See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/368455320

Development of the co-extrusion technology in the single production type.

(in English)

Book · February 2023

CITATIONS READS

0 35

1 author:

Виталий Валерьевич Леваничев

Podanfol S.A.
7 PUBLICATIONS   1 CITATION   

SEE PROFILE

Some of the authors of this publication are also working on these related projects:

highly permeable sausage casings View project

All content following this page was uploaded by Виталий Валерьевич Леваничев on 12 February 2023.

The user has requested enhancement of the downloaded file.

Edited by
VITALII LEVANICHEV

DEVELOPMENT
OF THE CO-EXTRUSION TECHNOLOGY
IN THE SINGLE PRODUCTION TYPE
(in English).

Monograph

2023

1
UDC 678+532
L48

Approved by the Academic Council of Volodymyr Dahl East Ukrainian

National University, Protocol No.6 of 25.02.2016.

Reviewers:
Glikin Marat, Doctor of Technical Science, Professor, Head of the Department of
Technologies of Organic Substances, Fuel and Polymers, Technological Institute of
EUNU named after named after V. Dahl, Severodonetsk.
Smolii Viktoriia, Doctor of Technical Science, Professor, Head of the Department of
Electronic Devices, Technological Institute of EUNU named after V. Dahl,
Severodonetsk.
Demin Dmitrii Doctor of Technical Science, Professor, Department of Foundry,
National Technical University, “Kharkiv Polytechnic Institute”

L48 Author:
Edited by Vitalii Levanichev
Development the co-extrusion technology in the single production type:
Monograph/ V. Levanichev . 2023. – 220 p. (in English)

This publication is the author’s translation of the monograph "Разработка технологии

соэкструзии в условиях единичного производства" which was published in 2016. In the
course of translation and editing, clarifications and updates were made to the text, which took
place on the issues under study from the moment of the first publication.
If you need to make the reference on this work, please us the Russian edition identification:
https://doi.org/10.15587/978-617-7319-02-2.

This monograph provides the analyzes of modern methods of changeovers accelerating in

coextrusion processes, methods of prediction and management of qualitative characteristics of
polymer products in the single production type. The mixing processes as well as the control of
the melt temperature, the extruder output with constant changes in formulations have been
studied. Also the methods for the calculating of the processes of plastic processing based on
representing the movement of the melt as a cork sliding on the surface of the flow channels. The
multilayer flow and the method of variable rotation speed of co-extruder screws were studied to
accelerate changeover by film color. This monograph is recommended for students, engineers
and researchers involved with co-extrusion technology of flexible packaging materials

Figures 69, Tables 74, References 84 items.

2
 All rights reserved. No part of this book may be reprinted or reproduced or utilized in any
form or by any electronic, mechanical, or other means, now known or hereafter invented,
including photocopying and recording, or in any information storage or retrieval system, without
permission in writing from the authors. This book contains information obtained from authentic
and highly regarded sources. Reasonable efforts have been made to publish reliable data and
information, but the author and publisher cannot assume responsibility for the validity of all
materials or the consequences of their use. The authors and publishers have attempted to trace
the copyright holders of all material reproduced in this publication and apologize to copyright
holders if permission to publish in this form has not been obtained. If any copyright material has
not been acknowledged please write and let us know so we may rectify in any future reprint. The
publisher, the authors and the editors are safe to assume that the advice and information in this
book are believed to be true and accurate at the date of publication. Neither the publisher nor the
authors or the editors give a warranty, express or implied, with respect to the material contained
herein or for any errors or omissions that may have been made. Trademark Notice: Product or
corporate names may be trademarks or registered trademarks, and are used only for identification
and explanation without intent to infringe.

Author:
VITALII LEVANICHEV, PhD, Associate Professor

ID ORCID: https://orcid.org/0000-0003-2962-1719

© Levanichev Vitalii, 2023.

6
 Abstract

Modern production, especially in the B2B business environment, is

characterized by an individual approach to each client. Features of the coextrusion
process are continuity, a rather narrow range of rational values of output, labour
intensity and cost of changeovers. Therefore, the organization and technology of
coextrusion in a single production type requires special methodologies.
The first chapter analyzes patents developed for accelerating changeovers
during extrusion, as well as methods open for commercial use. Particular attention is
given to processing additives, types and properties of surface coatings of extrusion
molding equipment. The problematic issues of existing approaches to modeling an
extruder, rheological behavior and multilayer flow are stated.
The second chapter is devoted to the research of coextrusion technology in the
conditions of a single production type. The processes of mixing, temperature control,
productivity and quality control are considered on the example of the triple-bubble
method.
The third chapter shows the results of modeling various designs of die
distribution channels. A new rheological model of the "corky" flow is proposed. The
advantages of this model are shown: coverage of the full rheological curve; the
dimension of viscosity has a pronounced physical meaning; allows you to
qualitatively evaluate the phenomena and effects of the near-wall flow. A new model
of polymer flow in the extruder has been developed, which takes into account the
slipping effects on the walls of the screw and barrel, has a more general character.
The fourth section is devoted to the study of multilayer flow, the method of
variable flow rate and technological requirements for the planning of coextrusion
production.

Keywords:
Coextrusion, multilayer flow, rheological model, extruder, changeover, near-
wall flow, polymer material, triple-bubble method.

7
Introduction ....................................................................................................................................... 10
Section 1. The analysis of changeover processes in the manufacture of flexible packaging materials
by coextrusion. .................................................................................................................................. 13
1.1 The main tasks and stages of creating multilayer structures. .................................................. 13
1.2 Comparative analysis of the waste structure during changeovers ........................................... 16
1.3 Technological operations carried out during the readjustment of equipment. ........................ 18
1.4 Analysis of the gravimetrical batch blender system in the changeovers process. ................... 20
1.5 Analysis of factors affecting on the raw materials replacement time in the extruder and die. 23
1.6 Analysis of existing methods to accelerate purging procedure. .............................................. 24
1.6.1 Disco Purge Variable Speed Method. .................................................................................. 25
1.6.2 Variable speed method for coextrusion. ............................................................................... 30
1.6.3 Methods of using cleaning additives. ................................................................................... 31
1.6.4 Methods for improving purging by improving instruments and equipment ........................ 33
1.6.5 Analysis of the use of processing additives. ......................................................................... 36
1.7 Some practical observations the wall flow influence in extrusion processes. ......................... 40
1.8 Types of coatings used for processing the channels of melt flow in the extruder and die. ..... 42
1.9 Modern problems of modeling the processes of polymer melt flow. ...................................... 45
1.9.1 Problems of modeling multilayer flow ............................................................................. 46
1.9.2 Problems of modeling the melt movement in the extruder screw. ................................... 47
1.10 Methods foresee properties for film quality control. ............................................................. 48
1.11 Characteristics of typical co-extrusion line for the production of shrinkage tubular films. .. 52
1.11.1 Typically technological scheme of production with the method triple-babble . ............ 52
1.11.2 Specifications. ................................................................................................................ 55
1.11.3 Range of products. .......................................................................................................... 56
1.12 Conclusions on the first section. ............................................................................................ 60
Section 2. Development of mixing technologies, extrusion and product quality control ................. 61
2.1 Research and development of supporting processes ............................................................... 61
2.1.1 The influence of deviations in the operation of mixing equipment on product quality. .. 65
2.1.2 Study of the criteria for estimating the mixing quality..................................................... 72
2.1.3 Development and analysis of the mixing index as a universal criterion .......................... 78
2.1.4 Method of mixing quality control ..................................................................................... 83
2.1.5 Development of a quality criterion for mixing in a single sample ................................... 86
2.2 Controlling the melt temperature............................................................................................. 88
2.2.1 Study of temperature regimes .......................................................................................... 92
2.2.2 The results analysis.......................................................................................................... 93
2.3 Extruder output control............................................................................................................ 97
2.3.1 Extruder output study ....................................................................................................... 98
2.3.2 The results analysis ........................................................................................................... 99
2.3.3 The extruder specific productivity calculation ............................................................... 102
2.4 Product quality control .......................................................................................................... 104
2.4.1 Investigation of the relationship of product quality characteristics and technological
modes ....................................................................................................................................... 106
2.4.2 Study description. ........................................................................................................... 108
2.4.3 Analysis of results .......................................................................................................... 110
2.5 Conclusions on the second section: ....................................................................................... 112
Section 3. Simulation of extrusion processes .................................................................................. 114
3.1 Shear flow modeling of die distribution channels. ................................................................ 114
3.2 Annular distribution channel optimization ............................................................................ 122
3.2.1 Design parameters influence .......................................................................................... 124
3.2.2 Technological parameters influence ............................................................................... 126

8
 3.3 Development the cork flow model ........................................................................................ 128
3.3.1 Characteristic points and analogies ................................................................................ 132
3.3.2 Method for calculating equipment channels based on corky flow model ...................... 134
3.3.3 Comparative analysis of complete rheological models of polymer melt flow ............... 139
3.3.4 Flow simulation results using the full rheological curve equation ................................. 140
3.3.5 Simulation of flow at different temperatures, comparative analysis of corky and power
model of melt flow .................................................................................................................. 143
3.3.6 Analysis of processes, effects and extrusion techniques based on a corky flow model . 146
3.4 Development of the melt flow model in the extruder ............................................................ 149
3.4.1 Flow between parallel plates .......................................................................................... 151
3.4.2 Development of the melt movement model in the screw ............................................... 153
3.4.3 Comparative analysis of the obtained equations with the classical extrusion equation . 158
3.4.4 Results of flow simulation in the dosing zone for different models ............................... 159
3.4.5 Simulation with different friction of the screw and cylinder surfaces. .......................... 162
3.5 Conclusions on the third section............................................................................................ 164
Section 4. Investigation of multilayer flow ..................................................................................... 166
4.1 The gravimetric dosing system investigations....................................................................... 166
4.1.1 The multilayer structure reproducibility for various formulations investigation ........... 167
4.1.2 The multilayer structure reproducibility for one formulation investigation ................... 168
4.1.3 Comparative analysis of data from the gravimetric control system and the layer
distribution in the die ............................................................................................................... 170
4.2 Comparative analysis of methods for dosing the melt. ......................................................... 177
4.3 Study of changeovers by color (recipe). ................................................................................ 182
4.3.1 Investigation of the mineral filler effect and the ratio of melts viscosities during color
changeover ............................................................................................................................... 184
4.3.2 Inner layer process purging (from colorless to white).................................................... 189
4.3.3 The color changeover investigation (from yellow to colorless) with varying screw speed
................................................................................................................................................. 189
4.3.4 Investigation of the color transition (from gold to colorless) with varying screw speed 195
4.4 Specificity of planning changeovers and orders queue ......................................................... 199
4.4.1 Analysis of the requirements for an order when placing it in the queue ........................ 202
4.4.2 Requirement for the series of production of films of different colors ............................ 203
4.5 Conclusions on the fourth section: ........................................................................................ 206
Conclusion ....................................................................................................................................... 207
References ....................................................................................................................................... 209

9
 Introduction

The global market of packaging materials is growing by 3.3% every year, and
the part of hard plastic and flexible packaging is growing faster than other materials
[1].
Multilayer flexible packaging has being constantly improved and developed,
and the co-extrusion method appears to be the most perspective method for producing
of multilayer materials, mainly because of its cost-effectiveness and producibility,
since a multilayer product is made in one stage.
The development of co-extrusion technology is moving towards the increasing
of the number of layers with reducing the thickness of each layer, not to change
significantly the overall film thickness. The equipment with 17 and 21 layers has
been created already, which ensure the minimal thickness of separate layers as far as
1μm, with a film width of 1200mm and a total thickness of 100-1000μm. This co-
extrusion technology is called nanolayer technology. The possibility of creating
2048-layer films is under the investigation now [2].
One can notify the following trend: large manufacturers of polymer materials,
such as BASF, LANXESS, Du Pont or UBE while focusing on particular polymers
and their consumer properties development along with producing their numerous
modifications, same time significantly expand the technological capabilities of much
smaller enterprises producing multilayer materials by co-extrusion method. It means,
that due to the use of new materials in multilayer structures and co-extrusion
technologies serious scientific research in the field of polymer materials have been
disproportionately strengthened.
Modern co-extrusion production of flexible multilayer packaging polymer
materials is multitopic, and in some cases it can small-scale or single production type.
Extrusion and co-extrusion technology studies have been conducted for steady
processes of mass production. The rules arising from changeovers between the ranges
of products are not studied yet.

10
 The number of such changeovers per shift can reach five for one co-extrusion
line. Depending on the structure of orders, coming into production, the operations
consolidation varies from 5 to 40, wherein type of production varies from large-scale
to single type. Time losses due to changeover can reach 20% per shift, subsequently
increasing wastes, decreasing quality and increasing the cost of finished products. At
the same time, the mass productivity of equipment constantly grows.
An output of co-extrusion film production comes 10 to 1000kg/h, the cost of
raw materials comprises 30-60% of the cost of polymer packaging, while the loss of
raw materials per shift due to changeovers can reach 10% of the nominal line
capacity. In contrast to, for example, metalworking cutting processes, the during the
process of extrusion the changeovers not only decrease the percent of equipment
exploitation, but also increases additionally waste materials and equipment wear.
Therefore, the acceleration of changeovers, reduction of raw waste is an urgent task.
For identical secondary molding processes (blowing, orientation, winding, etc.)
the coextrusion, has significantly more options for modifying the properties of the
package, if compared to the extrusion of single-layer films, since the introduction of
additives and super-concentrate in each layer can reach 30% compared to 10% for
monolayer films.
The expansion of the multilayer film materials range is caused by following
factors:
1. Significant widening of the raw polymer materials range which gives unique
properties for multilayer packaging and thus makes it outstanding in the market and
can be effectively used for commercial purposes.
2. A film made by coextrusion is often a semi-finished product and require
supplementary processes prior to the actual packaging process. Factories using a
multilayer film as a raw material set various additional requirements for the quality
and technical parameters of the film.
3. Development of supplementary processes equipment (printing, vacuum
forming, soldering packages, etc.), thus changing the nominal productivity of
machines, performing basically the same technological operation, by dozens or even
11
hundreds folds. Therefore, the volume of consumption and, thus, the volume of
orders for similar film sizes can vary significantly between different customers.
4. The availability of advanced packaging technologies and supplementary
processes equipment for small enterprises (for example bags making machine), which
make it possible to organize the production of competitive packaging without
significant investment.
5. Development of control systems for the coextrusion process based on
gravimetric or volumetric melt dosing, enabling to switch between the technological
conditions within a few minutes, which greatly increases the equipment flexibility.
Most the changeovers are require the raw material recipe changing. This affects
the temperature profile of the extruder and pressure, and thus, changes the extruder
specific output characteristic. Despite of the very fast changing of the technological
conditions, there are few operations that consume the main part of time during the
changeover: replacing of the raw materials in the storage bins, purging out and
stabilizing the extruder and die, and setting up the secondary molding process.
Thus, modern co-extrusion production can hardly be even called small-scale
production type, since some sorts of film can be unique and exclusive, i.e. client-
targeted.
Therefore, the development of special technologies for starting-ups, stoppings
and changeovers is required; it is necessary to guarantee the minimum time and raw
materials required for the changing of the productions of one kind of film to another.
The technology of changeovers should be universal and have generalized
methodologies and methods of changeovers, since some types can be produced once
or twice a year, while the conditions of production are constantly changing and same
time, quality and productivity must be maintained at the required level.
The author is grateful to his supervisor V.A.Ulshin for discussing of many
issues outlined in this monograph; to his colleagues V.V.Dyadichev, T.M.
Tereshchenko, T.I.Larchenkova for the analysis and processing of some experimental
data.

12
Section 1. The analysis of changeover processes in the manufacture of
flexible packaging materials by coextrusion.
The main direction of the use of plastic multilayer films, of course, is
packaging, though agricultural, medical and industrial purposes are of some
importance also. In food packaging, polymer films are used both on their own (shrink
films, stretch films, skin films, barrier, laminated, metalized, "breathable", "milk",
water-soluble, biodegradable films), for the manufacture of various kinds of bags and
bags, containers (hard films), and as part of a multi-component and multilayer
packaging [3].

1.1 The main tasks and stages of creating multilayer structures.

A wide range of packaging materials results from the variety of food products
and a wide range of packaging requirements. These requirements can be divided into
general and specific, depending of the product nature, conditions of its technological
processing and storage.
General requirements depend on obvious product requirements, since group of
products of a certain category simply cannot be packaged in certain package.
Firstly, it goes about the food safety of the package under the conditions of
filling, storage and maintaining, which have the maximum impact on the packaging
material. For example, if the product has been heated in the package, the
decomposing of the package as well as migration of hazardous substances on a level
harmful for human should not happen.
Secondly, the main product features; for example, for packing fish, the sharp
elements should be taken into consideration, and thus, the high resistance of the film
against perforation must be ensured.
Thirdly, the ensuring of the required level of barrier properties; packaging must
prevent the products spoilage throughout the whole storage period, i.e. it must
perform its basic function.
One cannot mention the general environmental requirement; the ability of
recycling of the packaging after use, without harm to the environment remains the

13
common problem for all polymer material, especially multi-layered films. However,
there are some promising exploratory works in this direction, including using of
coextrusion technology [4]. There is a recycling technology for any polymer
materials into composite products, when polymer waste is crushed and agglomerated,
then mixed with pre-dried sand, then 80% of sand and 20% of agglomerated plastic
are mixed with following melting of resulting mixture at 280-300oC in tunnel screw
feeders and then dosed and pressed into monolithic products. In this way the building
elements, such as paving slabs, shingles roof, sewer hatches and etc. can be produced.
Multilayer films are developed with reference to the properties, conferred by
the individual layers of the whole. When the general properties of packaging films for
the packaged product and packaging equipment have been determined, they must be
compared with the properties of single layers [3].
Basing on the analysis of the general requirements for packaging and the
properties of polymeric materials, one can determine the main configuration of the
multilayer structure, what materials will be used and possible options of their
position. In fact, having a set of polymers with different properties, you can create
any structure, depending on the needs of the market and the aim of the manufacturer.
The structures of multilayer polymeric materials used in co-extrusion
packaging technology are well studied [5]. However something new is being created,
hence no one can say exactly which multilayer structure would be optimal or even
sustainable. For example, only for the barrier packaging (artificial sausage casings)
more than 10 casing structures have been developed over the past 20 years (Table
1.1), which are still actual today and various companies use them for the industrial
production of casings. The application conditions for such a variety of multilayer
structures are the same and, in fact, the casings compete with each other. A lot
depends on product development, marketing, advertising, service, price-quality ratio
and specific requirements of the client [6].
Table 1.1 provides the stages of development of multilayer tubular heat-shrink
polyamide films (casings) manufactured by the triple blowing method (triple-bubble)

14
for the production of sausages and the main properties achieved by the using of these
structures.

Table 1.1
Structures of tubular heat-shrinkable barrier polyamide films (sausage casings)
№ Number Description
Typical structure
Stage of layers
Outer  Internal layer
Year
The properties of single-
layer casings are improved,
1
РА/Tie/PA, barrier properties are
3
РА/PA/PA, increased, thickness is
1995
reduced, colour hiding power
is increased
The moisture barrier is
increased due to
РА/Tie/LDPE/Tie/PA,
polyethylene, the raw
РА/Tie/LLDPE/Tie/PA,
material cost is reduced, the
2 РА/Tie/PP/Tie/PA,
elasticity is increased,
5 РА/Tie/ EVOH /Tie/PA
polypropylene enables the
2003 LDPE/Tie/РА/Tie/PA
sterilizing of the product
РА/EVOH/РА/Tie/PP
along with the low vapor
РА/EVOH/РА/Tie/Surlin
permeability, and the color
range is improved.
Increased mechanical
strength, improved barrier
3 РА/EVOH/РА/Tie/LLDPE/Tie/PA,
properties plus with cost
7 LDPE/Tie/РА/Tie/НDPE/Tie/PA
reduction, improved the
2012 PET/Tie/LLDPE/Tie/НDPE/Tie/PA
ability to introduce the
modifying additives.

Accepted abbreviations:
PP - polypropylene; PE - polyethylene; PA - polyamide; PET - polyethylene
terephthalate; Tie - adhesive; Surlyn - an ionomer (frost-resistant elastomer)
manufactured by DuPont; LDPE - low density polyethylene; HDPE - high density
polyethylene; EVOH - copolymer of ethylene with vinyl alcohol, LLDPE - linear low
density polyethylene.

15
 This description does not analyze big family of artificial multilayer permeable
casing, made from the mix of polyamides and different water-soluble polymers.
Those casings have been greatly developed from 2010 year up to modern time.
Thus, the basic structure and basic characteristics of multilayer packaging, such
as layer thickness, color and its manufacturing technology, are determined at the
design stage.
The next step is the clarifying the quality specifications of multilayer
packaging with respect to the specific requirements for the packaged product. At this
stage, some details and know-how, providing the competitive advantages of the
products are developed, and the required process productivity is calculated. Then, the
administrative and technical measures for the implementation of the product have
been developed and carried out.

1.2 Comparative analysis of the waste structure during

changeovers.
The co-extrusion process has more waste during the process recipe replacing,
compared to the single layer film extrusion.
Usually the changeover is the replacement of a recipe or in other words is a
purging out one layer, but without turning off of extruder of the other layers, because
it is necessary to keep the form and the melt strength of the tubular workpiece for
secondary molding. Also the turning off one extruder in co-extrusion line can lead to
extrusion of the melt through this extruder into the feeding zone, which can lead to
the emergency stop of the all line. There is also additional problem of the arising of
the polymer degradation in stopping extruder.
Therefore, a comparative analysis of statistical data on the level of waste spent
for changeovers during the production of single-layer and multi-layer films was
carried out (n - the period is 1 month).

16
 Table 1.2
Comparative wastes analysis for single-layer and five-layer film production.
Process Type of waste n1 n2 n3 n4
Total waste, kg 2787 2750 3864 1140

Extrusion of a single- Waste from 447 229 530 190

layer film (25kg/h) changeovers, kg
Waste from 16,0 8,3 13,7 16,7
changeovers, %
Total waste, kg 2827 2920 1765 3030
Co-extrusion of a Waste from 1530 1347 829 1607
five-layer film changeovers, kg
(40kg/h) Waste from 54,1 46,1 47,0 53,0
changeovers, %

Analysis of the data in table 1.2 shows that the proportion of changeovers
waste in the processes of co-extrusion increases by 3-5 folds against the extrusion of
a monolayer film. However this data show absolute values, which cannot be used for
the generalization of data.
To predict the expected cost-effectiveness due to increasing of the changeover
process efficiency, it is necessary to analyze the wastes structure more deeply and to
conduct this analysis with respect to the specific wastes in relation to the total
consumption of raw materials and time costs.
Table 1.3
Waste level in the volume of raw materials used.
Waste (extrusion) n1 n2 n3 n4 n5 n6 n7 average
Total, % 8,0 9,8 10,6 12,8 9,0 7,0 9,1 9,5±1,7
1. unplanned (emergency
equipment breakdowns,
3,3 4,5 4,9 7,6 3,8 2,4 4,4 4,4±1,5
functional process
instability),%
2. planned (process setup,
quality control, 4,7 5,3 5,0 5,2 5,2 4,7 4,7 5,0±0,3
changeovers),%
2.1 –including changeovers
1,0 1,5 0,8 1,5 1,3 1,8 1,4 1,3±0,3
waste,%

17
 Continuation of table 1.3
Waste (co-extrusion) n1 n2 n3 n4 n5 n6 n7 average
Total, % 6,4 6,7 7,5 6,6 8,6 6,0 9,5 7,3±1,2
1. unplanned (emergency
equipment breakdowns,
2,5 2,2 2,5 2,5 3,2 1,6 4,0 2,7±0,7
functional process
instability),%
2. planned (process setup,
quality control, 3,9 4,5 5,0 4,2 5,4 4,4 5,4 4,7±0,5
changeovers),%
2.1 –including changeovers
2,9 3,4 3,2 2,7 4,3 2,7 4,3 3,4±0,6
waste,%

An analysis of the data in Table 1.3 shows that, the co-extrusion process
compared with the extrusion of a monofilm is more stable and it can be explained by
the presence of a gravimetric dosing system and more reliable behavior of the
multilayer material during deformation, orientation the film. The multilayer structure,
as it were, redistributes the heterogeneities and defects that occurred at some point of
in the film layer, so small defects do not lead to breaking film and line emergency
stops. However a big difference between the processes is observed in the changeovers
waste level.
With an increase in the changeover efficiency, the saving of raw materials for
coextrusion processes can be 2% of the total amount of consumed raw materials. The
expected economic effect is also associated with an increase in actual productivity by
2%, since the line produces products instead of waste.

1.3 Technological operations carried out during the readjustment of equipment.

In the technological changeovers process the finished product parameters are
change, the main ones are as follows:
• film thickness, size (tube diameter and width);
• film color, decorative elements (roughness, structured surface, etc.);
• mechanical characteristics (stiffness, strength, perforate resistance, elasticity,
shrinkage);
• surface properties (surface energy, coefficient of friction);

18
 • barrier characteristics (gas permeability, vapor permeability, resistance to UV
radiation).
Let us analyze the operations, performed on the line, in the changeover
process.

Table 1.4
Line changeover operations for the new product type manufacture.
Operation Description Impact on time and waste
number
1 2 3
Replacing the recipe in the The operation is carried out before the
feed hoppers (recipe end of manufacture previous product
preparation dozing stations) type. With a good level of
1
organization and production
technology, waste can be minimized to
zero
Polymer melt purging out of Requires special techniques to
coextruded die and extruder minimize the loss of time, all
2
operations are "adjusted" by purging
out
Extruder thermal It is carried out during the purging
stabilization after changing process (operation No. 2)
3
the temperature profile (if
necessary)

19
 Continuation of table 1.4
1 2 3
Extruder output With the operators appropriate skill, is
4 stabilization carry out during the purging process
(operation No. 2)
Stabilization of secondary With the operators appropriate skill, is
5 molding processes. carry out during the purging process
(operation No. 2)

Each of these parameters requires special techniques to minimize time and

the waste, but the purging time is the most difficult to manage; provide the
maximum amount of the waste and the difficult to predict. The purging time
depends not only from the raw materials current parameters and technological
conditions, but also from the background: the previous type of film and impurity of
the flow channel surface and the co-extrusion die wear. The die wear depends of
the time after the last cleaning of the co-extrusion die, the total die wear, and the
mechanical service level [7].
The time spent on the changeover can be partially combined. Combining
operations depends of the staff skills, the work organization, the equipment
structural elements, degree of automation line.

1.4 Analysis of the gravimetrical batch blender system in the changeovers

process.
Replacing a recipe in feed hoppers is not a challenge for co-extrusion
technology. When designing the line, it is necessary to take into account design
solutions that provide free access to the hopper lower part. The recipe change time
in the hopper is can combine with the line operation time.
Problems arise when increasing static electricity on the transport, storage
elements, loading system and on the raw materials granules. In this case, part of the
granules “hang” in the hopper, stick to the storage elements walls, complete

20
cleaning becomes a time-consuming task, therefore, antistatic additives are
sometimes introduced into the raw materials.
If the line is equipped with a gravimetrical batch blender system, the dosing
system design, mixing and composition accumulation, the arrangement of sensors
and the control algorithm for the dozing element operation affect on the raw
materials replacement time. The functional diagram of the station recipe making
and placement options for sensors monitoring of the hopper filling was consider
(Fig. 1.1). For normal operation dozing element the one sensor to control the
amount of material is enough. The sensor position is selected based on the
performance of the transport system granulate material. When installing two
sensors (at the top and bottom of the hopper) it is minimizes the material amount
that must be replaced during changeover, this reduces the waste amount.

1 2

4
7

Fig. 1.1. Functional diagram of the recipe making station:

1 – the main component dozing element; 2 – the key component dozing
element; 3 - weight hopper; 4 - mixing hopper; 5 – extruder; 6, 7 - sensors for
monitoring the hoppers filling.

21
 The second factor that influencing to the changeovers time, this is the
volume of mixing, storage and intermediate bunkers. The bunker should have an
enough volume for the reliable operation of the automatic loading and batching
system and provide time for ongoing work on servicing the dozing system and
filling up new portions of raw materials. On the other hand, to speed up the
changeover, it is necessary to minimize the storage bunkers volume.
The automatic recipe making station does not guarantee the mixture
uniformity that fed to the extruder, since the recipe stability is determined by the
design and technological parameters of the mixer, and set of parameters that are
configured by the installer and are controlled by the station automatic control
system. It should be noted a wide variety of proposed structural elements and
know-how of manufacturers of this type of equipment.
The mixture (the batch) quality depends of: the uniformity size particle, a
static electric charge on the granules, the ability to accumulate static charges on the
bins surfaces, the components density, the mixing time, the batcher blades speed,
the one dose volume, the dozing station productivity. There is also some accuracy
in the dosage of each component, for example, for the component with 3% dosage,
the relative error can be up to 25%, another word in a single dose (or for single
batch), with a normally working dozing element, dosage can change from 2.25% to
3.75%. Also the use of a wide range of granular polymeric materials requires
constant monitoring and adjustment of mixing technology [8].
There are no criteria for check the quality of operation gravimetrical batch
blender systems; although practice shows that the recipe stability is the first
technological parameter influence on key manufacturing indicators: productivity,
cost and quality. Therefore, the development of dosing and gravimetrical batch
blender systems in co-extrusion processes requires new methods of process
control.

22
1.5 Analysis of factors affecting on the raw materials replacement time in the
extruder and die.
The co-extrusion die is designed to ensure the thickness uniformity of each
layer for a given range of viscosities, pressures and output. The residence time of
the polymer in the die is indirectly associated with stagnant zones. For same
productivity the biggest die volume, the greater probability of such zones and the
longer time recipe replacement (die purging time). Design parameters, if analyzed
residence time, contradictory. On the one hand, an increase in the distribution
channel volume is improves the die flexibility in terms of processing polymers
with different flow index and viscosity, on the other hand, an increases the
residence time.
Practical observations in the production process show that the main factors
that influence on the recipe time replacing in the coextrusion die and extruder, as
well as the level of waste during purging, are the viscosity ratio of the current and
new recipes m1/m2, the absolute values of the extruder volume Vеx and the die
Vd, the ratio of these volumes Vеx/Vd.
In the colored films manufacture, it is important to consider the amount of
colorant in the layer formulation and how the changeover is take place, from
lighter to darker or vice versa. While always the longest (costly) changeover - from
colored film to a colorless film [9].
When designing an extruder, the main parameters are productivity,
compression ratio, extruder diameter, length to diameter ratio, channel depth in the
dosing zone. The residence time is considered as secondary parameter. One of the
indicators showing the residence time in the extruder can be the so-called backflow
coefficient a=Qp/Qd, which predicts how much the melt is delayed by
backpressure in the die. If the coefficient higher, the degree of mixing higher, but
the residence time is longer.
Therefore, the actual task is to develop constructive and technological
solutions aimed at minimizing the polymer residence time in the die and extruder
while providing the required output and stable quality.
23
1.6 Analysis of existing methods to accelerate purging procedure.
According to studies [10] to speed up purging out proposed to apply the
variable screw speed, this method since different levels of shear deformations
leads to a change in the velocity profile and different channel parts are purging.
Low shear rates lead to purge our stagnant zones.
It is recommended to replace difficultly purge parts by making them quick-
change, for example, a melt filter.
Reducing the temperature by 5-100С for place where the flow rate is lower
and formation of stagnant zones is possible, thus increasing the melt viscosity in
this place and increasing the purging out intensity.
Cylinder temperature reduction when feeding purging polymer, that is
increase its viscosity and provide a good contact with equipment parts.
It is necessary to select materials with the possible similar rheology, only the
melt flow index (MFI) may not be indicative for rheology curve, and show only
viscosity in one point. Unknown dependence viscosity from shear rate and
temperature, can be lead to significantly reduced viscosity in the purging operation.
Different types of cleaning additives are available, in general they work, but
it can be difficult to clean the additives themselves, therefore, it is better that the
cleaning compound to be low viscosity. Need to take note - what recommended
temperatures using the cleaning compound.
Apply mixtures with adhesives that are well compatible with many polymers
for example the mixing EAA (ethylene acrylic acid copolymer) and LDPE 50/50
at start and little by little moving to the composition 90% LDPE and 10% EAA,
and in ending step completely removing EAA.
Abrasive materials (chalk, talc, glass sphere), surfactants, thermal stabilizers
are used as purging components of the cleaning compound. The compound base is
usually chosen to be the same as the material being purged, thus achieving
maximum compatibility and interfacial interaction. Various methods for the
cleaning composition preparation are aimed at increasing the compatibility and

24
components diffusion of the cleaning mixture into the cleanable component,
thereby increasing their level of influence and the cleaning intensity.
So a viscosity and rheology are the most uncertain parameters for purging
control. Since on the one hand, the new composition high viscosity is accelerates
the purging of the previous composition, but then it is difficult to purge the highly
viscous recipe itself.

1.6.1 Disco Purge Variable Speed Method.

Du Pont's Disco Purge cleaning method is variable extruder speed. The
method is deeply developed and open for commercial use.
It contains the following main sections:
1. Change in speed.
2. The use of foaming polyethylene with mineral filler.
3. The use of ethylene copolymers for accelerated purging.
4. Example of purging monitoring with quality rating.
According to [11], according to the Disco Purge cleaning method, purging is
carried out at different screw speeds
 1st minute at 30% of maximum RPM
 2nd minute at 90% of maximum RPM
 3rd minute at 50% of maximum RPM
 4th minute at 15% of maximum RPM
 5th minute at 70% of maximum RPM
 minutes 6-10 at 15-20% of maximum RPM
 minutes 11-15 -- repeat the cycling steps of the first 5 minutes
The specific rpm values do not matter (that is, the recommended % of
maximum speed can vary over a wide range). It is important that the velocities
structure and shear stresses is change and a new velocities distribution and shear
rates is created. One minute at each rotation speed is enough to development of a
new distribution of stresses and speeds. The polymer is better purged out at low
speeds, which stuck (stagnated) in the curve (bend) of the channel, there is a high

25
probability that an adhesive interaction will be between the purging and the
material in the stagnant zone.
At higher speeds, the materials speed on the wall is higher and the polymer
is purged away from the walls of the cylinder and dies. Periods of high
productivity are more important for effective cleaning.
The purging time varies from 15 minutes for the extrusion of sheets and
coatings to 30-45 minutes for blown film extrusion.
It should be noted that a purging time of 15 minutes can be offered as a kind
of standard, for example, Macro Canada, for its new coextrusion dies, also states
that purging out for a new color is no more than 15 minutes. But this is for testing
at the stage of checkout new equipment.
To evaluate the effectiveness of the proposed methodology, a comparison
was carried out under various conditions:
1. cleaning is carried out at constant speeds, and when a new polymer is fed,
the speed do not change;
2. cleaning by method Disco Purge as described above (30%, 90%, 50%,
15%, 70%);
3. simple cleaning when the screw speed varies between 90% and 10% of
the maximum every 5 minutes;
4. cleaning with a DuPont PE6611 cleaning mixture (polyethylene with a
foaming agent) with mineral filler silicon dioxide.
The following resins were used.
• Surlyn ® 1652, MFI = 5.0 g/10min (colorless),
• Nucrel® 1207, MFI = 7.0 g/10min (colorless),
• LDPE 1540, MFI = 6.5 g/10min (white color to control purging).
Two variants of the initial conditions are analyzed when the LDPE is purged
in the extruder and purged with Surlyn and Nucrel and vice versa.
The method purging with LDPE 1540 showed well. Because at processing
temperatures of 280-2900С, its viscosity was higher than that of Surlyn. An

26
average of 45 kg of raw materials and 15 minutes of time were spent on an
extruder with a diameter of 100 mm.
The use of cleaning material PE6611 led to a quick cleaning of the initial
material, but then the cleaning compound itself was difficult to purge. Total waste
amounted to 225 kg, so this method is not effective for standard purging during
changeovers, but the use of cleaning additives is recommended for heavy pollution,
when the material destruction in the extruder, for example, in emergency
situations.
The purging quality was estimated on a 10-point scale, the following criteria
were taken according to the quality level: 8 points are enough for the following
sale of the film, that is, a satisfactory level of purging quality; 10 points a complete
replacement of the material.
Table 1.5
Description of the changeover process when changing colors
Transition from white LDPE to Transition from transparent Nucrel
N transparent Nucrel N to white LDPE
0 new resin not yet visible 0 white not yet visible
1 new material begins to appear (to go) 1 white begins to go
can see clear transparent lines in
2 the film is still milky 2 the center
you can already see several
3 transparent bands (strips) 3 the wide of bands more then 1 inch
two bands more than 6 inches wide from 1/2 to 1 inch wide transparent
4 still white 4 bands
more than 5 inches two bands on
5 both sides 5 1/8 to 1/2 inch transparent bands
less than 1/8 inches of transparent
6 more than 4 inches of white 6 bands
thin transparent line clearly on two
7 more than 2 inches of white color 7 sides
8 less than 1 inch milky 8 very difficult to see the milky band
the white line has disappeared but
9 the milky color are still visible 9 the milky color are still visible
10 transparent film 10 completely white film

27
 Purging from Nucrel with LDPE Purging from LDPE with Nucrel

10 10
9 9
Disco Purge Disco Purge
8 8

Quality of purging
Quality of purging

7 7
6 Simple Disco 6 Simple Disco
5 Purge 5 Purge
4 4
3 N const =45rpm 3 N const =45rpm
2 2
1 1
N const=135rpm 0 N const=135rpm
0
10 20 30 40 10 20 30 40
Time, min Time, min

Fig. 1.2. The dependence of the cleaning time on the sequence (rotation) of
materials used
Operating at an increased speed of 135 rpm gives 20% time savings
compared to Disco Purge, but 30% higher waste.

Purging from Surlyn with LDPE Purging from LDPE with Surlyn

10 10
Disco Purge
Quality of purging

Quality of purging

8 Disco Purge 8

6 6
Simple Disco Simple Disco
4 Purge 4 Purge

2 N const 2
N const
0 =45rpm 0 =45rpm
10 20 30 10 20 30 40 50
Time, min Time, min

Fig. 1.3. The dependence of the cleaning time on the sequence (rotation) of
materials used
Differences in methods were more obviously at start up, where Surlyn was
used to clean the extruder from LDPE 1540. Disco Purge used 79 kg of material

28
and 25 minutes of time. The simple cleaning method took 20% more time, and
10% more material was used. Operating at constant speed at 45 revolutions
(maximum screw revolutions was 270) was with the smallest efficient.

Washing from LDPE with Surlyn и Nucrel Purging from Surlyn and Nucrel with LDPE

140 140

120 120

100 100
Waste, kg

Waste, kg
80 80

60 60
40 40
20 20
0 0
Purging N=45rpm with Surlyn

Purging N=45rpm with Nucrel

Purging N=135rpm with Nucrel

simple Disco with Surlyn
Disco with Surlyn

simple Disco with Nucrel

Disco with Nucrel

Purging N=45rpm from Surlyn

Purging N=45rpm from Nucrel

Purging N=135rpm from Nucrel

simple Disco from Surlyn
Disco from Surlyn

simple Disco from Nucrel

Disco from Nucrel

Fig. 1.4. Dependence of waste during purging, depending on the method and
material used
The analysis of this study shows that the influence of the dye on the time and
waste during washing is not taken into account. Changeovers using LDPE 1540
(colored white) to colorless Surlyn or Nucrel showed on average a 2X reduction in
waste and time, regardless of speed control method. The study claims this is the
effect of viscosity at processing temperature, but the MI quoted does not support
this.
Also, there is no analysis of the following fact: the Disco Purge method
when cleaning with Surlyn showed 3 times better results than when cleaning with
Nucrel; at the same time, when washing at a constant speed of N = 45 rpm, on the

29
contrary, cleaning with Nucrel showed 2 times better results than cleaning with
Surlyn.

1.6.2 Variable speed method for coextrusion.

Accelerated purging control systems provided by Macchi S.p.A. at the
exhibition K-2010 [12].
Co-extrusion 9-layer line was shown in operation in difficult exhibition
conditions. The line is equipped with 9 extruders with a diameter of 55mm. The
line produces a film with barrier layers sandwiched between ionomer and linear
LPDE layers using a special polymer to bond the layers. To keep the line running
successfully, Macchi engineers performed a nightly shutdown procedure with
purging of the melt channels so that decomposition of thermally sensitive polymers
would not cause problems with starting the line the next day.
The organization of such a procedure became possible thanks to the use of
Easy Control PPS software, which was developed by Macchi, which lets fast,
sequential changes in the screw speed. Full cleaning continues 15 minutes and
using 130 kg of material. Other purging methods may require 30 minutes of time
and about 500 kg of material.
According to the patent [13], a variable speed during coextrusion is used to
accelerate purging. The process diagram contains a control unit, which through the
controller provides control of extruder drives. Extruders are equipped with a
gravimetric dosing system. Co-extrusion die contains spiral flow distributor and
mandrel.
The technique is proposed for a system with four and seven extruders. For a
system with four extruders, the graphs [13] show how the change in the speed of
the extruder A is carried out in dynamics, where the material is purged out and the
change in the speed of the extruders B C D, while the overall output at the
beginning of purging decreases, and then keep in constant.
Methodology for seven extruders. Here, purging is carried out for the
extruder E, the speed of the extruders F, G, H, I, J, K is changed in such a way as

30
to compensate for the change in the output of the extruder E and the output of the
line to keep constant. In this way, the break of the extrudable multilayer film is
avoided and purging is intensified. It is also indicated that the purging time at
different speeds differs due to the use of cleaning materials, and in step a4-b1,
when the cleaning additive filled the channels, less time is required than in steps
a1-a3, when a cleaning additive is introduced in extruder and channels are start to
filled and purging.
It should be noted that the proposed variable speed method of one or more
extruders is the most possibility and technological in a single production type
conditions.

1.6.3 Methods of using cleaning additives.

According to [14], in modern extruders, the use of mixing elements, on the
one hand, they improve the melt quality and the process, but worsen the ability to
clean when changing to another color or polymer composition. It is proposed to
intensify the purge with a foaming additive, which is added to the composition in a
granular form and foams when going through the extruder when heated, so cleans
the melt channels flow from pollutions and residues of degraded material. Foaming
increases the local pressure inside the extruder and in this way is increase the
cleaning material effect on the channel walls by changing the flow rate in stagnant
zones.
According to [15], one of the polymer processing problems is gradual
accumulation on the walls of the screw, cylinder, die channels, which leads to an
increase in the average residence time of the polymer in the extruder by 5-500
times, this increase the polymer degradation and changes the product color. It is
proposed to use reactive compounds for cleaning equipment for polymer
processing, when catalysts for breaking the polymer chains of the polymer being
cleaning are used, in this case, its melting point and viscosity are lowered, and thus
cleaning is easier. It is proposed to use hydroxides and oxides of alkali metals as

31
catalysts, water is also added and a polymer base is used which does not react with
water in the catalyst presence.
According to [16], a composition consisting of a thermoplastic (A) with a
high melting point (above 200C) and a crystallinity of not more than 50% and a
thermoplastic (B) with a low melting point is used for purging. A significant
difference in the melting point leads to the fact that the thermoplastic (B) is used as
a carrier for a melt for a thermoplastic (A). The purging process must take place at
a temperature below the thermoplastic (A) melting point. The ratio of materials (A
and B) can be change significantly; the proportion of material (B) in a recipe can
range from 5 to 95%. This composition is very effective and does not lead to
equipment wear. The polymer (A) is easily deformed during purging and going
through the channel narrow parts, stretching into thin fiber.
The cleaning effect is probably explained by a change in the level of
polymer adhesion to metal at the softening temperature and polymer (A) high
viscosity.
Visible problem in the use of such a composition is the possibility of
stopping and stagnation of granules of not molten polymer (A) on the melt filters
or in channels of complex configuration, especially if the polymer (B) viscosity is
significantly lower than that of the polymer (A).
According to [17], it is proposed to use a composition consisting of a
pigment (the color to which we are starting now), a foaming additive, a binder
(preferably wax), for cleaning during the color changeover. The blowing agent
increases the melt volume by 30 times, the agent is chosen exothermic or
endothermic, or as a combination of both, it is important that the foaming take
place at least 25 ° C lower than the processing temperature.
According to [18], the problem is the formation of a melt film on the
equipment parts, high-quality purging is achieved using soft abrasive materials
(calcium carbonate, calcium phosphate, calcium silicate and aluminum silicate)
and sulfonated surfactants.

32
 According to [19], it is proposed to use a composition consisting of polymer
(B) and containing up to 10 weight percent of an alkaline earth metal salt for
cleaning. The level of the polymer (B) adhesion with the washing out polymer (A)
is important, it is suggested to choose the polymer (B) so that the adhesion is 50-
1500 grams / 15mm. Adhesion is tested on coextrusion cast film, a two-layer film
of polymer A and B layers.
Also, the polymer composition may additionally contain a third polymer (C),
which is added in a volume of 50% to the second polymer (B), while the mixture
viscosity parameters (B and C) should be provided: the melt index ratio of the MI-
mix60/MI-mix6 mixture should be in the range from 0.3/1 to 5/1, where
- MI-mix60 is the mixture melt index (g/10min) at 2160g and at a
temperature 20°C above the melting point of the mixture, after holding the mixture
in the melt in an MFI measuring apparatus for 60 minutes;
- MI-mix6 is measured under similar conditions, but the holding time is 6
minutes.
That is, an important parameter is the compatibility and thermal stability of
the cleaning mixture.

1.6.4 Methods for improving purging by improving instruments and

equipment
Purging acceleration developments are also being carried out in the direction
of equipment and tooling upgrades.
For example, according to [20], Alpine's new X-Series seven-layer film die
eliminates joint lines between materials with narrow molecular weight distribution
let is allows faster color changes. For the barrier film production, Alpine
showcased its new seven-layer X-Series die. Co-extrusion die with side feeding
holes let you to eliminate lines in the film from entry holes in the die, because the
spirals work in the cylinder inside, not in the outside. Alpine says the holes are
circular (don’t semicircular), which gives for a more laminar flow, which reduces
cleaning and color change times to 15 minutes. After the show, the seven-layer die
went to the Alpine lab for customer testing. It is especially correctly to use when
33
working with materials with low molecular weight distribution, which are
characterized by the formation of lines on the film (this lines can be lead to
different in thickness, color, transparent).
According to information [21], during blown film extrusion, there are
common cases of material degradations in the extruder stagnant zones, leading to
decrease in the melt quality, and then to the melt filter destruction. Last research
indicates that this problem is lead to impurity on the surface extrusion screws and
not in the blown die as previously thought. Even in custom-made mixing units,
where special elements are set up for intensifying mixing, you cannot avoid the
"stagnation zones" in which impurity on the surface are formed. The material
sticks to the screw, then the pieces are torn away from it, which leads to an
increase in the melt temperature, the screw efficiency and extrusion quality process
are decreases.
To solve the problem by Ibanez Extrusoras firms. S.L. and U.B.Tech GmbH
propose a new design of the mixing unit, where the number of stagnation zones is
minimized. The melt particularly going in the special holes in the screw and is
washed through its inner part, as well as from the outside, then mixed, which
creates a direct flow of material that provides a self-cleaning effect. This leads to
an increase in the screw efficiency as well as the cylinder direct functions.
According to the patent [22] The Japan Steel Works, Ltd. acceleration of
purging is achieved by switching the melt flow to the second die. A first pelletizing
unit (A) for extrusion a melt of one color and a second pelletizing unit (B) for
extrusion a melt of a different color. Granules of any color are fed into a twin-
screw extruder. Then the melt goes to the adapter, there is a flow switch after the
adapter, which directs the melt flow to the correspond die. Each die is equipped
with a gear pump and a melt filter.
According to the patent [23] of Gala Industries, Inc, acceleration of setting
up the granulation process is achieved by connecting two dies in series - with low
and high productivity. To speed up the start-up of a complex process, a process
with high productivity, and to reduce start-up losses, it is proposed to use a
34
switching valve with different operating positions. The melt is first fed into a die
No1 with a lower throughput of 2500kg/h, and then when the process is stabilized,
the required level of quality is regulated and the melt flow increases, the flap
directs the flow to the die No2 with a high productivity (throughput) of 4500kg/h.
This achieves significant savings in raw materials.
Bemis Manufacturing Company patent [24], for faster color change, it is
proposed to use liquid colorants and feed directly into the extruder feed zone. In
the cylinder loading zone, closer to the melting zone beginning, a dye is fed under
pressure in a liquid form through a special channel.
The advantage of this method is the high quality of the colorant distribution
and, accordingly, the uniformity of coloration, and also at the point of colorant
introduction as close as possible to the melting zone is provide minimal extruder
pollution with the colorant. An invention important aspect is the colorant supply
channel configuration and the use of a low pressure pump, which reduces the
device cost.
According to the patent [25] of The Japan Steel Works, Ltd there is a
problem of setting and control granulator continuous operation at high levels of
productivity (not less than 1000kg/h). During the granulation process, the process
output and melt viscosity can change. To provide optimal pelletizing, a die design
with a switching valve and at least two dies and corresponding pellet cutting units
is used. The dies have a different number of holes and are adapted to different
viscosities and/or extruder productivity.
In the patent [26], a design of a coextrusion die was developed, which has a
high cleaning speed and film quality. It is indicated that due to the fact that
polymers have a memory function, a matte stripe or turbulence area may appear on
film areas that had a negative effect of high shear stress and temperature. The
patented die makes it possible to produce a film where there are no clearly defined
boundaries between circulars melt flows, have the distribution channels special
design, the alternation of circular and spiral sections. Also, the spiral channels are

35
located not on the outer, but on the inner die surface. An important point is the
mirror surface of the melt distributors.

1.6.5 Analysis of the use of processing additives.

Research on ways to improve the pumping process of high-viscosity liquids
was carried out most intensively in the oil industry. According to [27], a method is
used when a high-viscosity liquid (fuel oil) is pumped inside an circular near-wall
layer of a low-viscosity liquid. According to this method, high-viscosity and low-
viscosity liquids are fed into the pipeline in such a way that the liquid with a lower
viscosity forms a stable ring at the pipe walls, inside which the high-viscosity
liquid moves. Since the maximum gradients of shear rates is observe on the near-
wall layer, this provides a noticeable decrease in pressure losses, which will be the
higher, if the more contrasting in the transported fluid viscosity and low-viscosity
fluid and higher the near-wall layer thickness. However, starting from some value,
increasing output by increasing the wall layer thickness is smaller because is
observe reduce, caused by a decrease in the proportion of high-viscosity liquid
fraction in the total flow. Therefore, it is not recommended to increase the
volumetric content of a low-viscosity liquid above 40-45%. The minimum content
is mainly limited by the wall layer stability.
Processing additives for polymer processing form a relatively stable wall
layer, which improves flow and improves the extrusion process efficiency by
acting as a lubricating layer. For example, in the patent [28] of the Kiev
Polytechnic Institute, it is proposed to introduce processing additives directly into
that extruder section and the die where their presence is required. Compared to the
standard use of additives, by mixing into the base composition, the proposed
method significantly increases the efficiency of their action and does not lead to a
change in the film quality.
The additives action leads to a decrease in degradation particles on the metal
surfaces of die channels and the extruder and improves the surface quality of the
extruded film. The studies were carried out on a laboratory extruder with a screw

36
diameter of 45 mm with an experimental tube die. As a polymer raw material, they
used LLDPE with a MFR of 5g/10 min; as a processing additive,
polydimethylsiloxane was introduced in an amount of 0.05%, which was fed to the
inner surface of the die body. The process was carried out without and with the
additive, at the same temperatures and output. In experiments without processing
additives, the pressure at the die inlet was 16-20 MPa, and in experiments with the
additives was 13-17 MPa. At the same pressure of 16 MPa, the productivity
without processing was 20 kg/h, and with a processing - 28kg/h. Thus, it was
possible to reduce energy consumption, increase output and improve the surface
quality of products without significant quantity input processing additives.
A similar technology called "encapsulation" is proposed for the processing
of thermosetting plastics (Macro, Canada), in this case an additional (enveloping)
layer is injected in the extruder adapter zone that processes the thermosetting
polymer.
For partial problem solving that arising during the extruder purging,
currently processing additives are propose with a dosage of 0.3 to 5%. The main
effect of processing additives are consists in forming on the die walls and extruder
lubricating layer [29].
At the same time, manufacturers of such additives declare the following
improvements:
- an extruder start-up acceleration with a decrease in the waste of raw
materials;
- increasing the film thickness stability;
- provide the possibility of making wider and thinner films without changing
the die;
- improving the quality of films from low quality raw materials;
- reducing the amount of degradation polymer in the extruder die;
- reducing the quantity of melt filter replacement;
- provide the full use of secondary raw materials when processing them into
film.
37
 To create a dynamic coating, it is recommended to start working by adding
5-8% concentrate during extrusion within 30-40 minutes, and 2-3% during
injecting molding for the first 5-10 products. The first sign of a positive effect of
input additive is a decrease in die pressure (or torque and current load on the
motor). Then you should wait for the parameters to stabilize at a reduced level (5-
10 minutes) and reduce the percentage of input to 0.3-0.5% for polyolefins and to
0.3% for polystyrene and polyamide. After that, you can increase the speed of
screw rotation and productivity or lower the operating temperatures in the extruder
last zones by 30-40°C. In this case, the pressure should increase, but stay on the
level little below of starting value. The extrusion additive concentrate forms a
dynamic layer, which is renewed with the constant input of a new portion of the
concentrate. From some time after stopping the input of the concentrate, this layer
disappears. In case of overdose the processing additive is possible the melt slipping
and reduced the extruder output.
According to [30], after the formation of a lubricating layer on the walls, the
melt slip along the metal walls, the shear rate decreases, and the velocity diagram
changes (levels out) (Fig. 1.5). As a result, the time for changing the melt in the
extruder is reduced by 20-30% (from 50 to 35 minutes). The presence of a
lubricating layer leads to a decrease in the torque on the screw, pressure in the die,
an increase in productivity while reducing energy consumption. At the same time,
the adhesion of degradation polymer in the die is eliminated, the extrusion of
compositions sensitive to temperature is provided, it becomes possible to produce
thinner films. In addition, processing additives have a washing effect and reduce
the cleaning time of equipment when changing colors.

38
 V1 = V0 V1 = V0

V1 << V0 V1 ≈ V0

V1 V1
V0
V0
V1
V1

Standard velocity diagram Velocity diagram when slip take place on

(high shear rate in the channel) the channel wall
(significant reduction in shear rate)

Fig. 1.5. Changing the velocity diagram of melt flow rates when using
processing additives
Some of the changeover problems can be solved with plasticizing and
cleaning concentrates. Plasticizing concentrates prevent crosslinking and thermo-
oxidative phenomena of secondary polymers, help their processing by improving
the melt properties (increasing MFI), and improve the physical and mechanical
characteristics of film products. Cleaning concentrates are used for quick and
economical cleaning of extrusion equipment during color transitions. The
concentrate contains mineral filler with a weak abrasive effect and a surfactant.
The use of various additives is one of the ways to solve technological
problems in a single production type. But a number of additional questions arise:
1. Influence of additives on film properties. An increase in strength is
declared with the use of processing additives, but the complex of physical and
mechanical properties and its connection with the complex of requirements for
quality characteristics is a constant issue in dynamically developing factories that
are continuously increasing the range of products.
2. Compatibility with all components that are commonly used in
formulations. There can be more than 100 components, and some types are used
once a year.
3. Operability the additives in the all range of temperatures and speeds. A
part of products numbers can be manufactured at the limit values of polymer

39
processing, accordingly, the additive should have a wider processing range than the
base polymer. For example, the masterbatch thermal stability at 300°C provides its
stable processing in the range of 220-260°C. If the heat resistance of the colorant
decreases to 260-280°C, problems arise during changeovers, start-ups and
shutdowns of the line, since in this case temperature “overshoots” may occur
during the stabilization of modes.
4. Criteria for estimating the additive, the economic practicability of its use.
5. Additives manufacturability, taking into account the fact that the
controlled parameters can be more than 100 and more than 30 technological
parameters can change during the changeover.

1.7 Some practical observations the wall flow influence in extrusion

processes.
When processing polyamide (PA6), when the line is stopped with the
heating turned on for 1 hour and the screw speed is zero, the raw material is
degradation. If you set the screw rotation speed to 1 rpm (while the extruder
operating speed is 100 rpm), there is no observe the degradations for 10 hours after
the line was stopped. At a low screw speed, the polymer residence time in the
extruder is 100 times longer than at the process operating speed. Therefore, the
melt small movement in the extruder provides that there is no polymer melt
degradation.
Such a conflict cannot be explained by melt flow models that assume that
the linear velocity at the channel wall is zero. There is a direct relationship between
die operating time and purging time for changeover between colors. That is, the
channel surface cleanliness and corrosion resistance surface is affect on the
purging time.
Here are some more observation results:
• the use of a 5% processing additive based on fluoroelastomer and
polyethylene, when purging the LPDE layer, during color changeovers, accelerates
purging by 1.5-2 times;

40
 • adding lubricants to the layer, improves its distribution, reduces the
thickness difference for a layer with a thickness of 12 microns by 1-2 microns, that
is, by 8-16%;
• addition of 0.5% lubricants or 10% white masterbatch with 50% titanium
dioxide, stabilizes the extruder output even when extruder is wear and tear.
So, the processes of near-wall flow affect the technological parameters of
extrusion and coextrusion, their analysis and control is required when changing the
recipe, when stopping and starting the extruder, when is purging from build-up
polymers in the melt flow channels.

41
1.8 Types of coatings used for processing the channels of melt flow in the
extruder and die.
To provide the sliding melt over the surfaces of modern molding equipment,
various coatings are used (Figure 1.6).

Fig. 1.6. The appearance of typical coatings of the melt flow channels
(Plamex company stand on the K-show)

The mechanism of coating action on the melt flow channels is similar to the
operation of processing additives, which form a lubricating layer on the walls and
ensure the melt sliding on the walls. That is, the presence of a coating leads to the
fact that the time for replacing the melt in the extruder decreases, the torque on the
screw and the pressure in the die decreases, productivity increases with a decrease
in energy consumption, the adhesion of degradations polymer in the die is
eliminated, the extrusion of compositions sensitive to temperature is provide, and
the time for purging equipment is reduced when color change.

42
 Table 1.6
Comparative characteristics of various coatings
Coating Thickness, Hardness, Wear resistance Corrosion
type μm HV resistance
Cr 25 950 4 2
Ni 25 550 2 5
PVD, TiN 4 2500 3 2
PVD, CrN 4 2100 3 3
PVD, CrN 8 2100 4 4
multilayer

Nickel or chrome plating is the standard, classic solution. Depending on

what is more important corrosion resistance or wear resistance, choose the type of
coating [31]. PVD coatings have higher hardness and lower adhesion to the melt,
therefore they are more preferred when processing heat-sensitive melts and
polymers with high adhesive properties. The disadvantages of PVD technology
include difficulties for made uniform coating in the deep holes (the depth-to-
diameter ratio must be not more than one). The properties of various types of
coatings [32] are shown in Table 1.7.

Table 1.7
Properties of various types of coatings
Parameter CrN CrN+OX Metall
CrN TiN TiCN
multilayer (CrN modified) amorph
2100 - 2300 - 2800-
Hardness, HK 2100 - 2500 2200 - 2700 1800
2500 2800 3300
Temperature,
650 650 700 500 400 700
max,°C
Plasticity
+++ +++ ++ ++ + +++
(Ductility)
Steel Gray,
Colour Steel gray Multicoloured Gold Copper
gray copper
Thickness,
2-5 3-9 3-9 2-6 2-3 2-4
micron

43
 New types of coatings include TiAlN, AlCrN and amorphous metals.
Amorphous metals coating have a lower surface roughness and a higher quality
structure (without pores and microcracks) compared to PVD coatings, while they
can be applied inside deep holes, with a depth-to-diameter ratio of up to ten.
The channels surface quality affects the waste during changeovers, research
in this direction is very laborious, since the extruder and the die work for 10-15
years and it is almost impossible to take into account all the factors that affect the
change in the washing time, and the coatings themselves and their application
technologies are constantly being improved.
From practical observations:
- If we compare a nitrided die and a die with a CrN-OX coating, then
the use of the coating, when working with the thermo-sensitive melt
(mix PA6+PVOH), reduces the so-called sweating effect of the “die
droop” by 2-3 times, thus the period between die cleaning increases
from 4 till 12 o'clock.
- When working on worn-out screw-cylinder pairs, situations are not
uncommon when, after change to a colorless composition (standard
transition of 0,5 hour), the extruder, in the reverse order,
"remembers" all the previous colors and is about one or two shifts
(12-24 hours) the rolls can be randomly colored with different colors
of the previous colorants. The colored level is very small, so this
effect visible only in the roll (in the mass).
- Co-extrusion five-layer die (with nitrided surface), which has
worked for 1 year in a single production type, after cleaning and
polishing, provides a 1.5-2 times reduction in waste during color
changeovers.
It should be noted that, of course, the channels coating is not a kind of panacea for
all the problems associated with purging; the channels design and balanced recipes
and correct operation with the die - plays an equally important role.

44
 1.9 Modern problems of modeling the processes of polymer melt flow.
The development of polymer melt flow models is in the direction of expanding the
physical characteristics used to predict the technological properties of polymer
materials based on the analysis results of the rheological curve.
The following generally accepted models can be cited:
• power law and polynomial equation, models allow determining the viscosity at
shear rates close to zero;
• Bueche-Harding, Ellis fluid model, Carreau model, Cross model additionally
include polymer relaxation time and viscosity constant at low and high shear rates.
• Cross-WLF model, where the relaxation time is replaced by the critical shear
stress at which there is a transition to the Newtonian flow in the region of high
shear rates.
The Ellis model, Carreau model, Cross model [33–37] are generally
accepted to describe the full rheological characteristic. There are other models for
the development of a power law, where it is proposed to use the relationship
between the flow index and the shear rate and temperature [38].
In connection with the expansion and modification of polymeric materials,
the creation of various compositions and copolymers, and the development of
technological additives, the question of creating flow models that take into account
sliding on the channel wall arose [39, 40]. Such models are also interesting for the
creation of equipment for the processing of thermosensitive polymers, where
coatings of equipment channels, technological methods (for example,
encapsulation) and processing additives provide melt slip and extrusion process
stabilization.
It is interesting to note that models that take into account slip on the channel
wall also use a power law, that is, the dependence nature is preserved, but the flow
process, the analyzed parameters and the melt diagram of flow rates, with this
approach, change significantly.
The melt flow near the channel wall affects many effects:
-elastic turbulence of the extrudate surface ”melt fracture”,
45
 -slow extrusion of the wall layer from the die, which comes out or in the
form of thermo-degraded melt pieces, sometimes in the form of a crown,
sometimes in the form of drops of superheated melt “die droop”.
That effects are not yet possible to calculate, and only directions for solving
such problems have been developed [41, 42].
Methods for calculating modern plastics processing processes are based on
simplified, empirical models that predict viscosity in a very narrow range of shear
rates and are built with limitations, which in practice significantly affect the
production process. The models parameters are difficult to correlate with the
physical, molecular characteristics of polymers, technological modes of their
processing. Therefore, the development of accurate and simple models of melt
flow taking into account the effect on the wall layer in the widest possible range of
shear rates is an urgent task.
1.9.1 Problems of modeling multilayer flow.
According to existing approaches for calculating multilayer flows at the
interface of two immiscible liquids, the following conditions must be satisfied:
continuity of both tangential and normal velocity components (this means no
slippage at the interface); continuity of shear stresses; difference balance between
normal stresses on the surface with surface forces. The boundary condition is also
the equality to zero of the flow velocity on the channel walls [43].
Modern gravimetric systems provide the required layer percentage by
controlling the output of each extruder at the required level. Moreover, a
proportional relationship is set up between the specified layer thickness and the
volumetric productivity of the corresponding extruder, excluding the layer position
in the die channel and/or the die design. On the one hand, this approach contradicts
the generally accepted theoretical description of a multilayer flow; on the other
hand, it gives high accuracy in controlling the thickness of each layer.
For example, for a three-layer LDPE/LDPE/LDPE material consisting of
identical mono-layers, with a layer ratio of 33.3/33.3/33.3, the theoretical velocity
diagram (Fig. 1.7) satisfying the conditions of multilayer flow shows that the
46
middle layer productivity should be ≈2 times higher than the outer and inner layers
productivity. In fact, to achieve the same layers thickness, the extruders output
must be the same or nearly the same.

Fig. 1.7. The theoretical diagram of the velocities of a multilayer flow

calculated on the basis of a power law
In coextrusion, the layer thicknesses are directly proportional to the
corresponding extruders output. At the same time, viscosity varying, filler amount,
flow index does not have a noticeable effect on the layers distribution. Such
experimental data contradict the theoretical results of multilayer flow modeling,
which are based on shear flow models calculations.

1.9.2 Problems of modeling the melt movement in the extruder screw.

The generally accepted models of the polymer melt flow in the extruder
screw dosing zone require modifications and changes.
The design improvement of a single-screw extruder is in the direction of
modifying the geometry of the screw and barrel, increasing the purity and hardness
of their surface. Bimetallic screw-cylinder pairs have been developed and are
widely used, and the coating grades are adapted to the tasks of increasing abrasive
or corrosion resistance, various combinations of screw and barrel coatings have
been selected for optimal extruder operation [44].

47
 A significant increase in the single-screw extruder productivity is achieved
through the use of a barrier screw in combination with longitudinal grooves along
the entire barrel. Such an extruder was named Helibar-extruder and is considered
as one of the most effective means of resource saving in plastics processing [45].
Moreover, resource saving is associated with a decrease in energy consumption
and loss of raw materials, since the extruder purging is significantly accelerated.
These practical results are largely don’t conform to the modern theoretical
concept of the dosing zone operation as a pump for pumping liquid.
Very often, theory in plastics processing processes goes behind practice,
perhaps one of the reasons is that the melt is analyzed as liquid, and the real
movement is closer to the sliding of a solid on the surface.

1.10 Methods foresee properties for film quality control.

The complex of quality characteristics of film materials and the development
of methods for predicting them in a single production type is becoming one of the
technological process key methods. Moreover, the skill and experience of the
operator in coextrusion processes often does not help to speed up the equipment
setup, since the relationship between the technological process parameters and
quality characteristics is multifaceted.
The products quality characteristics are an indication that the changeover is
complete, the fact that operations No. 3, 4, 5 (Table 1.4) have been completed, that
is, the secondary molding has been stabilized and the line has been set up to a
standard output and produces high-quality products.
Quality control of film polymeric materials is carried out from 30 minutes to
5 hours. It depends from the number of controlled parameters and the time of
testing. For example, only conditioning film samples before measuring mechanical
properties should be at least 2 hours. The control time is comparable to the line
changeover time; therefore, the technology must provide a 100% guarantee of a
high-quality product without process additional regulations.

48
 The KPI patent [46] proposes a method for predicting the properties of an
epoxy composition, which is made using ultrasonic modification. The problem of
increasing efficiency, simplifying the forecasting process and increasing the results
accuracy is being solved when determining the effective ratio of the ultrasonic
processing parameters, which will allow the directed implementation and
prediction of the epoxy composition parameters. A method for predicting
properties is proposed, where the effective values of the studied variable
parameters of ultrasonic treatment (input) are determined, which are selected as the
frequency, amplitude, intensity of ultrasonic vibrations, as well as temperature,
time and predict the quality properties (output) using a first-order mathematical
model ( linear regression equation) for each variable, which looks like this:
Yi (X) = c0 + c1*X1 + c2*X2 + c3*X3 + c4*Х4 + c5*X5,
Хi - input parameters of ultrasonic treatment.
Yi- output parameters, technological and operational properties of the epoxy
composition.
c0, c1, c2, ..., c5 - equation constants to be determined.
Analysis of literary sources on this issue shows that there are no reliable
methods and models, the above study is the beginning of work in this direction.
When describing technology, it is often limited to trends or analysis of the
relationship of one or two technological parameters to characteristics. For example,
for the orientation process, an increase in the stretching coefficient - intensify the
orientation and, accordingly, increases the film rigidity (module) in the direction of
orientation, but the whole complex of technological parameters and control
methods is not given.
At the same time, the development of secondary molding processes is as
rapid as arise of new polymer materials for processing in extrusion processes.
For example, Macro (Canada) [47] offers several secondary molding
schemes for one and the same set of equipment (Fig. 1.10). The secondary molding
method choice is determined by which polymer is chosen as the main barrier to

49
gases - PA terpolymer, EVOH, PA or PVdC, it is also possible to install an
electron-beam processing module.
At the same time, it is the secondary molding technology that provides about
50% of the total variety of nomenclatures. Moreover, if the nomenclature is created
by varying the raw material or thickness, that is, it is set by primary molding, then
the result is that the change in quality characteristics is quite easy to control. When
varying the technological parameters of secondary molding, it is difficult to
evaluate the results of monitoring the physical, mechanical and shrinkage
properties when the required properties are not achieved and additional regulations
of technological modes is required.
Therefore, the actual task is to develop methods and models that make it
possible to comprehensively predict characteristics and efficiently control the
process. Such methods are especially important in make-to-order production, for
example, with several changeovers during a one shift, when it is necessary to
accurately and quickly regulate the line if there are deviations in the process.

50
51
 1.11 Characteristics of typical co-extrusion line for the production of
shrinkage tubular films.

1.11.1 Typically technological scheme of production with the method triple-

babble .
The technological process for the manufacture of multilayer polymeric
materials by the co-extrusion method consists of the following main stages:
• extrusion of polymer melts;
• molding a multilayer tube and stabilizing the first diameter;
• orientation in the MD and TD directions and stabilization of the second
bubble diameter;
• heat setting (thermo-fixation) and control of the film shrinkage in the MD
and TD directions, stabilization third diameter;
• cooling of tubular or flat multilayer polymer material;
• control winding of multilayer polymer material.
In this technological process (Fig.1.9), the transportation of raw materials is
carried out by a vacuum unit. To prepare the outer (A) and inner (E) layers
composition of the multilayer film, the process of components mixing (PA6,
PA6/66, antiblocking, slipping additives) is carried out in the recipe preparation
station. The station consists of receiving hoppers for loading each component, a
gravimetric dosing unit, a mixing hopper and a storage hopper for loading into the
transportation system.
The finished mixture is fed into hopper, which is equipped with a weighing
system. When the actual output of raw materials from this hopper is measuring, the
gravimetrical system can controls the output of the extruder. The relative error in
dosing the melt for each layer is not more than ± 1.5%.
The extruder provides melting, mixing of basic polymers with additives,
creates pressure, provides polymer material compression, thus from a semi-
crystalline, polymer passes into an amorphous state. The creation of an amorphous
polymer mass is an important stage in the technological process triple-bubble,

52
because the next operations of secondary molding can only be carried out with an
amorphous structure. If the crystalline formations in the granules PA are not
transferred to the amorphous phase, it is difficult to make a high-quality film. The
extruder must provide stable output and pressure while minimizing polymer
degradation.
Next, a melt filtration unit is installed. This is an important element for
formulation changes and especially when using polymers and colorants and
additives with low thermal stability. The filtration unit design should provide for
quick replacement of filters.
The coextrusion die have four blocks; in the first one the extruders are
connected and the melt flows distribute from each extruder to the second block,
where the flow are divided and prepared for the spiral melt distributors. The third
block is spiral melt distributors, where each layer is separately formed, and the
fourth is a block of joint flow of layers and formation of a tubular multilayer
preform. The die has a device for adjusting the thickness difference of the final
multilayer first tube.
To cool the multilayer tube, a water-oil cooling system is used. Vaseline oil
is fed inside the tube, outside the tube is cooled with water. By regulated the oil
and water level, operator provide the required diameter of the first tube (first
bubble).
The first pulling rolls is installed in a bath of cold water. Its rotation speed is
automatically set by the gravimetric control system so as to provide the required
thickness of the first tube while keep in the extruders output.
After quick cooling the tube, the required amorphous structure of the first
bubble is fixed. The tube is transform to flat tape, bended and fed through a system
of additional rolls to the IR heating unit where the material is heated to the
temperature of a highly elastic state. Then the tube is blowing in tensile direction
(TD) and at the same time the tube is stretched in the machine direction (MD) by
means of the pulling rolls, so provide the film biaxial orientation (second bubble).
In the process of orientation, when macromolecules are in a highly elastic state,
53
they straighten, the packing density of macromolecules increases, when the
maximum possible increasing of the length macromolecules is reached (for a given
material, at a given temperature) – the second bubble is stabilization.
Further, through the system of additional rolls, the tubular film is fed to the
fourth pulling rolls, where it is heated to the temperature of the maximum
crystallization rate. Heat setting is providing formation of hydrogen bonds between
PA macromolecules, the film structure is strengthened, and the final crystal
structure is formed. By controlling the pull rollers speeds and changing the bubble
diameter in heat setting unit forms a regular, controlled packing (relaxation)
macromolecules in the required direction and thus regulated the film elasticity in
this direction. In the process heat setting the diameter (triple bubble), mechanical
properties and shrinkage properties are stabilized, and the difference in film
thickness is slightly reduced.
Next, the tubular film with the help of additional rolls is led by the rolls to
the winding device. To reduce the winding forces, a tension regulator is installed in
front of the winding device. After winding, the bobbins are set on pallets and
transported to next processing.

54
 Fig.1.9. Functional diagram of the manufacture typical process of a
multilayer heat-shrinkable tubular film by the method of coextrusion
1-loading hopper for gravimetric dosing; 2-extruder; 3-co-extrusion die; 4-
unit for forming the first babble dimensions; 5-cooling bath; 6-first pulling pair of
rolls; 7-additional rolls; 8-unit for heating the first tube; 9- unit for blowing the
tube and forming the film (second babble); 10-fourth pulling pair of rolls; 11-unit
for heating and the film heat setting; 12-unit for control the third babble after film
heat setting; 13-winding device.

1.11.2 Specifications.
Product: Co-extrusion tubular five-layer shrink barrier film.
Film structure: A / B / C / D / E, tubes width: 60-300mm, roll diameter max
410mm, film thickness 25-60 microns, thickness variation ±7% (for ±3σ range)
and if 7% is more than 5 microns then deviation no more than ±5 microns.
Productivity: max 80kg/h, max speed 200m/min.

Table 1.8
Configuration extruders by layers
Extruder А E
B C D
outside inside
Screw diameter, 45 25 45 25 30
mm
L/D ratio 30:1 30:1 30:1 30:1 30:1
Screw revolutions, 160 150 160 150 160
maximum, RPM
Output, max, kg/h 30 5 30 5 15
PA6 Tie LDPE Tie Resins PA6
Resins
PA6/66 LDPE LLDPE Plastomers PA6/66
Polymer
LDPE LLDPE HDPE LDPE LDPE
configuration by
LLDPE HDPE PP LLDPE LLDPE
layer
HDPE EVOH PA6 HDPE HDPE
PP PA6/66 PP
mLLDPE

55
1.11.3 Range of products.
Let us consider how the nomenclature of a five-layer polyamide heat-
shrinkable tubular film for packaging sausages is formed. What properties are
provided and how these properties are achieved.
The base film PA/Tie/PE/Tie/PA has the following main characteristics:
• outer polyamide layer provides high mechanical strength, low permeability
to oxygen and other gases, has a high gloss and printability;
• middle layer, consisting of polyolefins, gives low vapor permeability and
high elasticity, reduces the loss of weight of the product during storage (drying);
• adhesive layers, consisting of ethylene copolymers, ensure the multilayer
material operation as a whole;
• inner polyamide layer in contact with the product is biologically neutral,
highly resistant to food acids and fats, and ensures optimal casing adhesion to the
meat product.
Table 1.9
Formation of the basic casing range
Qualitativ How is it achieved Number of
e
standard sizes
parameter
Color Coloring one or two layers by adding 1% to 50
20% color masterbatch in the layer recipe
Diameter Change in diameter of a casing at constant from 30 to 200
tensile coefficients with step 1мм,
total 170
Thickness Change in thickness of a first tube at constant 35μm, 40μm
tensile coefficients 50μm, total 3

56
 Total 50*170*3=25500 standard sizes of the basic nomenclature film, due to
different colors, diameters and thickness.

The production of new types is achieved:

• use of additives (mineral fillers, foaming agents) that fundamentally
change the appearance, organoleptic properties, roughness and surface structure;
• modification of physical and mechanical parameters that influence on the
shape of the sausage product, pilling the casing from the product (before cutting
and vacuum packing), provide the possibility of cooking in metal molds and
bending the casing to give it a ring shape;
• use of additives that change the permeability of the film for various
applications (UV barrier, permeability for smoke);
• use of additives and technological methods that modify the surface
properties of the outer or inner layer to improve adhesion with special types of
paint or change the adhesion with various types of meats.
In addition, the standard sizes for the new type are developed according to
the technology of the main range by adding different colorants, different diameters
and thicknesses. (Table 1.10).
Table 1.10
Methods of developing new types
Qualitative How is it Color, Diameter, Thickness, Total types
Type

parameter achieved pcs pcs pcs

1 2 3 4 5 6 7
Appearance, Additive N1 to
1 organoleptic outer layer 10 100 1 1000
characteristics
Roughness, surface Additive N2 to
2 10 100 1 1000
structure outer layer
Surface activity Additive N3 to
3 and layer outer layer 10 50 1 1000
compatibility

57
 Continuation of table 1.10
1 2 3 4 5 6 7
Increasing the Additive N4 to
4 barrier to UV middle layer 10 100 2 2000
radiation
Forming a sausage Change of
5 in the form of a technological 20 50 2 2000
ball, ellipsoid parameters
The casing is Change of
pilling when technological
6 20 100 3 3000
cutting in a form of parameters
spiral
Appearance, Additive N5 to
7 organoleptic middle layer 10 100 1 1000
characteristics
- - - - - SUMM 11000

It should be noted that the total number of items is 36500 pcs. does not
reflect all the equipment capabilities and can be expanded. For example, radical
UV inks are used to reduce the cost of UV printing on casing. Such paints have
much higher adhesion to PE than to PA, and to solve the problem, in the casing we
change the places of the middle and outer layers, as a result we get a new look with
the structure PE/Tie/PA/Tie/PA, which has the technology specifics, as the outer
polyethylene layer has its own characteristics of slipping along the pulling rolls of
the extrusion line and printing equipment, and has a specificity of its application at
a meat processing plant.
On the other hand there are 80-150 popular nomenclatures, which take 80-
90% of the total monthly production volume, but the company provides the ability
to product the all range, because even one small order can influence the client and
argue him to give larger orders in the future. Actually it depends from factory

58
management policy in relations to customers and strongly depends on what
competitors offer.
For the studied line, based on practical observations, the time values were
measured for each type of operation in the technological changeovers process to a
new type of product (Table 1.11).

Table 1.11
The range of time variation in the technological changeovers process
Unit,
№ Т, Т,
Describe Process module of
operation min max
equipment
Recipe change in
Recipe
feed bins(recipe Dosing
1 20 30 making,
station
preparation station) mixing

Melt purging in
coextrusion die and Extruding Extruder,
2 10 90
the melt Die
extruder
Thermal stabilization
of the extruder after
Extruding Extruder,
3 10 30
changing the set the melt Die
temperature
Secondary
Units from
forming
Extruder output first tube
(sizing,
4 10 30 forming
stabilization orientation,
unit….to
heat set,
rewinder
winding)
Secondary
Stabilization of Units from
forming
first tube
secondary molding (sizing,
5 5 30 forming
orientation,
processes unit….to
heat set,
rewinder
winding)

59
 Thus, it is confirmed that the most difficult to predict operation No. 2, and
purging the extruder and the die can be long in time.

1.12 Conclusions on the first section.

1. The production of flexible multilayer packaging materials by the
coextrusion method is small-scale, in some cases single type, therefore, it is
necessary to develop methods for controlling the technological process in
conditions of changeovers in order to improve the three main production indicators
- productivity, cost, quality.
2. There is an obvious contradiction between the developed practical
methods for accelerating the changeover and blowing, aimed at intensifying the
flow at the channel wall, and the theoretical description of the polymer melt flow
process, in which the flow at the wall is taken to be zero, semi-empirical models
are used that do not explain the observed effects in the flow of polymer melts.
3. It is required to develop express methods for control and analysis of the
coextrusion technological process and the rules for developing control actions,
development of methods and models for predicting the quality characteristics of
film materials depending on the technological modes of secondary molding to
reduce the process time stabilization after the changeover.

60
 Section 2. Development of mixing technologies, extrusion and product
quality control

2.1 Research and development of supporting processes

Each layer is designed for its functionality and usually consists of several
materials. The mixture preparation for each layer can be carried out in two ways:
1. In a simplified method, preparation and mixing of all components (before
feeding them into the extruder gravimetric hopper) is carried out in a concrete
mixer or rotating barrel, where each component is manually weighting and filled.
2. An automatic station is used for loading, dosing (weighing), mixing and
feeding into the extruder each component used in the layer recipe.
Obviously, the complication and rise in the cost of equipment service
(Figure 2.1.). Moreover, a number of questions arise about the manufacturability of
automatic mixture preparation for each layer.
1. How much does product quality improve?
2. How much will the stability of production increase?
3. How, at the design stage of the technological process, to determine the
required amount of automatically dosed components for each layer?
4. Where to look for the economic effect from the recipe preparation system
introduction?
5. How will this affect on the production system flexibility?

61
 a b

Fig.2.1. Variants of schemes for automatic recipe preparation stations, a-

gravimetric principle of recipe preparation (using a weighing and mixing bunker),
b - gravimetric dosing by continuous monitoring of weight change

At the design stage, first of all, it is necessary to determine which layers will
be colored, and it is for them that it is imperative to provide for automatic dosing
of the colorants. This solves a number of issues related to the manufacture of
colored films. First of all, the problem of on-line color control is solved if color
deviations are associated with the masterbatch instability.
When is going the changeover by color, in the production of minimum
volumes of film with the so-called "exclusive" color, difficult to predict and
calculate accurately is how much colored mixture to prepare for the small batch of
products, especially when the products mass is comparable to the mixing bunker
volume, this usually leads to waste of colored raw materials, or underperformance
the required volume of a batch of products. The use of a dosing system solves this

62
problem, simplifying batch control, minimizing the mass of waste production
colored mixtures.
For conditions single production type, if we view which dosing method -
with one weighing bunker or with continuous control of the weight of each
component, to use for dosing colorant, then the principle of continuous weight
control clearly wins here, as the result is achieved with a simpler (compact) design
and the colorant loading is as close as possible to the extruder loading zone, which
will allow for more efficient color control.
About scheme Fig.2.1-a should say that can see granulometric composition
influence on the mixing quality, therefore there is a need to vary the mixing time
and dose volume, when changing particle size distribution of the introduced
components, for example when changing the masterbatch density. The reason is
the density and size of granules of modern masterbatchs is instable (different
suppliers used different pigments, equipment, recipe) and density is in 1.3-2.0
times higher than the basic polymer density, as the super-concentrate contains the
big percent of the mineral filler. Therefore, it is not always possible to produce a
homogeneous mixture of granules in the mixing bunker. It is especially difficult to
homogenously mix when the colorant percentage is low (0.5-5.0%). At the same
time, for 15-40% colorant dosing, the first method (Fig. 2.1a) may be more
preferable, because in first, the quality of mix in this case can be make on
satisfactory level and in second for provide high output of the dosing unit that
working on the principle of weight changing, it is necessary to provide the
correspondent volume of the bunkers which is not always ergonomic. But if it is
necessary to cover the all range of possible dosing of the colorant from 0.5% to
30%, you can go to the complication of the dosing system design but provide the
color reproduction stability. So for colorants dosing, the second method (Fig. 2.1b)
is more preferable.
The next task solved by the use of automatic batch preparation stations is the
introduction of the so-called key components into the recipe, that is, components
with a dosage volume of 0.5% to 3%.
63
 In plastics processing technology, practice is far ahead of theory. New
polymers and compounds appear every year. Moreover, their use is often non-
standard, that is, not the way the developer imagined it. The constant search for
technological solutions aimed at modifying various mechanical, chemical, barrier
properties of polymer films and packaging by introducing various additives leads
to completely unexpected results, for example, combining polymers in a single-
layer film that do not adhere to each other in multilayer film.
Therefore, the introduction of key additives into the existing recipe, as well
as the high flexibility of the recipe preparation technology with guaranteed stability
of its reproduction, gives significant advantages in the development and
modification of the film properties.
The use of an automated control system for the process of preparing the
composition recipe for each layer of a multilayer polymer product provide the
minimum influence of the human factor on the accuracy of making a working
composition. This increases the efficiency of technological process control as a
whole, improves product quality and process stability. Additionally, the tasks of
accounting and control of raw materials consumption can be solved.
Based on practical observations, the introduction of an automatic recipe
preparation station can reduce waste by 1.5 times.
In general, there is often a temptation to attribute many organizational and
technological problems related to product quality and production waste to batch
preparation operator errors. Eliminating this factor in itself is a huge step in
improving technology.

64
2.1.1 The influence of deviations in the operation of mixing equipment on
product quality.
To study the supporting processes of weighing and mixing the composition,
two periods of mixing equipment operation were chosen (the dosing device output
is not more than 250 kg/h, dosing mixing of 6 components). The first period is the
stable process, that is, there were no systematic lines failures and operator
comments about problem with dosing station, and the second period, when alarms
and failures in the dosing system appeared daily. The main reason for the case of
periodic alarms in the mixing station is problems in the compressed air system,
compressed air pressure instability (fluctuations) was 5-7atm, with a frequency of
3-6 hours. The instability of the compressed air pressure led to alarms from the
mixing station diagnostic system, but was not clearly reflected in the extrusion
process, the film was produced without stopping and of satisfactory quality. It
should be noted that the main coextrusion equipment units do not require high
pressure (7-8atm) in the compressed air system, at the same time the station's
dosing elements required a stable and high level of air pressure, and this was
reflected in the dosing station operating manual.
The work of the recipe preparation station is that dosing is led by controlling
the speed of opening the damper using a pneumatic cylinder, the damper reaction
time is less than 0,1 second, therefore, high compressed air pressure stabilizes the
dosing process. The station is equipped with an air pressure sensor, which is set to
an alarm limit of 5 atm.
For analyzed the stability of mixing, the following technique was used: 2
parallel samples were taken from the extruder feed hopper with a volume of 8 liters
(≈7 kg of raw material) (where the mixing composition was located). Sampler is in
the form of a metal glass with a handle, length about 0.5m. The samples total
weight P∑ was from 24g to 28g, then the sample was disassembled by components
from one granule to other and the components percentage was calculated.
In many sources [48-52], there is no of mixing analysis a multicomponent
system, or it all comes down to estimate of the key component distribution.

65
 The proposal, shown in [53], to determine the stability of mixing by the
uniformity of distributions of one or two key components, also does not allow a
process comprehensive analysis, since:
• there can be three or more key components (a given percentage from 1% to
10%);
• each component can have different properties influence on the stability of
its dosage, uniformity of distribution, electrification, granulometric indicators, etc.;
• deviations can occur due to errors in the working meter of one of the key
components, while the other metering units were working stably;
• and finally, probably the most important thing, that the technologist needs
to see the accumulated dosing error, as this will allow a deeper analysis of the
process, draw parallels with other process parameters and quality characteristics.
Although it should be noted, further research has shown that for quick
estimate, a method based on the analysis of one component is applicable as a
express method.
To develop a comprehensive methodology for monitoring a multicomponent
system, the deviation in each sample from a given percentage was calculated
taking into account the deviations of all components used, that is, as a total
deviation, according to the formula:
1. Δj = ∑│Xex ij – Xset ij│
Where
Xex ij - the measured percentage of the component with index (i), in the
sample with index (j);
Xset ij - is setting percentage of the component with index (i) in the sample
with index (j);
i - is the number of the component in the sample;
j – is the sample number.
The parameter Δj can be as a criterion for the quality of mixing at a certain
constant value of the sample size P∑.

66
 The sample size P∑ depends on a number of dissimilar technological factors:
the maximum sample analysis time, the extruder volume, the mixing ability of the
extruder, and the raw material granule size . In this study (when choosing a sample
of no more than 30g), the following initial data were taken into account: the
volume of the extruder is 700cm3, the volume of the dosing zone is 135cm3, the
ratio of the return flow coefficient to the forward flow coefficient is ~ 0.15, and the
sample analysis time is no more than 60 min.
The mixing error, depending on the dosing equipment configuration,
consists of the following components:
Δj = Δ1 + Δ2 + Δ3 + Δ4
Where
Δ1 = balance error, or the weighting error;
Δ2 = error due to the different particle size distribution of the components,
especially the level of electrification and the pellets weight, which leads to
different conveying speeds;
Δ3 = mixing error in the mixing device itself, design flaws, technology
errors;
Δ4 = error caused by a combination of three factors: sample size, mass of
one granule, mass fraction of a component, that is, when the mass of one granule is
comparable to the mass of a component in the sample.
The results of studying the mixing quality for dosing system various settings
are shown in Fig. 2.2. The mixing in the barrel "concrete mixer" was taken as a
standard, when the mixing error is practically constant and caused by only one
element Δ4.

67
 % 16

14

12
Graph N1
10

8
Graph N3
6

2
Graph N2
0
0 10 20 30 40 50 60 70 80
N sample

Fig. 2.2. Change in the total percentage of dosing deviation in the sample under
different operating conditions of the dosing system (Graph 1 and Graph 3 ) and
changing the mixing method Graph 2
Table 2.1
Mixing quality research results
Average value of the total
Experim Process Number of Standard
dosing error
ent No. description samples deviation
Δav
Before regulating
Graph
(before fix) 43 6,8 2,3
№1
dosing system
Graph Etalon
10 3,34 1,12
№2 "concrete mixer"
After regulating
Graph
(after fix) dosing 35 4,08 1,43
№3
system

To search for the process regularities, an absolute and relative errors analysis in the
determination of each component in the sample was carried out.
Δij = │Xex ij – Xset ij│
εij = Δij/Xset ij * 100
During the study, it was determined that the mixing error is related to the
component percentage. For higher the component percentage, the absolute dosing
68
error can be higher, but at the same time the relative mixing error will be lower.
Figure 2.3 shows this pattern.

100
relative error of component content

10

1
0,1 1 10 100
% in the sample

Fig. 2.3. Dependence of the relative mixing error and the component dozing

Table 2.2
Relationship between a given percentage of a component in a sample and a mixing
error (typical values)

Name Xij set Δij εij

Component 1 90 1,7 1,9
Component 2 8 1,3 16,3
Component 3 1,5 0,5 33,3

The effect of mixing stability on product quality was measured by analyzing

the mechanical properties. For this, film samples were taken and tested on a Zwick
2.5kN tensile testing machine (sample dimensions 70x10mm, thickness 20±2μm,
test speed 100mm/min). The assessment was carried out according to the tensile
strength and relative elongation (average values and coefficient of variation). The
minimum values obtained during the tests were analyzed separately.
69
 One of the parameters, that show the characteristics stability of any process,
is the coefficient of variation. In particular, to estimate the elongation stability of
polyamide monofilaments, the tolerance for the coefficient of variation is set at no
more than 15% [54].

3
Force, kg

0
0 10 20 30 40 50 60 70

-1
Elongation, %

Fig. 2.4. Typical mechanical characteristics of film oriented polyamide material

Table 2.3
Example of stability analysis of mechanical characteristics
Coefficient of
Elongation, % Average Standard deviation
Parameter variation
Х1 Х2 Х3 Х4 Хav S S/Xav*100%
Value 50 40 60 55 51,25 8,5 16,7

Comparative results are presented in tables 2.4 and 2.5. Presented are the
mechanical characteristics of film materials with different dosage stability.

70
 Table 2.4
Product quality with dosing stability Graph No.1, Fig. 2.2, the number of
tested samples n = 299
Parameter Breaking force Elongation at break
Average value, Хav 4,92kg 37,25%
Standard deviation, S 0,52kg 6,60%
Coefficient of variation,
S/Xср*100% 10,58% 17,71%
Minimal value, Хmin 4,10kg 29,00%

Table 2.5
Product quality with dosing stability Graph No. 3, Fig. 2.2, the number of
tested samples n = 315

Parameter Breaking force Elongation at break

Average value, Хav 4,83kg 38,29%
Standard deviation, S 0,44kg 6,13%
Coefficient of variation,
S/Xav*100% 9,15% 16,01%
Minimal value, Хmin 4,20kg 29,00%

For the two variants of dosage stability, the coefficients of variation of the
elongation at break of 17.71% and 16.01% were obtained, accordingly. At the
same time, the minimum breaking force increased from 4.1kg to 4.2kg.
So, with a decrease in the total deviation, when mixing from 6.8% to 4.08%,
the mechanical characteristics stability increases by 10%. The minimum breaking
force is increased by 2.3%.
The technique for estimate the quality of mixing by the total deviation of the
components is applicable to control the state of technology and equipment. But it
requires a long-term connection to the current process by analyzing various states
of equipment, formulations and reference processes. Also, the disadvantages
include the lack of flexibility and uniform criteria for mixing quality. The
experiment did not include points with a dosage of 11-89%.

71
2.1.2 Study of the criteria for estimating the mixing quality
To estimate the mixture quality, various methods were analyzed and three
main statistical criteria were identified:
1. The standard deviation of the components content in the samples that are
taken during the experiment.
2. Coefficient of heterogeneity (coefficient of variation).
3. The degree of distribution deviation from the random one, or the mixing
index.
These criteria are developed, in fact, for two-component systems. Modern
recipes usually contain up to 10 ingredients, and the criteria for mixing quality
need to be developed. On the other hand, no clear relationship was found between
the quality of mixing in the recipe preparation and the product quality. Therefore, it
is necessary to develop criteria for estimating the quality of mixing of
multicomponent systems, a method for controlling the quality of mixing and to
determine the quality effect of mixing on the finished product characteristics.
To study this task, research was carried out in a production environment
[55]. Every 1-3 shifts, two parallel samples of the finished mixture were taken
from the extruder hopper. Each sample taken was disassembled into components
(k) and the percentage of components in the sample was determined. The data
obtained for the observation period, the results of the analysis of samples were
averaged and analyzed statistically - the mean content of the Xki component and
the standard deviation Ski were calculated.
As an output characteristic, the physical and mechanical characteristics of
the film in the MD and TD directions (force and elongation at break, modulus,
yield strength, coefficient of variation of elongation) were analyzed. The E-
modulus is calculated over the range from 0.5% to 1% elongation. Measurement of
mechanical characteristics was carried out several times per shift, at the same time,
the mixture analyze from the bunker was performed 1 time in 1-3 shifts. This is
due to the process control system, the analysis time, the quality control system.
The analysis results of the sample representativeness are shown in table. 2.6, the
72
number of tests performed at the inlet (Kts) and outlet (Kfm) of the system - in
table. 2.7.
The mechanical characteristics for each test were determined using 4
samples, and the coefficients of variation for the MD and TD elongation were
calculated. Then the results were averaged over the observation period. 1 month
was chosen as the observation period. That is, all the observation results were
averaged and analyzed after they were collected for one period. The study was
carried out for 5 months (see P1-P5, Table 2.7). And then the observation periods
were compared with each other. During the observation period, a wide range of
films was produced in terms of diameter (20mm-40mm), thickness (16-25
microns), color (colorant content from 0% to 3%) (more than 30 standard sizes).
The extruder bunker with a volume of 10 liters, holds 7.0-8.0kg of raw materials,
the recipe preparation is automated, the mixture was created in a gravimetric
batcher. The weight of one sample for laboratory analysis is from 0.025kg to
0.03kg. Extruder with a diameter of 45 mm, operating speed range 80-110 rpm.
Die back pressure 150–240Bar. Table 2.6 is an analysis example of one sample. It
is known that the spread in the concentration values of the dispersed phase in the
"ideal" mixture obeys the binomial distribution law.
The total number of particles in each sample and their content must satisfy
the relationship [49]:
9
N
c1  c  , (2.1)
where с is the components concentration.
Then the binomial distribution can be replaced by the normal distribution.
To estimate the sample representativeness, a check was made for the minimum
required number of granules in the sample. The mass of one granule of each
component was determined as the arithmetic mean of ten granules. Table 2.6
shows that to estimate the quality of mixing of Component 1, it is enough to select
66 granules, to estimate Component 6, 1938 granules are needed. The actual

73
sample size ranged from 2100 to 2500 granules. Therefore, the distribution of
components in the sample can be considered normal. Additionally, to check the
sample representativeness, a calculation was performed according to [51]. For non-
clumping materials, the minimum required sample mass

10 4  d 3  p
Gm 
2.5  c0
, (2.2)
where: d - pellet diameter; p - the bulk density; c0 - component concentration.
Since the system is multicomponent, the weighted average pellet weight M =
0.0124 g was calculated. Based on the ball shape, the granule diameter is 0.26 cm.
The results of calculating Gm are shown in Table 2.6. According to this
calculation, it was determined that for two materials K4 and K6 with a
concentration of 0.6% and 0.5%, respectively, the sample mass of 30 g is
unsatisfactory (104 g and 125 g are required). It also follows from formula (2.2)
that the minimum concentration of a component for a 30 g sample should be 2.1%.
In the course of further research, it was determined that for components with a
concentration of less than 2.1%, the ± 3S range falls into the area of negative
concentration values, which is physically impossible. But, firstly, the sample size is
enough for estimating other components, and secondly, in this study, the
distribution histograms of components are not studied, while the standard deviation
was enough to estimate the quality of mixing, thirdly, this would increase the
experiment complexity by 4 times and could lead to operator errors.

74
 Table 2.6
Representativeness analysis for sample

N - the
Actual Gm - the
Components

Component minimum
number of minimum
weight in Component Granule required
granules in required
the sample, content,% weight, g number of
the sample, sample
g granules in the
pcs mass, g
sample, pcs
К1 25,12 83,7 0,0118 2127 66 0,7
К2 2,20 7,3 0,0118 186 132 8,6
К3 1,18 3,9 0,0177 66 238 16,0
К4 0,17 0,6 0,0137 12 1597 104,2
К5 1,14 3,8 0,0211 54 246 16,4
К6 0,14 0,5 0,0209 7 1938 125,0
SUMM 30 100,0 - 2452 - -
Table 2.7
Study results table
Кts Period XК1 SK1 XК2 SK2 XК3 SK3 XК4 SK4
21 P1 87,07 1,66 7,37 1,10 1,90 0,59 1,75 0,78
10 P2 86,76 1,36 7,06 0,79 1,99 0,20 2,11 0,77
29 P3 87,38 1,21 7,21 1,01 1,82 0,65 1,86 0,68
29 P4 87,54 1,45 7,23 0,89 1,96 0,64 1,52 0,43
21 P5 87,59 1,02 7,46 1,09 1,83 0,57 1,75 0,59
Кts Period XК5 SK5 XК6 SK6 Ssum Кm F% VF
21 P1 1,23 0,95 0,42 0,18 5,25 110 34,0 15,3
10 P2 1,44 0,67 0,64 0,24 4,03 148 37,9 11,4
29 P3 1,15 0,41 0,53 0,18 4,14 228 37,2 13,2
29 P4 1,04 0,47 0,67 0,49 4,37 225 41,0 13,5
21 P5 0,83 0,34 0,46 0,21 3,81 226 40,2 11,7

Initially, an analysis was carried out of using the standard deviation of one
of the components as an input parameter, that is, they tried to find a component, by
which the entire mixture quality could be assessed, but there was no such
component (see Fig. 2.5).

75
 2,5 6

SK1
5
2
SK2
4
1,5 SK3
Sk1-Sk6

Ssum
3
SK4
1
2 SK5

0,5 SK6
1

Ssum
0 0
P1 P2 P3 P4 P5
Period of research

Fig. 2.5. Changing the standard deviations of S1-S6 components

The change in the total (Ssum) standard deviation for different periods does
not correspond to the dynamics of changes in any of the six components, that is,
the criteria for assessing the stability of mixing for one component are unreliable.
This is shown by the research results analysis given in Table 2.7 in the most stable
period P2 (Ssum is minimal), but the stability of the components K1, K4 and K6 is
not the highest.
Therefore, the parameter was chosen as the input characteristic - the total
standard deviation Ssum for all components. The Ssum value can be a complex
criterion for mixing quality for a multicomponent system.
The search for the output characteristic was carried out by the method of
regression analysis by searching for an equation:
Y = m1x1 + m2x2 + ... + b where the values x1, x2 ... xn are the mechanical
characteristics and Y is Ssum.
Further, according to the Student's criterion, a significant factor was found -
the coefficient of variation of transverse elongation, which reflects the mechanical
characteristics stability . Table 2.8 shows the average value of the elongation F% in
the transverse direction and its coefficient of variation VF.
76
 The regression equation VF = 1.72 + 2.62Ssum, has a coefficient of
determinism R2 = 0.87 and the value of Fisher's criterion F = 19.5 which is higher
than the critical Fcr = 10.13 (for degrees of freedom V1 = 5-3-1 = 1 and V2 = 5-1-
1 = 3 and level α = 0.05). The relationship between the parameters is reflected in
the graph (Fig. 2.6).

The relationship coefficient of variation of elongetion and the total deviation

6 18

16
5
14

4 12
coefficient of
variation, Vf
10
S sum

Vf
3
8

2 6 the total standard

deviation, Ssum
4
1
2

0 0
1 2 3 4 5
Period of research

Fig.2.6. The relationship between the coefficient of variation for elongation and the
total standard deviation

As said above, the coefficient of variation of the relative elongation F%

shows the stability of the physical and mechanical properties. The level of the
coefficient of variation VF = 15% can be taken as critical.
Therefore, only the period P1 can be accepted as unsatisfactory from the
point of view of the mechanical characteristics stability. On the other hand, the
coefficient of variation minimum value in individual tests achieves VF = 1%;
stabilization of this level is the task of further research.

77
 Additionally, we analyzed the dosing accuracy influence of each of the six
components (in turn) on the mechanical properties stability, the level of
interconnection decreased.
So, as a result of experimental studies of the mixture samples
representativeness and the film mechanical characteristics, it was determined that
there is a statistical relationship between the mixing quality and the mechanical
characteristics stability, therefore, in the development of extrusion technological
processes, especially in a single production type with changing formulations, it is
imperative provide for systemic quality control of mixing.
The total standard deviation Ssum lets you to estimate the mixture quality, but
is not a universal criterion for the quality of mixing of a multicomponent system,
since it will vary from the number of components and their percentage. It is
proposed to use the mixing index as a universal criterion [48].

2.1.3 Development and analysis of the mixing index as a universal criterion

First of all, we note that for a multicomponent system, the mixture
coefficient of variation (heterogeneity), as a universal criterion, cannot be applied,
since the ratio Vi = Ski/ Xki * 100% varies depending on the component percentage,
for example, in the first period P1: V1 = 1,91%, and V2 = 14.9%, and the mixing
process was the same.
Let us analyze the various calculation formulas of the mixing index
proposed [48].
In this case, it is necessary to push off from the next mixture indicators:

s0  c * (1  c)
2
. (2.3)
where c - is the component concentration (in parts relative to one).
S02 - is the dispersion of an absolutely unmixed system.

s0  c * (1  c)
(2.4)
S0 – standard deviation of the component content for a completely unmixed
system,
78
 S - standard deviation of the component content in samples taken during the
experiment.
In this case dispersion S2 calculated by the formula:
n

 (C i  C av ) 2
S2  i 1

n 1

where Ci and Cav - are the current and average component concentration in
the sample; n - is the number of samples.
σ2 – general dispersion for an absolutely mixed system calculate:
c * (1  c)
2 
N
Where N is the number of particles in the sample.
It is proposed to calculate the mixing indices according to the following
ratios:

I1 = σ2 / s2 ,
I2 = 1- S2 / S0 2 ,
I3 = 1- S / S0 ,
I4 = (S0 2- S2)/(S0 2 - σ2 ) ,
I5 = 1-( S 2 - σ2 ) /(S0 2- σ2)

To analyze the indexes sensitivity, let us analyze an example from [49]

where four variants of the component distribution are studied.

79
 Table 2.8
Analysis results of the mixing quality of various model systems
System Nr 1 2 3 4

Mixtures structure

Completely
Mixing is Mixing is Mixed
Overall mixing rating unmixed
unsatisfactory unsatisfactory system
system

Particle distribution regularized regularized regularized random

Visual estimate of the mixture

quality on a 10-point scale
0 3 6 9
Dispersion measured (s2 ) 0,105 0,0125 0,0021 0,00109
Standard deviation measured
during the control of samples (s)
0,324 0,1118 0,04583 0,03302
Dispersion of an absolutely
mixed system *100 (σ2*100)
0,1056 0,1056 0,1056 0,1056
Dispersion of an unmixed system
(s0 2)
0,1056 0,1056 0,1056 0,1056
Standard deviation for unmixed
system (s0)
0,325 0,32496 0,32496 0,32496
Mixing index 1 (I1) 0,010 0,084 0,503 0,969
Mixing index 2 (I2 ) 0,006 0,882 0,980 0,990
Mixing index 3 (I3 ) 0,003 0,656 0,859 0,898
Mixing index 4 (I4) 0,006 0,891 0,990 1,000
Mixing index 5 (I5) 0,006 0,891 0,990 1,000

Table 2.7 shows the estimates of the mixing quality. The I1 and I3 indices
are the most acceptable, since they are as close as possible to the visual assessment
of unmixed systems. Indices I2 I4 I5 are not sensitive in the area of almost mixed
system. The I3 index is easier to apply in practice, since it does not contain the
parameter N - the number of particles in the sample, which is very important for
methods of volumetric sampling. Also, I3 has the maximum sensitivity for high
mixing levels (score 9 or more).
80
 It should be noted that for the 4th system, where the distribution was
obtained by the method of generating random numbers, the mixing index is I3 =
0.898, therefore this level can be taken as a boundary level for deciding on the
quality of mixing, this value was confirmed by further studies (see table 2.12).
So, according to the study results of the multicomponent mixture (section
2.1.2), the relationship between the total standard deviation of the mixture
components Ssum and the coefficient of variation of the elongation VF was shown.
For this experiment, the mixing index I3 was calculated. The results of calculating
the mixing index are presented in table 2.9
Table 2.9
The results of calculating the mixing index
I3 – average
Name К1 К2 К3 К4 К5 К6 Ssum VF
value
Period 1 0,95 0,96 0,96 0,94 0,91 0,97 0,949 5,25 15,30
Period 2 0,96 0,97 0,99 0,95 0,94 0,97 0,962 4,03 11,40
Period 3 0,96 0,96 0,95 0,95 0,96 0,98 0,960 4,14 13,20
Period 4 0,96 0,97 0,95 0,97 0,95 0,94 0,956 4,37 13,50
Period 5 0,97 0,96 0,96 0,96 0,96 0,97 0,962 3,81 11,70

All mixing index values are higher than 0.898, therefore, the mixing quality
of all components in all periods can be considered satisfactory. The mixing index
I3 does not depend on the component percentage, therefore it is a universal
estimate.
The regression equation VF =259–256.81*I3 has a coefficient of determinism
R2 = 0.90 and the value of Fisher's criterion F = 27.4 which is higher than the
critical Fcr = 10.3 (for degrees of freedom V1=5-3-1=1 and V2=5-1-1=3 and alpha
level =0.05), calculations were performed using the Excel analysis package. The
relationship between the parameters is also visible on the graph (Fig. 2.7). It should
be noted that the Fisher criterion value for the equation VF=1.72+2.62*S∑ is
F=19.5, therefore, the mixing index I3 has a deeper relationship with the film
quality characteristics than the total standard deviation Ssum.

81
 16,0
Coefficient of variation for relative elongation, VF

15,0

14,0

13,0

12,0
y = -256,81x + 259
R2 = 0,9014
11,0

10,0

9,0

8,0
0,946 0,948 0,950 0,952 0,954 0,956 0,958 0,960 0,962 0,964
Mixing Index, I3

Fig.2.7. Relationship between the mixing index and film mechanical properties

In this study, the range of changes of the coefficient of variation is from

11.4% to 15.7%. Moreover, these are the average values in the periods P2 and P1,
respectively. The 15.7% level can be considered critical; it is preferable to stabilize
the 11% level. On the other hand, each value of the mixing index is also the
average value for the component in the study period. In this study, it is 1 month.
But the technological process requires control based on the results of point control.
Therefore, it is of interest to develop criteria for estimating each sample.

82
2.1.4 Method of mixing quality control
To develop criteria for evaluating a single sample, we will analyze the
distribution of deviations for various components.
Table 2.10
Results of monitoring the content of various components in different periods
Hittin
Average Standard Tolerance Tolerance
№ Min Max g the
value, % deviation, % min max
range
Period Хav Si Xmin Xmax Хср-3Si Хср+3Si ±3S
Component №1 study.
P1 87,07 1,66 83,00 89,70 82,10 92,04 +
P2 86,76 1,36 85,50 89,40 82,68 90,84 +
P3 87,38 1,21 85,40 90,90 83,74 91,02 +
P4 87,54 1,45 82,50 90,80 83,19 91,89 -
P5 87,59 1,02 86,20 90,00 84,52 90,66 +
Component №2 study
P1 7,38 1,10 4,90 10,30 4,07 10,69 +
P2 7,06 0,79 6,10 8,50 4,69 9,43 +
P3 7,21 1,01 5,60 9,80 4,18 10,24 +
P4 7,23 0,89 5,90 9,20 4,54 9,91 +
P5 7,46 1,09 5,80 10,20 4,20 10,72 +
Component №3 study
P1 1,90 0,59 1,30 3,90 0,13 3,68 -
P2 1,99 0,20 1,60 2,20 1,38 2,60 +
P3 1,82 0,65 0,50 2,70 -0,12 3,76 +
P4 1,96 0,64 0,80 3,40 0,05 3,87 +
P5 1,83 0,57 0,60 2,90 0,12 3,55 +
Component №6 study
P1 0,42 0,18 0 0,70 -0,12 0,96 +
P2 0,64 0,24 0,2 1,00 -0,07 1,35 +
P3 0,53 0,18 0,2 0,94 -0,01 1,07 +
P4 0,67 0,49 0,2 2,20 -0,80 2,15 -
P5 0,46 0,21 0,1 1,00 -0,17 1,09 +

Statistical data analysis in Table 2.10 shows that the ±3S range almost
completely covers the range of values recorded in the period. In periods of
maximally stable P2, P3 and P5, there are no exits beyond the range of ±3S, in
periods P1 and P4, mixing fluctuations of more than ±3S are observed. Therefore,
a single sample over a tolerance of ±3S already indicates an unstable mixing.
Let's carry out the distribution deeper analysis using the K1 component on
example. The results are shown in Table 2.11.

83
 Table 2.11
Statistical analysis of the sample control results for component K1 in
different periods
Total
Standard numbe
Observatio Average The number of samples lying
value, %
deviation, Min Max r of
n periods % in the range
sample
s
Хav Si Xmin Xmax ±S ±2S ±3S ±4S
P1 87,07 1,66 83,00 89,70 22 16 21 22 22
P2 86,76 1,36 85,50 89,40 10 8 10 10 10
P3 87,38 1,21 85,40 90,90 30 22 28 30 30
P4 87,54 1,45 82,50 90,80 30 24 28 29 30
P5 87,59 1,02 86,20 90,00 22 17 20 22 22
SUMM - - - - 114 87 107 113 114
SUMM, % - - - - 100 76,1 93,8 99,1 100
Only in one period is there an overshoot ± 3S range. 93.8% of all
measurements are in the ± 2S range. Therefore, a tolerance of ± 2S can be taken as
a standard for the control of a single sample.
Setting the normative for SN value is possible if a certain boundary level of
the mixing index is specified. For example, in this study, it can be assumed that the
mixing index standard value should be I3≥0,96. This mixing index value is typical
for the periods P2, P3 and P5. Therefore, 0,96=1-SN/S0 and taking into account the

fact that the standard deviation value can be calculated: s0  c * (1  c)

The normative for SN value can be calculated:

S N  0,04 * с * (1  с) (2.5)
or as a percentage:

S N (%)  0,04 * с * (1  с) *100 (2.6)

Thus, the standard deviation required value of the component can be
calculated depending on the component concentration in the recipe and the mixing
index required value (mixing quality) [56].

84
 2,5

Calculated value
SN(%) for
2 I3=0,96
Standard daviation, %

1,5
Experimental
values, measured
values for
1 standard
deviation S

0,5 Experimental
values, additional
measured
intermadiate
0 values S
0 20 40 60 80 100
Component content, %

Fig. 2.8. Components standard deviation dependence on its percentage in the

formulation in a quality mixture at I3 = 0.96

Therefore, we can offer the following decision-making methodology based

on the results of a single sample control:
1. For each component K, depending on the given concentration c,
according to the formula (2.6), the standard deviation in percentage SN (%) is
calculated.
2. The controlled sample is analyzed for hitting into the range of Хav±2S N or
ХS±2SN, where ХS - the setting value of the component percentage (in a normally
operating dosing system ХS≈Хav). That is, the absolute deviation Δi=|Хi-Хs| must
satisfy the condition Δi≤2SN, where Хi is the percentage measured value of the i-th
component in the sample.
3. If the result Δi lies in the range of Хav±2SN, then the work of the dosing
system is normal. Moreover, it is necessary to check for all components.

85
 4. If the result Δi is outside the range of Xav±2SN, the analysis is carried out
in the range of Xav±3SN, if the result is outside the range Xav±3SN, then the dosing
system operation is of poor quality.
5. If the result Δi is outside the range of Xav±2SN, but the result falls within
the range Хav±3SN , two additional samples are analyzed, if at least one of the
samples is outside the range of ±2SN, it can be considered that the mixing is of
poor quality and it is necessary technical service the mixer. Otherwise, it is
considered that the error was single and the work in the dosing system is normal.
To control the process overall stability is based on the results of work for a
period (more than 1 month), the actual standard deviation S fakt is analyzed and
compared with the standard SN. If the deviation is above (Sfakt> SN), it can be
considered that the mixing as a whole for the period is of poor quality and it is
necessary provide the technical service the mixer.
It should be noted that with a significant number of components in the recipe
(for example, more than 5), the analysis for each component is a rather laborious
task. Therefore, the technologist needs to determine the number rational value of
controlled components based on the analysis of their influence on the properties of
the multilayer film and the control labor intensity.

2.1.5 Development of a quality criterion for mixing in a single sample

Since the parameters SN and I3 are related to each other, and it is determined
that a single sample should be in the range of ±3SN, it can be proposed to estimate
the distribution of a single sample by the inequality I 3≥0.90, which was found for
the model system (Table 2.8).
To clarify this criterion, an investigation was conducted of problematic
events on the extrusion line associated with significant failures in the dosing
system. Observations were carried out for 12 hours by analyzing the extrusion
process state and the mixture preparation quality.
During the observation period, the dosing system was repaired on the line.

86
 Since when analyzing samples it is more comfortable to work with the
component percentage (and not with the concentration in fractions of a unit), the
calculation was carried out according to the formulas:

s0  Х av * (100  Х av ) (2.7)
where Хav – average (or setting in the system) component percentage, %
n

(Х i  Х ср ) 2
S2  i 1
(2.8)
n 1
where, Хi - measured percentage of a component in a single sample, %
When analyzing the process operability, the set of estimates is similar to that
of [57].

Estimate criteria for Automatic production line

Unacceptable
waste level 10 Actual
failure
(Alarm)
Waste, %

8
Acceptable
waste level
Conditional
6
failure
(Alert)
Standard 4
waste level 0 4 8 12 16 20 24
Time, day
Line is working Line is defective
Line is operational Line is inoperative

Fig. 2.9. The automatic line operation estimate.

87
 Table 2.12
Analysis of samples under various conditions of the extrusion process
Period Process status estimate Component Хav S0 X 11 X12 S I3
К1 43,30 49,55 23,35 29,96 24,00 0,52
The line is defective and К2 50,90 49,99 73,90 65,93 27,48 0,45
inoperative, (unstable line К3 2,10 14,34 1,02 1,44 1,27 0,91
1
operation, unstable К4 2,10 14,34 1,63 1,43 0,82 0,94
extruder output) К5 1,10 10,43 1,09 0,82 0,28 0,97
К6 0,50 7,05 0,56 0,40 0,12 0,98
К1 43,30 49,55 30,56 30,00 18,42 0,63
The line is defective but
К2 50,90 49,99 63,50 62,10 16,86 0,66
operational, conditional
К3 2,10 14,34 1,70 2,74 0,75 0,95
2 failure condition (output
К4 2,10 14,34 2,70 3,03 1,11 0,92
pulsation occurs
К5 1,10 10,43 1,10 1,76 0,66 0,94
periodically)
К6 0,50 7,05 0,44 0,37 0,14 0,98
К1 43,30 49,55 43,60 37,30 6,01 0,88
К2 50,90 49,99 50,05 57,28 6,44 0,87
The line is working and К3 2,10 14,34 1,90 2,17 0,21 0,99
3
operational К4 2,10 14,34 2,51 1,62 0,63 0,96
К5 1,10 10,43 1,60 1,22 0,51 0,95
К6 0,50 7,05 0,34 0,40 0,19 0,97

We see a clear relationship between the unstable operation of the equipment

and the mixing quality. It should be noted that an error of the dosing and mixing of
the main components was found.
In the third period, the index values are 0.87, 0.88, which is less than the
critical 0.90, therefore the operation of the mixing equipment has deviations that
did not influence on the "point" estimate of the process as - stable operation, but
additional monitoring of the dosing station operation is required until the process is
normalized.

2.2 Controlling the melt temperature

To adjust the temperatures in the extruder zones, a certain range is usually
set where it is possible to process the polymer. Based on the process parameters:
the viscosity and strength of the melt, the presence of incomplete melts fractions,
degradation gels, the output stability, the motor current, and the die pressure -
technologist adjusts the extruder temperatures [58].
88
 For coextrusion, it is necessary to additionally take into account, firstly, the
relative influence of coextruded layers, since the melt temperature is equalized
with the cooperative flow in the die and, secondly, the temperature range of their
cooperative processing, since the intersection of temperature ranges decreases the
temperature control range in comparison with the processing of a monolayer [43].
Figure 2.9 shows the processing temperatures of various polymers. It can be
seen that the range of their cooperative processing (intersection of temperature
ranges) is much narrower than for the processing of a monolayer. Melt temperature
prediction is especially important for temperature-sensitive polymers (EVOH,
PVDC, PVOH, PVP) and multilayer (multicomponent) compositions processed in
a narrow temperature range.

EVOH

PVDC

EVA

PA6/66

PA6

PP

LLDPE

HDPE

LDPE

100 120 140 160 180 200 220 240 260 280
Temperature, С

Fig. 2.10 Temperature range for processing some polymers

Modern multilayer structures are created to optimize various types of films

(shrink with a selective barrier, high-barrier for sterilization of packaged product,
films with a twist effect). At the same time, complex structures PA-EVOH-PA-
TIE-LDPE, EVA-PVDC-EVA-PA are used, which are manufactured not only due
89
to the correct selection of technological modes, but also know-how in the design of
equipment [33], for example:
• coextrusion die heating systems, which make it possible to set the
difference in temperature, between nearest layers in the die, is about 40°C, the
standard design gives 10°C;
• technology of encapsulation, which makes it possible is feeding a heat-
sensitive melt with a temperature of 160°C into a die with a temperature of 220°C,
without material destruction.
But in general, the methodology of setting the temperature profile of the
coextrusion unit is quite constant:
• firstly, the cooperative flow temperature in the die (Td) is determined, as
satisfying all polymers of the multilayer structure;
• secondly, the extruder temperature profile and the melt temperature are
selected as Text = Td±(10÷50)°C, while Tw=Tw+(10÷50)°C if the polymer works
(flows in the die) in a low temperature region, and Tw=Тw-(10÷50)°C if the
polymer works in the upper temperature range.
• thirdly, the temperature of the "upper", die initial zones is determined,
where the formation of monolayers, adapters (Ta) takes place, depending on the
calculated temperature of polymer processing of each layer in the extruder Text
and the die Td, that is, they tend to approach the average value of the selected
temperature range of polymer processing.
The issues of heat transfer are deeply studied in works [34, 49, 52, 59]. The
process of melting and heat transfer during the polymer movement from the
loading zone to the die is considered in detail. The main design parameters and
screw speed, polymer thermo-physical characteristics are taken into account. The
polymer temperature calculation is carried out on each screw pitch by analyzing
the heat release due to viscous friction, taking into account the cylinder wall
temperature.
But theoretical studies were carried out for certain boundary conditions for
the screw standard geometry, without taking into account the heat transfer in the
90
cylinder itself and the accuracy of keeping the temperature, heating power, the
capabilities of the process control system, and equipment wearing. At the same
time, the accuracy of rather complex models is not very high. For example, in [60],
the results of a study of melting in a single-screw extruder are given, in particular,
it is shown that if the Melting Model predicts the final melting at 16 screw pitch,
then in a real process this take place at 20 pitch, with a total of 21 pitches in the
screw. Taking into account that the beginning of melting is on the 6 pitch, the
relative error is 50%.
Usually, the technologist sets some permissible limits, where regulates the
temperature profile and melt temperature depending on the viscosity and recipe
thermal stability, taking into account the screw drive capabilities and the melt
pressure. Moreover, there is always a linear relationship between the temperature
in the extruder zones and the melt temperature.
Actually, in fact a simple method is proposed in modern studies [41], where
the polymer temperature characteristics (points of crystallization, softening,
melting) are taken into account, and the temperature profile is set up during the
technological process debugging. This situation is due to the fact that practice in
plastics processing technologies is significantly ahead of theory. For example, in
article [61] the method of temperature control during coextrusion, which is used by
the operator, is analyzed, while the author believes that the operator's actions as a
whole are wrong, since the temperature changes only based on the analysis of
temperatures in the extruder zones, and does not take into account productivity,
viscosity , pressure limits in each extruder, etc.
Therefore, it is of interest to study the effect of temperature in the extruder
zones on the melt temperature, to find simple dependences for engineering
calculations and technological process operational control, to determine the
adequacy of the melt temperature linear dependences and the level of possible
errors.

91
2.2.1 Study of temperature regimes
For the study, 18 extruders are considered which are installed on 4
coextrusion units [62]. The observation period is 1 month.
Temperature control for each zone is provided by a microcontroller with a
built-in PID controller. Extruder temperature zones are equipped with a heating
and cooling module. The regulators show not only the current and set temperature,
but also the percentage of the heater or cooler turned on, so you can see in which
mode (cooling or heating) each extruder zone is operating.
This heating system design provides the temperature in each zone is kept
constant and practically does not depend on the heat release in the extruder. The
accuracy of temperature control (with optimal settings of the PID controller
parameters) is ±1°C.
To assess the effect of technological modes on the melt temperature, a
regression analysis was carried out. The search for a solution was carried out in the
form of dependence: у=a1х1+а2х2+ + аnхn +b.
Table 2.13
Design parameters of the research coextrusion lines
Parameter / layer А В С D Е
(outside) (inside)
Screw diameter, mm 45 25 C1,2,4=45 25 30
C3=30
Maximum speed, rpm 160 150 160 150 160
Material (main) PA-6 Tie LDPE, Tie PA-6
EVA EVA PVDC EVA EVA
Power of heaters in extruder zones, kW 2,0 1,0 2,0 1,0 1,5
Quantity of heating zone in extruder 5 3 5 3 4
Drive power, kW 30 15 30 15 20

The factors variation range was determined by technological modes, which

have a fairly wide range due to the small-scale nature of production. The
investigated parameters and the range of their variation are shown in Table 2.14.

92
 Table 2.14
The factors variation range for coextrusion unit No. 3 (as an example)
Factors input output
Extruder Р N Q Q/N I Tav Тm
o o
Bar rpm kg/h kg/rpm A C C
А min 135 25 12 0,45 17 257,8 250
max 245 50 22 0,52 25 263,2 265
В min 83 5 0,3 0,04 1,4 183,3 205
max 131 15 0,8 0,06 2,1 193,3 215
С min 139 80 7 0,06 9 228,5 220
max 309 160 12 0,11 17 241,3 240
Д min 93 5 0,3 0,05 1,5 172,8 205
max 147 15 0,6 0,07 2,3 187,3 225
Е min 107 40 5 0,12 4,7 244,5 225
max 279 75 10 0,15 9,1 266 260

2.2.2 The results analysis

In all extruders, a statistical relationship was revealed between the analyzed
technological parameters and the melt temperature, since the calculated value of
the Fisher criterion is greater than the table value.
The analysis shows that the significant factor (for the level α = 0.05) in 17
out of 18 extruders is the average temperature across the extruder zones Tav, and
in all experimental data there is a directly proportional relationship between Tav
and the melt temperature Tm.
For the remaining factors are significant arises in separate experiments. For
example, for an A1 extruder, the most significant factor is the melt pressure.

93
 260 250

258
200

256
Temperature, oC

Pressure, Bar
150

254

100
252

50
250

248 0
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47
Experiments number

Melt temperature Melt pressure

Fig. 2.11. Dynamics of changes in pressure and melt temperature for the extruder
A1
For extruder C3, the effect of rotation speed N on Tm was found, but for
extruder D3 this dependence is negative. Also, for the extruder A1, the influence of
the Q/N ratio was found, but for the other extruders this factor was not confirmed.
No significant influence the motor speed and current were found, although
the level of speed variation for the extruders C and E was in a wide range, and for
C3 a wide range of rotation speeds up to 79-158 rpm was recorded. But at high
screw speeds, the thermal control system keep in the temperature by air cooling
and no melt overheating is observed due to the forces of viscous friction. Although
it should be noted that the analysis of individual points shows that in the range of
rotation speeds of 150-160rpm for a screw with a diameter of 45mm, an
uncontrolled increase in the melt temperature is periodically observed.
Regression analysis was carried out to determine the coefficients in the
equation Tm = a1*Tav.
The graphs show the experimental values of Tm and the average temperature
prediction for the extruder zones.
94
 270

260

250
Temperature, ºС

240

230

220

210

200

190
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41
Experiment number

prediction Тm (В3)=Тav*1,106 experiment Тm (В3)

prediction Тm (А2)=Тav*0,99 experiment Тm (А2)

Fig. 2.12. Predicting the melt temperature from the average temperature across the
extruder zones
The temperature prediction error according to the equation Tm = a1*Tav, for
the range ±2S is ±12.8%. Different extruders have their own level of coefficient
a1. Analysis of technological modes shows that the coefficient depends on the
extruder temperature profile.
Table 2.15
Average temperatures by zone for different extruders
Extruder
Line Coeffi
Extrud Materi temperature
numb Т1 Т2 Т3 Т4 Т5 Т6 cient
er al profile
er а1
description
A1,
1, 2, 3 225 273 277 273 268 250 PA6 0,98
А2, А3 Temperature
C1, with increasing
1, 2, 3 175 235 258 253 245 242 LDPE 1,00
С2, С3 in the middle
E1, Е2, zones
1, 2, 3 226 268 275 270 265 252 PA6 0,90
Е3
A4 4 150 165 170 170 175 170 EVA 1,06
B4 4 150 160 170 170 170 170 EVA 0,96 Smooth profile
С4 4 128 142 150 155 155 155 PVDC 1,01
B1,
1, 2, 3 118 156 193 208 223 224 EMA 1,10 Temperature
В2, В3
with a gradual
D1,
1, 2, 3 106 144 182 198 214 223 EMA 1,18 increase
D2, D3

95
So, the higher the temperature in the first zones, the lower coefficient a1 value in
the equation Tm = a1*Tav (for a1 the range is 0.9-1.2).

300

280

260

240 A1, А2, А3

C1, С2, С3
Temperature, C

220
E1, Е2, Е3
200
A4

180 B4
С4
160
B1, В2, В3
140 D1, D2, D3

120

100
Т1 Т2 Т3 Т4 Т5 Т6
Extruder zones (T1-T5 extruder, T6 adapter)

Fig. 2.13. Typical temperature profiles

Table 2.16
Recommendations for the temperature profile controls at the coextrusion
Temperature profile Generalized equation for Recommendations for the
description predicting the melt temperature profile uses
temperature
Stepwise increase Тm=1,15*Тav Universal most widespread
in temperatures
Smooth profile Тm=1,05*Тav For single, non-optimized
processes
With an increase in Тm=0,95*Тav To intensify melting and
the first zones mixing

During of this research, a new technological parameter of the extrusion process

was found - the percentage of heaters and cooling fan output. That is, this
parameter shows the quantity of supplied or removed energy in the heating zone.
The parameter is standard for a microprocessor controller.

96
 Table 2.17
Typical heaters output percentage level
Nr heating 1 2 3 4 5 RPM The extruder The melt
zone screw temperature, temperature,
°C °C
Percentage 25 5 0 -5 -25 100 230-255 250
of 30 20 10 5 0 50 235-270 250
supplied
Increasing the screw speed requires a decrease in the setting average heating
temperature, since more heat is generated by friction.

2.3 Extruder output control

A large change in formulations, a wide spread in the nomenclature of
colorants (the use of more than 50 items at one workplace during a month), as a
result, a significant fluctuation of the mineral filler in the layer composition (from
0% to 20%), affecting fluctuations in rheological characteristics and an unstable
dependence of productivity on the screw speed.
So becomes difficult to predict output when choosing equipment and
determining the screw design; standard methods require additional calculations,
because a wide range of recipes is planned.
Gravimetric dosing systems provide automatic control of the screw speed
depending on the set output. But even here problems arise: oscillatory processes
(output pulsation), long-term selection of the required rotational speed due to
unstable productivity, screw acceleration to the maximum rotational speed due to
melt overheating and a sharp decrease in the extruder specific output [63].
The parameter by which the control action is generated in gravimetric
systems is the ratio of output to rotation frequency Q/N (specific productivity).
To guarantee control and technological process analysis in a single co-
extrusion production type, it is necessary:
• perform a statistical analysis of the Q/N parameter;
• set the boundary values (tolerances) Q/N for predicting and preventing
rejects and breakdowns of equipment;

97
 • set the principles of control by the parameter Q/N to increase the process
stability.

2.3.1 Extruder output study

The study was carried out on 3 coextrusion lines equipped with a gravimetric
dosing system. The number of experimental points is 729; the total number of
recipes is 21 types.
Table 2.18
Investigated parameters of coextrusion lines
Parameter /Extruder А В С D Е
(outside) (inside)
Screw diameter, mm 45 25 C1,С2=45 25 30
C3=30
Drive power, kW 30 15 30 15 20
Maximum speed, rpm 160 150 160 150 160
Material (base) PA TIE LDPE TIE PA
Output min-max, kg/h 10-25 0,3-1,1 7-14 0,3-1,1 5-15
Percentage of colorant addition min- 0-25 0 0-30 0 0-30
max, %

Table 2.19
The results of measurement for parameter Q/N
№
Line Parameter/Extruder А В С D Е
Q/N av 0,474 0,055 0,091 0,063 0,133
Standard deviation 0,015 0,005 0,008 0,004 0,008
3 Q/N min 0,435 0,038 0,061 0,052 0,120
Q/N max 0,514 0,063 0,109 0,070 0,152
Drag flow ratio α 0,459 0,064 0,127 0,064 0,159
Q/N av 0,328 0,058 0,196 0,057 0,097
Standard deviation 0,010 0,003 0,018 0,006 0,013
1 Q/N min 0,315 0,053 0,160 0,043 0,084
Q/N max 0,357 0,062 0,233 0,068 0,129
Drag flow ratio α 0,359 0,064 0,260 0,064 0,127
Q/N av 0,465 0,054 0,293 0,059 0,132
Standard deviation 0,017 0,003 0,053 0,005 0,011
2 Q/N min 0,428 0,050 0,224 0,042 0,118
Q/N max 0,494 0,059 0,406 0,065 0,162
Drag flow ratio α 0,459 0,064 0,459 0,064 0,159

98
 0,8

0,7

Parameter Q/N, kg/h/rpm

0,6

0,5

0,4

0,3

0,2
2,0
2,0
1,0
1,0
1,0
1,0
1,0
1,0
1,0
1,0
1,0
1,2
2,0
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,1
5,3
5,3
5,3
2,0
2,0
2,0
3,2
3,2
3,2
3,2
3,2
3,2
11,0
11,0
11,0
11,0
11,1
8,0
4,0
5,4
5,0
5,0
5,0
5,0
5,0
Recipy number

Extruder A Extruder C Extruder E

Fig. 2.14. Dynamics of changes in the Q/N parameter during changeovers and the
line number 1 for different recipes

2.3.2 The results analysis

The specific productivity analysis (Q/N parameter) shows that this
parameter, with a stable flow of the extrusion process, can vary in the range:
• ± 3% for one recipe and stabilized process;
• ± 7% for one recipe and the full range of variation of technological modes
in terms of productivity and melt temperature;
• ± 15% if you analyze different recipes (nomenclature) and the full
operating range of screw rotation speeds and extruder temperatures.
Moreover, a significant deviation appears when more than 15% of the
mineral filler is used (Figure 2.14).

99
 0,14

0,13
Parameter Q/N, kg/h/rpm

0,12

0,11

0,1

0,09

0,08
0 5 10 15 20 25 30 35
Percentage of colorant in recipy

Extruder Е Line 1 Trend (Extruder E Line 1)

Fig. 2.15. The filler influence on the Q/N parameter

The using of a mineral filler or master-batch of a polyamide colorant based

on TiO2 (40% PA6 + 60% TiO2), leads to an increase in the Q/N parameter. The
maximum Q/N values are fixed on the maximum colored recipes (Fig. 2.14). A
noticeable increase in the Q/N parameter by 5-10% occurs already at dye content
more then 7%.

100
 0,25

y = -0,0002x + 0,2339
0,2 R2 = 0,5468
Parameter Q/N

0,15

y = -0,0002x + 0,1265
0,1 R2 = 0,6939

0,05

0
-50 0 50 100 150 200 250 300 350
Pressure, Bar

Extruder С Line3 Extruder С Line2

Trend (Extruder C Line3) Trend (Extruder C Line2)

Fig. 2.16. Relationship between the Q/N parameter and pressure. Maximum
value prediction when pressure is zero

It should be noted that the viscosity of super-concentrate colorant is usually

lower than that of the main raw material, therefore, theoretically, the Q/N
parameter should decrease with an increase in the amount of colorants, but in
practice the opposite can be observed (Fig. 2.14 and 2.17). The reason for this
phenomenon may be a change in the melt flow nature in the extruder. On the other
hand, the stability of the Q/N parameter usually decreases when the extruder is
operated at high temperatures.

101
 16
Changing the kind of flow,
increased output
14

12

10
Output, kg/h

Extruder С Line1 45mm

8 Extruder С Line2 45mm
Extruder С Line3 30mm
6

Changing the kind of flow,

4 "frozen" extruder,
decreased output
2

0
0 50 100 150 200
Screw rotation speed, rpm

Fig. 2.17. Dependence of output on rotation speed for different extruders.

Extrusion of LDPE Blends and LLDPE Color Masterbatches

The Q/N parameter makes it possible to predict critical situations in the

technological process, for example, for extruder C Line 3, the minimum value of
0.061 is found for a "frozen" extruder where the frequency is 158rpm and
productivity is sharply reduced (Figure 2.16). Such situation leads to uncontrolled
melt heating because of to intense internal friction.

2.3.3 The extruder specific productivity calculation

The Q/N parameter can be calculated from the screw design parameters at
the stage of developed the technological process.
Total flow = Drag flow - Pressure flow - Leak flow
It is known [34] that the drag flow in the extruder Qd is determined from the

relation Qd = α*N, where α is the drag flow coefficient, N is the screw speed.
Drag flow coefficient α =V/2, where V is the screw pitch useful volume in the

102
metering zone. Approximately,   DH D  e / 2 where D - is the screw
diameter, H - is the screw channel depth in the metering zone; e - is the screw
flight.
Analysis of the design parameter α and the measured values of the Q/N
parameter shows that the maximum values of the Q/N parameter are in the range
(0.9-1.1)*α, that is, they can be determined at the stage of developed the
technological process.
It should be noted that during polymer extrusion in a high temperature
region, for example, LDPE processing at a temperature of 240°C (i.e., at low melt
viscosity), the level of Q/N parameter values can be in the range (0.6-0.7)*α.
When controlling technological modes, a decrease in the Q/N parameter
lower than 50% of α indicates failures in the technological process (a significant
increase in pressure or a decrease in viscosity, overheating the melt), a extruder
temperature correction is required (Fig. 2.16).

0,36 Сolorant quantity

22%
0,355

0,35
Parameter Q/N, kg/h/rpm

0,345

0,34
Сolorant
0,335 quantity 0%

0,33

0,325

0,32

0,315

0,31
90 110 130 150 170 190 210
Pressure, Bar

Extruder А Line 1

Fig. 2.18. Influence of mineral filler and pressure on the Q/N parameter.

103
 Theoretically high values (level 1.1*α) may show a low level of mixing in
the extruder as the so-called pressure flow (reverse flow) decreases which increase
the extruder mixing action. But there is melt sliding intensification on the screw
walls, and at such values, the extruder proceeds purging is more quickly and
efficiently. For this reason mineral filler is most often used as the component of
cleaning additives. Although the author's practical observations show that a change
in the coefficient α from 0.6 to 1.1 does not visually change the color stability of
multilayer film (when screw has a dispersive and distributive mixing elements).
It should be noted that the high-speed region is more unstable. When the
extruder is operating in the lower region of the screw rotation frequency range,
with a decrease in output, an automatic increase in the rotation frequency by the
gravimetric control system stabilizes the process. At high Q/N values, there are
also no problems with stabilization the output, so there is a reserve for controlling
the rotation speed.
Also of interest is the control of temperatures across the extruder zones to
stabilize the Q/N characteristic and equalize the flow rate. When determining the
zones for controlling temperatures, it is necessary to analyze the set range and
current values, take into account that a decrease in the Q/N parameter can have
place from low productivity of the loading zone or an increase in pressure due to
problems in the die area.

2.4 Product quality control

The quality characteristics of the flexible multilayer material can be divided
into:
1. Geometric parameters (thickness, width, weight, length).
2. The film material appearance in transmitted and reflected light (different
gel types, inclusions, stripes, mechanical defects, irregular structures, wrinkles,
matting, surface structure, etc.)
3. Winding appearance, uniformity and density of winding in a roll.

104
 4. Physical and mechanical properties (strength, shrinkage, permeability,
hardness, etc.).
As a rule, the control quality of 95% characteristics of film polymeric
materials is carried out within 30-60 minutes from the moment of sample
manufacture. Measurement of other parameters, in particular permeability, can
take up to 24 hours, depending on the technique and equipment.
It is necessary take into account the post-crystallization processes that take
place in polymer film materials during storage. Such processes are typical for
semi-crystalline polymers. In other way, we can say that the material properties are
normalized, 80-90% of normalization is take place during 1-2 days after
production, when the film material is stored under standard production conditions.
During this time, mechanical, shrinkage, and geometric properties are stabilized.
The right balance must be found between acceptable control time and quantity of
estimate quality parameters.
When developing quality requirements, a difference should be made
between:
• requirements that characterize, differ one nomenclature of serial production
from another;
• requirements that show the stability of quality characteristics in a product
sample, into a certain nomenclature.
The properties stability can be estimate to using the coefficient of variation:
s
  *100
x
where
- S is the standard deviation,
- x is the average value.
Polymer materials stability studies and coefficient of variation analysis
showed the following regularity:
• v <10% - characteristics have high stability;

105
 • v is from 10% to 15% - the stability of the parameter is satisfactory, the
process is into the normal range;
• v is from 15% to 25% there are malfunctions in the technological process,
correction is required;
• v > 25% the parameter is unstable, there are disturbances in the
technological process that require prompt elimination.
The requirement for the quality characteristics of a certain nomenclature is
normalized by setting the minimum-maximum range for each measured
characteristic.
An important element that provides the stability of product quality is the
classification and grouping of various nomenclatures for the development of
common (uniform) methods, parameters and quality control tables. Such tables let
you to clarify the requirements for each nomenclature, simplify the development of
new types of products, summarize the requirements for the operation of equipment,
help to the operational training of personnel, and let improving the quality of
products in a complex for several product ranges.
Grouping of technological processes (for the analyzed production) it is right
to carry out according to the used unity of technological equipment. It's connected
with the wide variety of designs, models and control systems of modern equipment
designed for the manufacture of identical multilayer structures of flexible
polymeric materials.

2.4.1 Investigation of the relationship of product quality characteristics and

technological modes
In the processes of manufacturing polyamide tubular films by the Triple-
bubble method, the barrier characteristics are determined by the multilayer material
structure and the formulation of each layer [64], control is carried out selectively,
especially if problems are detected in the processes of preparing mixtures or with
raw materials.
The main qualitative parameters that are measured and controlled at each
changeover are the mechanical and heat-shrink properties of the polyamide tubular
106
film [65], which in the Triple-bubble processes are regulated by the corresponding
coefficients of stretching and shrinkage [66, 67].
For a certain nomenclature (formulation), the elongation coefficients can
vary for different periods of production due to changes in the properties of raw
materials, which in turn requires the selection of extrusion temperatures, the
cooling intensity, wear of the pulling rollers, the speed of motion of the film
material and, accordingly, the rate of heat-setting can also change. Therefore, the
regulation range is set for each coefficient. It is important to define tolerances and
regulation rules in such a way as to guarantee the required product properties in
one step.

Fig. 2.19. Triple-bubble process scheme, production of a single-layer tubular

film, 1-extruder; 2- extrusion head; 3 - cooling and calibration unit; 4 - pulling rolls
N1; 5 - unit for heating the primary tube for blowing and orientation; 6 - unit heat
setting; 7 - winding unit into a roll; 8 - pulling rolls N2; 9 - pulling rolls N3; 10 -
pulling rolls N5.

107
 Table 2.20
Polyamide film technological parameters production, diameters of finished
tubular shrink films 20-40mm
№ Parameter name Regulation Symbol
range
1 Melt temperature in the coextrusion die, оС 235-255 Т1
2 Cooling water temperature of the primary 8-14 Т2
tube in the calibrator, оС
3 Primary tube temperature before blowing 70-80 Т3
and orientation, оС
4 Tube temperature after heat setting, оС 130-150 Т4
5 Temperature before winding, оС 20-35 Т5
6 Diameter of the primary tube, after the 5-15 D1
calibrator (before the heating unit), mm
7 Tube diameter after orientation (before the 20-60 D2
pulling rolls N3), mm
8 Tube diameter on winding (between the 20-40 D3
rolls N5 and winding unit), mm
9 Speed of pulling rolls №1-5, m/min 100-300 V1-5
10 Stretch ratio in MD (machine direction) 2,3-2,7 V3 /V1
11 Shrinkage ratio in MD 0,8-0,9 V5 /V4
(V3 ≈V4 )
12 Stretch ratio in TD (transverse direction) 3,4-3,7 D2 / D1
13 Shrinkage ratio in TD 1,10-1,25 D2 / D3

The effective methods for determining the relationship between technological

parameters and product characteristics is the method of regression analysis.

2.4.2 Study description.

The film samples were taken 1-3 times per shift from each of the 3 lines.
During the observation period - 1 month, n = 277 product samples were taken.
Mechanical characteristics were measured for each sample in the machine (MD)
and transverse directions (TD). At the same time, to obtain one characteristic (one
point), 4 breaks were carried out; the average value was taken as the result. In

108
parallel, the technological modes were recorded in which the tubular film samples
were made.
During the observation period, a wide range of films was produced in
diameter (19mm-24mm), a total of 6 different calibers, and color (colorant content
from 0 to 3%), and a total of 5 different color options.
Extruder with a diameter of 45mm, operating speed range 80-110 rpm.
Pressure in the die was 150 - 240Bar.
The coefficients of MD and TD stretching and shrinkage are taken as input
factors.
Table 2.21
Technological factors range variation
Value Factors input (X)
D2 / D1 D2 / D3 V3 /V1 V5 /V4
Х1 Х2 Х3 Х4
Xmin 3,49 1,14 2,39 0,82
Xmax 3,64 1,22 2,64 0,90
x 3,57 1,18 2,53 0,85
S 0,02 0,01 0,04 0,02

The film mechanical characteristics in the MD and TD were in series

analyzed as output characteristics: stress Rm and relative elongation Fmax at break,
Module (Rm/Fmax) as the ratio of stress to elongation at break.
Table 2.22
Film mechanical properties statistics
Factors output (Y), n=277
Thiсkness, MD TD
Value
mic Rm, Fmax, Rm/Fmax Rm, Fmax, Rm/Fmax
МPа % МPа/% МPа % МPа/%
Ymin 17 156 80 1,4 215 38 4,1
Ymax 22 234 136 2,6 345 70 6,7

Y 19 201 111 1,8 273 53 5,2

S 1 14 10 0,2 20 6 0,4

109
 The search for the output characteristic was carried out by the method of
regression analysis, by searching for an equation of the form Y = m1x1 + m2x2 +
... + b, where the values x1, x2 ... xn are the coefficients of stretching and
shrinkage, and Y is one of the mechanical characteristics.

2.4.3 Analysis of results

The coefficients in the regression equation for various mechanical
characteristics, and the corresponding Fisher coefficients (F) and determination R2
are given in Table 2.23, the calculations were carried out using the Excel Analysis
Tool-Pak.
Table 2.23
Regression analysis results between technological modes and films
mechanical characteristics
Mechanical characteristics (Y) Coefficients in regression equation
F-test R2
m4 m3 m2 m1 b
Fmax -141,0 -33,0 -199,0 -65,9 785,7 17,7 0,21
MD Rm 290,3 34,4 177,6 -91,5 -17,4 14,1 0,17
Rm/Fmax 5,03 0,94 5,01 0,23 -11,62 49,6 0,42
Fmax -16,3 -40,6 82,9 -65,4 304,7 13,0 0,16
TD Rm -92,4 -122,6 -279,0 -126,1 1442,4 7,2 0,09
Rm/Fmax -0,73 1,47 -13,80 3,90 4,54 21,2 0,24

The freedom degrees for the experiment were f1 = 4, f2 = 272.

For the freedom degrees number f1 = 4, f2 = 200, the Fisher criterion critical
values are:
• for the significance level alpha =0.05, Ft = 2.42;
• for the significance level alpha =0.01, Ft = 3.41.
The F-criterion calculated values for all six equations are higher than the
tabular one, so all equations have statistical significance.
It is necessary to note the low level of the coefficient R2, therefore, the
relative prediction error at individual points (for example, for the Rm parameter in
MD) reaches 26%, but for most of the experimental points, (for the ± 2S range) the
relative prediction error using regression equations is less than 15%.

110
 350

330

310

290

270
Rm, MPa

250

230

210

190

170

150
1 10 19 28 37 46 55 64 73 82 91 100 109 118 127 136 145 154 163 172 181 190 199 208 217 226 235 244 253 262 271
Experiment number

Rm MD experiment Rm MD prediction Rm TD experiment Rm TD prediction

Fig. 2.20. Stress at break, experimental data and prediction according to

regression equations

Using the Student's t-test, important factors were found, that is, the
coefficients that regulate the corresponding mechanical characteristics.

Table 2.24
Values of Student's criterion for the investigated technological factors
Factors output Factors input
V5/V4 V3/V1 D2/D3 D2/D1
Mechanical characteristics m4 m3 m2 m1 b
Fmax -4,61 -2,34 -5,09 -2,68 7,32
MD Rm 6,38 1,63 3,05 -2,50 -0,11
Rm/Fmax 10,18 3,96 7,96 0,51 -6,72
Fmax -0,87 -4,68 3,46 -4,34 4,62
TD Rm -1,36 -3,91 -3,22 -2,31 6,05
Rm/Fmax -0,53 2,30 -7,85 3,53 0,94

111
 The Student's criterion critical values, with the number of degrees of
freedom f2 = 200, are:
 for a significance level 0.05 → t = 1.97;
 for the significance level 0.001 → t = 3.34.
Analysis of the data in Table 2.24 shows that the coefficients have a
complex effect, and the shrinkage factors (V5/V4 and D2/D3) have a more
significant effect than the stretch factors (V3/V1, D2/D1). It should also be noted
that changing only the diameter D2 changes both transverse coefficients and taking
into account the fact that V5/V4≈V5/V3, changing the speed V3 changes both
longitudinal coefficients (in machine direct). Stretch coefficients influence more
predictably - they change the Module of the corresponding mechanical
characteristic. Therefore, when developing a technological process for one
nomenclature, it is necessary to work out and set such tolerances for physical and
mechanical characteristics so that the operator has the opportunity to achieve the
specified characteristics by changing only the stretch ratios V3/V1 and D2/D1. In
this case, the operator must regulate the stretch ratios by changing the parameters
V1 and D1.
At the same time, to develop new types of products with a different ratio of
physical and mechanical characteristics, the technologist should, first of all, work
out and set the suitable shrinkage coefficients.

2.5 Conclusions on the second section:

1. Quality control of mixing is required in extrusion technologies using
multi-component formulations, as the mixing process influence on the film quality.
2. The mixing index I3≥0.96 is a complex and universal criterion for the
quality of mixing when analyzing and comparing the equal periods of mixing
equipment operation.
3. Control and analysis of a single sample must be carried out on the basis of
statistical methods, by analyzing the standard deviation of each component in a
single sample and it’s within the standard range of ±3Sн.

112
 4. The mixing index level I3≥0.88 is the critical point for the component
with any percentage.
5. The melt temperature is easy to predict from the average temperature of
the extruder zones, taking into account the nature of the temperature profile. The
relative forecast error for the ± 2S range is ± 12.8%.
6. Controlling and analyzing specific Q / N productivity will avoid problems
in the coextrusion process and reduce changeover times.
7. To develop technological parameters and control the quality
characteristics of products, it is quite effective to use the linear regression method.

113
 Section 3. Simulation of extrusion processes

3.1 Shear flow modeling of die distribution channels.

The polymer product quality is depends from melt uniformity distribution in
the extrusion die channel. Stability of layer thickness during coextrusion provided
by design parameters dies distribution channels, as well as technological
parameters of polymer material processing.
The extrusion die distribution channel main goal is the annular shape of the
molten polymer with minimal thickness variation, additional plasticization and
homogenization of the polymer material, equalization or a slight increase in the
polymer melt temperature, as well as creating resistance to the polymer movement
is necessary to maintain a certain extrusion mode.
Various shapes and geometries of distribution channels have been
developed, but in coextrusion dies for the manufacture of tubular multilayer films,
distributors with side feed of material are used, of which two types can be noted -
see Fig. 3.1.

a b c
Fig. 3.1. The main types of distribution channels used in coextrusion dies
(‘a’ - a channel in the form of a ring with side feed, ‘b’ - a die with spiral
distribution channels, ‘c’ - the channel design is development of the scheme ’a’ at
the point of flow connection).

114
 Ring type channel fig. 3.1a, although it seems "outdated", widely used
especially for heat-sensitive polymers, at the same time, this channel geometry is
very diverse and is constantly being improved. In particular, channels have been
developed with an offset unbalanced connection point of streams, to eliminate
possible stagnant zones and accelerate purging fig. 3.1c, during changeovers and
layer recipe replacement.
Therefore, it is of interest to carry out a comparative analysis of typical
designs of annular distribution channels Fig. 3.2.
For research, a two-dimensional channel model was developed. The model
is create using the method of electro-hydraulic analogies, where the selected die
areas are represented as resistance, and a step-by-step back pressure calculation
and the flow velocity is carried out starting from the channel equivalent resistance
to the outlet resistance at the end of the channel. The power law is adopted as the
law describing the melt flow. The channel is divided into 100 elementary tubular
sections, and forming a cylindrical channel with 50 elementary sections of the flat
slot type. Since the channel can have a different cross-sectional shape (trapezoid,
circle, rectangle), which affects the melt flow time, the model provides the ability
to calculate the flow rate at various points of the channel cross-section. The models
adequacy was confirmed in an experimental study of the operation of distribution
channels with various polymeric materials [68, 69, 70].
The input data for the model are the following technological parameters: the
rheological characteristic of the polymer in the form of a power-law model, the
productivity is 7.5kg/h, the channel design parameters (Table 3.1).
Polymer melt flow mathematical study was provided for next distributive
channels design (Fig. 3.2):
1. The tubular channel part of constant diameter is located along the line of
flow entry (extruder adapter) and has no gradient of the circular conical
channel part (simple, linear).

115
 2. The tubular channel part has a gradient relative to the line of the extruder
adapter, with constant diameter; the circular conical channel part height is
changes linearly (simple, linear).
3. The tubular channel part has a gradient, a variable diameter that changes
linearly; the circular conical channel part height also changes linearly
(complex, linear).
4. The tubular channel part has a gradient and a variable diameter, the circular
conical channel part height and the diameter change nonlinearly (complex,
nonlinear).

Fig. 3.2. The investigated distribution channels

The model give possibility calculating: the velocity profile at the outlet from
the tubular and cylindrical distributive channel, the pressure distribution at all
channel points, the distribution of velocities and shear stresses. The general design
diagram of the investigated distribution channels is shown in Fig. 3.3. Next design
parameters are taken into account in the mathematical model: the tubular channel
diameter at the inlet and outlet; the cylindrical conical channel height at the inlet
and outlet, the molding gap width, the cylindrical conical channel diameter at the
inlet and outlet (Table 3.1).

116
 Fig. 3.3. Design diagram of the distribution channel

Table 3.1
Geometric parameters of the studied distribution channels
№ Parametr 1 2 3 4
1 Inlet tubular channel diameter - d in, mm 25 15 27,5 18
(Channel element number 1)
2 Outlet tubular channel diameter - d out, mm 25 15 6 6
(Channel element number 50)
3 Inlet cylindrical channel diameter - D in, mm 190 190 190 190
4 Outlet cylindrical channel diameter - D out, mm 70 70 70 70
5 The molding gap width of the conical channel part - S, mm 2 2 2 2
6 The cylindrical channel height at the inlet -L1, mm 178 178 178 178
7 The cylindrical channel height at the outlet -L2, mm 178 134 134 134

This designs is choice for research from next reasons: firstly, it is necessary
to understand how the design complication and, accordingly, the rise in the die cost

117
will improve the layer thickness stability; secondly, similar designs are still used
nowadays, especially for thermo-sensitive polymers; thirdly, after analysis it is
possible to draw parallels with flat dies. All structures have the same purpose - to
form the most uniform melt flow over the cross section in the form of a tube [71].
Limitations on the distributive channel back pressure were set - 110-120Bar,
because the total back pressure for the all die should not more than 350Bar. This is
associated with the limitation of pressure-flow in the extruder, as the channel must
be suitable for processing thermosetting plastics with high thermal sensitivity. The
height and die body diameter at the inlet and outlet did not vary.
Optimization of geometric dimensions for each design option was carried
out according to two parameters:
• the melt flow velocity profile at the outlet from the channel, that is, the
deviation from the average velocity was minimized;
• the average residence time the distributive channel should be minimal.
Each channel design has been optimized for the processing of two types of
polymers (with different flow indexes), by selecting the tubular channel diameter
at the inlet and outlet. To carry out the optimization, the tool "Analysis package"
Microsoft Excel was used. Three parameters were taken as a channels design
comparative assessment:
 the maximum percentage of velocity deviation from the average -
Smax [%];
 the maximum residence time in the die - Tmax [minutes];
 the pressure level in the channel - Pnom [Bar].
For comparison, as a reference percentage of output deviation, it can be set
up that there is a difference of less than 15% between the minimum and maximum
outputs at the distribution channel outlet; in fact this means that the layer thickness
will lie in the range of ±7.5% of the average thickness. This deviation is the
standard for many well-known manufacturers of extrusion equipment. Thus, the
criterion of optimality (Kopt) is the minimum of the SUMM:
Kopt=[Smax+Tmax]→min.
118
 Modeling was carried out for two variants of the flow index 0.3 and 0.65.
This range covers a wide range of plastics used in industry. Grades of PVDC
polymers were selected as the studied rheological characteristics, the processing
temperature was taken as constant Text=165°C. Next rheological characteristics
are used:
0,01(Tp 140)
IXAN 303
m  28579   0,7  e ,
0,01(Tp 155)
IXAN 813
m  9695   0,35  e .
The results of modeling the polymer flow process are presented in Table 3.2.

Table 3.2
Modeling results the flow process in the study channels

Channel number 1 2 3 4
Melt index 0,3 0,65 0,3 0,65 0,3 0,65 0,3 0,65
Difference between the minimum
and maximum output along 33 4,3 15 25 24,6 23 18,5 21,2
distribution channel, %
Residence time in the distributive
channel, calculated from the
velocity profile at a distance of 1 178 207 31 38 3,6 3 3 2,8
mm from the channel wall,
minutes
Range of variation (min-max) of
shear rates in the channel, 1/s
0,038-2,14 0,22-9,93 1,61-6,75 3,25-5,82
Shear rate change percentage 5587 4365 319 79
Pressure, Bar 120 118 116 112 111 108 115 111

119
 the point of inlet in the scheme of flow in the point of outlet
tubular channel distributive tubular from tubular
channel channel
12

10
Shear rate, 1/s

0
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
Channel element number

1 2 3 4

Fig. 3.4. Shear rate distribution in the study channels (flow index 0.3)

Output, m3/s
5,0E-08

4,8E-08

4,6E-08

4,4E-08

4,2E-08

4,0E-08

3,8E-08

3,6E-08

3,4E-08

3,2E-08

3,0E-08
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
Channel element number
1 2 3 4

Fig. 3.5. Output distribution in the study channels (flow index 0.3)

120
 Pressure, Pа
140000

120000

100000

80000

60000

40000

20000

0
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35 37 39 41 43 45 47 49
Channel element number
1 2 3 4

Fig. 3.6. Pressure distribution in the study channels (flow index 0.3)

Graphs analysis let us to conclude that all designs of distributive channels

can be used in the processing of plastics, that is, "have the right to life." Channel
design No.1 can only be used for plastics with low thermal sensitivity and for a
small range of flow indexes. The use of channel No.2 let to reduce the maximum
residence time in the channel, and the design is more flexible. The designs of
channel No.3 and channel No.4 can be taken to be equivalent in terms of flexibility
and polymer residence time; such designs reduce the distribution channel pressure,
which is important for reducing the backflow in the extruder and improving the
processing of heat-sensitive polymers.
Output distribution graphs analysis (Fig. 3.5) showed that the design of
channel No.2 and channel No.4 provides the productivity increase at the outlet of
tubular channel (channel element number 47-50), which reduces the a stagnant
zone possibility at the point where two melt streams join.
The channel No.3 design is the most undetermined, on the one hand, there is
a short polymer residence time in the channel, the design is not difficult to

121
manufacture, and the shear rates distribution nature is close to channel No.4; on the
other hand, in channel No.3 observation a sharp decrees the output in the exit from
the tubular channel (channel element number 47-50), which can lead to the
stagnant zone region and prolonged melt purging during changeover (in color and
recipe). The most optimal is the channel design No.4, that provides flexibility for
processing different plastics and a minimum residence time in the die.
The investigated distribution channels differ significantly in the shear rate
deviation in the tubular channel. The simulation results showed that the shear rate
constancy in the channel is an integral criterion for rating the channel operation
quality (Fig. 3.4). The channel design No.4 best correspond with this requirement.
is to provide
The rational design criteria (for the selected materials and productivity) can
be a minimal level of shear rates in the distributive channel. This level must be
more than 1,6s-1 for analyzed cannels, in this case, the estimated residence time in
the die channel is no more than 3 minutes, which is important for changeovers
acceleration issue.

3.2 Annular distribution channel optimization

In the previous chapter, it was shown that a distribution channel with a
constant diameter (see Fig. 3.2 (2)), having a relatively simple configuration,
provides a thickness difference of ± 7.5%. This layer thickness variance level is
acceptable for many modern processes film materials production.
The working time of the extrusion dies is more than 20 years. At the same
time, cleaning is depend from the polymer thermal stability, and can be at intervals
from 1 to 12 months. The cleaning operation is laborious and increased thermal
and mechanical influence on the cannels surface, which naturally gradually
changes the geometry and surface hardness.
Therefore, it is of interest to determine:

122
 1. How to design parameters changing and the extrusion processing
characteristics will affect to the thickness variation.
2. Develop practical recommendations for analyzing and eliminate
deviations in film thickness.
3. Determine the critical level of canal geometry change when die
replacement is required. It is also important to determine the relationship between
the design and technological parameters of the molding equipment in the extrusion
process with the products quality characteristics.
As an example, let us study a channel where the tubular channel part has a
gradient relative to the extruder adapter, with constant diameter; the of the circular
conical channel height changes linearly (Fig. 3.7).

123
 Fig. 3.7. Distribution channel design diagram. L, h, Dtub, Dout - variables for
studying the effect on speed stability, simulated section No.1 corresponds to Din,
simulated section No.50 corresponds to Dout
Modeling was carried out for a material with a flow index of 0.3. This range
covers wide plastic types that used in industry. The polymer grade PVDC -
IXAN303 was chosen as the studied rheological characteristic, the processing
temperature was taken constant tp=165оС. Productivity is 7.6 kg/h.
Rheological characteristic: m=28579γ-0,7exp{-0,01(tр-140)}.
The criterion for assessing the channel is the percentage of speed deviation:
ΔVi=(Vi max-Vi min)/Vi max*100%.
Film thickness variation is directly proportional to the percentage of speed
deviation. A speed deviation of no more than 15% can be considered the norm.

3.2.1 Design parameters influence

30 160

140
25
120
Speed deviation Vi, %

20

Pressure, Bar
100

15 80

60
10
40
5
20

0 0
10 20 30 60 90 120 180 210 240 270 300
Diameter D out, mm

Fig. 3.8. Distribution channel outlet diameter influence on the technological

parameters of extrusion

124
 That estimate distribution channel outlet diameter Dout (Fig. 3.8). The
influence is insignificant, with standard design solutions, when the channel tilt
angle is in the range of -30о +30о . It is important that there is an optimal value for
this parameter, in this example it is Dout = 180mm when channel inclination angle 2
degrees.

100 350

90
300
80
250
Speed deviation Vi,%

70

Pressure, Bar
60
200
50
150
40

30 100
20
50
10

0 0
0,5 1 1,5 2 2,5 3 3,5
Molding gap h, mm

Fig. 3.9. The molding gap influence on layer distribution.

In this study, the gap changes from 0.5mm to 3.5mm. The optimal value is
2mm (for a tubular channel with a diameter of Dk = 15mm). Gap is the most
important factor in terms of influence on speed deviation. When the gap changes
by 5% (from 2mm to 2.1mm), the speed deviation changes by 49% (from 9.56% to
14.2%).
For single-layer dies, the gap is calculated based on the required pressure
and the maximum shear stress. For coextrusion dies design, it is also necessary to
take into account layers thickness and sequence, avoid the formation stagnation
zones and unstable layers thickness when they are connected.

125
 70 250

60
200
50
Speed deviation,%

Pressure, Bar
150
40

30
100

20
50
10

0 0
20 50 100 133 200 250 350
Channel height L, mm

Fig. 3.10. Distribution channel height influence (at the outlet, at the point of
joining of two flows) on the technological parameters of extrusion

The channel height L influence. The standard design solution lies in the
range of 100-150mm. This range is confirmed in this study. The question is: why
increasing the channel height constantly decreases the velocity deviation ΔV?
Other words: why is there an optimal back pressure for the gap width h, but, for
the changing channel height L, the higher the back pressure is better for
distribution. Probably, with an increase in the channel height, cross flows arise due
to the shear stresses equalization in the channel cross section; at the same time,
with a decrease in the gap, the equalization of velocities does not have time to be
realized. The increase in the channel height (length) is limited by a maximum
pressure of 350 Bar, above this value, critical tensile stresses appear and the
problems with extruder mechanical elements connections may occur.

3.2.2 Technological parameters influence

The paper [43] presents the results of flow simulation for a flat-slot die. It is
shown that a change in productivity, processing temperature has an insignificant
126
effect on the initial distribution of speeds at the exit from the die (the flow rate
deviates by 5% when the productivity changes by 10 times). At the same time,
changing the material from PS to LDPE leads to a sharp speed deviation by 100%,
in practice this means that the film thickness will differ twice and such a deviation
is unacceptable.
In this study, the results presented in [43] are confirmed. Varying the
processing temperature and productivity does not lead to a change in the speed
distribution.
From material characteristics, only the flow index has an impact. Viscosity
constant, melting point, temperature constant do not affect to the velocity
distribution. Moreover, there is an optimal flow index value of 0.3 and a region of
rational values from 0.25 to 0.5, where the speed deviation does not more than
15%.

160 400

140 350

120 300
Speed deviation Vi, %

Pressure, Bar
100 250

80 200

60 150

40 100

20 50

0 0
0,1 0,2 0,3 0,4 0,5 0,6 0,7 0,8 0,9
Flow index

Fig. 3.11. The flow index influence on the technological characteristics of

extrusion

It should be noted that the power law gives the following error: the flow
index is taken constant for the entire studied range of speeds and processing

127
temperatures; in a real process, the flow index depends on both temperature and
shear rate [38].
The relationship between flow index, temperature and shear rate is shown in
Table 3.3.
Table 3.3
Melt flow index n and viscosity constant μ0 for LDPE 15813-020
Temperature, С

Shear rate on the flow parts, s-1

20-40 40-100 100-200 200-700

n μ0 n Μ0 n μ0 n μ0

170 0,39 31289 0,30 43192 0,28 48645 0,20 74193

190 0,59 12346 0,43 22057 0,42 22827 0,27 50952
210 0,66 7173 0,56 10403 0,49 14535 0,37 27493
230 0,68 5443 0,61 6991 0,57 8374 0,40 21181

Therefore, temperature and capacity control should not be avoided, so they

insignificantly, but affect the flow index and in some cases it is the only possible
tool for the technologist.
Usually, in the developed technology, such a variation is very limited,
including the process inertia, for changes and stabilizes the temperature in the
coextrusion die at 10С it takes from 30 minutes to 120 minutes. Temperature
variation across the extruder zones is more preferable.
An increase in temperature and/or a decrease in productivity can be
suggested as a general recommendation, as this increases the flow index and
reduces its effect on velocity deviation (Figure 3.11).

3.3 Development the cork flow model

Consider the following mechanism (model) for the non-Newtonian fluid
flow. First of all, because the polymer chains are in relative adhesion, for stabilized
flow, a cork flow character always observed. Other words, the macromolecules
interdiffusion is block to arise of a smooth velocity profile (from zero on the

128
channel wall to a maximum in the center) and the real velocity diagram is
telescopic. In any case, this concerns the channels dimensions of modern extrusion
equipment and rheometers [72].
During the polymer flow the wall-layer W3 is formed. Wall-layer molecules
are compressed and practically do not relax. The central-layer W1 (cork) is slides
on the wall-layer. The central-layer W1 is compressible and elastic. The wall-layer
thickness is 0.5-1% of the all channel width.
Interaction goes by macro-roughness and segments of molecules that
protrude (stick up) from the tangled ball and adhere to the wall-layer molecules.
The area, where the interaction takes place, can be called a low-viscosity interlayer
W2, its thickness ranges is about 1% to 8% of the all channel width (according to
the studies layers distribution during coextrusion, see Section 4).

Fig. 3.12. The photo near-wall flow region cut.

The wall area (shades of black and dark brown) is have the three areas: 1 -
the area melt contact with the nozzle (near-wall layer); 2 – the area low-viscosity
melt; 3 – the area normal viscosity melt (central layer); 4 - white purging
compound (fed to the die to replace the brown melt).
The color and structure of:
 central layer is near to standard film;
 low-viscosity layer is characterized for under-heat melt;
129
  near wall layer is characterized for degradation polymer.
Macroroughnesses (conglomerations, bundles of macromolecules) are
characterized by the height H and the angle of inclination α. Microroughnesses –
protruding (stick up) macromolecules segments, are not taken into account in this
model, but their presence and influence on the flow parameters are assumed. The
flow diagram is shown in Fig. 3.14.
Interaction and flow occurs as follows
1. High viscosity Newtonian region - the speed of Vt is small and
macroroughness and the segments of central layer molecules have
time to relax almost completely, the intermolecular bond is
completely restored, so there is no noticeable decrease in viscosity.
2. Non-Newtonian region, when the relaxation rate Vr and the flow
rate Vt are close, that is, the macroroughnesses do not have time to
relax, but have already moved to a new position, here η is
noticeably reduced - the length of the line η=f(Vt ) where the
molecules of central and wall layers come into contact, therefore, a
decrease in viscosity is observed.
3. Low viscosity Newtonian region - the speed of movement increases
so much that the macromolecules do not have time to relax and
stick, adhere each other, that is, the interaction macromolecules is
along the upper part of the macroroughness, thus the viscosity
stabilizes.
The actual structure of the melt surface, that is, the interacting macro-
irregularities geometry, can be seen at the exit from the die, since the rectangular
velocities profile don’t change when the melt leaves the molding channel.
The area where the interaction takes place can be called a low-viscosity
interlayer W2 (Figure 3.13).
In fig. 3.13 shows the velocities diagrams, generally accepted, calculated
according to the power law and proposed telescopic, where the flow goes with
sliding on the channel wall, with different thicknesses of the low-viscosity layer
130
W2 (the productivity of three flows is the same). Design diagram of the non-
Newtonian fluid corky flow model shows in fig.3.14 .

12

10

8
theoretical
V*100, m/s

(power law)
6

slip on the wall

4 W1 (thickness the
wall layer 5,5%)

2 slip on the wall

(thickness the
W2 wall layer 2,5%)
0
0 W3 5 10 15
point of channel

Fig. 3.13. Diagrams melt flow rate polymers.

Fig. 3.14. Graphical interpretation of the Corky flow model a compressible

fluid.

131
 As a result of the analysis of the motion of the central layer, the equation was
obtained:
H H
 
sin  Vr
1 . (3.1)
Vt * tg
It should be noted that for transition from the 2D to 3D flow model, the
parameter η can be considered as viscosity.
In other words, the corky flow model (C-Model) is formulated as follows:
the central-layer (cork) W1 flows (moves) in the channel, the layer W1 interacts
with the wall-layer W3 through the low-viscosity interlayer W2.
The wall-layer W3 also moves along the channel wall, because the
molecular chains of the wall-layer W3 and the interlayer W2 constantly interact
and adhere each other and the central-layer W1, as it were, "pull out" the wall-
layer W3 towards the exit from the channel.
I am suggesting a more general name for the proposed mechanism can be
trigonometric flow model (T-Model), since the formula 3.1 can be used to
analyze the shear flow.

3.3.1 Characteristic points and analogies

So for the first time the full rheological curve equation of a non-Newtonian
fluid is obtained on the basis of a physical model without empirical power
dependences.
Equation (3.1) allows calculating the viscosity constants and transition points
between the flow regions:
H Vr
at low shear rates  0  V 
sin  ; tg ;
t1

H Vr
at high shear rates     H ; Vt 2 
 1 .
sin  tg *   1
 sin 

132
 At an angle α≈0, a Newtonian flow is modeled, that is, a shear of layers
without relaxation is realized.
An analogy of the proposed model with a turbulent fluid flow can be
analyzed; the macroroughnesses in the near-wall region are transverse whirls
penetrating into the central part of the turbulent fluid flow, the angle α and height
H in fact the characteristics of a whirl.
The understanding of the non-Newtonian fluid viscosity in the corky flow
model differs from the generally accepted one: the large interaction area is the
reason for the observed high viscosity. The observed decrease in viscosity is a
peaks decrease and smoothing, the melt compaction and a decrease in the effective
contact area.
The model assumes that viscosity is always linked (connected) with the
effective interaction area. The model also relates stress relaxation in the polymer to
flow characteristics.

133
3.3.2 Method for calculating equipment channels based on corky flow model
In the tables 3.4 and 3.5 shows the corky model with the standard calculation
parameters, formulas for recalculating the flow parameters in channels of
characteristic geometry are given.
Table 3.4
Fluid flow equations for a capillary (tube channel) with length L and radius R
Shear model, Newtonian fluid Corky model, non-Newtonian Relationship
fluid of parameters
Viscosity
4
η, 
(effective Near-wall Pа * s 
μ, [Pa*s]  
viscosity for viscosity  m  R
polymers)
Shear rate
γ,   Vt,  
(visual or 1 m
effective or s s R
average shear 4Q Cork flow rate Q V t 
  3 V  4
R R
rate for t 2
polymers)
ΔPn, [Pa] Back pressure ΔPc, [Pa]
Back pressure due to melt Pn 4
 1
due to shear Q 8 L sticking Q 2 L  P c R
rate flow Pn  (adhesion) to the Pc  ΔPn = ΔPc
R 4
channel walls R 3
τn, [Pa] τc, [Pа]
Pn R Pc R
Shear stress  n 
2L Shear stress  c 
2L n c
 n    c  Vt

134
 Table 3.5
Equations of fluid flow between parallel plates of length L, width w and
height h
Shear model , Newtonian fluid Corky model, non-Newtonian Relationship
fluid of
parameters
Viscosity
6
η, 
Pа * s 
(effective
μ, [Pа*s]
Near-wall
  
viscosity for viscosity  m  h
polymers)
Shear rate
γ,   Vt,  
1 m
(visual or
effective or s Cork flow s h
average shear 6Q rate Q V t 
rate for
  2
V t  6
wh wh
polymers)
Back pressure
ΔPn, [Pа] due to melt ΔPc, [Pа]
Back pressure Pn 6
sticking  1
Pc h
due to shear Q12L (adhesion) to Q 2 L
rate flow Pn   P c  ΔPn = ΔPc
wh 3 the channel wh 2
walls
τn, [Pа] τc, [Pа]
P h P h
Shear stress n  n Shear stress c  c n c
2L 2L
 n    c  Vt

In the cork flow model, the back pressure is determined by the viscous friction
force Ft that arises in the interphase layer W2, that is, between the channel walls
(surface) and the melt cork; therefore, the basic relations during the melt polymer
movement in channels of characteristic geometry are calculated as follows:
Ft VtS p Vt 2RL Vt 2L Q 2L
tube channel : P      , (3.2)
Sс Sc R 2 R R 3

Ft VtS p Vt 2wL Vt 2L Q 2L

slit channel: P      , (3.3)
Sс Sc wh h wh 2

135
 where Sс - channel cross-sectional area; Sр - channel surface area; Ft is the
force resisting to cork shear, which characterizes the melt adhesion to the channel
walls.
Let's analyze the wall viscosity dimension:
 Pa * s   pressure  force
 m  = rate  output . (3.4)
In this understanding, viscosity, as a value showing resistance to flow, has a
obvious physical meaning.
It should be noted that in the standard dimension viscosity [Pа*s] is
practically not used in plastics processing technology. Usually the technologist
analyzes the melt flow index (MFI). The author has come across situations when
the application of viscosity and shear rate was used for a process deeper study, but
led to erroneous results. At the same time, the use of the melt flow index [g/10min]
always gives adequate and predictable results in technological process. Melt flow
index ‘MFI’ is the same as Output ‘Q’ which is measured under some standardized
conditions.
The standard conditions for the process of measuring the MFI are the force
(pressure ΔPc) and the capillary geometry (R, L), or in other words the standard
shear stress. As can be seen from the comparison tables (3.4, 3.5), shear stress is
calculated regardless of how (in which model) we calculate viscosity and shear (or
flow) rate, therefore some standard shear stress is a more universal indicator of
flow.
As clearly as possible, this is seen in the equations where a more detailed
calculation of the shear stress is shown.
Table 3.6
Comparative analysis the shear stress calculations
Shear flow model Corky flow model

 n    c  Vt
R 4 R 1
 n  Pn Q 3   c  Pc Q 2
2L R 2L R

136
 Shear stress τ is a constant for a given weight (method MFI). We measure -
output - Q , which varies from viscosity and the result does not depend on which
model we use to calculate the viscosity and shear rate. Therefore, the melt flow
index is a measure of the real viscosity of the polymer. Another question is how

(with which model) we calculate the viscosity (Newtonian μ or Corky η or

another) and the corresponding shear rate.
If we imagine (to additional) that we are using a power-law model where the
term is:
- “true viscosity” is used, for μt is the viscosity of a power-law fluid;
- “effective viscosity” μ is the viscosity of a Newtonian fluid.
4n
This two viscosities [33] is related by equation  t  
3n  1
Then there is even greater confusion with the estimation of the viscosity,

because the flow index n can be calculated only in a certain range of shear rates,
and without this limitation it is not clear where the limits of applicability of the
measured and calculated viscosity are.
Therefore, when a rheological curve is given, it is necessary not only to
know how (equipment) it was used but also a model of how the viscosity and shear
rate were calculated. Without this information, the rheological curve is not
connected to the real process.
The same approach to measuring viscosity is observed in flexo-printing
technology. Measuring the viscosity flexo-printing inks and various additives (in
the form of viscous liquids) with a Brookfield viscometer (time for a certain
volume of viscous liquid to flow through a standard capillary) always gives a
correct estimate.
Let's take a closer look at the formulas in the table. That is, by measuring the
4 1
 
MFI, we practically estimate the value
R 3 or R 2 .
It is interesting to analyze the dimension of this parameter
137
  Pa * s   pressure  pressure 
 m3    output    speed * area
   

So this understanding of viscosity, as a value showing resistance to flow,

also (similar to corky model) has an obvious physical meaning. This explains why
the MFI is better used to assess the viscosity of a polymer than the actual classical
‘viscosity’.
I think that the main problem is that the classical dimension of viscosity
[Pa*s] or dimension [Pressure*time] has no physical meaning. The same problem
with kinematic viscosity. Dimension [mm2/s] has no physical connection with
viscosity as a criterion for resistance to flow.
Mixing two, three or more liquids with a spoon, it is always easy to visually
and organoleptically assess their viscosity. But at the same time, many methods
and standards have been developed for visually understandable and simple
characterization of a liquid.
Table 3.7
Comparison of two polymers flow measurement on a standard capillary
rheometer
Param Power
eters -law Viscosity
Effective fluid as the
Melt viscosity, viscosi Corky value of
flow Weigh Shear Newtonia ty, flow reverse
index t stress Pressure n flow n=0,6 viscosity to MFI
symbol

MFI F τ=8,97F ΔP=15,2τ μ μt η τ/Q

dimensi [g/10mi
on n] [gram] [Pa] [Pa] [Pa*s] [Pa*s] [Pa*s/m] [Pa*s/m3]
LDPE 1,14 1116 10011 152541 4774 4092 1,83,E+07 5,28E+12
15813- 3,90 2607 23385 356340 3247 2783 1,24,E+07 3,59E+12
020, 10,9 4905 43998 670443 2195 1881 0,84,E+07 2,43E+12
190C 64,3 13007 116673 1777871 983 843 0,37,E+07 1,09E+12
0,25 1116 10011 152541 21841 18721 8,37,E+07 24,2E+12
Elvax
1,04 2607 23385 356340 12235 10487 4,69,E+07 13,5E+12
3165,
190C 3,16 4905 43998 670443 7552 6473 2,89,E+07 8,36E+12
19,7 13007 116673 1777871 3204 2746 1,23,E+07 3,55E+12

138
 The table shows the viscosity calculations for different models and flow
index. The differences are huge, so the standardization of viscosity as a parameter
of resistance to flow is an urgent task.

3.3.3 Comparative analysis of complete rheological models of polymer melt

flow
Let us determine the error in predicting the viscosity using the corky flow
model in the widest possible range of shear rates.
Rheological curves HDPE (200оС, Alaton TM7040) and PP (190оС, CD460)
in the range of shear rates γ from 10-2 to 104 are taken from [34].

Carreau model selected for comparative analysis:

  
 
n 1
 1   
2 2
0   (3.5)

The Carreau model parameters for the selected HDPE and PP grades are
given in [34], but to cover the full range of shear rates (γ from 10 -2 to 106 ) and to
improve the approximation accuracy, the Carreau model parameters were
corrected, calculations were performed using the Excel Tool-pack "Solution
search”.
Corky model:
The Model (formula 3.1) to create for a corky flow, but for clarity of
approximation by two models, instead of the flow velocity Vt [m/s], the shear rate
γ [1/s] and the usual understanding of viscosity as resistance to shear flow are
used:
H H
 
sin  r . (3.6)
1
 * tg
After this transformation, we will use the term - Trigonometrically model, or
T-Model name for equation 3.6.

139
 So shear rate is applied, the formulas for calculating transition points between
flow regions are transformed:
H r
at low shear rates 0  
; t1  ;
sin  tg
H r

at high shear rates    H ;  
sin   1 .
t 2
tg *   1
 sin  
If we setting the values µ0 and µ∞ , we determine the model parameters and
find the angle α according to the equation:

sin( )  1 
0 (3.7)
Further, setting the value of γt1 we calculate the relaxation rate γr.

3.3.4 Flow simulation results using the full rheological curve equation
The model parameters final values are shown in Table 3.8. Table 3.9 shows
the calculated value at each analyzed point of the rheological curve. Also given is
the standard deviation σ for predicting the viscosity using the two considered
models (the number of points n = 6) [73].
Table 3.8
Flow Model Parameters
Material
Parameter Description
HDPE PP
α, degree 82,1 85,6
γr, 1/s 2732 102 T-Model parameters
H, Pа*s 1040 5035
γt1 , 1/s 380 8
γt2, 1/s 39520 2679 T-Model calculated
μ 0, Pа*s 1050 5050 values
μ∞ , Pа*s 10 15
μ 0, Pа*s 1100 4700
μ∞ , Pа*s 10 1 Model Carreau –
n 0,3 0,39 parameters
λ, s 0,01 0,51

140
 Table 3.9
Experimental and calculated values of viscosity according to the analyzed
models
Viscosity,
Viscosity,
experimental and
Shear rate experimental and
calculated values for
calculated values for PP
HDPE
T- T-
-1 Carreau Carreau
γ, с µ exp Model µ exp Model
µ calc µ calc
µ calc µ calc
1,0E-02 - 5044 4700 - 1050 1100
1,0E-01 5000 4988 4696 1000 1050 1100
1,0E+00 4000 4489 4380 1000 1047 1100
1,0E+01 2000 2250 1720 950 1023 1096
1,0E+02 500 387 428 900 833 865
1,0E+03 100 55 106 400 296 227
1,0E+04 21,6 19 27 50 48 53
1,0E+05 - 15 7 – 14 19
1,0E+06 - 15 3 – 10 12
Standard deviation –
σ, Pa * s 230 231 65 110

10000

1000
Viscosity, Pa*s

100

10

1
1,0E-02 1,0E-01 1,0E+00 1,0E+01 1,0E+02 1,0E+03 1,0E+04 1,0E+05 1,0E+06
Shear rate, 1/s

PP PP T-Model PP model Carreau

HDPE HDPE T-Model HDPE model Carreau

Fig. 3.15. Rheological characteristics of HDPE and PP for the different

temperatures and approximation by equations (3.5 and 3.6) with parameters
according to table 3.8.

141
 Note the following relationship between the two models. First, the close
values of the viscosities μ0 and μ∞. Second, the relaxation rates γr in the T-Model
are inversely proportional to the relaxation time λ in the Carreau model, and the
rates γr ratio for two polymers have same level as the ratio of relaxation times λ.
The T-Model has the following advantages:
• developed on the basis of a physical flow model;
• has fewer parameters;
• allows to calculate the transition points between the flow areas and the
limiting values of viscosity;
• T-model has a universal character, at an angle α≈0, a Newtonian flow is
modeled, that is, a shear without relaxation;
• T-models graph shape is closer to the typical S-shaped of a non-Newtonian
anomalous viscous fluid flow curve, which is given in [43; 74].
Table 3.10 shows the C-Model parameters for the studied rheological curves
(in the parameters of wall viscosity and corky flow rate). The viscosity constant Hс
and relaxation rate Vr calculation was carried out for a standard capillary (D
=2.1mm, L =8mm) according to the equations: η=3810*μ; Vt=γ/3810.
Table 3.10
Corky flow model parameters
C-Model
Parametr
HDPE PP
Interaction angle α, deg 82,1 85,6
Relaxation rate Vr m/s 0,719 0,027
Height of interacting elements (constant of wall
viscosity)
Hc, Pa*s/m 3,97E+06 1,92E+07
Viscosity at zero flow rate η 0, Pa*s/m 4,01E+06 1,93E+07
Viscosity at infinite flow rate η ∞ , Pa*s/m 3,82E+04 5,73E+04
Flow speed, transition at low speeds Vt1 , m/s 0,1 0,0021
Flow speed, transition at high speeds Vt2, m/s 10,4 0,705

142
3.3.5 Simulation of flow at different temperatures, comparative analysis of
corky and power model of melt flow
When developing plastics production processes, an analysis is required over
the full temperature range where a viscous-flow state is observed, that is, it should
cover the possible range of temperature conditions for polymer processing.
The power law is widely used to calculate the processes of melt flow in the
extruder and the die, but it gives you to calculate the flow only in a curve limited
part. For example, for polymers, which were analyzed in the previous section, it
covers the range of shear rates γ from 101 to 104s-1 for PP, and from 102 to 104s-1
for HDPE (Fig. 3.15). It should be noted that it is sometimes indicated that the
region of shear rates, which are sufficiently with enough accurately covered by the
power law, satisfy with the characteristic region of polymer processing from 10 0 to
104 [33], but when analyzing specific characteristics, it can be seen that the
transition (linear region in logarithmic coordinates) is much less.
For the rheological characteristics of LDPE at two temperatures, parameters
were calculated according to the corky flow model (Table 3.11) and the power law
model (Fig. 3.16).
Table 3.11
Rheological characteristics of LDPE
Viscosity Pa*s/m
o
LDPE 170 C LDPE 230oC
Flow Power
velocity*, Cork Power law Cork law
m/s Experimental model 1 model 1 Experimental model 2 model 2
0,0001 - 1,9E+07 - - 2,8E+06 -
0,0015 - 1,6E+07 - - 2,7E+06 -
0,0053 1,0E+07 1,1E+07 1,1E+07 2,4E+06 2,4E+06 2,7E+06
0,0105 6,8E+06 7,8E+06 6,8E+06 1,9E+06 2,1E+06 1,9E+06
0,018 4,6E+06 5,5E+06 4,5E+06 1,5E+06 1,7E+06 1,5E+06
0,026 3,6E+06 4,2E+06 3,4E+06 1,3E+06 1,5E+06 1,2E+06
0,053 2,2E+06 2,4E+06 2,1E+06 9,9E+05 1,0E+06 8,8E+05
0,105 1,2E+06 1,4E+06 1,2E+06 6,5E+05 6,9E+05 6,3E+05
0,184 8,0E+05 8,9E+05 8,2E+05 4,6E+05 5,0E+05 4,8E+05
0,263 6,1E+05 6,9E+05 6,3E+05 3,7E+05 4,1E+05 4,1E+05
0,40 - 5,2E+05 - - 3,3E+05 -
3,00 - 2,3E+05 - - 1,9E+05 -
10,0 2,0E+05 1,78E+05

143
 The flow velocity from 0.0001m/s to 10.0m/s is corresponds to shear rate
from 0,38s-1 to 38100s-1, if rheological curve was measurement on a standard
capillary D=2.1mm, L=8mm.

1,0E+08

1,0E+07
Viscosity, Pa*s/m

y = 235800x-0,7366
R2 = 0,9981

1,0E+06

y = 213136x-0,4818
R2 = 0,9856
1,0E+05
1,0E-04 1,0E-03 1,0E-02 1,0E-01 1,0E+00 1,0E+01
Flow velocity Vt, m/s
LDPE, 170ºС Model 1 LDPE, 230ºС
Model 2 Point Vt1 model 1 Point Vt2 model1
Point Vt1 model 2 Point Vt2 model2 Power law model (LDPE, 230 C)
Power law model (LDPE, 170 C)

Fig. 3.16. Rheological characteristics of LDPE at different temperatures and

approximation by equation (3.1) with parameters according to table 3.10.

It can be seen from the graph that the corky flow model approximates the
rheological curve quite well, even in the area where the viscosity changes linearly
in logarithmic coordinates, that is, where the power model is applicable.
Approximation by a power-law model was carried out in the region of a non-
Newtonian flow.
Table 3.12 shows the corky flow model parameters for the rheological
characteristics of LDPE at various temperatures.

144
 Table 3.12
Parameters flow models
Parameter Model 1 (170оС) Model 2 (230оС)
α, degree 82 70
Vr m/s 0,05 0,07
H, Pa*s/m 1,91E+07 2,67E+06
ηₒ 1,92E+07 2,84E+06
η∞ 1,87E+05 1,71E+05
Vt1 0,007 0,026
Vt2 0,711 0,396

The C-model parameters analysis shows that temperature affects all three
parameters: angle, relaxation rate, and viscosity constant. In the power-law model,
two parameters, the viscosity constant and the flow index, change. To build models
taking into account the temperature, it is necessary to additionally find the models
parameters functional relationship from the temperature.
The approximation accuracy analysis in the velocity range from 0.005 to
0.25m/s (or in the usual shear rate from 20 to 1000s -1) at 230°C shows that the
maximum relative error in predicting the viscosity using the cork model and power
model is approximately the same and does not more accordingly 12.9% and 12.4%.
For a temperature of 170°C, the cork model gives a higher relative error - up to
19.6%, while the power-law does not exceed 7.6%, while the correlation
coefficient for all four models is r> 0.99, the determination coefficient is R2> 0.98.
The corky flow model advantage is obvious - the full range of velocities coverage,
with comparable forecasting accuracy with the power-law model in the non-
Newtonian flow region.
An obvious problem in applying the power law model, and this is clearly
seen from the example under consideration, is that the shear rate from 0.1 to 20s -1
is also interesting for modeling the plastics processing, therefore, two or three
power-law models with different viscosity constants and index are needed to
adequately describe one rheological curve.

145
3.3.6 Analysis of processes, effects and extrusion techniques based on a corky
flow model
The corky flow model shows that as a result of periodic relaxation of
macroroughnesses in the melt, transverse vibrations arise, and their frequency
increases with increasing flow velocity.
It can be assumed that when they coincide with the frequency of internal
(temperature) oscillations of macromolecules, resonance appears and the
phenomenon chaotic changes in the extrudate surface or, as it is called,
“sharkskin”, is observed. That is, the macroroughnesses increase sharply in size
due to resonance. This explains why lowering or raising the melt temperatures
eliminates the "shark skin" effect, as well as the super-extrusion mode - operation
at very high shear rates when the resonance boundary is overstep. The critical
shear stress τсr, at which surface distortion is observed, is 0.1–0.4MPa [33], the
period of melt near-wall vibrations (for the considered polymers) when the range
of τсr is achieved is 10-5 –10-8 s.
The proposed method for calculating the channels and the corky flow model
make it possible to study the wall and central layers interaction. The near-wall
layer W3 formation nature is also interesting. It is clear that there is a dependence
on the coefficient of melt friction on the metal and the polymers thermal stability.
The die temperature affects in two ways, on the one hand, an increase in
temperature reduces the viscosity on the channel wall and the near-wall layer
becomes thinner and accelerates, on the other hand, the melt destruction grows and
degradation particles on the walls grow. With a decrease in temperature, the
process is reversed, an increase in viscosity occurs, the near-wall layer grows, but
the melt decomposition decreases, this improves the near-wall layer W3 stability.
Let us carry out a qualitative analysis the wall layer W3 nature. According to
the design scheme in Fig. 3.14, the relaxation of melt microroughness is analyzed,
which in section are presented in the form of triangles, that is, the change in the

146
contact line length is calculated with a change in the flow rate η=f(Vt). But if we
consider the channel surface and, accordingly, the volumetric flow, then instead of
the length, it is necessary to analyze the change in the contact surface area of the
bunches (bundles) of macromolecules (macroroughness). Depending on the
assumed shape of these bunches (beams), the area calculation will change. The
most probable is a spherical shape or, to simplify calculations, a pyramidal shape
in the form of a triangular pyramid, which is closer to the design scheme of a corky
flow. But in any case, for a sphere or a triangular pyramid, the interaction area will
be proportional to the interaction line length square, that is, in the model, this is the

wall viscosity, S  
2
Actually, in the corky flow model of a non-Newtonian
liquid, it is assumed that the observed viscosity is the superposition of two factors
of the effective interaction area and intermolecular interaction. Therefore, the force
acting on the wall layer W3 will be proportional to the viscosity square:

FW 3   2 * Vt Such a function has an extremum (convexity) at the first

transition point in the region of low shear rates – Vt1 [76].
That is, for each channel section and each rheological curve, there is an
optimal output, at which the impact on the near-wall layer W3 is most effective.
Such a change in the force FW3 (that is, the presence of extrema) explains why the
extrusion dies effective washing is provided by a variable melt flow rate in the die
(periodic changes in the output and/or extruder pressure in the min-max range)
[11].
The minimum force FW3 in the region of high shear rates Vt2 explains why
there is an optimal injection rate in the injection molding process. The pressure
curve on the injection rate has a minimum (extremum) in the region of high flow
rates [84]. Injection in the range of optimal injection speeds is one of the factors
that increase the process and products quality.

147
 0,00001 0,0001 0,001 0,01 0,1 1 10 100 1000
Flow velocity, m/s
Model 1, 170°С Force of viscous friction, 170°С
Model 2, 230°С Force of viscous friction, 230°С
Transition points model 2 Transition points model 1

Fig. 3.17. Graph of viscosity and viscous friction force on the flow rate.

The following dependence can be noted: on the part of the curve (where a
decrease in viscosity is observed) decrease of the effective area of interaction
going faster than increase the shear stress, therefore, the viscous friction force
decreases, in this time the shear stress increases continuously.
The method for calculating the flow based on the corky model requires
further development, the parameters H, α, Vr characterize the interaction strength
between the layers and depend on the intermolecular interaction, temperature,
polymer branching, and molecular weight; therefore, it is necessary to find how the
model parameters are related with the polymer molecular characteristics. It is also
of interest to study the force acting on the wall layer and calculate the layers W3
and W2 velocity. Based on experimental data, their speed is several times lower
than the central layer W1 speed and strongly depends on the quality and properties
of the forming channel coating (type of material, hardness, roughness, corrosion
resistance, adhesive properties to polymer melts, wear resistance, presence of
micropores in the surface) ...

148
3.4 Development of the melt flow model in the extruder
Flow models of a Newtonian, non-Newtonian power-law fluid in an extruder
screw have been worked out in detail by many researchers [33, 34], but these
models use a limit - the velocity on the wall of a stationary channel is zero. It is
also assumed that the main element that creates pressure in the extruder is the
moving surface. That is, when the screw rotates, the model assumes that the melt
as a liquid adheres to the surface and the maximum speed develops near the screw
wall in the direction of its rotation. The melt adhesion to the all surface that is
moving is a prerequisite for the extruder standard operation.
When analyzing the methods of creating pressure, it is indicated [34] that the
extruder main idea is that it is a surface coiled into a spiral, so if you feed the melt
with two moving surfaces, you can significantly increase the extruder productivity.
To implement this idea, an experimental device was developed, consisting of two
heated, rotating discs, where the melt was supplied by the discs surfaces, the
device worked reliably in the laboratory, but had a number of disadvantages, in
particular, the flow channel limited length. The screw does not have such a
limitation; therefore, the extruder design development [34] was proposed as
follows: the flights are not connected with the screw, the screw root and the
cylinder rotate in the same direction. In such a device, the melt, adhering to the
screw root and to the cylinder, is carried away to the outlet by two surfaces. In this
case, it is better to rotate the flights in the opposite direction. Thus, in theory,
productivity will be doubled compared to conventional extruder designs (due to
drag flow).
But the Helibar extruder, where the productivity is increased by 30-50%,
without increasing the screw diameter, is designed with completely different
structural elements. Note that it is claimed [45], including a reduction in energy
consumption by 10–60% and accelerated purging when changing formulations,
although at first view it seems that the channels in the cylinder in the zone of melt

149
movement should increase the number of stagnant zones and to reduce the
extruder's adaptability to color change.
Let us analyze the Helibar extruder design based on the available
information [45, 77-81]. Longitudinal grooves improve heat transfer by increasing
the cylinder surface area, mixing and plasticizing action due to the barrier screw,
increasing productivity due to the fact that the plasticized material is additionally
fed along the grooves (0.5-1.0 mm high) [81], which run along the entire cylinder.
But it should be noted that the grooves depth decreases towards the exit from the
extruder and at the very end the cylinder is smooth (at a length of about 5D), if the
grooves went to the very end, it would be impossible to stably melt the polymer
material, since the channel depth in the dosing zone and the degree of compression
strongly affect the extruder plasticizing effect, that is, the grooves do not affect
productivity as a simple additional melt conveyor. So it was possible to simply
increase the channel depth instead of adding the grooves length.
The grooves can be straight or spiral, at least one groove is needed, and if
the groove is spiral, then it runs perpendicular to the screw thread axis [45].
Almost all thermoplastic materials and secondary raw materials are extruded. And
what is very important - the productivity calculation of the Helibar extruder is
possible using the “screw-nut” model [79]. It is confirmed that the movement of
the polymer melt (even in such a complex configuration of channels) can be
considered as the movement of a nut (cork) screwed onto a screw, and which
moves due to friction with the cylinder walls and sliding relative to the rotating
screw. Consequently, the grooves do increase productivity, but above all they
create additional braking (friction) on the melt cork surface.
It can be assumed that the polymer melt, which wraps around the screw in a
spiral, has a structural strength - it “forms a nut”, therefore, the grooves braking
effect in the barrel enhances the melt sliding (spiral) relative to the screw, and
therefore the extruder output increases.

150
 Table 3.13
Characteristics of standard extruders in comparison with HELIBAR

Pnom, Nmax, Qmax, *

Firm Extruder description, ø45мм L/D Qmax/Nmax
kW rpm kg/h

Smooth cylinder, loading

area smooth or with small 26 13,2 100 50 0,50
grooves (1950г)
The cylinder consists of two
Komax parts, a groove in the
loading zone at a length of 30 35 200 160 0,80
5D, a smooth cylinder at a
length 25D (1980г)
Extruder HELIBAR (2000г) 30 37 210 180 0,86

Extruder HELIBAR/
EXTRU 30 34 150 135 0,90
standard
DEX
GmbH Extruder HELIBAR / with
36 75 275 300 1,09
high output
*
parameter Qmax/Nmax was calculate by author.

Analysis of the Helibar extruder characteristics, which are declared by the

equipment manufacturers [77, 78], shows that, in comparison with the extruder
with a smooth loading zone, the specific output increases in 2.18 times (1.09/0.5),
the maximum rotation speed and output also increases.

3.4.1 Flow between parallel plates

Let us consider the process of flow between two parallel plates located at a
distance h, based on the generally accepted shear flow and flow in the form of a
"cork". One plate is stationary, the other moves at a speed V0 (Fig. 3.18).

151
Fig. 3.18. Velocity profile for different flow models: a - shear flow, c - corky flow.
The corky flow analysis is carried out according to the equations from Table 3.5,
while we assume that the melt adheres to the plates with the same force and the
plates area is the same. The final velocity diagram for such a flow is rectangular,
the melt is carried away by the moving plate.
F fr  VtS p ; F0  V0  Vt S p ;
where
Ffr - is the force preventing shear of melt corky, which characterizes the melt
adhesion to the stationary plate;
F0 – is the force acting on the melt cork from the moving plate side with the
velocity V0;
Sр – is the plate surface area;
Vt – is the melts cork speed;
η – is the near-wall viscosity, which characterizes the cork shear resistance
on the plate wall.
In steady state the force acting on the melt cork from the moving plate side
and entraining it in the plate movement direction, is equal to the stopping force
from the fixed plate side, therefore:
VtS p  V0  Vt S p ; Vt  V0 / 2 .
That is, with the same contact area and the same melt friction (sliding) on
the movable and fixed plates, the cork speed will be half the moving plate speed.

Therefore, the output for the width: q A  V0 h 2 .

152
 In this way, the generally accepted shear flow analysis approach [34] and the
corky motion analysis presented above, give the same output calculation result.

3.4.2 Development of the melt movement model in the screw

The melt movement analysis in the dosing zone is similar to the movement
analysis in the extruder feeding zone. In fig. 3.19 is a diagram showing the various
forces acting on the cork element of the polymer melt. The pointing (symbols) of
the screw geometrical parameters are generally accepted and correspond to the
symbols in [34].

Fig. 3.19. Diagram of forces acting on the cork of the polymer melt: F s -
friction force acting on the melt from the screw; Fb is the friction force acting on

153
the melt from the cylinder; Fp - force acting on the polymer cork due to back
pressure in the die.

Fig. 3.20. Velocities melt diagram in the screw dosing zone: V0 - the screw
- -
rotation speed; Vts the cork speed relative to the screw; Vtb the cork speed
relative to the cylinder; Vx - the cork speed useful component along the screw
axis; Vmax - the cork useful maximum speed; Vp - the cork back pressure speed; φ -
the helix angle; θ - the friction angle.

According to the developed diagram of speeds (Fig. 3.20), the screw

movement and the melt movement are related by the following relationships:
V0
Vx  V  DN .
 1 1 ; 0 (3.8)
  
 tg tg 

Vx  Vtb sin  ; V x  Vts tg . (3.9)

154
 The melt movement without back pressure at the dosing zone outlet
The forces acting on the cork element can be calculated through the screw
geometrical parameters, the wall viscosity and the screw speed, for this we analyze
the equation of steady motion under the condition Vp=0, Fp=0, projection onto the
helix axis Y:
Fb cos(   )  Fs . (3.10)
According to the corky flow model:
V0  Vts
S b bVtb cos(   )  S s s , (3.11)
cos
where Sb - the cylinder surface area; Ss - the screw surface area; Sw- helix
pitch sectional area, section perpendicular to the Y-axis.
After transformations, taking into account equations (3.9), we obtain an
equation for calculating the angle of friction θ:
1 S s s
  tg . (3.12)
tg Sbb sin  cos

Simplified algorithm for calculating "drag flow":

1. For rheological characteristics, wall viscosity constants (3.1), we calculate

the ratio  s  b  H s H b .
2. Determine the friction angle according to the equation (3.12).
3. According to the equation (3.8), for the screw rotation speed N, we can
determine the cork speed Vx.
4. Calculate the dosing zone output Q  VxDh(1  e t ) .
5. After calculated the movement velocities Vtb and Vts according to equations
(3.9), we can determine the corresponding near-wall viscosity on the wall of
the cylinder ηb and the screw ηs according to equation (3.1).

155
 Cork movement with the back pressure at the dosing zone outlet
If the back pressure ΔР at the dosing zone outlet is arise, the melt flow speed
decreases. The cork deceleration, the "reverse flow rate", is calculated using the
plug flow model (Table 3.5) in the helix axis direction:
PS w
Vp  , (3.13)
Sbb  S s s
The viscosity on the wall of the cylinder ηb and the screw ηs is calculated
from the cork velocity relative to the screw Vtb and the cylinder Vts according to
equations (3.8, 3.9) without taking into account the back pressure, this is
permissible, since the shear rate level in the screw channel is usually calculated
from the rotation speed without taking into account the back pressure. To calculate
ηb and ηs , it is required to apply the corresponding rheological model according to

equation (3.1), where the viscosity constants  s  b  H s H b .

The cork speed along the screw axis:
V  Vx  Vp sin . (3.14)
The final equation of the screw metering zone operation we obtain after
using the variables from equations (3.8), (3.12), (3.13) in (3.14):
DN sin  cos P S w sin 
V 
S s s Sbb  S s s (3.15)
1
Sbb
For a metering zone with a length L, a channel width w and metering depth
h:
Lw L ( w  2h)
S w  hw ; Sb  ; Ss  . (3.16)
sin sin

If we accept that,  s   b   , where η is the average wall viscosity in

the channel, is then the equation of metering zone work is transformed to a form
more suitable for engineering calculations:

156
 w  DN sin  cos Ph sin 2  
V    (3.17)
h  w  2 2  L 

Channel shape factor:

Fd =Fp = w (h  w) . (3.18)

0,8

0,6
Fd, Fp

0,4

0,2

0
0 0,4 0,8 1,2 1,6 2
h/w
Fd (shear model) Fp (shear model) Fd=Fp=w/(h+w) (cork model)

Fig. 3.21 Channel shape factors for standard shear model from [34] and
calculation from cork flow model (3.18).

Output for metering zone:

Q  V Dh(1  e t ) . (3.19)
If we assume that the areas of the screw and the cylinder are the same and
equal to the cylinder area (when w  h ), then with this simplification, the motion
between the parallel plates melt cork is simulated, and the equation for the dosing
zone work is transformed to the form:
DN sin  cos P h sin 2 
V  . (3.20)
2 L 2
After calculated the speed V value, it is necessary to check the friction angle,
which changes under the back pressure action:
V  Vts tg . (3.21)

157
3.4.3 Comparative analysis of the obtained equations with the classical
extrusion equation

We transform the classical equation of a Newtonian fluid extrusion

P
Qc  NFd   F p to a form where only the melt velocities along the axis of


a single-pass screw will be taken into account Vc  Vxc  V pc :

Qс P
Vc   1 NFd  1 F
Dh1  e t   p (3.22)

Without taking into account the channel shape factor Fd, Fp (when w  h ):
DN cos sin  P h 2 sin 2 
Vc   (3.23)
2 L 12
Let us analyze the calculations using equations (3.20) and (3.23)
The direct flow is the same for both models. For equality of reverse flow, it

is necessary that: 1   h 6
The same viscosity ratio is obtained when analyzing the flow between
parallel plates using the shear and cork flow models (Table 3.5). Thus, equations
(3.20) and (3.23) are identical.
Equations (3.15) and (3.17), are more general than the classical extrusion
equation, take into account the non-Newtonian nature of the melt flow, at the same
time, they are simple enough for understanding and practical application. Equation
(3.15) takes into account the surface quality of the screw and barrel, which affects

the ratio  s b and gives an understanding for a well-known practical observation

- the surface quality of the screw should be better than that of the barrel, then the
extruder works stably; in the opposite case, when the melt sticks to the screw and
slides along the cylinder, the melt output pulsation is observed.

158
3.4.4 Results of flow simulation in the dosing zone for different models

As an example, let us analyze the calculations by equations (3.15) and (3.22).

PE material, processing temperature 2300С, density ρ = 1g/cm3, rheological
characteristics, measurement on a standard capillary D = 2.1mm, L = 8mm:
Table 3.14
Rheological characteristics PE
Parameter Volume
Shear rate, s-1 1 20 100 400
Viscosity, Pa*s 738 625 350 170

Based on the rheological characteristics, the material flow models parameters were
calculated.
Table 3.15
Flow models parameters of the PE material
Flow model Volume The range
Parameter
of rates
Corky Interaction angle α, [deg] 70
H H Relaxation rate Vr [m/s] 0,07 Vt , [m/s]
 
sin Vr  Pa * s 
Wall
 1 constant
viscosity
  2,66E+06 0;
Vt tg H,  m 
Viscosity constant m0, [Pa*s] 2976
Power law γ , [s-1 ]
Flow index n 0,52
  m0 n1
Viscosity at zero
flow rate
μₒ, [Pa*s] 745 20;1000

Further, when simulating the flow in the dosing zone, the cork speed Vt
(Vtb,Vts) is calculated according to equations (3.9) , the wall melt viscosity in the
barrel η b and screw ηs is calculated according to the model parameters from
Table.3.15. The viscosity for the classical model was determined by the power-law
model, with the parameters from table. 3.15; shear rate   DN h .

159
 The ratio of reverse flow to forward flow according to the equation:
  V p Vx *100

It should be noted that for a standard capillary, there is a relationship

between the wall viscosity constant H and the viscosity μ1 it is H  3810* 1
[73].
The screw geometrical parameters: D=45mm, φ=17,50 , e=5mm, L=600mm,
h=4mm, w=37.7mm. According to equation (3.12) at ΔP=0, the angle of friction is
θ=12,420.
The simulation results given in table 3.16 shows that both models (3.15) and
(3.22) give similar results, the difference in prediction output is no more than 10%,
for rotation speed from 10rpm to 200rpm. The flow model and the level of shear
rate and viscosity is the main influence factor in the difference of calculations
output.
Table 3.16
Comparative calculations for two models of the extruder dosing zone
Parameter Simulation results
1 2 3 4 5 6
ΔР, [Bar] 20 300 20 300 20 300
N, [rpm] 10 10 40 40 80 80
Corky model
θ , [deg] 11,28 -5,25 11,88 4,19 12,01 6,24
Q, [kg/h] 4,96 -2,29 20,94 7,30 42,35 21,75
α , [%] 9,45 141,76 4,45 66,71 3,36 50,37
Shear model
Qc , [kg/h] 5,19 -2,27 21,87 7,36 44,37 24,13
αc , [%] 9,3 139,6 4,5 67,9 3,2 47,3

Let be note, in the calculations given above, the melt rheological

characteristics are the same for sliding on the screw and barrel ηb≈ηs, and the
results of output calculating according to formulas 3.17 and 3.15 differ by less than
2%, so in the formula 3.17 can uses the average viscosity value
  ( s   b ) 2 with a small error. But if the flow rate Vt (for estimate

160
average viscosity η ) is calculated by analogy as for the shear model, that is, to

accept that the cork speed will Vt  V0  DN , in this case the difference
between calculating the output according to formulas 3.17 and 3.15 will be more
then 15% (Tab.3.16; Fig. 3.22).
Table 3.17
Melt flow model influence on calculate the pressure flow and extruder
output
Parameters Simulation results (ΔР=200Bar)
Rotation
Flow model N 0,1 1,0 5,0 10,0 40,0 80,0 120,0
speed
Newtonian,
Qn
viscosity is constant -9,0 -8,5 -6,2 -3,4 13,8 36,7 59,6
(3.22)
μₒ=745Pa*s
Power-law Qc
-0,5 -1,2 -1,0 0,4 12,5 31,4 51,2
Tab 3.13 (3.22)
Output
Corky Q
-3,4 -3,1 -1,6 0,3 12,2 29,1 47,0
Tab 3.13 (3.15)
Corky
Q
Tab 3.13, -3,4 -3,2 -2,2 -0,8 8,7 23,8 40,8
(3.17)
Vt=3,14*D*N

Let be note, in the region of low speeds of screw rotation from 0.1 to 5.0 rpm,
the use of a power-law model leads to significant errors in the estimate of output,
so the power law “does not see” the right level viscosity in the region of low shears
rates.
40,0

30,0

20,0
Q, kg/h

10,0

0,0
0,0 20,0 40,0 60,0 80,0 100,0
-10,0
Speed rotation screw N, rpm
Qn - viscosity is constant for revers flow (tab 3.13)
Q - corky model (tab.3.13), where Vt (Vtb, Vts) - according to equations (3.9)
Qc - power-law model for revers flow (tab 3.13)
Q - corky model where Vt=3,14*D*N

161
 Fig. 3.22 Extruder characteristic in different models, when pressure is
200Bar.

3.4.5 Simulation with different friction of the screw and cylinder surfaces.
The results of calculating the output with a significant difference in melt
sliding (friction, level of adhesion) along the screw and barrel are given in the table
3.17.
According to the results shown in table 3.17, by controlling the parameter
 s b , you can control the extruder output. The maximum possible angle of
friction predicted by equation (3.12) is 72.5 degrees, while the productivity will be
97kg/h.
When the maximum melt adhesion on the barrel wall and sliding on the
screw wall is reached, the extruder productivity increases in 2.21 times (97/43.8),
this level is in good agreement with an increase in the specific productivity in 2.18
times, in the Helibar extruder according to the data in Table 3.13.

Table 3.18
The wall viscosities influence on the dosing zone productivity
Simulation results (N=80rpm)
Parameter
1 2 3 4 5 6 7 8 9 10
ΔР,
Bar
 s b 10,0 5,0 3,01 2,01 1,02 0,53 0,37 0,24 0,13 0,07

θ ,[deg] 0,4 0,9 1,6 2,7 6,2 13,5 20,0 29,8 43,1 53,0
300
Q,[kg/h] 2,2 4,5 7,7 11,6 21,8 35,3 43,3 51,9 59,7 63,8

θ ,[deg] 1,3 2,7 4,4 6,5 12,4 22,4 30,1 40,8 53,6 62,3
0
Q,[kg/h] 7,4 13,7 20,9 28,3 43,8 60,4 69,1 78,0 86,5 91,4

162
 100

90 The melt sticks to the barrel and slip on

the extruder screw (helibar extruder)
80

70
The melt adheres to the barrel and the screw of
60
Output, kg/h

the extruder equally (Classical model)

50 300 Bar

40 0 Bar
The melt sticks to the screw
and slip on the extruder barrel
30

20

10

0
0 1 2 3 4 5 6 7 8 9 10 11
The ratio of the viscosity melt near the screw and barrel

Fig. 3.23 Change in the extruder output from the ratio of friction on the
screw and barrel.
It should be noted that both models complement each other. Cork flow is
more typical for high-viscosity, high-molecular-weight polymers, with a large
amount of fillers, in technologies where processing, non-stick additives are used
that affect the melt sliding relative to the extruder channels surface.
Shear flow develops during high-temperature processing, extrusion of low
molecular weight polymers. Also, at the flow nature are influences the channels
dimensions, the surface coating type, and the equipment wear.
The mixing ability of the extruder in the cork model can be analyzed taking
into account the transverse vibrations of bunches (beams) of macromolecules, such
vibrations cause diffusion and mixing processes in the melt. The integral
assessment of the flow time and shear stress in the dosing zone shows the
accumulated volume of mixing actions on the melt.
It is known from practical observations that the standard screw has poor
mixing ability. Although the shear flow model assumes the circulation of the melt

163
in the dosing zone and, as it were, mixing should theoretically be present as a result
of shear flow, in practice, different mixing elements are used.
The design elements of the mixing elements are often selected by semi-
empirical methods depending on the achieved mixing level and the observed
degradation of the melt.

3.5 Conclusions on the third section

1. When designing the distribution tubular channels of coextrusion
dies for operation in a single production, it is necessary provide a
constant and maximum shear rate along the all length of that
channel.
2. The main technological parameters affecting the distribution of
melt flows in the extrusion die are the flow index, temperature and
productivity. The range of flow index rational values is 0.25 to 0.5.
3. An increase in the processing temperature and a decrease in the
productivity improve the melt distribution process in the die, since
they increase the flow index, but it should be borne in mind that
there is an optimal value for the flow index (that is, temperature
and productivity).
4. The non-Newtonian behavior of polymer melts is associated with
complex flow geometry, entanglement of macromolecules, and the
elasticity of a high-molecular-weight liquid.
5. The corky flow model is developed on the basis of a physical
model and more accurately, in comparison with empirical models,
approximates the rheological curve in the full range of melt flow
rates. The model makes it possible to study the interaction in the
flow near-wall region, which is important for high-speed extrusion
processes, in the conditions of small-scale production with large
quantity changeovers and change of formulations.

164
6. A method was developed for calculating the flow main parameters
of a non-Newtonian fluid in the full range of velocities, which is
based on the analysis of melt adhesion to the channel surface; a
new dimension for viscosity, as the ratio of pressure to linear
velocity, and a formula for converting a shear flow into a cork flow
are proposed.
7. A qualitative explanation is given to the effect of “shark skin” as a
resonance region due to the coincidence of the relaxation
oscillations frequency in the near-wall region and internal
(temperature) macromolecules oscillation. The efficiency of the
technological method of variable screw speed used for purging
extrusion equipment is explained by the presence of an optimal
flow rate when the force acting on the wall layer is maximum in the
region of low shear rates.
8. The representation of the polymer melt flow in the form of a cork,
which has a certain shape and slides over the channel surface,
complements the theory of plastic processing processes, provides a
new theoretical understanding of the single-screw extruder
operation, and explains the practical observations the screw surface
high quality effect on the extrusion process stability.

165
Section 4. Investigation of multilayer flow

Equipping modern coextrusion lines with gravimetric or volumetric melt

dosing systems is the standard solution for controlling extruder output on a per
layer basis. The melt dosing system is the key modules of the coextrusion line.
An important task in the technology of coextrusion is the multilayer
structure control, which mean the layers distribution is prediction for a certain ratio
of the extruders productivity.

4.1 The gravimetric dosing system investigations

The study was carried out on a coextrusion line equipped with a gravimetric
system [76].
Table 4.1
Technological parameters of the investigated process
Parameter А В С Д Е
(outside) (inside)
Screw diameter, mm 45 25 45 25 30
Rang of output, kg/h 2-30 0,5-5 2-30 0,5-5 1-20
Motor power, kW 30 15 30 15 20
Screw rotation, max, rpm 160 150 160 150 160
Polymer PA TIE LDPE TIE PA
MFI (190С, 2,16kg)
Basic material (80-100%) 2,0-3,0 2,0-4,0 2,0-3,0
Colorant super-concentrate (0-20%) 1,2-11,7
MFI (230С, 2,16кг)
Basic material (80-100%) 2,5-5,5 2,5-5,5
Colorant super-concentrate (0-20%) 8,0-22,0 8,0-22,0

Co-extrusion die for forming a multilayer tube has spiral 8-way distributors.
The co-flow channels have a gap of 3-5mm and a diameter of 120mm, a forming
nozzle with a diameter of 50mm, a gap thickness of 1.5mm, a channel length of
25mm. The melt temperature at the exit from the die was 230-2500С (control with
a pyrometer). The colorants masterbatches had a base corresponding to the layer
material, the masterbatches heat resistance was 250-3000С. The gravimetric dosing
system accuracy was 0.01 kg.

166
 The gravimetric system, based on the current value of the parameter α=Q/N
(ratio of productivity to rotational speed), calculates the required output of each
extruder, taking into account the material density and automatically sets it. Then
every 0.5 minute measures the extruder productivity and, if necessary,
automatically adjusts the screw speed.
The layer thickness stability was in the range of ± 0.5% for all layers, the
measurement was carried out according to the gravimetric control system data.

4.1.1 The multilayer structure reproducibility for various formulations

investigation
Film materials with a five-layer structure 35-45 µm thick were measured on
an SVC video control system.
The measuring absolute error of the layer thickness was Δ = 0.4μm. Taking
into account that the film thickness is 40μm, the absolute error (when analyzing the
percentage of layers) was Δ = 1%.
At the same time, the influence of the following factors was studied: MFI of
a layer, a setting layer thickness on gravimetry, structure on the final layer
thickness in the film. The MFI range for recipes №1-25 ranged over the range
according to the table 4.1.
The number of experimental points N was determined by the recipe entrance
frequency in production plans, the research period was 1 month.

167
 Table 4.2
Summary table of measurement results
Gravimetric control set,
Material N Δ=0,5% Measuring layer thickness with a video system, Δ=1%
Е D С В А Е D С В А
Recipe №1-10 53 20 2 31 2 45 20,4±2,0 3,3±0,7 31,2±3,2 3,1±0,8 42,0±3,1
Recipe №11-15 10 20 2 40 2 36 20,4±2,0 4,2±1,0 33,6±2,6 4,2±0,3 37,6±2,4
Recipe №16-18 5 10 2 21 2 65 10,5±1,2 4,0±1,3 19,7±1,9 3,1±0,9 62,6±2,4
Recipe №19-25 31 20 2 50 2 26 21,7±2,1 3,4±0,9 47,3±3,2 3,3±0,7 24,3±2,2
Recipe №1
In the layer С colorant is
10% 11 20 2 31 2 45 20,5±1,6 3,6±1,0 32,7±2,0 3,7±1,0 39,6±2,3
Recipe №2
In the layer С colorant 3%,
in the layer Е 15% 8 20 2 31 2 45 19,2±2,0 3,3±0,3 30,8±2,9 3,2±0,7 43,6±4,3
Recipe №8 without colorant 5 20 2 31 2 45 20,6±1,9 3,7±1,2 31,2±3,0 3,2±1,4 41,3±1,4
Recipe №3
In the layer С colorant 3%,
in the layer Е 15% 6 20 2 31 2 45 19,1±1,7 2,8±0,7 31,8±4,5 2,7±1,0 43,6±4,0
Recipe № 4
In the layer С 20%,
in the layer Е 3% 8 20 2 31 2 45 21,0±2,7 3,6±1,1 33,0±3,9 3,6±0,8 38,9±2,9

The data analysis in Table 4.2 shows there are no noticeable effect the
viscosity and the layer position in the die, on its final thickness. Everything is
mainly determined by the volumetric capacity installed on the extruder. The
measuring layer thickness high standard deviation can be noted, but a high
measurement error affects here, so the film is very thin and the interface between
the layers is an unclear.

4.1.2 The multilayer structure reproducibility for one formulation

investigation
The next experiment was carried out in this way: a different percentage was
set in a multilayer structure (PA/TIE/LDPE/TIE/PA), the coextrusion line
productivity did not change. The primary tube multilayer structure was analyzed
on an SVC video control system with a magnification of 300 times.
Measurement of 1 slice was carried out. The error in measuring the layer
thickness (in comparison with the study in 4.1.1) was reduced by 10 times, since
the analyzed primary tube (350μm), which has a thickness 10 times greater than

168
the film thickness, therefore, the absolute error in measuring the layers thickness
was Δ=0.1%. The recipe N 8 (without colorants) used.
Table 4.3
Comparative results of set and actual layer thickness
Measuring layer thickness with a video system,
Gravimetric control set, Δ=0,5%
Δ=0,1%
№ А В С D Е А В С D Е
1 18,5 2,5 36,6 2,8 39,6 15,8 3,75 32,7 2,41 45,3
2 18,5 2,5 36,6 2,8 39,6 15,8 3,75 32,7 2,41 45,3
3 18,5 2,5 36,6 2,8 39,6 19,2 2,82 32,1 3,38 42,5
4 18,5 2,5 36,6 2,8 39,6 19,2 2,78 31,1 3,33 43,6
5 17,6 2,4 34,9 2,7 42,4 18,0 4,0 36,6 4,57 36,9
6 17,6 2,4 34,9 2,7 42,4 20,1 2,83 41,1 2,83 33,1
7 17,5 2,4 30,3 2,7 47,1 17,6 2,85 24,7 2,3 52,6
8 39,9 2,6 30,3 2,9 24,2 47,1 1,63 30 2,45 18,8
9 20,0 2,5 38,5 2,5 36,0 23,8 2,58 35,4 2,58 35,7
10 45,0 2,5 30,0 2,5 20,0 45,2 1,69 25,7 1,69 25,7
11 39,6 2,8 36,7 2,5 18,5 43,2 5,09 31,9 2,95 16,9
12 47,1 2,7 30,3 2,4 17,5 51,6 2,02 23,9 2,27 20,2
13 39,9 2,5 30,5 2,8 24,2 46,2 1,36 29,9 1,63 20,9
Average 27,6 2,52 34,1 2,68 33,1 29,4 2,86 31,4 2,68 33,7

Regression analysis of layer thicknesses, controlled by gravimetric method

and measured in the SVC system, shows that the correlation coefficient is 0.95, the
Fisher criterion calculated value Fр = 1411 is much higher than the table value Ft =
7.04 for the significance level α = 0.01. The number of experimental points is n =
65; k is the number of factors studied, k=1; degrees of freedom v1=n-df-1, 65-63-
1=1 and v2=df=63; therefore, there is a statistical relationship between the
parameters.
The data from Table 4.3 shows that the middle layer is in fact thinner by 3-
6% of that set by gravimetry, while the outer and inner layers, on the contrary, are
thicker by 0.5-5%.

169
 60

50

40
layer thickness, %

30 Gravimetry
(volumetric
dosing)
20 SVC video-
microskope

10

0
1 2 3 4 5 6 7 8 9 10111213 1 2 3 4 5 6 7 8 9 10111213 1 2 3 4 5 6 7 8 9 10111213
A C E
N experiment

Fig. 4.1. Comparison of data monitored by gravimetry and data measured on

the SVC system.

4.1.3 Comparative analysis of data from the gravimetric control system and
the layer distribution in the die
To clarify the conclusions from the previous experiment, the distribution of
the layer in the die was studied, that is, for one cut, the layers thickness was
measured in a circle in different sections. The primary tube was 350 microns thick.
The layers B, C, D were measured together because visually the adhesive looks
more like polyethylene, and the border with polyamide is clearer.

170
 Table 4.4
Technological modes of extrusion when made a sample according to recipe
No. 8 (colorless)
Parameter A B C D E Summ
N, rpm 49 19 113 19 44
Q, kg/h 19,9 1,1 17 1,1 11,1 50,2
Q/N, kg/h rpm 0,406 0,058 0,150 0,058 0,252
Percent, % 36 2,5 39 2,5 20 100
ρ, g/sm3 1,14 0,9 0,9 0,9 1,14
I, А 27 2,4 15 2,1 8,1

Table 4.5
Summary data by layer distribution
Recipe number 8 colorless Layer
Parameter А В+С+D Е
Structure set by gravimetry,% 36,0 44,0 20,0
Output, kg/h 19,9 19,2 11,1
Structure, measurement on a video system, based on
the results of 7 measurements on one section,% 37,3±0,78 41,4±4,38 21,3±4,16

Table 4.6
Summary data by layer distribution
Recipe number 1 in layer C brown colorant
10%. Layer
Parameter А В+С+D Е
Structure set by gravimetry,% 45,0 25,0 30,0
Output, kg/h 12,7 5,6 8,4
Structure, measurement on a video system, based on
the results of 3 measurements on one section,%
46,0±1,4 22,4±1,7 31,6±0,5

The layer thickness deviation from the average can be considered

satisfactory, since modern coextrusion dies have a deviation from the total
thickness for the range of ± 2S no more than 7% and if 7% is more then 4µm, this
deviation is normalized to ± 4µm (according to the materials of Macro, Canada).

171
 The data in Tables 4.5 and 4.6 show that, as in the second experiment, the
thickness of the middle layer is 2.6% less than that set in gravimetry, respectively,
the outer layers are the same thicker.

0,035
E D B
0,03
C
0,025
A

0,02
V, m/s

0,015
C
A
0,01
E D B

0,005

0
0 10 20 30 40 50 60 70 80 90 100
Layer thickness, %

Fig. 4.2 Diagram of multi-layer flow velocities calculated from experimental

results
0,035

А
0,03
В+С+D
0,025
E

0,02
V, m/s

0,015

B+C+D
0,01
E A
0,005

0
0 10 20 30 40 50 60 70 80 90 100
layer thickness, %

Fig. 4.3. Diagram of multi-layer flow velocities obtained on the basis of

experimental data, layers B, C, D are combined into one layer

172
 Typical coextrusion Layer The structure Extruder The
parameters and the measured in output, structure set
resulting multilayer the photo, kg/h in
structure. % gravimetry,
%
1 25,8 5,5 20
2 3,5 0,5 2,5
3 34,3 8,4 38,5
4 3,0 0,5 3,0
5 33,3 9,8 36

Fig. 4.4. The structure of a multilayer material and technological parameters

of its production.
The velocity diagrams analysis (Fig. 4.3, 4.4) and the study of sections using
a video control system (Fig. 4.5, 4.6, 4.7) show that during coextrusion, the flow
has a cork character, in the results of melt sliding on the die channel surface
formed wall layer with the thickness of 0.5-8% . That is, the outer and inner layers
have, as it were, a two-layer structure.
The structure 5 layer Layer Q Gravimetric
material kg/h structure set
(PA/TIE/LDPE/TIE/PA).
Thickness 350 micron
PA wall layer W2 3,0%
1 9,5 18,5%
РА outer layer 16,1%
Tie layer 2,8% 2 1,02 2,5%
LDPE Middle layer 31,1%
3 14,9 36,6%
Tie layer 3,3% 4 1,14 2,8%
PA inner layer 40%
5 22,95 39,6%
PA wall layer W2 3,6%

Fig. 4.5. Analytical description of a typical multilayer structure, above, you

can see the touch with a ballpoint pen.
The corky flow model assumes that transverse vibrations arise in the outer
and inner layers in the zone of melt contact with the channel surface. Perhaps this

173
effect (during flow) leads to further surface layer transcrystallinity, when
macromolecules line up perpendicular to the surface.

174
175
176
4.2 Comparative analysis of methods for dosing the melt.

There are two methods for the manufacture of a given multilayer structure
and, accordingly, for dosing the melt during coextrusion (Fig.4.8):
• gravimetric dosing by measuring and controlling the output of raw
materials Q = f(ΔF) from the extruder hopper and corresponding control of the
extruder screw speed Ne;
• volumetric dosing with a gear pump, the layer thickness is provide by
controlling the rotation speed of the corresponding gear pump Np, while the
extruder provide constant pressure P2 by controlling the screw rotation speed Ne.

Fig. 4.8. Diagram of methods for dosing melt during coextrusion

It is believed that the melt pump limitation is an increase the polymer

degradation. The melt pump advantages include, first of all, a practically stable
output that does not depend on the melt viscosity.
Practical observations and a comparative analysis of the two dosing methods
show that the control productivity and, accordingly, the layer thickness is
practically the same for both systems.
Table 4.7 shows observations of two extruders, screw diameter 30mm,
operating in the same seven-layer coextrusion unit, but having a different method
of dosing the melt. In extruder No.1, dosing with the use of a melt pump, extruder
177
No.1 is also equipped with a weighing hopper for measuring the consumption of
raw materials, but the information on the consumption is for reference only, and
the dosage is controlled by the melt pump. Extruder No.2 has gravimetric dosing.
General structure PA/PA/PA/Tie/LDPE/Tie/PA layer numbers and,
accordingly, extruders from outer to inner 1///7, the percentage of layers is
10/10/30/5/25/5/15. Table 4.7 shows productivity and pressure for extruders No.1
and No.2, the observation period is 1 hour.
Table 4.7
Comparative characteristics of melt dosing methods.
Pressure Р3, Output, Melt temperature ,
0
Bar kg/h С
Equipment min max min max min max
Extruder №1 with melt pump 217,6 220,9 3,03 3,38 259,3 259,6
Extruder №2 gravimetrical
control 219,5 222,5 4,6 5,16 260,3 260,7

The data shows that the three main indicators of the dosing process are
comparable for both extruders.
Five-layer coextrusion machine observations for the PA/Tie/LDPE/Tie/PA
structure, the study were made for adhesive feed extruders No.2 and No.4. But
there is no weighing hopper for extruder No.2 equipped with a melt pump
therefore output data are not shown (table 4.8). Extruder No.4 controls the set
pressure P2 = 100Bar by adjusting the screw speed. The observation period is
0.5hours.

178
 Table 4.8
Comparative characteristics of melt dosing methods.
Pressure, extruder-melt pump-die, Bar
Melt temperature, 0С
Equipment P1 P2 P3
min max min max min max min max
Extruder №2 with
gravimetrical control 289 290 - - 274 276 225,2 225,4
Nе=24,7rpm
Extruder №4 with melt
pump 112 116 99,9 100,1 167 169 222,7 222,9
Nе=22,0rpm, Nр=5,3rpm

Table 4.9
Comparative characteristics of melt dosing methods.
Pressure, Extruder-Melt pump-Die, Bar
Melt temperature, 0С
Period observation 2h P1 P2 P3
min max min max min max min max
Extruder №2 with
gravimetrical control 299 301 - - 283 286 223,6 224,8
Nе=24,7rpm
Extruder №4 with melt
pump 132 138 99,9 100,1 170 174 216,4 217,1
Nе=23,0rpm Nр=5,4rpm

The data in tables 4.8, 4.9 shows almost the similar stability of the pressure
in the die and the melt temperature, as a consequence the extruder productivity. So,
from the point of view of analyzing the dosing process stability, it makes no
difference which system to use: gravimetric or volumetric.
It seems that it makes little sense to complicate the design and install an
extra module. But practical observations show that the use of the melt extruder-
pump system is, first of all, the most optimal in the conditions of multi-product,

179
one-off production, when often (on average 1 time per shift) product formulation
and/or process parameters changes.
It is common knowledge that an extruder is a connection of two pumps.
Therefore, when changing the recipe or productivity, it is necessary to select the
optimal temperature profile. It is also important to take into account the back
pressure in the die, so that there is no significant increase in "backflow", which
causes overheating of the melt due to an increase in the forces of internal friction.
The use of the extruder-melt-pump system separates the tasks of preparing
the melt and feeding it into the die. The extruder operates with a stable outlet
pressure, the pressure is small (less than 120Bar), therefore the “counterflow” of is
stable and small. That is, the main extruder task is to provide melting and supply of
the melt with low pressure. At the same time, automatic control of the screw speed
within ± 3 rpm, to stabilize the pressure at the pump inlet, does not lead to
pulsation of the melt, because the pump equalizes the output curve. It should be
noted that no increase in the melt degradation take place in the pump. In any case,
the author has repeatedly observed just the opposite effect: during the extrusion of
thermosensitive polymers, the technological process is more difficult to control
when there is no melt pump. It is likely that the main reason is the effect of back
That is, the melt pump lets it to operate at a low and stable back pressure, which in
turn allows you to select temperatures and optimize the polymer flow in the
extruder.
It should be noted that we are talking about comparing the technological
process stability over a fairly long time from a week to a month. If you try to
compare the processes even for several hours, days (after cleaning the extruder and
the die), the difference will not be noticeable. But when batches of raw materials,
operators change, melt filters are replaced, changeover are made according to the
nomenclature, repairs are carried out on the line, the line is periodically in a
stopped state (when the extruder is at low speed) - the use of a melt pump reduces
waste, increases the stability of output and the stability of product quality.

180
 As shown in Section 3, the melt flow representation in the form of a corky
lets you to more accurately describe the rheological curve, calculate the multilayer
flow, and calculate the melt movement in the screw dosing zone. Stable and low
back pressure at the exit from the extruder lets to stabilize the wall viscosity and
the residence time in the extruder.
In the absence of a melt pump, an increase in back pressure (for example,
due to filter blocking) leads to increased wall friction, local melt overheating on
the screw (or barrel) surface and increased degradation, thus the degradation
process “like an avalanche” intensifies with increasing filter blocking.

Table 4.10
Comparative analysis of melt dosing methods
№ Gravimetric dosing with an extruder screw. Volumetric dosing with a melt pump.
п/п
1 2 3
1 Requires developed of extruder temperatures Temperature control is carried out
depending on the recipe and productivity. only when it is necessary to eliminate
non-melting or destruction of raw
materials.
2 Requires a wider temperature range across the Narrower temperature range across
extruder zones. extruder zones.
For example, for the extrusion of an LDPE For example, for extrusion of an
layer, the range can be 200-245C. LDPE layer for a similar range of
additives, the range is 220-240C.
3 Requires complex temperature profiles across It is enough to apply a flat
extruder zones. temperature profile along the extruder
zones
4 The pulsation of the melt feed is equal to the The pulsation of the melt is equal to
volume of the screw coil. the chamber volume formed by two
teeth (10-20 times less than the
volume of the screw coil)

181
 Continuation of table 4.10
1 2 3
5 Work in a narrower range of formulation Stable extrusion in the full range of the
viscosities. When working with polymer viscous-flow state, work in the
formulations with different viscosities, for widest possible range of viscosities.
example when using different colorants and
varying the percentage of their introduction
into the formulation, it is necessary to
optimize the extruder temperature profile
for each formulation.
6 More requiring to extruder wear. So the More requiring to pump wear. So the
extruder operates at a higher pressure, extruder creates little pressure, defects
imperfections on the screw surface, burned on the surface of the screw or barrel do
melt on the screw, can lead to unstable melt not lead to a decrease in the dosing
flow. quality of the extruder-pump system.
7 One melt pressure sensor is required. Requires three melt pressure sensors.
8 The average time of purging the extruder The average time of purging the
45mm (PA6 or LDPE) when changing color extruder 45mm (PA6 or LDPE) when
is 10min, the amount of waste is 5kg. changing color is 10min, the amount of
waste is 5kg.

Table 4.10 shows the practical results of observing the operation of two
dosing systems during coextrusion of the same five-layer structures with a wide
range of products.
Thus, the use of an extruder-pump system is preferable in a single
production type..

4.3 Study of changeovers by color (recipe).

Color transitions play a key role in changeover processes, so all equipment
modules are used (recipe preparation - extruder - secondary molding), the most
time-consuming and difficult to predict for the resulting waste.

182
 If the maximum number of changeovers in thickness and diameters can
reach 7 changeovers per shift, but a maximum of changeovers per shift is can be
planes in color (for lines with a output of 30-60 kg/h).
The initial data on the waste of raw materials for the color changes are
reflected in the extrusion equipment characteristics. For example, if the output is
100kg/h, the maximum purging time for new equipment is 15minutes, the loss of
raw materials for the changeover is 25kg. But this is an approximate value, because
it does not take into account the raw materials type and the gradual "clogging" of
the melt flow channels, which gradually increases the losses at the same
changeover, the operating personnel experience, the Maintenance and Repair
System in the factory.
The norms can be presented in the form of table 4.11, where the cells
indicate the loss of time or raw materials during the transition between all the
product colors, the index shows the transition direction (from which and to which
color the transition is going). It should be noted that the table is asymmetrical, that
is, there can be a significant difference between the transition from color No. 1 to
color No. 2 and the transition from color No. 2 to color No. 1, therefore, for each
ordered assortment, there is an optimal plan for their production.
Table 4.11
Typical table of losses (waste) during changeovers
Color Color №1 Color №2 Color №3
Color №1 0 Х12 Х13
Color №2 X21 0 X23
Color №3 X31 X32 0

Similar tables are developed for all colors and size of products into each
type. In a simplified accounting option, averaging over all transitions is possible,
but this also depends on the dispersion of the actual waste values from the average
and on the requirements of the set accounting and production planning system.
It should be noted that the actual waste, even for the same changeover, has a
fairly wide range of variation, for example, at a rate of X12 = 10kg, actual waste

183
can lie in the range of 6-14kg (depending on the wear of the equipment, personnel
experience, the previous quantity and complexity of different changeovers). For
the most difficult washing from a dark color (black, brown) to colorless, at a rate of
30kg, the actual waste can be up to 100kg. It is clear that such a significant
deviation from the norm has reasons and requires corrective action, but for the
production planning system, such a deviation leads to a significant decrease in the
accuracy of predicting the realization of a shift task and, as a consequence, to
disruptions in the timing of orders. Therefore, it is required to assess the realization
of the set waste standards every shift, analyze the causes of deviations, and develop
and carry out corrective actions to improve the accuracy of predicting the
realization of the set waste standards.

4.3.1 Investigation of the mineral filler effect and the ratio of melts viscosities
during color changeover
Changeover description:
• middle LDPE layer “C” replacement of the brown dye formulation with the
blue dye formulation;
• inner PA layer “E” replacement of a colorless layer with a white one.
The screw rotation speed is constant.
The time between samples No.1 and No.6 is 6 minutes.
Table 4.12
Technological modes of extrusion during the changeover
Parameter C (LDPE) E (PA6)
N, rpm 100 50
Q, kg/h 20 17
The melt 240 250
temperature, 0С

In the process of color changing, we observe (Fig.4.11) how a spiral-type die

with 8 distributors with a nominal diameter of 7 mm is washed out (Fig.3.1b).

184
 The process of washing out the middle layer (brown-blue transition) analysis
will be carried out on the basis of information on the rheology, recipe, and the
dynamics of each layer coloring.

100000
LDPE
15813-020

Braun dye
polybatch
10000 1340
Viscosity, Pa*s

Blue dye
polybatch
4021

1000 Yellow dye

2028Е

Gold dye
7797

100
0,10 1,00 10,00 100,00 1000,00
Shear rate, 1/s

Fig. 4.9. Rheological characteristics, (rheological curve was measurement on

a standard capillary D = 2.1mm, L = 8mm, the temperature 1500С).

We calculate the viscosity of the mixture using the equation [52]:

lg c  M1 lg k1  M 2 lg k 2
μс – viscosity of the mixture, μk1 – viscosity of component 1, μk2 – viscosity
of component2, M1 - mass fraction of component 1, M2 - mass fraction of
component 2.
Table 4.13
Rheological characteristics of components and mixtures of the middle layer.
Viscosity MFI (1500С, Percentage composition of
Component name when a shear 4,9kg), the middle layer (recipe)
rate is 10s-1 g/10min Braun Blue

185
LDPE 15813-020 8000 1,1 79% 76%
Braun dye Polybatch 1340 2500 7,9 21% -
Blue dye Polybatch 4021 1500 30,1 - 24%
Viscosity of mixture μс, Pa*s - - 6266 5353

Although in the standard parameters of masterbatches it is rarely possible to

find the MFI characteristic, but this characteristic is quite important for the
technological process. The standard MFI of a dye masterbatch can be considered
three to four times greater than the base polymer MFI. That is, for the example
under consideration, this would be a level of about 3-4 g/10min. But it can be seen
that the brown and especially the blue dye are much more fluid. Such low viscosity
values of dyes lead to the need for additional temperature control, which is usually
not difficult to adjust, but it still requires operator time, process control, and
sometimes additional waste.
Analysis of sections of a multilayer sleeve during purging (Fig. 4.10) shows
the following regularities: when a less viscous melt is fed into a die with a more
viscous melt, the flow is closer to shear, the melt gradually displaces the more
viscous melt from the die (washing out with blue - brown color). It can be
imagined that a high-viscosity melt, as it were, forms a narrower channel for a low-
viscosity melt, while itself adheres to the channel walls, so it is more difficult for a
low-viscosity melt to wash out a more viscous melt.

186
 № Structure photos Descriptions of purging
sample
The inner layer is unchanged.

Start changing the middle layer color.

1

Inner layer without noticeable color

changes.
The middle layer color has changed by
2
80%,

The inner layer is whitish (about 5%

white).
The middle color changed 90%, but the
3 appearance (see Figure 4.11) changed
30%.

The inner one is whitish (about 5%

white)
Medium color changed by 95%
4

Medium color changed by 99%

Inner color (about 90% white)
5

Inner layer color (about 90% white)

Middle layer color changed by 99%
6

Fig. 4.10. Coloring layers in the changeovers process when changing colors.

187
 № Photos of the sleeve appearance
sample

Fig. 4.11. The tube appearance during the color changeover. The sample
number Fig. 4.11 corresponds to the sample number Fig. 4.10

188
4.3.2 Inner layer process purging (from colorless to white)
Table 4.14
Inner layer recipes
Color PA6 PA6/66 Anti-block White dye super-
concentrate.
Colorless 87 10 3 -
White 65 10 - 25

The relative viscosity (in 96% H2SO4) of polyamides and the polyamide
base of additives is 3.3-3.8.
The white dye super-concentrate contains 60% TiO2, that is, the final
mixture is a highly filled composition characterized by a corky flow [52]. The
multilayer tube sections shows that during the purging process, at the all layer
thickness the highly filled composition gradually changes the layer color (from
colorless to white). That is, the mixture color change is take place in the extruder
where two colors are mixed and this change in the mixture is immediately visible
throughout the all layer thickness and therefore purging is faster. Mineral filler
(titanium dioxide) enhances the melt sliding, which leads to the cork nature of
replacing one layer with another. If we compare the changeover time between two
layers, then the brown→blue transition takes 1.5-2 times longer than the
colorless→white transition. Of course, it should be borne in mind that the white
layer is a substrate and the blue color is very deep and bright, therefore the overall
transition end is primarily determined by the blue color. Small stripes of the
transparent inner layer may simply not be noticeable, but nevertheless, a structure
photos shows that the flow and the replacement nature are different.

4.3.3 The color changeover investigation (from yellow to colorless) with

varying screw speed
Description of the transition:
• middle layer C - the yellow dye formulation replacement with a colorless
one;
189
 • inner layer E - the white layer replacement with a colorless one.
Table 4.15
Rheological characteristics of components and middle layer mixtures
Viscosity when The middle layer composition
MFI, g/10min
Component name a shear rate is (recipe)
(1500С; 4,9kg)
10s-1 Yellow Colorless
LDPE 15813-020 8000 1,1 75% 100%
Yellow dye 2028E 2000 6,69 25% -
Viscosity of
- - 5656 8000
mixture μс, Pa*s

Table 4.16
Technological modes of extruders during the changeover
Time
Parameters A C E
h - min
N, rpm 50 68 33
10-35 I, А 22 13 6
Q/N, kg/rpm 0,43 0,17 0,24
N, rpm 25 92 90
10-55 I, А 13 13 10
Q/N, кg/rpm 0,37 0,16 0,25
N, rpm 25 80 100
10-59 I, А 14 14 14
Q/N, кg/rpm 0,38 0,16 0,25
N, rpm 54 75 39
11-23 I, А 25 12 7,1
Q/N, кg/rpm 0,43 0,16 0,25
The structure in the
№
process of color Time А С Е Notes
sample
transition
0 - 10-35 50 68 33 Standard screw speeds
Start of purging, intense yellow
color of the middle layer and
1 10-37 30 92 70
white of the inner layer are
visible

Discoloration of the middle

layer (yellow changes to
2 10-41 25 92 80 colorless) and discoloration of
the inner layer (white changes
to colorless)

190
 The yellow is still visible in the
layer.
3 10-42 25 92 80
A white stripe is visible in layer
E

Yellow stripes are visible

4 10-45 25 92 90
(yellow dye trace)

White stripes are visible, also

5 10-47 25 92 90
yellow trace.

White is still visible.

6 10-50 25 92 90

Almost invisible white color,

7 11-02 25 80 100
whiteness of the inner layer.

Almost transparent structure,

8 11-16 53 75 48
start of set blowing process.

Fig. 4.12. Changing the layers color during the transition (the time from 11-
16 to 11-23 setting up blow molding)
The multilayer structure is investigated in relation to process speed, time and
output.

191
 120

100

80
N, rpm

А
60

40
Е

20

0
0 2 4 5 8 10 13 25 30 35 40
The time from starting purging procedure, min

Fig. 4.13. Diagram of the screws control in the changeovers process (from
yellow to colorless)

The time from 10-34 to 10-45 The time from 10-45 to 10-53

Fig. 4.14. The tube appearance during the changeover, on the samples
indicate the time and the screws rotation speed

192
 The time from 10-53 to 11-04 The time from 11-04 to 11-16

Fig. 4.15. The tube appearance during the changeover, on the samples
indicate the time and the screws rotation speed
Table 4.17
The relationship between the waste and the percentage of color change in
layer C
Time, h- Cumulative time, Percentage of The waste Notes
min min color residues cumulative, kg
10-37 0 100 0 Purging ~97%
dye
10-41 4 50 0,84
10-42 5 10 1,05
10-45 8 3 1,68 Purging near
wall layer ~3%
10-47 10 2 2,1
10-50 13 1 2,73
11-02 25 1 5,25
11-16 39 0 8,19 -

In fig. 4.12 and 4.14, the yellow layer is displaced by the colorless layer,
which has a higher viscosity.
For the changeover from yellow to colorless, it is characteristic that the
yellow recipe is washed out with a more viscous colorless recipe, therefore, the
cork character of the washing is observed.
For washing from white to colorless, there are two factors that complicate
washing, firstly, there is no mineral filler in the colorless recipe and its flow is

193
closer to shear flow, which worsens the conditions for replacing the white layer;
secondly, washing with a colorless composition requires the highest quality
washing, which increases time and waste (fig. 4.15). So, as a result of research in
production conditions, it has been established that the most difficult washing
during the transition from a colored film to a colorless one occurs in three stages.
At the first stage, the color disappears by 90% during 10 minutes. The second stage
takes a long time - 30 minutes. In this case, the color practically disappears, the
film is transparent, but some degree of coloration is observed in the mass of the
film (roll, reel). The third stage is complete washing, when a completely colorless
film is extruded (Table 4.18).

Table 4.18
Purging observation results for coextrusion line changeover to colorless
formulation
Color
Stages of The degree of The time of The total
matching
transition color change,% purging, min time, min
quality level
Basic 0 – 90 10-15 10-15 Low
Additional 90 – 99 30-40 40-55 Good
Final 99 – 100 30-40 70-95 Excellent

194
 120

100

Percent of ending changeover, % 80

60

40

20

0
0 10 20 30 40 50 60
Time, min

The standard technology The technology with increase wall slip

Fig 4.16. The recipe replacing is depending on the slip on the channel wall.

In fig. 4.16 shows the dynamics of color change for different melt flow
conditions because of the processing additives use.

4.3.4 Investigation of the color transition (from gold to colorless) with varying
screw speed
Description of the transition:
• middle layer replacement of the Gold dye formulation with a Colorless
one;
• inner layer replacement of the White layer with a Colorless one.
Table 4.19
Rheological characteristics of components and mixtures of the middle layer
Viscosity Percentage composition of
MFI (1500С,
Component name when a shear the middle layer (recipe)
4,9kg), g/10min
rate is 10s-1 Gold Colorless
LDPE 15813-020 8000 1,1 80% 100%
Dye GOLD 7797 2700 3,95 20% -
Viscosity of mixture μс,
- - 6437 8000
Pa*s

195
 № Photo of the five
Е С А Notes
sapmle layer structure

0 - 25 40 50 Standard screw speeds

Increase the purging speed of the

1 25 60 20
gold middle layer

2 25 60 20 Middle layer purging

3 25 60 20 Middle layer purging

4 20 80 15 Middle layer purging

5 20 80 15 Middle layer purging

Middle layer purging, increase

6 40 80 15
washing of the inner layer

7 80 40 15 Inner layer purging

8 80 40 15 Inner layer purging

9 80 40 10 Inner layer purging

10 40 80 10 Middle layer purging

11 25 40 50 Setting the standard screw speed

Fig. 4.17. Changing the layers color when going from gold to colorless

196
 90

80

70

60

50
N, rpm

Е
40
С
30
А
20

10

0
0 2 4 6 8 10 12 14 16 18 20 22
The time from starting purging procedure, min

Fig. 4.18. Speed rotation control of the screw for changing the color from
gold to colorless (according to Fig.4.17).

In Figure 4.19, the gold-colored layer is replaced by a colorless one, which

has a higher viscosity. The flow nature is similar to the previous study, since the
golden color recipe is washed out by a more viscous colorless recipe, therefore, the
cork character of the washing is observed. Separately, it is necessary to describe
the problems of washing out "stripes" (samples No. 7-10). Because of channel
wear or gradual melt degradation, stagnant zones are formed in the coextrusion die,
therefore, the flow rate decreases in this place and the melt of the current color
accumulates. Therefore, to simplify painting the previous color, it is advisable to
build the series of transitions setting to the principle from light to dark (from white
to black), so that when the lighter layer is washed out, it would be easier for the
dark one to paint over it.

197
 Samples №1-6

Samples №7-11

Fig. 4.19. The appearance of the tube when the color changes from gold to
colorless; the sample number corresponds to the photograph number in Fig. 4.17.
198
 Also important to select the optimal geometry of the die distribution
channels so that the channels volume has the minimum required dimensions to
ensure the highest possible flow rates (see Section No. 3). The following practical
observation is interesting, when the coextrusion line successively produced various
intensely colored films (containing 15-25% deep dye super-concentrate in separate
layers), and then switched to a long-term production of a colorless film, so the line,
like "remembers" the previous colors in reverse order. Coloring is very weak, it is
visible only "all at all", that is, in a roll, when many turns of the film are connected
on each other, some film areas do not have a visible color. Moreover, it seems that
the purging on a colorless film has already ended, but the coloration take place
after a few hours of work on a colorless recipe. This indicates that the wall layer
may not be washed out immediately; it is also a signal of significant wear on the
inner surface of the extruder and the die.

4.4 Specificity of planning changeovers and orders queue

According to studies [82] of the functioning of flexible production systems
(FPS), the determinism or stochasticity of the queuing system (QS) is influenced
by:
1. The coefficient consolidation of operations.
2. The load factor of the serving subsystems.
3. The method of acceptance orders for production.
Analysis of the operating conditions of modern multi-product co-extrusion
production shows that such a production system should be classified as stochastic
queuing systems, due to the inconsistency of incoming orders for production, there
is no rhythm in the volume and types of incoming orders.
The following factors are specific to the co-extrusion process:
1. The asymmetry of the tables of transitions between kinds, colors, types of
products.

199
 2. Transition not only takes time and reduces productivity, but also results in
waste.
The presence of the first factor leads to the fact that there is always one
optimal order production queue. The presence of the second factor leads to the fact
that there is a minimum volume for one product range when setting it up in the
production plan, and the minimum order volume for loading one production line,
because of the waste grows intensively when the queue decreases below a certain
critical value. This dependence for a production line with a capacity of up to
80kg/h, for a total possible number of product standard sizes 25500 (see Table 1.9)
is shown in Figure 4.19.

16

14

12

10
Waste, %

0
0 5 10 15 20 25 30 35
Orders queue, days
Waste min, % Waste max, %

Fig. 4.20. Typical dependence of waste level on order queue in multi-

product coextrusion production [83].

It should be noted that 40-50% of all kinds of incoming orders are 3-5
popular diameters and 5-8 colors of products, that is, 15-40 standard sizes, which is
less than 1% of all possible standard sizes of products.

200
 At the same time, even a little increase in waste, for example, from 4% to
8%, leads to a significant load of operators for additional work on line setup, waste
cleaning and sorting, and write of production reports. Thus, the time for increasing
the process stability and control the line, improving the quality characteristics of
products during the shift is reduced.
Therefore, the most rational planning strategy is to add standard sizes to the
incoming orders in the amount of 20-25% of the order queue, to reduce waste, for
increase the utilization rate of production capacities and the formation of
warehouse stocks to reduce the lead time for the most popular product positions.
The popular positions can change, therefore, a monthly analysis is required and it
is possible to revise the list of standard sizes that are manufactured without the
presence of specific orders for products.
Now let's analyze the factors influencing the formation period of the order
queue. It is clear that the longer the period for which orders are collected, the more
likely it is that similar colors, types and calibers will arrive, and there are more
opportunities to group and optimize the queue (minimizing waste). But the
limitation is the order lead time, which is formed by the market, since the
maximum lead time for any order is the queue formation period multiplied by two.
And here a very difficult question arises of how to compare (compare) your
products: from point of view of quality, number of types and cost price with a
competitor. Without such a comparison, it is impossible to compare the terms, for
example, you can produce 10 colors and 10 diameters and have them constantly
available in the warehouse, thus reducing the time until the time of transportation.
Another option is to work on specific orders, having thousands of product types in
the assortment and satisfying customers as much as possible in the range of
products, but in this case, the terms for individual types of products can increase
significantly, the availability of an assortment of raw materials and the timing of its
delivery, the operability and availability of all equipment and personnel begin to
influence.

201
 4.4.1 Analysis of the requirements for an order when placing it in the queue
The next planning task is to analyze each order in the queue for its cost to
assess the possibility of its production (into the current queue) and analyze waste in
the context of each client.
So, the order queue contains the terms and the level of losses for it
manufacturing.
Table 4.20
Queue of orders in the rang of their coming (unoptimized)
The coming date Quantity, Changeover waste, Changeover
(order number) Type km Weight, kg kg waste, %
10 Color №1 50 500 10 2,0
15 Color №3 1 10 20 66,7
20 Color№2 1 10 30 75,0
25 Color №1 50 500 20 3,8
- SUMM 102 1020 80 7,3

After searching options for manufacturing orders (Table 4.22). The queue is
grouped and optimized, and then each order is analyzed.
Table 4.21
Waste norms for transitions between film colors
→ Color №1 Color №2 Color №3
Color №1 0 10 20
Color №2 20 0 10
Color №3 10 30 0

Table 4.22
Optimized order queue
The coming date Quantity, Changeover Changeover
(order number) Type km Weight, kg waste, kg waste, %
10 Color№1 50 500 10 2,0
25 Color№1 50 500 0 0,0
20 Color№2 1 10 10 50,0
15 Color №3 1 10 10 50,0
- Summ 102 1020 30 2,9

The following options for analyzing the order queue are possible, if the total
percentage of waste exceeds the standard, it is necessary to remove from the queue

202
orders that have the highest percentage of waste (for example, above 20%) until
the entire queue has an acceptable level of losses (about 4%). But even if the queue
has a low level of waste (for example, 2.9% as in Table 4.23), this does not mean
that it is optimal, since it contains two very large orders (50 km each) same
standard size and two very small orders (1 km each). As a result, significant losses
on small orders (waste 50%) are compensated by savings on large orders (waste
2%). The question arises as to how correct such a production plan is. For
production, in general, the final figure of losses in the whole queue is important,
but if the production of small orders depends on the entry of large orders, then
small customers will not always be able to receive their orders, or it is difficult to
plan the timing of their production. It is also necessary to monitor when these small
orders become in a shift task, since this shift will have an increased amount of
waste and an increased workload of personnel, it may be necessary to strengthen
such a shift with more experienced operators. Another variant of a heterogeneous
queue arise, when one client at the same time ordered both large and small orders
in the range. Such a complex order must be analyzed separately for waste and for
the lead time of all sizes for this client. It is difficult to establish any rules here,
but the main criterion will be the utilization of production capacities, the total
volume of open orders, if there are more of them, then it is easier to refuse a small
order and vice versa.

4.4.2 Requirement for the series of production of films of different colors

It should be noted the technological requirement of building a queue from
light to dark colors, then purging to colorless and then again from light to dark, etc.
As already indicated (Tables 4.17, 4.18), the flow nature affects the fact that the
color remnants can be washed out most part of the time that spent on the
changeover. Therefore, if the new color is more intense or darker, then even with
the previous color remnants, the product will have a normal appearance (color) for
commercial use. This is clearly shown in Fig. 4.20.

203
№ Photos of colored films Notes
Original films / percentage
of dye in the film:
1-blue / 1%
2-green / 2%
3-white / 20%
1 4-black / 3%

Transitions:
1 Black-green
2 White-blue
Black is strongly translucent
through weakly colored
2 green. Intense white is
noticeably visible through
the blue film.

Transitions:
1 Blue-white
2. Green-black
A more preferable
sequence, since the original
3 (lower) color is almost
invisible, black colors more
intensely than white.

Fig. 4.21. Simulation of a different sequence of transitions by color

204
№ Photos of colored films Notes
Transitions:
1 - blue-green
2- white-black
Weakly colored blue
strongly changes the green
4 film color.
White practically does not
show through the black
color.

Transitions:
1 Blue-black
2 Green-black
3 White-black
Black dyes any color well.
5

Transitions:
1 Blue-white
2 Green-white
3 Black-white
White quite intensely colors
6 blue and green, but black is
translucent, contrary the
high content of dye in the
white film.

Fig. 4.22. Simulation of a different sequence of transitions by color

205
 Analysis of Fig. 4.21, 4.22 shows that the rational sequence of color
transitions for the considered colored films:
1. Blue - green - white - black
2. Green-blue-white-black
Naturally, when one standard size is made in a sufficiently large volume and
the waste for the transition is reduced to the required level, the sequence of color
may not be followed. For example, with the standard for the transition of 30 kg
colorless film, with an order volume of 30,000 kg, the waste is reduced to 0.1%
and the question becomes more important - will other customers suffer due to the
fact that production facilities are loaded with one order of one client? Since with an
average productivity of 50 kg / h, such an order will be fulfilled for 25 days.
Therefore, if the factory has dozens of customers and the average order
production time for them is 20-30 days, that is, the average volume of one order of
one standard size of film is 1000 kg, then it is necessary to develop rules for
working with very large orders.

4.5 Conclusions on the fourth section:

1. Modern coextrusion lines equipped with gravimetric dosing systems allow
investigating the parameters of multilayer melt flow for a wide range of polymer
materials.
2. Investigation of multilayer structures and modes of their production shows
that there is an almost "corky" character of the multilayer flow. The deviation from
the "cork" character shows the redistribution of the set and the actual layer
thickness. The thickness of the outer and inner layers can be 0.5-3% higher than
that setting by gravimetry.
3. Low-viscosity wall layer W2 has a stable thickness for a set recipe and
modes of its production. The tendency of an increase in the wall layer thickness
with an increase in the thickness (productivity) of the corresponding layer is fined.

206
 4. Improvement of the coextrusion technology, especially in the conditions
of single and small-scale production, requires the development of multilayer flow
models taking into account the wall slip.
5. Methods of planning orders in extrusion processes in a small-scale
production, based on groupings by color, leads to a 3-5-time reduction in waste.
This needs the development of limitations on the volume of one order, production
time, waste level, quality level, number of types.
6. A background for the functioning of a single extrusion production is the
development of individual approaches to each client, including the main
production indicators - the acceptable level of waste, nuances of quality, minimum
order volume.

Conclusion

Representation of melt movement processes in the form of a cork sliding on

the surface, allowed for the first time to obtain a full rheological curve, to explain
the effect of surface crushing (or “sharkskin”) and the technological method of a
variable melt feed rate during purging of the extrusion equipment. In the further
development of a full rheological curve model, it is necessary to take into account
the polymer molecular characteristics, to investigate the interaction of the low-
viscosity and the near-wall layer, and the interaction of the near-wall layer with the
channels surface, to find the dependence of the die coating material on the flow
rate of the near-wall melt layer.
The developed model of the melt movement in the extruder, taking into
account the interaction (viscous friction) on the walls of the screw and barrel, gives
a new understanding of the process and shows ways to improve the extruder. For
example, it is interesting to investigate the Helibar extruder system with the melt
gear pump. At the same time, the Helibar extruder can be upgraded by reducing the
L/D ratio and simplifying the screw design. Such a system should theoretically

207
operate at low pressures in the extruder and develop a high specific productivity,
quickly and easily purged when changing recipes.
The management of a modern flexible manufacturing enterprise should be
built at least using a Materials Requirements Planning (MRP) system, the basic
principles of which are JIT (Just In Time) and Kan Ban (On time to produce). In
modern single co-extrusion production, it becomes an important task to take into
account the requirements of each client, the production of individual configurations
of goods "to order", that is, it is necessary to implement the so-called planning
systems CSRP (customer synchronized resource planning, resource planning
synchronized with the client). An important element of such a system is an
individual technological process developed for the client. The technology
(technological modes, raw materials, quality requirements, etc.) must be formed
when an order is opened and transferred to production, reflected in a shift task, and
controlled before the order is shipped.
Modern co-extrusion production is characterized by a wide variety of types
(ranges) of the manufactured flexible multilayer packaging polymer materials, in
some cases it may be small-scale or single production type.

208
 References

1. Grimm, A. (2012.06.14). Vzglyad BASF na upakovochnye materialy. Doklad

na 3-m plenochnom simpoziume, Sankt-Peterburg.
2. Lu, B., Sudre, G., Serghei, A., Maazouz, A. (2020). Unveiling the Effects of In
Situ Layer–Layer Interfacial Reaction in Multilayer Polymer Films via
Multilayered Assembly: From Microlayers to Nanolayers. Macromolecular
Materials and Engineering. DOI: 10.1002/mame.202000076.
3. Polimernye plenki: materialy, tekhnologii i naznachenie, poslednie tendencii
rynka. Specialnyj vypusk "Vse o plenkah". (2008). – Unipack.Ru:
http://www.unipack.ru/paper/Plenki_Unipack_Ru2008.pdf Last accessed:
25.07.2021
4. Dyadichev, V.V. (2003). Soekstruzionnaya obrabotka vtorichnyh polimernyh
materialov (teoriya, tekhnologiya, oborudovanie). Dissertaciya doktora
tekhnicheskih nauk, Lugansk: publ. SNU im. V. Dalia.
5. Admer, fields of application. (2021). Official website MITSUI CHEMICALS
EUROPE GMBH. Available at: https://admer.eu/fields-of-
application/packaging/flexible-packaging Last accessed: 25.07.2021
6. Levanichev, V. V. (2008, May). Kompleksnyj podhod k sozdaniyu obolochek
dlya kolbasnyh izdelij. Zhurnal “Myasnaya industriya”, 44-45.
7. Ulshin, V. A., Levanichev, V.V., Tereshchenko, T.M. (2010) Analiz processa
perenaladki soekstruzionnogo oborudovaniya s celyu minimizacii poter
vremeni. Lugansk: Visnyk SNU im. V. Dalia. 9(151), 43-49.
8. Ulshin, V.A., Levanichev, V.V., Tereshchenko, T.M., Levanichev, A.V. (2012).
Eksperimentalnye issledovanie vliyaniya kachestva smesheniya na
harakteristiki gotovogo izdeliya. Lugansk: Visnyk SNU im. V.Dalia. 9(180),
194-198.
9. Ulshin, V.A., Levanichev, V.V., Tereshchenko, T.M. (2011). Issledovanie
processa techeniya rasplava polimera v kanalah soekstruzionnogo
oborudovaniya. Lugansk: Visnyk SNU im. V.Dalia. 3(157), 80-86.
209
10. Foederer, Beth. (2010). Efficient extruder and slot-die purging. The official
website of the Society of Plastics engineers. Available at:
http://www.4spepro.org/view.php?source=003231-2010-11-03
11.Disco purge procedure for extrusion coaters (2010). The official website of the
company Du Pont. Available at:
http://www2.dupont.com/Nucrel/en_US/assets/downloads/disco_purge.pdf
12.Naglyadnaya soekstruziya. Ekstruziya tekhnologicheskie novinki. (2010).
Zhurnal Plastiks, 7(89), 34.
13.Paetzold, R., Krause, U. (2005). Assignee: Windmoeller & Hoelscher. Pat. No.
US6875382 В2. Process to purge polymer or plastic melt guiding parts of film
extrusion systems. Appl. No.: 09/954216; prior. 18.09.2001; publ. 5.04.2005.
14.Ertle, R. T., Ertle R. J. (1995). Assignee: Cylatec Corp., Pompton Plains, N.J.
Pat. No. US005424012A. Method for purging thermoplastic extruders. Appl.
No.: 179,978; prior. 11.01.1994; publ. 13.06.1995.
15.Shida, M., Grove, L. (2011). Assignee: MSI Technology LLC., Pat. No.
US008080506B2. Reactive purge compound for polymer purging. Appl. No.:
12/502,556; prior. 14.07.2009; publ. 20.12.2011.
16.Koch, U., Klenz, R., Friel, P., Gareiss, B. (2004). Assignee: BASF, Pat. No.
US006673759B. CLEANING MATERIAL FOR EXTRUDERS. Appl. No.:
09/868,096; prior. 14.06.2001; publ. 6.01.2004.
17.Nitzsche, N. E. (2004). Assignee: Polyone Corporation, Pat. No.
US006916770B2 Multi-functional color concentrate compositions. Appl. №:
10/150, 305; prior. 14.06.2001; publ. 6.01.2004.
18. Bailey, F. W. (1990). Assignee: Phillips Petroleum Company. Pat. No.
US4954545. Process for cleaning polymer processing equipment. Appl. No.:
283350; prior. 12.12.1988; publ. 4.09.1990.
19. Chandraker, Vinay Kumar., Oda, Hidemasa. (2000). Assignee: EVAL
Company of America, Pat. No. US6060445A. Polymer cleaning compositions
and methods. Appl. No.: 08/829401 prior. 31.03.1997, publ. 9.05.2000.

210
20. Progress v ekstruzii na NPE. (2007). Oficialnyj sajt. Available at:
http://www.polymery.ru/blog.php?id_company=54&n_id=1965&category=ite
m&page=91 Last accessed: 27.07.2021.
21. Ekstruziya bez mertvyh zon. (2010). Ekstruziya tekhnologicheskie novinki.
Zhurnal Plastiks 7(89), 33.
22.Mizuguchi, Hideki., Ishida, Masaharu. (2000). Assignee: The Japan Steel
Works Ltd, Pat. No. US006019916A. Manufacturing method of different color
pellets and manufacturing apparatus therefore. Appl. No.: 08/987,423; prior.
09.12.1997; publ. 01.02.2000
23.Eloo, M. (2012). Assignee: Gala Industries, Inc., Pat. No US008187512B2.
Method and device for granulating plastics and/or polymers. Appl. No -
I 11/884462; prior.15.02.2006; publ. 29.05.2012
24.Bemis, P. F., Albrecht, L. C., Schick S., F. (1996). Assignee: Bemis
Manufacturing Company, Pat No. US5486327. Apparatus and method for
injecting or extruding colored plastic. Appl. No.: 184,826; prior. 21.01.1994;
publ. 23.01.1996.
25.Yoshida, M., Mizuguchi, H., Kobayashi, N., Ishida, M. (1999). Assignee: The
Japan Steel Works, Ltd., Pat. No. US005879720A. GRANULATING DEVICE
FOR THERMOPLASTIC RESIN. Appl . No.: 20,383; prior. 09.02.1998; publ.
09.03.1999.
26.Mahler, F., Baier, K., Heineker, M., Lybovski, Y. (2008). Assignee: Khosokava
ALPIN Aktsiienhezellshaft. Pat. No. UA81589C2. Ekstruziina holivka dla
vyrobnytstva rozduvnoi rukavnoi plivky. MPK: B29C 47/20. No. a200702503;
declareted: 17.08.2005; publ. 10.01.2008.
27.Agapkin V.M. Truboprovodnyj transport mazuta. Vebsajt «NEFT'-GAZ
elektronnaya biblioteka». Available at: http://www.dobi.oglib.ru/bgl/4477/53.html
28.Sivetskyi, V. I., Sokolskyi O. L ., Sivetskyi A. V. (2006). Pat. No. UA18494U.
Sposib ekstruzii polimernykh materialiv. Natsionalnyi Tekhnichnyi Universytet
Ukrainy "Kyivskyi Politekhnichnyi Instytut" MPK: B29C 47/00, No.
u200604717; declareted: 27.04.2006; published: 15.11.2006; bul. № 11, 2006.
211
29.Koncentraty ekstruzionnyh (processingovyh) dobavok “Basko” P0025. (2013).
Oficialnyj sajt OOO NPF «Bars-2». Available at:
http://bars2.com/colors/marks/p0025/.

30.On Cap Additives for Blow Molding. (2013). The official website of PolyOne
Plastic Compounds . Available at: http://www.polyone.com/en-
us/products/colorantadditive/Pages/default.aspx
31.Screw coatings (2016). The official website company Bernex Bimetall AG.
Available at: http://www.bernexgroup.com/mm/coating.pdf
32.CrN PVD high-perfomance coating(2016). The official website company
Oerlikon Metco, Switzerland . Available at
http://www.oerlikon.com/metco/en/products-services/coating-services/pvd-
coatings/pvd-coatings-processes
33.Rauvendaal, K. (2008). Ekstruziya polimerov. Perevod s anglijskogo pod red.
Malkina, A.J. St. Petersburg: Professiya, 768.
34.Tadmor, Z., Gogos, C. (1984). Teoreticheskie osnovy pererabotki polimerov.
Perevod s anglijskogo. Moscow: Himiya, 632.
35.Hammarström, D. (2004). A Model for Simulation of Fiber Suspension Flows.
KTH Mechanics, Royal Institute of Technology SE-10044 Stockholm, Sweden,
125.
36.Vinogradov, G. V., Malkin, A. J. (1977). Reologiya polimerov. Moscow:
Himiya, 434.
37.Han, Chang Dae. (1979). Reologiya v processah pererabotki polimerov.
Perevod s anglijskogo pod red. Vinogradova, G.V., Fridmana, M.L. Moscow:
Himiya, 368.
38. Dyadichev, V., Levanichev, V., Tereshtchenko, T. (2003). Metodika opisaniya
reologii rasplava polimera v shirokom diapazone skorostej sdviga.
Resursozberihaiuchi tekhnolohii vyrobnytstva ta obrobky tyskom materialiv u
mashynobuduvanni. Lugansk: Visnyk SNU im. V.Dalia. 68–72.
39.Wei, C., Yaqiang, S., Chunqian, L., Qian, L., Changyu, S. (2011). Effect of
micro-viscosity and wall slip on polymer melt rheology inside micro-channel.
212
 Materials conference ANTEC 2011. Available
at: http://www.plasticsengineering.org/polymeric/node/4897
40.Hatzikiriakos, S. G., Dealy, J. M. (1991). Wall slip of molten high density
polyethylene. I. Sliding plate rheometer studies. Department of Chemical
Engineering, McGill University, Montreal, Canada. Available
at: http://www.chem.mtu.edu/~fmorriso/cm4655/Hazikiriakos_Dealy.pdf
41.Rauwendaal, C., Pilar Noriega, E., Harris, H. (2008). Vyyavlenie i ustranenie
problem v ekstruzii. Perevod s anglijskogo pod red. Volodina, V.,
St.Petersburg: Professiya, 328.
42.Brian Black, W. (2000). Wall slip and boundary effects in polymer shear flows.
[Doctoral dissertation, University of Wisconsin- Madison]. Available
at: http://grahamgroup.che.wisc.edu/pub/black_dissert.pdf
43.Michaeli, W. (1992). Extrusion dies for plastics and rubber: design and
engineering computations. Hanser Publishers, Munich, 340.
44.Screw and barrel combinations (2015). The official website of company Bernex
Bimetall AG. Available at: http://www.bernexgroup.com/mm/Barrel-
Screwcombination1.pdf
45. Bonten, C., Kast, O. (2015). Resource Efficiency in Plastics Technology.
Institut für Kunststofftechnik Stuttgart, Germany. Materials Мotiva Group,
Helsinki. Available
at: http://www.motiva.fi/files/9729/02_Resource_efficiency_in_plastics_industr
y_Bonten_Kast.pdf
46.Kolosov, O.Y. (2009). Natsionalnyi Tekhnichnyi Univerytet Ukrainy “Kyivskyi
Politekhnihnyi instytut. Pat. No. 43672U UA Sposib prohnozuvannia
vlastyvostei epoksydnoi kompozytsii, oderzhanoi z vykorystanniam
ultrazvukovoi modyfikatsii. MPK: C08L 63/00, C08J 3/28, C09J 5/08, B29C
61/00, B29C 61/06. No. u200903203; declareted: 04.03.2009; published:
25.08.2009, Bul. No.16, 2009.
47.Barrier Biax Film Lines. (2016). The official website company Macro, Canada.
Available at: http://www.macroeng.com/barrier-triple-bubble-lines.php
213
48. Kim, V.S., Skachkov V.V. (1988). Dispergirovanie i smeshenie v processah
proizvodstva pererabotki plastmass. Moscow: Himiya. 240.
49.Torner, R., Akutin, M., (1986). Oborudovanie zavodov po pererabotki
plastmass. Moscow: Himiya, 400.
50.Borshchev, V.Ya., Gusev Yu.I., Promtov, M.A., Timonin A.S. (2006).
Oborudovanie dlya pererabotki sypuchih materialov : uchebnoe posobie.
Moscow: “Izdatelstvo Mashinostroenie-1”, 208.
51.Shubin I.N., Sviridov M.M., Tarov V.P. (2005). Tekhnologicheskie mashiny i
oborudovanie. Sypuchie materialy i ih svojstva: Uchebnoe posobie. Tambov:
Izdatelstvo TGTU, 76.
52.Basov, N., Broy, W., (1985). Tekhnika pererabotki plastmass. Moscow:
Himiya, 528.
53.Shlegel, I.F. Shaevich, G.Y., Rukavicyn, A.V. Noskov, A.V., Slemnev, D.A.
(2012). Opredelenie effektivnosti smeshivaniya pri plasticheskoj podgotovke
syrya. Institut Novyh Tekhnologij i Avtomatizacii promyshlennosti stroitelnyh
materialov. Stroitelnye materially, № 8. Available at:
http://www.inta.ru/pub/opredelenie-effektivnosti-smeshivaniya-pri-
plasticheskoy-podgotovke-syrya-stroitelnye-materialy.-2012.-8/ Last accessed:
01.08.2021
54.Fiziko-mekhanicheskie pokazateli poliamidnyh (PA-6) mononitej. (2021). The
official website company OOO “Shagraj”. Ukraine. Available at:
http://www.shagraj.com.ua/pages/ru/mononiti-leska.html
55. Levanichev, V.V., Tereshchenko, T.M. (2010). Issledovanie vliyaniya
kachestva smesheniya na fiziko-mekhanicheskie harakteristiki plenochnyh
materialov. Lugansk: Visnyk SNU im. V.Dalia. 2 (144), 91-95.
56. Ulshin, V.A., Levanichev, V.V., Tereshchenko, T.M., Levanichev, A.V.,
(2012). Kriterii kachestva smesheniya mnogokomponentnoj sistemy. Eastern-
European Journal of Enterprise Technologies, 6(6(60), 28–31.
https://doi.org/10.15587/1729-4061.2012.5544

214
57. Cherpakov, B.I. (1990). Ekspluataciya avtomaticheskih linij. Moscow:
Mashinostroenie, 304.
58.Yakovlev, A.D. (1972). Tekhnologiya izgotovleniya izdelij iz plastmass.
Leningrad: Himiya, 344.
59.Torner, R., (1977). Teoreticheskie osnovy pererabotki polimerov (mekhanika
processov). Moscow: Himiya, 464.
60.Altınkaynak, M., Gupta, M., Spalding, S., Crabtree., (2011). Melting in a Single
Screw Extruder: Experiments and 3D Finite Element Simulations. Magazine
International Polymer Processing XXVI (2), 182-196.
61. Process temperature specifications – a sad story (2013). Technical magazine
AIMCAL. Available at: http://www.convertingquarterly.com/blogs/substrate-
secrets/id/5173/process-temperature-specifications-a-sad-story.aspx
62.Levanichev, V. (2013). Upravlenie temperaturoj rasplava v processah
soekstruzii. Eastern-European Journal of Enterprise Technologies, 5(5(65), 4–
6. https://doi.org/10.15587/1729-4061.2013.18100
63. Ulshin, V.A., Levanichev, V.V., Tereshchenko, T.M., Levanichev A.V. (2012).
Gravimetricheskie sistemy dozirovaniya v soekstruzii, novye tekhnologicheskie
parametry processa. Lugansk: Visnyk SNU im. V.Dalia. 3(174)2, 175-179.
64.Levanichev, V.V. Larchenkova T.I., (2003, Jan.). Issledovanie barernyh svojstv
poliamidnyh obolochek. Zhurnal “Myasnaya industriya”, 10-11.
65.Levanichev, V.V. Larchenkova, T.I., Sharapova, A.V., (2002, March)
Issledovanie processa termousadki v poliamidnyh kolbasnyh obolochkah.
Zhurnal “Myasnoj biznes”, 8-9.
66.Levanichev V.V. Kriula K.V. (2010). Pat. No. 54505 UA. Bakterytsydna
kovbasna obolonka na osnovi poliamidiv. MPK: A22C 13/00. No.
U201006310; declareted: 25.05.2010; published: 10.11.2010, Bul. No. 21.
67.Levanichev V.V. Kriula K.V. (2010). Pat. No 54503 UA. Bahatosharova
dvovisnoofiientowana rukavna obolonka dlia upakuvannia kharchovykh
produktiv. MPK: A22C 13/00. No. U201006308; declareted: 25.05.2010;
published: 10.11.2010, Bul. No. 21
215
68.Tereshchenko, T.M. (2007). Sovershenstvovanie tekhnologii i oborudovaniya
pererabotki vtorichnyh polimernyh materialov kombinirovannym
vydavlivaniem. Dissertaciya kandydata tekhnicheskih nauk. Lugansk: publ.
SNU im. V.Dalia.
69.Levanichev, V.V., Tereshchenko, T.M., Gaponov, A.V. (2009).
Matematicheskaya model processa techeniya polimera v kolcevyh
raspredelitelnyh kanalah ekstruzionnyh golovok. Resursozberihaiuchi
tekhnolohii vyrobnytstva ta obrobky tyskom materialiv u mashynobuduvanni:
zbirnik naukovych prac, Lugansk: Zb. nauk. pr. SNU im. V.Dalia, 229-238.
70.Levanichev, V.V., Tereshchenko, T.M., Gaponov A.V., (2010). Rezultaty
matematicheskogo modelirovaniya techeniya polimera v kanalah ekstruzionnyh
golovok. Kyiv: Zbirka materialiv V Mizhnarodnoi naukovo-tekhnichnoi web-
konferentsii «Kompozytsiini materialy», 75-77.
71.Levanichev, V.V. Safronov, K.N., Dyadicheva, I.V., (2010). Issledovanie
harakteristik kolcevogo raspredelitelnogo kanala ekstruzionnoj golovki.
Lugansk: Visnyk SNU im. V.Dalia. 9 (151), 59-65.
72.Levanichev, V. (2013). Model techeniya rasplava polimera. Eastern-European
Journal of Enterprise Technologies, 4/7(64), 39–41. Available
at: http://journals.uran.ua/eejet/article/view/16685/14175
73.Levanichev, V. (2015). Analiz polnoj reologicheskoj modeli techeniya rasplava
polimera. Eastern-European Journal of Enterprise Technologies, 2(6(74), 11–
16. https://doi.org/10.15587/1729-4061.2015.38951
74.Tager, A. A. (2007). Fiziko-himiya polimerov. 4th edition. Moscow: Nauchnyj
mir, 576.
75.Levanichev, V. (2015). Razrabotka modeli dvizheniya rasplava v
ekstrudere. Eastern-European Journal of Enterprise Technologies, 5(5(77), 7–
13. https://doi.org/10.15587/1729-4061.2015.51338
76.Levanichev, V. (2014). Study of multi-layer flow in coextrusion processes.
TEKA Commission of motorization and power industry in agriculture, 14 (1),

216
 144–153. Available at: http://www.pan-
ol.lublin.pl/wydawnictwa/TMot14_1/Teka_14_1.pdf
77.Grunschloss, E. (2006). Assignee: Krauss-Maffei Kunststofftechnik Gmbh. Pat.
No. US 7083321 B2. Single screw extruder. Appl. No.: US 10/600217;
declareted 06.05.2004; published: 01.08.2006.
78. Extruder with long helical grooves (RANGE HELICAL). (2021). The official
website company Komax. Available
at: http://www.komax.pro/en/extrusion/extruder-long-helical-grooves
79. HELIBAR® – single-screw extruders. (2015). The official website company
EXTRUDEX GmbH. Available at: http://extrudex.de/en/helibar
80. HELIBAR® Plastification Unit. (2015). The official website company HELIX
GmbH. Available at: http://www.helixgmbh.com/index.php?id=7&lang=en
81. EXTRUDEX introduces economic single-screw HELIBAR® extruder at
K2010. (2010). The official website company Messe Düsseldorf GmbH.
Available at: http://www.k-online.com/
82. Kolosov, A.N., (1991). Organizaciya i ekonomika gibkogo
avtomatizirovannogo proizvodstva. uchebnoe posobie. Kiev: Vyshcha shkola,
167.
83.Levanichev, V.V. Girkin E.J., Levanichev, A.V., (2012). Planirovanie zakazov
v edinichnom ekstruzionnom proizvodstve. Lugansk: Visnyk SNU im. V.Dalia.
3 (174) 2, 65-70.
84.Barvinsky, I.A., (2015). Osnovy inzhenernyh raschetov litya termoplastov:
tekhnologicheskie parametry. CADmaster. 2 (81).70-77. Available at:
https://issuu.com/cadmaster/docs/cadmaster-2015.2_81_

217

View publication stats