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High Quality Dispersing Agents For Masterbatch
High Quality Dispersing Agents For Masterbatch
Contents
Theory 4
Range of products 7
Product data 8
Technology 10
Ceridust 17
Safety information 27
3
Theory
MECHANISM MODEL
·
Drop point
Pigment wetting
·
Viscosity
(dispersing agent)
·
Polarity
Surplus of dispersing agent
(e. g. wax) is beneficial
· Viscosity
Dispersion · Thermal an color stability
Stabilization Polarity
·
·
Compatibility
Prevention of flocculation ·
Viscosity
5
Theory for
Coloring Plastics
EXPLANATION OF SINGLE
PIGMENT CONCENTRATES
Pigment preparations where dispersions of
mainly one (single pigment concentrate =
SPC) or more pigments exist in a polymeric
carrier system are usually described as
»pigment concentrates«.
Montan
This quality control assures the high level of reliability for the wax
processing of waxes from Clariant.
Ceridust
Polyethylene Licocene Polypropylene
wax Licolub wax
Licowax
Amide
wax
Structure of some Polyolefin Waxes taken from our Range Structures of some Amide and Montan Waxes from our Range
Drop point Acid number
Product Structure Drop point [ °C ] Product Structure [ °C ] [ mg KOH/g ]
7
Product data
overview
Drop point Acid value Density at 23 °C Viscosity at 140 °C Color Supply forms1
[ C° ] [ mg KOH/g ] [ g/cm3 ] [ mPa·s ]
Polyolefin waxes
Licowax PE 520 ~ 120 – ~ 0.93 ~ 650 White Granules, Fine grain, Powder
Licocene PP 1302 ~ 90 – ~ 0.87 ~ 200 [ 170 °C ] White Granules, Fine grain
Licocene PP 1502 ~ 86 ❖ – ~ 0.87 ~ 1800 [ 170 °C ] White Granules, Fine grain
Licocene PP 6102 ~ 145 – ~ 0.90 ~ 60 [ 170 °C ] White Granules, Fine grain
Licocene PP 6502 ~ 148 ❖ – ~ 0.90 ~ 1700 [ 170 °C ] White Granules, Fine grain
Licocene PP 7502 TP * ~ 165 ❖ – ~ 0.90 ~ 1800 [ 170 °C ] White Granules, Fine grain
Amide wax
Drop point Acid value Density at 23 °C Viscosity at 100 °C Color Supply forms 1
[ C° ] [ mg KOH/g ] [ g/cm3 ] [ mPa·s ]
Ceridust
Montan waxes
9
Technology I
Manufacturing
of Masterbatches
The most important considerations in molded part production may In the two-stage masterbatch production, SPCs are produced
be factors such as short cycle times and therefore of high output in the same manner as the one-stage process. In the first stage,
rates. Surface properties, gloss or maintenance of mechanical the process can be optimized because only one colorant is used.
properties can also play a major role in processing requirements. A single-screw extruder often meets the needs for homogeneous
The production of masterbatch can be done in different ways. The mixing of ingredients in this second stage.
most common procedure is to manufacture concentrates on twin-
screw extruders. There are two methods for this, the single-stage There are other well-known processes for the manufacturing of
and the two-stage process. In single-stage masterbatch production, masterbatches which can be utilized for special requirements
all components in the concentrate are mixed in one processing step. and alternative forms.
In general there are two main possibilities for the masterbatch In addition to a highly concentrated masterbatch often melts
carrier systems. With so called universal carrier systems a and disperses much faster if the carrier has a lower viscosity
polymer matrix is chosen that is compatible with as many resins and melting point compared to the host polymer. Masterbatch
as possible. The masterbatch can then be utilized in different producers choose the appropriate combination of carrier and
polymer systems. Such carrier systems consist in the first place dispersing agents depending upon the requirement profile of
of waxes, polyethylene & polypropylene resins or similar polymers. their product in order to meet the technical requirements.
Such generated masterbatches are a good alternative when it is
neither possible nor economical to make use of the host polymer Even though pigment concentrates were primarily used in color-
itself – especially when coloring small quantities of raw materials. ing polyolefins and other commodity polymer. Due to constant
technological development, more efficient processing plants,
Nowadays plastics are often specially modified for their end new areas of application, cost savings etc, there is a daily demand
application and molded parts are becoming more and more for new solutions and more and more efficient and sophisticated
complex, so special masterbatches have to be developed. products as a result.
Carrier systems consist of polymer that is identical to that used
by the part manufacturer. This practice is often applied for the Only with the aims of the pigment concentrate producer remain
coloration of most thermoplastics. the same: The highest possible pigment concentration at the same
time as the highest possible dispersion quality. Here the use of
Unfortunately, often it is impossible to use the same polymer special waxes – in particular high quality dispersing agents – and
as carrier for the mastebatch. The selection of the carrier their optimal matching with the demands of the relevant pigments,
depends strongly upon shear sensitivity, wettability, polarity carrier systems and processing technology allows the efficient and
and also economics. consequent realisation of these aims.
11
Technology III
CARRIER SYSTEMS
Manufacturing
13
Technology III
CARRIER SYSTEMS
Because of its high dispersion quality, efficiency and wide range The processing of the three components (wax, carrier resin and
of application, this type of concentrate is widely used. pigment) is carried out either in an internal mixer or after produc-
ing a premix with an extruder. The uncomplicated handling and
In general, concentrates of this type contain between 5 % and high dispersion quality have resulted in their widespread use for
30 % wax, as long as a polyolefin carrier system is involved. With the most sophisticated applications in diverse polymers.
styrenics and engineering plastics, between 1 % and 5 % of a
suitable wax is used. The »breading« procedure is also possible with easily dispersible
pigments and concentrates for thick-walled parts without any
By using a combination of wax and resin, the advantages of the demand for high quality. This involves about 40 % polymer, roughly
other two concentrate types are combined. The wax component – the same amount of pigment and about 20 % of wax being mixed
partly used in micronized form – allows high pigment concentra- in a high speed mixer until the wax softening point is reached by
tions as well as a good pigment wetting and thus helps to reach warming up the mixture.
a good dispersion. The carrier resin makes the handling of the
concentrate easier. Then the pigment is wetted with the wax, which makes the mixture
virtually dust-free. When the temperature is raised further by
Both technical and commercial advantages over the first mentioned about 10 Kelvin, the pigment-wax mixture forms a thin skin around
type of concentrate can be obtained by judicious selection of both the polymer granulate, with the result that the wax functions as a
of these components and by optimal conformity to the specific de- binder. So that the skin is not peeled or the mixture is made lumpy
mands of pigment, processing technology and areas of application. as a result of uneven cooling, the »coated« granulate must be cooled
down gently in a controlled manner.
60
~15 m/s (Polymer wetting)
40
~7 m/s
20
110.0 2.0
105.0 1.0
100.0 0
0 5 10 20 30
Content of wax [ % ]
■ Color yield ■ Filter pressure value
The production of high-filled concentrates of basic pigments with the desired shade of color, blended with the polymer to
in pure wax provide an economical and technically convincing be colored and diluted to a certain concentration required for
solution – in particular for the production of smaller quantities easy dosage.
of pigment concentrates. These can then be mixed in accordance
15
Licocene
as a sole carrier
internal method
3.0 120
14 μm, 724 mesh/square [bar/g] pigment
115
2.5
■ Rel. color yield [ % ]
110
■ Filter pressure value
2.0
105
1.5 100
95
1.0
90
0.5
85
0 80
LLDPE 35 %
Licowax PE 520 15 % Extruder: Berstorff ZE 25 x 48 D: Screw CP3 /
Licocene PP 6102 10 % 48 L-D, speed 500 min -1, 5 kg/h
Temperature: Licocene 90-140-150-120-100-100-
Ceridust 6050 M 10 %
120-120-120 °C, Die: 130 °C; LLD-PE polymer MB
Licocene PP 1502 40 % 40 % 120-140…
Under the tradename Ceridust Clariant offers a wide range of re-agglomerating, eases pigment dispersion and, last but not least,
micronized waxes with a particle size below 40 μm. Ceridust stabilizes the dispersion.
particles are closer in size to those of organic pigments than all
fine grain or powder grade wax particles. A mixture of standard powder and Ceridust already improves the
dispersion remarkably. Therefore for the first trials we recommend
Finer particles give a better statistical distribution than bigger ones. the use of a combination of two parts Licocene/Licolub/Licowax in
The fine Ceridust particles can act as »distance keeper« between powder form and one part of Ceridust as micronized-powder form.
the pigment particles. The micronized wax particles, sidewise close
to the pigment particles and being (almost) statistically ideally The remarkable increase in color strengt allows a possible r eduction in
distributed, show a high likeliness to find a place between pigment amount of pigment. This will be the way to have economical f ormulation
particles, thus separating them from each other. Consequently those costs and a good performance without processing problems.
pigment particles will not form agglomerates.
Ceridust types Approximate particle size
When the mixture is being processed, e. g. when passing kneading [ d50 µm]
blocks in the metering zone of an extruder, the distance keeping, Ceridust 3620 8.5
micronized wax particles will melt right where they are. This Ceridust 3910 6.5
means between the »agglomeration prone« pigment particles are Ceridust 5551 8.5
coated with a fine film of wax. This kind of particle coating neutral- Ceridust 6050 M 9.5
izes the binding forces of the pigment particles, prevents them from Ceridust 8020 8.0
135
12
130
■ Filter pressure value [ bar/g ]
10
■ Rel. color yield [ % ]
125
120
8
115
6
110
4 105
17
Recommendations for
POLYOLEFINS
Figure 8: Licocene and Ceridust for concentrates and masterbatches (40 % Disazo condensation in PP)
internal method
10 6 (bad)
8 5
■ Filter pressure value [ bar/g ]
■ Film note
6 4
4 3
115
■ Filter pressure value [ bar/g ]
7.5
■ Rel. color yield [ % ]
110
5.0 105
100
2.5
Formulation: 40 % Pigment Violet 23
95
60 % - x % Polypropylene
x % Test product
0 90 Filter value: DIN-EN 13900-5
20 % Licocene PP 6102 13 % Licocene PP 6102 Filter: 14 μm, 724 mesh
+ 7 % Ceridust 6050 M Color yield: DIN 55986
19
Recommendations for
POLYOLEFINS
Thanks to their well balanced properties, Licowax PE 520 and Polyolefin [ % ]
Ceridust 3620 are universally suitable for pigment concentrates Organic pigment 40 25 – – – –
to color polyolefins. Being a polyethylene wax, it is fully Carbon black – – 30 20 – –
compatible with high necessary compliance with our customers’ TiO2 – – – – 70 60
specific demands; our service team is at their disposal for PE 520 ~ 20 ~ 10 15 – 10 –
discussion. Compared with various competitive polyethylene PE resin ~ 40 ~ 65 55 80 20 40
waxes, Licowax PE 520 is characterised by its advantageous
thermostability, which in practice becomes noticeable in good
color fastness when melting as well as in absence of smell.
Depending on pigment and type of application, the following
basic recipes can be recommended:
Figure 10: Influence of particle size and amount of wax (30 % Cu-Phtalocyanine in LLDPE) –
Decrease of filter pressure value (FPV) due to finer particle size and higher amount of wax
internal method
16
Filter pressure value [ bar/g ]
12
4
Formulation:
30 % Pigment Blue 15:1
0 70 % - x % LLDPE (MRF 25)
Without 10 % Licowax 15 % Licowax 20 % Licowax 15 % Licowax 20 % Licowax x % Test product
PE 520 PE 520 PE 520 PE 520 PE 520 Filter value: DIN-EN 13900-5
+ Ceridust 3620 + Ceridust 3620 Filter: 40 μm, 725 mesh
(2:1) (2:1) Premix: Cold mix
Polyamide 65 65 65
Polycarbonate 77 77
Polyester 67 67 67 67
Polystyrene 65 65
TPU 65
Pigment 30 30 30 30 30 30 30 30 30 20 30 30
Ceridust 3910 2
Ceridust 5551 3 1 1 1
Licowax C 5 3
Licowax E 5 3 3 2
Licolub WE 4 3 2 5 2
Licolub WE 40 3 2
Licolub WM 31 ( 5 ) 3 3 2
21
Recommendations for
ENGINEERING RESINS
Figure 12: Pigment dispersion in polyamide 6 using Licowax, Licomont and Ceridust
20 130
■ Filter pressure value [ bar/g ]
120
■ Rel. color yield [ % ]
15
Formulation: Polyamide 6
10 110
+ 30 % Pigment Blue 15:1
+ x % Test product
Filter value: DIN-EN 13900-5
5 100 Filter: 14 μm
Extrusion:
Temperature: 240 –> 250 °C
Screw speed: 500 rpm
0 90 Throughput: 6 kg/h
Without 1 % Licowax 1 % Licomont 1 % Ceridust Licomont Licomont Licomont Screw: MB 6
E CaV 102 5551 CaV 102 CaV 102 CaV 102 Co-rotating twinscrew
+ Licowax E + Ceridust 5551 + Ceridust 5551 extruder ø 25 mm
( 1 + 1 % ) ( 1 + 1 % ) ( 2 + 3 % ) L/D= 40, cold mix
internal method
16 130
■ Filter pressure value [ bar/g]
12 120
■ Rel. color yield [ % ]
8 110
4 100
Formulation: Polyester + 30 % Pigment
PV Fast Green GNX + x % Test product
Filter value: DIN-EN 13900-5
0 90 Filter: 14 μm
1 % Licolub WE 4 3 % Licolub WE 4 5 % Licolub WE 4 2 % Licolub WE 4 Processing: Screw MB 6, 300 rpm and 8 kg/h
+ 1 % Ceridust 5551 Premix: Cold mix
23
Recommendations for
ENGINEERING RESINS
For the coloring of PC it is very common to disperse without TEM Photographs of Polycarbonate Samples
wax, the polarity of the polymer wetts the pigments reasonably
well. As a montan wax, Licowax E ideally combines polymer No wax 3 % Licowax E 2 % Licowax E
1 % Ceridust 5551
compatibility, pigment wetting, lubrication and mold release
when removing injection molded parts from the mold. Magni-
fication
The proportion of wax in the pigment concentrate on the basis
of the polymer to be colored should be selected in such a way
4000 x
Tabelle mit rein ?
that the finished product contains 0.1 to 0.3 phr Licowax E.
By using Licowax E it is possible to improve the color yield
considerably, but the combination with Ceridust 5551 provides Color yield 100 % 117 % 131 %
even better results.
Formulation 17.0 % Pigment Green 7
3.0 % Montan wax
80.0 % Polycarbonate
(MFR 25 g / 10 min)
internal method
30 140
Highest color yield with
mixture of Licowax E
and Ceridust 5551
25 130
■ Rel. color yield [ % ]
120
■ Correlated haze
20
Lowest correlated haze
with Ceridust 5551
15 110
10 100
5 90
Extruded hoses stick together when being wind up and can not
be unstucked again. Here the concentrate producer is afforded the
opportunity of both improving the pigment dispersion and also
counteracting specific, a.m. processing problems.
25
Recommendations for
STYRENICS
110
100
The usual precautions to be taken when Toxicological and ecological Technical Data
handling chemicals should be observed. properties For further information on the physical and
Safety data sheet can be supplied for each For data on toxicological and ecological chemical properties, detailed application
individual product upon request. When properties of the product groups mentioned, and packaging of our products please refer
handling organic powders the domestic please refer to the relevant safety data sheet to our product data sheets, our various
regulations must be observed in order to or the corresponding product data sheet. application brochures and product flyers.
prevent durst fires and dust explosions.
Status according to the Storage
European chemicals law (REACH) The products described in this leaflet have
The products mentioned in this leaflet or a minimum shelf life of two years after
the monomers are either pre-registered, delivery when stored in a dry place at
registered or as polymers exempt from room temperature.
registration (EC 1907/2006).
27
Clariant International Ltd
Rothausstrasse 61
4132 Muttenz
Switzerland
www.additives.clariant.com
www.clariant.com
This information corresponds to the present state of our knowledge and is intended as a general
description of our products and their possible applications. Clariant makes no warranties, express or
implied, as to the information’s accuracy, adequacy, sufficiency or freedom from defect and assumes
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information waives any of Clariant’s General Terms and Conditions of Sale, which control unless it agrees
DA 8270 E | 01.2014
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