Resin Manual (Rev0)

Client: Kamdhenu Paints, Gurgaon SPC.
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Dexter Technologies 19/05/2010
Dexter Technologies
RESIN MANUAL
KAMDHENU PAINTS
PROJECT KPJ-101
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RESIN
Resins are the condensation / addition polymers which form by reacting monomer units. It
is the film forming material of the paint and provides gloss and adhesion to the paint.
Resin is the main ingredient of the paint system. Durability of paint depends on the quality
and quantity of resin used in the overall paint formulation.
Resin plays an important role in overall paint formulation. As different quality and quantity
of resins are used in the paint, it provides
(1) It converts liquid coating into solid film after application as a thin film by air-drying or
drying mechanism.
(2) It provides gloss to paint film.
(3) It gives flexibility and hardness to the paint film.
(4) Makes paint adhere to the surface.
(5) It provides resistance to water, alkali and abrasion.
(6) It disperses pigment and extender in uniform way on the substrate.
Resin is used as film forming substance and also used as binder, which binds the
pigment and extender to the substrate.
Very wide ranges of resins are used in surface coating industry. They are as follows
(1) Alkyd resin.

(2) Acrylic resin
(3) Epoxy resin.
(4) Amino resin.
(5) Polyurethane resin.
(6) Others (Water Thinnable Resins)
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RESIN – CLASSIFICATION IN PAINT INDUSTRY
Resin
Alkyd Emulsion Acrylics Epoxy Amino Miscellaneous
ALKYDS
Kienle originally used the Term “Alkyd” in 1927 to describe the reaction product of
polyalcohols and polybasic acids.
The word alkyd was coined as Al [ cohol ] , [ A ] cid or Alk [ C ] y [ I ] D ==> Alkyd .
However, definition become lucid when the esterification reaction with polyhydric Alcohol
and Polybasic acids, were termed as polyester formation but subsequently the usage of
the term “alkyd “ now tends to specify polyester products composed of polyhydric
alcohol‟s, polybasic acids and monobasic fatty acids obtained from oils. These materials
are used chiefly in the coating industry.
In coating industries the terms Alkyd, Alkyd Resin and Alkyd solution are used
interchangeably, even though most alkyds are handled as solutions in hydrocarbon
solvents.
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Classification of Alkyd Resins
On The Basis
On The Basis of Drying
of oil Length Characteristics
Short Oil Long Oil Drying Non Drying

Alkyd Alkyd
Medium Oil Semi Drying
Alkyd
On The Basis of oil length

In this method alkyds are classified on the basis of amount of oil % present in the alkyd.
The general recognised compositions are as follows: -
Alkyd Type Oil Contents ( % )

Short Oil Alkyd 35 - 45 %
Medium Oil Alkyd 46 - 55 %
Long Oil Alkyd 56 - 70 %
On The Basis of Drying Characteristics

This classification depends on the type of oil or fatty acids present in the particular alkyd.
Broadly every alkyd can be classified as a drying, semidrying, or non-drying alkyd.
Drying Alkyd: - These are based on the oils having higher iodine value( more than 160)
.It has higher unsaturation, which in the presence of oxygen at room temperature cross
links to form a thin film. e.g.
Linseed oil, Tung oil based alkyds.
Semidrying Alkyd: - These are based on the oils or fatty acids having Iodine values in
the range of 160 - 120.
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Soya, Sunflower, Tobacco seed, Niger seed oil based alkyds are the examples of
semidrying alkyds.
Non-drying Alkyd: - Normally has oils having iodine value less than 120.
Examples are Palm oil, Castor oil and Coconut oil based alkyds.
On the basis of oil content classification and the drying concept, an alkyd can be
described as 60 % oil - drying alkyd OR with less precision, a Long oil drying alkyd.
Question arises, what will be the nomenclature if monobasic fatty acids used in
place of oil? Comparison between the long oil, short oil systems and the fatty acid system
can be made by stoichiometrically converting the weight of fatty acid to the weight of an
equivalent molar amount of triglyceride.
Commonly in paint industry, the classification of long / short / medium oil alkyd can
be understood on the basis of the series. Examples the long oil alkyds are always named
as R 2---, Medium oil alkyds are named as R 3 ---, short oil alkyds are named as R 4---. (--
- Are the different numbers used for naming the different alkyds)
Raw Materials
The most common alkyd ingredients are as follows: -
Polybasic Acids
Phthalic anhydride Ajelaic Acid
Isophthalic Acid Succinic Acid
Maleic Anhydride Adipic Acid`
Tetra hydro phthalic anhydride Fumaric Acid
Oils
Linseed Oil Sunflower Oil
Soya Oil Cotton seed Oil
Castor Oil Dehydrated Castor Oil (DCO)
Tung Oil Coconut Oil
Polyhydric Alcohol
Glycerine Sorbitol
Pentaerythritol Propylene glycol
Ethylene glycol Trimethylol ethane
Trimethylol prophthalice Di propylene glycol
Neopentyl glycol Di ethylene glycol
Monobasic Acids
Fatty Acids obtained from oils Synthetic saturated fatty acids
Benzoic Acids
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Monoglycerolysis Catalyst
Lead Acetate Trihydrate ( LATH ) Litharge
Cerium Octoate 6% Lithium Stearate
Calcium Oxide / hydroxide Sodium Naphthalene
Di-butyl tin oxide ( DBTO) Sodium Hydroxide
Anti Oxidant
Hypophosphorous Acid ( HPA ) Triphenyl phosphite ( TPP )
Solvents
Xylene M.T.O.
C - IX
Polyhydric Alcohol (polyols)

The 3 predominant Polyhydric alcohol used in alkyd resins are :-
CH2OH
CH2OH CH2OH CH2OH
CH OH
C CH OH HO CH
CH2OH CH2OH CH2OH CH OH
CH OH
Pentaerythritol Glycerol
CH2OH
Sorbitol
The high functionality of Pentaerythritol makes it of wide interest as the polyol for long oil
alkyds containing 60 % or more fatty acid, because of its high functionality, Pentaerythritol
is often blended with either glycerol or glycol in alkyds containing less than 60 % fatty
acids.
Pentaerythritol containing alkyd tends to have higher viscosity and molecular weights, dry
more rapidly and give coatings of greater hardness with lower flexibility, better gloss and
gloss retention, better heat and yellowing resistance better chemical resistance, better
water resistance and better exterior durability than glycerol based alkyds of comparable oil
contents.
In paints, Pentaerythritol types also shows antisagging at equal brushing, brushability and
flow.
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The higher functionality of pentaerythritol over glycerol is the main reason for many of
above mentioned advantages.
Our major quantity of the polyol used is pentaerythritol. We get three types pentaerythritol.
They are named as Penta - 88, Penta -98(Penta nitration grade) and Penta technical
(Kanoria Penta). The differences between these are based on the purity. Penta exists as
mono penta and dipenta.
Penta 98/nitration grade contains 98% of monopenta and 2% of dipenta. Penta 88
contains 88% of mono penta and 12% of dipenta and penta technical/ penta Kanoria
contains 96% of mono penta and 4% dipenta.
CH2OH CH2OH CH2OH CH2 CH2OH

C C C
CH2OH CH2OH CH2OH CH2 CH2OH
mono penta di penta
The higher the dipenta content higher the reaction rate. Hence there will be separate
formulation for every type of pentaerythritol. The formulation can be used depending on
the availability of penta.
Though Sorbitol has six hydroxyl groups, It undergoes intermolecular dehydration at alkyd
esterification temperature 210 - 260 deg C that‟s why use of Sorbitol is restricted.
CH2OH CH2
CH OH CH OH
At 210 - 260 deg C

HO CH HO CH O + H2O
CH OH CH OH
CH OH CH
CH2OH CH2OH
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Polybasic Acids
COOH COOH
3
CO COOH
4
2
CH COOH
O ||
CHCOOH
1
5
CO COOH COOH 6 COOH Maleic Anhydride
Phthallic Anhydride Isophthallic Anhydride Tetrahydrophthallic Anhydride
Terphthallic Anhydride
( Cis - 4 - cyclohexene -
1,2 dicaroxylic Anhydride )
Phthalic anhydride is the most extensively used polybasic acid in Alkyd resins because of
its low cost and the excellent properties it imparts to Alkyd resin products.
In recent years Isophthalic acid has been more extensively used in place of phthalic
anhydride. Isophthalic acid compared to orthophthalic acids are claimed to have higher
molecular weight and higher viscosity, to have better drying characteristics and to give
hard and more durable films with better heat and chemical stability.
Isophthalic acid is more reactive than phthalic anhydride. The reason is intermolecular
cyclization in phthalic anhydride makes it less reactive than Isophthalic acid.
The para isomer of phthalic acid, terphthalic acid has very poor solubility in alkyd
ingredients It also has very high melting point (436 deg C), has made processing of
terphthalic acid based alkyds very difficult.
Other dibasic acids used in alkyds in limited amount includes THPA (Tetrahydro phthalic
anhydride), Maleic anhydride etc.
Maleic acid / anhydride often used to replace part (upto 10 % max on a molar basis) of the
phthalic anhydride in the alkyd resin. It reacts with the unsaturation in fatty acids, Its effect
is to increase the total functionality of the alkyd system, viscosity and polymer molecular
weights.
When Maleic anhydride is used in small amounts in phthalic anhydride alkyds they dry
more rapidly and give harder films with improved colour, better alkali resistance, better
exterior durability because of improved water resistance .
Catalyst
Alkyds are manufactured through different routes. One of the routes is through
Monoglycerolysis. Here a catalyst is required to convert oil (triglyceride) into
monoglyceride. E.g. Lead acetate Trihydrate (LATH), Di butyl tin oxide (DBTO), Cerium
Octoate 6%, Liocat etc.
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Fatty Acids and Oils

Chemically oils are carboxylic esters derived from the single alcohol (glycerol
HOCH2CHOHCH2OH ) and are known as glycerides . More specifically, they are
triglycerols.
O
||
H2C-O-C-R
|
H C-O-CO-R'
|
H2C-O-C-R"
||
O
A Triglycerol (A glyceride) {here R, R', R'' are fatty acids )
Oil is made up of glycerides derived from different fatty acids.

Usually the fatty acids are all straight chain compounds ranging from 3 to 18 carbon. Oil
contains fatty acids of even no. of carbon ( except C3 and C5 ).
The extent and kind of unsaturation in the fatty acids has a strong effect on the properties
of the final alkyds.
In general, triene (3 double bond) unsaturation contributes more to drying rate, colour
properties and film hardness than di-ene (2 double bond) unsaturation. Conjugated
systems are slightly better than nonconjugated systems in the development of initial
drying.
The effect of oil on alkyd properties are as follows :-
Triglyceride or Fatty Iodine Speed of Color Gloss

Acid Source Value Drying Retention Retention
Approx.
Linseed oil 189
DCO oil 155
Soya oil 135
Castor oil 85
Coconut oil 9
If an oil or fatty acid has Iodine value of 125 - 135 or more, indicating about 1.5 double
bonds per fatty acid, it gives satisfactory drying properties to the alkyd. Below this range of
iodine value, the oil either don‟t dry or take extremely long time to form a dry films.
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DCO and linseed oil gives the best drying time because in these oils, fatty acid groups of
multiple unsaturation predominate over others.
The oils or fatty acids, with higher iodine values not only show faster drying properties but
also give coating of greater hardness and better gloss.
Anti Oxidants
All these oil-modified alkyds are processed at higher temperature (210 - 265deg C).
Oxidation of oil will take place at higher temperature resulting in charring of the oil and
hence high colour of the resin. To prevent this anti oxidants are added. E.g. Triphenyl
phosphite (TPP) and Hypo phosphorous acid. The oxygen present in the reaction vessel
will react with TPP and tri phenyl phosphate will get generated. Also nitrogen purging is
done to create an inert atmosphere inside reaction vessel. This will further prevent material
coming in contact with air inside the reaction vessel at high temperature.
Azeotropic solvent
In alkyd, it is a condensation reaction between polyol and polybasic acid. Water will get
generated and it will be removed azeotropically by using a solvent. E.g. xylene, butanol
Azeotrope:- Two immiscible liquid of different boiling point when mixed will boil at a lower
boiling point of both the liquids.
E.g. water boils at 100 deg C and xylene boils at around 145 deg C. A mixture of xylene
and water boils at around 95 deg C.
Modifiers
Alkyd modification was defined as a chemical reaction during alkyd preparation which
incorporates the alkyd chemical agents which don‟t fit in the classification of alkyd
ingredients: - namely Polyhydric alcohol‟s, polybasic acids or oils / fatty acids.
The primary reasons for modification are either for economy (cost factor) or to confer some
desired properties.
The amount of modifier may be as high as 40 % of the total alkyd, but usually 10 - 25 %
are common.
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Effects of modifier
Modifier Advantage Disadvantage

 Faster Dry  More yellowing
 Better Brushability  Decreases exterior
Rosin  Greater hardness durability when used in
 Better mar resistance excess
 Better adhesion
 Reduces alkyd  Poor solubility
functionality ( Chain  Poor flexibility
Terminator ) and acts as
Benzoic Acid a gelation inhibitor
 Greater hardness
 Higher viscosity
 Faster dry
 Improved colour and
gloss
 Improved chemical
resistance
 Better water resistance  Greater yellowish tone
Iso cyanates  Faster dry  Toxicity problem ( During
 Better abrasion raw material handling )
resistance
Processing Of Alkyd Resin

Chemical Reactions involved in Alkyd Processing
The chemical reaction occurs during the alkyd processing are as follows: -
1. Condensation reaction among alkyd ingredients or alkyd modifiers, including

esterification; ester, alcohol, or acid exchange; and etherification.
2. Addition reaction of the unsaturated hydrocarbon portions of the monobasic fatty acids,
including free - radical or Diels - Alder reactions with other alkyd ingredients, modifiers or
oxygen.
3. Addition reactions, especially free- radical types with other unsaturated alkyd
ingredients.
4. Side reactions such as decarboxylation.
Examples of Above named reactions during alkyd processing are: -

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A). Esterification and ester exchange: -
The basic reaction involved in an alkyd processing is esterification. This is happening

during the reaction of an alcohol with an acid. It is a reversible reaction (In all alkyd
preparation we have polyhydric alcohols and polybasic acids). The reaction is: -
R1COOH + ROH R1COOR + H2O

Ester exchange or tranesterification reaction is: -
R1COO R2 + R3COO R4 R1COO R4 + R3COO R2

As this reaction can occur in any two-ester molecules, it is of important in alkyd
preparations, especially for its effect on the molecular weight distribution in the final
product.
B) Etherification: -
At the alkyd processing temp (210 deg to 250 deg C) etherification reaction can occur in
alcohols: -
2ROH ROR + H2O
In an observation made by a scientist, he found that at 240 deg C temp with glycerol 7-8 %
esterification can be possible. He reported lesser etherification
(Approximately negligible) with pentaerythritol.
While sorbitol is found to be more prone to etherification than glycerol because it is
capable of internal etherification: -
CH2OH CH2
CH OH CH OH
At 210 - 260 deg C

HO CH HO CH O + H2O
CH OH CH OH
CH OH CH
CH2OH CH2OH
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C) Alcoholysis and Acidolysis
These reactions are special cases of esterification as only hydroxyl, carboxyl, and ester
groups are involved.
A partial alcoholysis of a triglyceride is: -
CH2(OCOR)CH(OCOR)CH2COOR + C(CH2OH)4
CH2OHCHOHCH2COOR +(CH2OH)2 C(CH2OCOR)2

A partial acidolysis of a triglyceride is: -
CH2(OCOR)CH(OCOR)CH2COOR + C6H4(COOH)2
CH2(OCOR)CH(OCOR)CH2OCOC6H4COOH
+ RCOOH
Both alcoholysis and acidolysis are reactions used in the preparation of alkyds from oil. If
polyol and phthalic anhydride are added to the oil simultaneously, substantial amount of
insoluble polyol phthalate forms. To avoid this difficulty, either alcoholysis or acidolysis is
employed to make partial esters of the polyol or acid, respectively before proceeding.
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Manufacturing of Alkyd Resins
Flow chart of manufacturing of a resin
Oil and Solvent Charging Powder

Charging Charging
Heating Processing Cooling

( Reactor Stage )
Solvent Thinning
Charging ( Blender Stage )
Filteration Approvel from

QAD
(A) Alkyd Resin is manufactured by four processes (In Reactor Stage)

(1) Mono Glycerolysis Process or M.G. Process
(2) Acidolysis Process or Half Ester Process
(3) Homogeneity Process
(4) Fatty Acid Process
(B) Thinning and Filtration Stage (Blender stage)
(1) Alkyds by Mono Glycerolysis:
In M.G. Process, Oil, which is triglyceride, is first converted into monoglyceride by reacting
it with polyol. The resulting mixture is reacted with polybasic acid for further polymerisation
reaction.
The systematic processing steps are given below
(a) Charging:
 General Checks
 Charge Oil to the reactor.
 Maintain appropriate water level in separator.
 Start heating as per SPI, stirring and pass N 2 through the batch at approximate 200
litres/hr.
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 Charge the Catalyst and stir for 5-10 minutes and then charge Polyol (Part-1) Raise to
M.G. temperature as specified in SPI.
 Maintain the temperature till the desired tolerance for M.G. with specified alcohol is
obtained. If the tolerance for M.G. is not in range, proceed further only after passing
phthalic anhydride compatibility test.
 Cool the batch to 1800C or below and stop N2 purging.
(b) Post M.G. Charging:
 Charge Polyol (Part-2), Polybasic Acid, Monobasic Acid, antioxidant & Xylene in
sequence.
 Start heating and N2 purging.
 Heat and maintain at 170+-5 for 1hr.
(c) Esterification Stage:
 Continue N2 purging, heat to esterification temperature. Remove water of reaction

azeotropically. Check acid value and viscosity periodically.
 After attaining desired viscosity and acid value stop heating and start stripping if
specified in the SPI.
(d) Stripping and Thinning Stage :
 Strip Xylene till discharging viscosity is achieved.

 Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix in the reactor.
 Discharge the batch to a blender containing pre-arranged solvent under stirring.
Reactor Stage Process map of Alkyd Processing by M.G. Process

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Oil Charging Heating of Oil Catalyst Polyol Charging

Charging
Temp of Oil 100 - 120 deg C Temp of Oil 70 to 100oc Temp of Oil 100 to 160oc
N2 Purging
No. of coil operated
TP Outlet temperature
TPP Charging , Post Cooling the batch M.G. Check Heating for M.G. Temp
M.G. Charging to 150 - 160 deg C Cleared for 240 - 250 deg C
M.G.
No
No
D
Heating kept open
Maintain Temp.
N2 Purging
TP Outlet temperature Removal of WOR
D No
Maintenance of reflux rate
Check
Heating to 170 -180 deg Maintenance for 1 hrs. Heating for poly. for dv Is dv &Dil.Visc.= 68 - 80 sec
Acid Value = 10 - 16
Max. 250 deg & AV AV ok
Yes
Agitation of blender
Blender should have
some material
Flushing of
Discharging to Cooling of the batch Stop heating / reduce
Reactor Blender Quenching & temp. Red. 200 deg C RPM
 Clean Reactor Temp. at 180 - 200 deg C Batch cooled to 200 deg C
References :- ISTM test method :- M.G. tolerance checking

phthalic compatibility ;
Viscosity ; %NVM ; Acid value
GPI :- General Processing Instruction
SPI :- Specific Processing Instructions
WI :- Work Instructions
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Chemistry involved in above-mentioned process is :-

Alkyd preparation by M.G.Process
CH2OH CH2OH CH2OCOR1 CH2OH Tri Glyceroides

| |
CH OCOR2 CH OH +
C + | |
CH2OCOR3 CH2OCOR3 Diglyceroides
CH2OH CH2OH
Pentaerythritol Oil ( Triglycerides) Monoglyceroides
M.G. + Phthallic Anhydride + Pentaerythritol Alkyd
(CH2OH)2 O O CH2OH
CH2OCOCH2 - C - CH2O O-- C O O-C C - O - CH2 - C - CH2 - 0 - C
COOH
CHOCOR2
CH2OH n
CH2OCOCH2
O O CH2OH O
----------------- O - C C - O - CH2 - C - CH2 - 0 - C -----------------

CH2OH
Fatty Acid Fatty Acid Benzoic

Acid
PAN Penta
Alkyd
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(2) Alkyd by Acidolysis Process
Acidolysis process is also known as half ester process. In this process, oil (CCO) reacts
with phthalic anhydride. During this, one acidic group of phthalic anhydride reacts with
hydroxyl group of ricinoleic acid which is present in the castor oil and ester groups are
formed without removal of water. In the second part, when pentaerythritol or sorbitol is
added along with phthalic anhydride or rosin further esterification reaction takes place.
The systematic processing steps are given below.
(a) Charging :
 General Checks
 Charge oil to the reactor.
 Start heating, stirring and N2 purging at the rate of 200 litre / hr.
 Charge Polybasic Acid (part-1) and xylene part I.
 Raise the temperature to 170 -1800C.
 Maintain the temperature till the desired acid value is obtained in the specified
time and range . Cool the batch to the desired temperature.
(b) Post Acidolysis Charging :
 Charge Monobasic Acid (Rosin) if specified, Sorbitol solution in the specified time at
specified temperature.
 Remove water of Sorbitol and charge other Polyol and Polybasic Acid (part-2), Xylene
and add antioxidant.
(c) Dehydration and Esterification Stage :
 Raise to dehydration temperature. Remove water of reaction azeotropically.

 Check the samples periodically for achieving the desired M.T. tolerance, acid
value and viscosity to complete dehydration.
 After achieving the desired constants, cool the batch to 230 - 220 deg C , add xylene
as per specification and then start heating and process the batch at 230-2400C.
 Sample should be checked periodically.
 After attaining desired viscosity and acid value stop heating and start stripping.

 Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix it in the reactor.
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Reactor Stage Process map of Alkyd Processing by Acidolysis Process
N2 Purging
TP Outlet temperature
Castor Oil Charging Heating of Oil Polybasic Acid and Heating for Acidolysis
Xylene Charging 170 - 180 deg C
Keeping the Agitation on

Cooling the batch A.V. Check
Heating to 140 - 150 Deg C Rosin Charging Yes forAcid
to 100 - 120 deg C Attained
Value
Charging At Right Rate No
at 140 - 150 temp continual
Removal of WOS No
Sorbitol Charging
Cooling to 120 deg
Post Sorbitol Charging
( Polybasic Acid , Polyol ,
Xylene , Antioxidant )
170 - 180 deg C
D
Maintain the temp at
Is MTO Check
Tol., dv for dv Removal of WOR
Heating For Dehydration
& AV & AV Dehyd. at temp 260 - 265 deg C
N2 Purging
Achieved Maintenance of reflux rate
MTO
NO tolerance
Keep Heating on and
Maintain temp. at 260 - 2650
Removal of WOR
D No
N2 Purging
Maintenance of reflux rate
Yes Cooling of the batch to
Check
210 - 220 deg and
Heating for poly. for dv Is dv &
Xylene part III addition Max. 240 deg & AV AV ok
Max. Temp. 240 deg C
Yes
Blender should have
some material
Flushing of
Reactor Blender Quenching & temp. Red. 180 - 200 deg C RPM
Clean Reactor Temp. at 180 - 200 deg C Batch cooled to 180 - 200 deg C
References :- ISTM test method :- Viscosity ; %NVM ;

Acid value ; MTO tolerance
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(3) Alkyds by Homogeneity Process

In this process, Oil, Rosin and Polyol form a homogeneous mixture first. And then
polybasic acid and other raw materials are added and further esterification takes place.
The systematic processing steps are given below as
(a) Charging :
 General Checks
 Charge Oil to the reactor.
 Start heating, stirring and N2 purging at the rate of 200 Lit/hr.
 Charge Monobasic Acid (Rosin) at 100-1250C, Polyol and Xylene.
 Raise to homogeneity temperature within 2-4
 Maintain the temperature till the desired acid value for homogeneity is obtained.
 Cool the batch to 1800C or below and stop N2 flow.
(b) Post Homogeneity Charging :
 Charge other raw materials.

 Start heating and N2 purging. Heat and maintain at 170+-50C for 1hr.
(c) Dehydration and Esterification Stage :
 Heat to dehydration temperature. Remove water of reaction azeotropically. check the

samples periodically for achieving the desired M.T. tolerance, acid value and viscosity
at dehydration.
 After achieving the above constants, process the batch at the final temperature.
Sample should be checked periodically.
 After attaining desired viscosity and acid value, stop heating and start stripping.

 Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix it in the reactor.
References :- ISTM test method :- Viscosity ; %NVM ; Acid value

MTO tolerance
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(4) Alkyds by Fatty Acid Process
In this process, all the raw materials viz. fatty acid, polybasic acid , polyols , monobasic
acid , xylene are charged at single stage.
The systematic processing steps are given as under.
(a) Charging :
 General Checks
 Charge fatty acid into reactor.
 Charge all other raw material into reactor.
 Raise the temperature to 1700C or as specified and maintained for 1hour.
(b) Esterification Stage :
 Continue N2 purging, heat to esterification temperature. Remove water of reaction

azeotropically. Check acid value and viscosity periodically.
 After attaining desired viscosity and acid value stop heating and start stripping if
specified in the SPI.
(c) Stripping and Thinning Stage :

 Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix in the reactor.
References :- ISTM test method :- Viscosity ; %NVM ; Acid value

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Reactor Stage Process map of Alkyd Processing by Fatty Acid Process
Fatty Acid Charging
Polybasic acid , Polyol

Monobasic acid , Xylene charging
Heating kept open

Maintain Temp.
N2 Purging
TP Outlet temperature Removal of WOR
D No
Time of maintaining the temp. Maintenance of reflux rate
Check
Heating to 170 -180 deg Maintenance for 1 hrs. Heating for poly. for dv Is dv &Dil.Visc.as per SPI
Acid Value as per SPI
Max. 240 deg & AV AV ok
Temperature at 170-180 deg C Max. Temp. 240 deg C
Yes
Blender should have
some material
Flushing of
Reactor Blender Quenching & temp. Red. 200 deg C RPM
Clean Reactor Temp. at 180 - 200 deg C
Note :- General Checks :- It involves following Activities
 Checking the reactor hygiene

 Check the Reactor Bottom valve getting closed / not bypassing
 Check and ensure that no line is open to reactor .
 Check and ensure that the all RMs are available in sufficient qty. at shop floor before
starting the batch
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(B) Thinning and Filtration stage
Dil .Viscosity % NVM , Gardner

Adjust blender to reach reqd.
Adjusted as per SPI
Viscosity & % NVM
Heat input from Thermopac Heat blender to Materail at 140 - 150 deg C temp.
Agitation kept on 140 - 150 deg C
Start Filtration
Check
Finish
No
No Check
Should be 7
Is Finish
O.K.? D Finish
Is Finish
Should be 7
O.K.?
Yes
Yes
Transfer to tank / Barrel
References :- ISTM test method :- Viscosity ; %NVM

GPI :- General processing instruction
SPI :- Specific Process Instruction
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Points to be taken care during processing of Alkyd batches

Raw material related Points
1. Oil
 If the quantity of Soya / RLO charged in any Soya / RLO based formulation is more,
then the viscosity pick up in the batch will be slow, resulting in higher cycle time. If the
quantity charged is less, then the pick up in viscosity of the batch will be higher.
 If the quantity of DCO (m) charged in any Soya + DCO (m) based formulation is more,
then the viscosity picks up in the batch will be higher. If the quantity charged is less,
then the pick up in viscosity of the batch will be higher due to lesser oil content in the
batch.
 If the quantity of CCO charged in acidolysis batch is more, then AV at acidolysis stage
will be low and if the quantity is less, then the AV will be high. The effect this low / high
AV on the batch are as follows
Acid Value Dehydration rate Further reaction Final properties

Lower Higher Higher pick up High AV
Higher Lower Stagnancy Low AV
2. Catalyst
 Catalyst needs to be charged at specified temperature. Addition at lower temperature

will result in catalyst poisoning, which will result in higher time for achieving MG or less
Alcohol tolerance. Less alcohol tolerance will result in filtration problem.
 If the quantity of the catalyst charged is less, it will result in higher time for achieving
MG or less Alcohol tolerance.
 Extra quantity addition of catalyst will effect the clarity of the medium, further process
and filtration. LATH reacts with phthalic anhydride and forms lead phthalate, which is
an insoluble , sticky compound . During filtration , it sticks to filter cloth and affects the
rate of filtration.
3. Polyol
 Higher quantity of polyol in pre MG stage will result in low clarity in MG tolerance and
lower quantity of polyol, results in lesser MG tolerance.
 Higher quantity of polyol in post MG/acidolysis stage will result in stagnancy in

viscosity pick up. Lower quantity results in high viscosity pick up and higher acid
value.
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4. Phthalic anhydride
 Less quantity of phthalic will result in lower acid value and stagnancy in viscosity
pickup.
 Higher quantity will result in high acid value , high viscosity pickup. The reaction may
go uncontrollable.
5. Maleic anhydride
 The quantity of maleic is very critical, a slight higher quantity can lead to very high
viscosity pick up and gelation .
6. Xylene
 If the quantity of the xylene charged in less, this will result in low reflux rate, high acid
value, reactor temperature shoot up, wrong discharging of the batch( batch will be
under polymerised), stripping at wrong viscosity ( this will cause stagnation of the
batch)
 If the quantity of xylene charged is higher, this will result in high reflux rate, low acid
value ( lower than the specification), maximum process temperature will not be
achieved (this will effect the cycle time), wrong discharging of the batch( over
polymerised batch - this may result in filtration problem.)
7. Antioxidant
 If not charged as per sequential order or not charged than colour value of the batch will
be higher.
8. Nitrogen purging
 If not done colour value of the batch will be higher. Nitrogen purging also helps in
enhancing the reflex rate, hence reduction in acid value.
Operation related
If the temperature of batch is not raising
 Check heating valves whether it is closed or open

 Check thermopak is running or not.
 Check thermopak temperature settings. ( Return and Outlet temperature )
 Check cooling valves whether it is open or closed
 Check water level in separator. If it is high drain the water to specified level)
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 Check xylene content in the batch by keeping controlling solids .( Controlling solid is
less means higher solvent contents )
If cooling is not achieving
 Check cooling tower is running or not

 Check the pressure on the cooling water head
 Check heating valves
 Check cooling tower fun running or not
 Check water level in the cooling tower bin / basin
 If the viscosity pickup is very high in the batch, this also may result in inefficient cooling
of the batch.
If temperature is going high
 xylene content is lesser in the batch

 Vent losses in the batch resulting in less xylene content ( Check cooling in the
condenser)
 Water is drained suddenly from separator
 Reflux line choked
 Check thermopak setting
Phthalic deposition in reflux line and separator
 High phthalic content in the batch.

 Maintenance ( 170 deg ) in the batch not done.
 Water draining from separator is not uniform.
 Maintain the water at lower level in separator
Acid value of the batch is coming on higher side
 Check the normality of KOH

 Slow down the heating of the batch, increase the N 2 purging in the batch, and
increase the reflux rate of the batch.
Very high viscosity picks up in the batch
 Check sample at smaller intervals

 Start cooling of the batch as soon as discharging viscosity is achieved and discharge
the batch
 During cooling also check the sample of the batch.
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Pump is not lifting material
 Check the inlet and discharge valve of the pump

 Check the rotation of the pump
 Check the strainer before the pump
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ACRYLIC RESIN
Acrylic resins are the homopolymers or copolymers based on acrylic acid and their esters .
However polymers based on styrene are also classified as acrylic resins . Thus acrylic
resins are structurally macromolecules of saturated C-C chain obtained by addition of the
individual monomer units across the vinyl group.
Raw Materials :-
A) Initiators :-
Initiates free radical Reaction. E.g. di tertiary butyl peroxide(DTBP), AIBN and Di benzyl
peroxide.
CH3 CH3 CH3 CH3 C=O

|
-
NC C - N = N - C - CN -
H3C C - O - O - C - CH3 O
| Di Benzyl
CH3 CH3 CH3 CH3 O Peroxide
|
AIBN DTBP C=O
Bet Temp. 20 - 100 deg 80 - 150 Deg 40 - 90 Deg

for Use
B) Monomer :-
Examples are as follows :-
ACRYLATES CH2 = CH - C O O R
CH = CH2 Methyl acrylates R - > CH 3 ( 8 Deg )
Ethyl acrylates R - > C2H5 ( -22 Deg )
n-Butyl acrylate R - > C4H9 ( - 54 Deg )
CH2 = CH - CO O H CH3
|
CH2 = C - C O O H METHACRYLATE CH3
|
ACRYLLIC ACID METHACRYLLIC STYRENE CH2 = C - C O O R
ACID
MMA R - > CH3 ( 105 Deg )
EMA R - > C2H5 ( 65 Deg )
HEMA R - > C2H4OH
( 55 DEg )
In order to prevent the premature polymerisation of monomers during storage or transport

the monomer are inhibited by adding suitable inhibitor.
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[C] Solvents:-
(1) Acrylic ester polymers with short side chain are polar and require polar solvents like
ketone, esters ethers or alcohol.
(2) As the side becomes longer the polymer becomes less polar and can dissolve in non
polar solvents like aliphatic hydrocarbon.
Choice of solvents also depends on their evaporation rate.
Processing of acrylic resins
Most widely used commercial process in preparing acrylic co polymers is the free radical
polymerisation, which involves three stages-
a) Initiation:
initiator splits to give the free radical
CH3 CH3 CH3
NC - C - N = N - C - CN 2 NC -C . + N2
CH3 CH3 CH3
I-I 2 I .
b)Propagation:
Initiator free radical attacks the monomer molecule to propagate the reaction.
I . + CH2 = CH - R I - CH2 - CH - R
.
I - CH2 - CH - R + CH2 = CH - R
.
I - ( CH2 - CH - R ) n - ( CH2 - CH - R )
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C) Termination:
This takes place when reactive sites on the polymer chain have rendered inactive.
-
2 I -( 2- CH - R ) n - ( CH2 - CH - R I ( CH 2 - CH ) n - 2- CH - 2-CH- ( 2-CH )n-

| | | |
R R R R
Free radical polymerisation of acrylic monomer may be carried out in any of four basic
polymerisation system.
Bulk - Absence of any solvent.

Solution - Polymerisation carried out in presence of solvent.
Suspension - Polymerisation carried out in the presence of non solvent.
Emulsion - Polymerisation carried out in the presence of non
solvent , usually water but with water soluble initiator.
Controlling of molecular weight during process
 Rate of addition : Degree of polymerisation depends on the rate of addition . Faster

rate of addition will tend to increase the monomer concentration resulting in higher
molecular weight resin . On the other hand slower addition rate will give low molecular
weight resin .
 Initiator Concentration: As initiator concentration increases molecular weight

decreases.
 Type of initiator : AIBN gives lower molecular weight than DTBP
 Processing Solids- High processing solid polymerisation reduces chain transfer activity
of solvents resulting in higher molecular weight system.
Viscosity or molecular weight is proportional monomer concentration and inversely

proportional to initiator concentration.
Precautions to be taken during processing of acrylic resins

a) Temperature:
Since the molecular weight is highly sensitive to temperature, proper temperature

maintenance is necessary.
b)Proper weighing of monomers and initiator :

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Since monomer concentration and initiator concentration play important role in determining
the molecular weight of resin , the weighing should be perfect.
c)Use of metering pump:
Molecular weight also depends upon monomer concentration or processing solids. Faster
rate of addition will tend to increase the monomer concentration resulting in higher
molecular weight resin . On the other hand slower addition rate will give low molecular
weight resin . Hence controlled rate of addition using metering pump is necessary to have
desired molecular weight and viscosity.
d) Storage of monomers, initiators, intermediates (Need to be adhered strictly to the

storage condition).
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AMINO RESIN
Amino resins are produced as a result of condensation reactions between amino
compounds and formaldehyde . The most common amino compounds used are urea ,
melamine , hexamethoxymethyl melamine and benzoguanamine.
Commonly used raw materials in amino resin processing are :-
(a) Paraform
(b) Melamine / Urea / Benzoguanamie
(compound containing -NH2 group.)
(c) Alcohol (methanol / butanol)
A. Formaldehyde and paraform
Preparation of formaldehyde
Ag/Cu catalyst
CH3OH HCHO +H2 -20kcal.
CH3OH +1/2 O2 HCHO+H2O+38 kcal.

Product gases absorbed in water , and gives formaldehyde solution which contain mixture
of CH2(OH)2 and H(CH2O)2 where n=2-3.Paraform is obtained by vacuum concentration of
solution.
Paraform - HO(CH2O)n where n =8-100
=93-99% formaldehyde content
In paraform due to moisture formaldehyde contents drops to 91% or lower.
B. Melamine/Urea/Benzoguanamine (-NH2 group containing compounds)
NH2
C C
// \ O // \
||
N N H2N - C - NH2 N N
| || | ||
C C C C
\\ / \\ /
NH 2 N NH 2 NH 2 N NH 2
Melamine Urea Benzoguanamine

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C. Alcohol‟s
Methanol
Butanol
Isobutanol
Processing of amino resins
Alcoform formation stage Methylalation stage Etherification and

self condensation stage
Filtearion stage Solvent stripping stage

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EPOXY RESINS
 These are the condensation product of Bis phenol (Bis A) and epichlorohydrin(ECH).
Alkali is used as condensing agent [lye= NaOH in DM water]
 Chemically epoxy means a compound containing 3 members cyclic ring of “oxirane”
O
C C
TYPE OF EPOXY RESINS
Solid epoxy Liquid epoxy
Less EPCL More EPCL

Higher soft point Low soft point
High M.Wt. Low M.Wt.
n>2 n=2
Better chemical Inferior chemical
resistance resistance
Manufacturing of epoxy resins

There are two processes by which epoxy resins are manufactured :-
A )Taffy process:
Bis A + ECH
using stoichiometric NaOH
B). Advancement process: (fusion process)
catalyst
Liquid epoxy -----------------------> highly polymer products
(low mol.wt.) Bis A
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TAFFY PROCESS ADVANCEMENT PROCESS
1. Side reactions No side reactions

2. By products No by products
3. No control over material Better control over mat.
4. Long PCT Less PCT
5. Branching No Branching
6. Low cost More cost
Properties imparted by epoxy resins :-
 Toughness
 Flexibility
 Adhesion
 Chemical resistance
 Hardness
 Solvent resistance
 Electrical resistance
 Poor exterior durability
 High stowing schedule
 Little compatibility with other resins
 Interior water resistance
 Less stability in solvents
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EMULSION
What is emulsion polymerisation ?
In this polymerisation reaction , low molecular weight monomers are converted to high
molecular weight polymer . When a solvent is used as a vehicle for polymerisation than
such process is termed as “ solvent polymerisation” and when water is used as a vehicle
than such process is termed as “ Suspension polymerisation “ or “ Emulsion
polymerisation “.
In general , the emulsion is prepared by adding monomer to an aqueous solution

containing water , surfactants , catalyst , buffer , protective colloid at an elevated
temperature of 70 - 80 deg C. The monomers get dispersed in the aqueous phase by
entering into the surfactant miscelles . The catalyst generates free radicals, which initiate
the polymerisation reaction . The monomer polymerises almost completely in the miscelles
to fine solid polymer particles . These polymer particles remain in disperse state . This
dispersion in known as “ Emulsion” .
Role of raw material of emulsion :-

Raw material used in emulsion preparation
Following are the main ingredients of emulsion :-

 Monomers
 Emulsifiers ( Surfactant )
 Catalysts ( Initiator )
 Water
 Buffer
 Chain transfer agent
 Chaser catalyst
 Protective colloids / Thickeners
 Preservatives
 Alkali
 Monomers
Most of the properties of emulsion depend on the nature of monomers. Among the
commonly used monomer some are often termed as „hard‟ as their homopolymers are
very hard and brittle ( High Tg monomer ) . While some monomers are termed as „ soft „
monomer as their homopolymer are tacky , soft and flexible ( Low Tg polymers ).
A combination of hard and soft monomer is often used to produce a emulsion having
intermediate properties like toughness , flexibility , tack freeness etc.
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E.g. :- Methyl methacrylate , Glacial methacrylic acid , Butyl acrylate , Styrene monomer ,
2 - Ethyl hexyl acrylate monomer .
 Emulsifier ( Surfactants )
Surfactants reduces the inter facial tension between two insoluble phases i.e. water and
monomer as a result the monomer gets dispersed in the form of fine droplets , which are
stabilised by the surfactant layer on their surfaces.
Mainly 2 type of surfactants is used for emulsion polymerisation :-

a) Non-ionic surfactant :
These are the most commonly used surfactants for emulsion polymerisation. They are
alkyl phenol ethylene oxide condensate products.
B) Anionic Surfactants :
These are characterised by negative charged large molecules that consists of a
hydrocarbon chain or aromatic ring and the hydrophilic portion is most frequently a sodium
/ potassium or ammonium sulphate or sulfonate
 Catalysts ( Initiator )
Catalysts used for emulsion polymerisation are also known as “ free radical initiators “. On
heating they form free radicals which initiate polymerisation of monomers .
 Water
Almost 50 % of the emulsion are water . Water containing insoluble as well as soluble
impurities like salts are very harmful for polymerisation reaction as well as for emulsion
stability . Filtered and de - ionised water of certain specification is only recommended for
emulsion polymerisation.
Use of deviated property water can result in following problems :-
Acceleration or inhibition of reaction
Discoloration of product
Variation in particle size of product
Coagulation in emulsion during or after processing
 Buffers
During polymerisation disturbance in the specified pH of the solution affects the rate of
reaction as well as emulsion stability hence buffers like sodium bicarbonate are used to
stabilise the pH of the system.
 .Chain transfer agent
The role is to control the molecular weight . E.g. . Tertiary dodecyl mercapten
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 Chaser catalyst
To eliminate the possibility of free monomer in emulsion system , IInd part addition of the
catalyst is done and it is known as chaser catalyst
 Alkali ( Neutralisers )
Certain emulsion i.e. 100 % acrylic , styrene acrylic , should be neutralised for stability
before packing . Alkali like ammonia is used for the same .
 Protective Colloids
Protective colloids are a water soluble polymer added in small quantity during emulsion
polymerisation of Vinyl acetate co - polymer to stabilise the emulsion . No protective colloid
is necessary for 100 % acrylic as well as styrene acrylic emulsions.
 Preservatives
There are several ingredients in emulsion like surfactants , protective colloids which are
prone to bacterial attack due to bacterial attack surfactants and protective colloids get
degraded as a result the emulsion looses viscosity and stability . To eliminate the
possibility of the same , preservatives are added into emulsion system.
 Defoamer
It reduces the foaming hence reduces the packing time of material.

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TEST METHOD
Following are the regularly used test methods :-
1. Water tolerance test for water reducible resin

2. MT tolerance
3. Non volatile matter of hydrocarbon resin solution
4. Determination of acid value
5. Test for monoglycerolysis (MG) and phthalic compatibility
6. Viscosity of resins by ford viscosity cup
7. Viscosity by Gardener bubble viscometer
1. Water tolerance test for water reducible resin

Apparatus:
 100 ml glass beaker.

 Glass rod or spatula.
 Reference glass plate (8 inch x 6 inch x 3mm) with paper label .
Procedure:
 Take 20 grams resin sample in a 100ml glass beaker .

 Dump 20 ml D I water (without stirring) at a stretch in a beaker.
 Stir the mixture with a glass rod or a spatula .
 Observe the solution clarity as such as well as by keeping the beaker on the glass
plate with marked block . Sample is considered free from haze if you can clearly
read/see the writing /marks through material.
 If the sample is free from haze in above test , further repeat step 2 to 4 by additional 20
grams of water and observe for clarity and haze.
2. M T O Tolerance
Reagents :
 Mineral turpentine ( HP/BP 1:1)
Apparatus:
 100 ml measuring cylinders-2Nos.

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Procedure:
 Take 10 ml of the resin in a clean and dried measuring cylinder.

 Add mineral turpentine at a volume of 1ml at a time .
 Mix the contents thoroughly and note the clarity or development of any haze.
 Continue the test till it develops the haze .Continue further till 100ml mark of the
measuring cylinder if it does not develop any haze.
 If it develops haze during addition of mineral turpentine stop addition and note down
the quantity of mineral turpentine added.
 If it does not develops haze even up to 100 ml mark of the measuring cylinder, transfer
10ml of the content to the other measuring cylinder and repeats procedure no. 2,3,4,
and 5.
3. Non volatile matter of hydrocarbon resin solution
Apparatus :
 Flat bottom circular dish of tin or glass approximately 70 mm in diameter .

 Air circulated oven maintained at 120o C .
 U clip - 30 mm bright (nickel plated) .
Procedure:
 Weigh dish containing U clip and about 1-1.2 gm castor oil (M1).
 Transfer 0.8-1.2 gm (M2) of well mixed sample to the dish and note the weight
accurately and quickly before there is a loss of weight due to evaporation.
 Spread the material evenly with the help of U clip
 Make sure that castor oil and material is evenly spread over the surface of disk.
 Heat the content (dish along with material ) in oven, which is being maintained at
120oC for 2 hours.
 Remove the dish after two hours and cool it to room temperature.
 Weigh the dish .(M3).
4. Determination of acid value

Apparatus:
 150 ml conical flask

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Reagents:
 0.1 N Alcoholic/Methanolic KOH Solution.

 Xylene/Butanol or Toluene/Isopropanol(Neutralised)
Procedure:
 Weigh accurately to the nearest 0.01 gm ,about 1-2 gm ,depending on the free acids of
material into a conical flask .
 Add nearly 10-15 ml of Xylene/Butanol mixture (1:1 Xylene:Butanol neutralised with
0.1 N alcoholic potassium hydroxide solution) or Toluene -Isopropanol mixture(1:1
toluene: isopropanol neutralised
 with 0.1 N alcoholic potassium hydroxide.
 Shake and warm if necessary.
 Titrate the solution with standard 0.1 N potassium hydroxide solution using
phenolphthalein as indicator.
5. Test for monoglycerolysis (MG) and phthalic compatibility

Apparatus:
 10 ml measuring cylinder.
 SS cup and spatula.
 Hot plate.
Reagents:
 MG reagent comprising of a mixture of AR grade methanol and Absolute alcohol in

the ratio of 10:3 by weight or as specified in Specific Process Instructions(SPI)
 Phthalic anhydride.
Procedure:
MG Test
 Take 1 ml sample in a clean and dry 10ml measuring cylinder.

 Cool it to room temperature.
 Add 0.5 ml of M.G. reagent to it.
 Shake well to form a homogenous solution.
 Check the clarity and if it is clear, repeat step-3,4 and 5 till slight haze is observed.
 Note the quantity of M.G. reagent added till the clarity persists.
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Phthalic compatibility test
 Take M.G. sample and Phthalic anhydride in SS cup in ratio by as the quantities of
resin charge.
 Stir with the spatula and heat the mixture till the melting temperature of phthalic
anhydride is attained
 Keep the mixture stirring till the sublimed Phthalic Anhydride starts getting collected
along the edges of the cup.
 Take a drop of sample on glass plate and cool it to room temperature.
 Check for the clarity .It should be clear.
6. Viscosity of resins by ford cup

Apparatus:
 Calibrated Ford cup B4

 Timer - A stop watch graduated in division of 1.0 seconds.
 Thermometer -accurate to 1.0 oC
 A suitable stand, provided with levelling screws.
 A spirit level.
 Sieve /Nylon cloth -About 20-40 mesh.
 A suitable receiver.
Procedure :
 Place the ford cup on the stand. Level the cup by adjusting the screws of the stand
.The same may be ensured by using screw level.
 Strain the sample through sieve or nylon cloth ,wherever required.
 Adjust the temperature of the resin and the Ford Cup to the specified temperature( upto
30oC )
 Close the orifice by the forefinger . Fill the cup slowly to avoid formation of air bubbles
till the sample overflows into the gallery.
 Scrape the excess with a spatula over the entire rim of the cup.
 Place the receiver under the cup .The distance between cup and orifice and the base
of the receiver should be about 15 cms.
 Remove the finger and simultaneously start the stop-watch. Stop it as soon as first
break occurs in the stream.
 Time in seconds until the first break occurs denotes viscosity of the resin at that
temperature.
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7. Viscosity by PRS tubes
Apparatus:
 Constant temperature water bath : Any suitable constant temperature bath capable of
maintaining the temperature at 25.0 +_ 1.0 deg oC or any other temperature as
specified in the specifications of the product .
 Empty PRS Tubes of clear glass and flat bottoms.
 Standard PRS tubes
 Viscosity tube corks
 Thermometer
Procedure:
 Fill a viscosity tube with the material under test till the meniscus touches lower
marking line .Fit the cork properly.
 Transfer the tube to a constant temperature water bath maintained at 25 oC or at a
temperature as specified in the specification of the product . Keep it for 10 min. Adjust
the level of the liquid so that bottom meniscus will be in level with the 100mm line .Fit
the cork so that the bottom of the cork is in level with the 108 mm line . This will
ensure a bubble of suitable and uniform size.
 Choose the proper standard tubes(based on expectation ) or as indicated in the
specification for comparing t he viscosity . Allow these standard tubes along with the
tube filled with sample to remain in constant temperature bath for 20 minutes.
 Take out the tubes and invert the tubes ( sample and standard) quickly in such a
manner that the tubes are in perfect vertical plain and the bubble start rising towards
the flat end of the tube .The bottom meniscus of the bubble should be used for
comparing the speed of the bubble . The slower the speed the higher the viscosity .For
this tube holder may be used.
 Due to differences in bubbles sizes and shapes of the ends of the ,it may be necessary
to align the positions of the bubble at the same level initially in-order to have a proper
comparison of the speed of the speed of the bubble .Ensure the observation by
repeating the above procedure.
 Identify the standard tubes that matches with the speed of the bubble in the sample
tube or one having viscosity higher and lower than the sample.
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STANDARD PROCEDURES OF REAGENT
1. Standardisation of alcoholic KOH
 Crush 16 to 20 grams of primary standard potassium hydrogen phthalate and dry in a

petridish at 120oC for two hours .Stopper the container and cool in a dessicator .
 To standardise a 0.5 N solution , weigh accurately 1.5-1.75 grams of dried phthalate
and transfer to a 500 ml volumetric flask .Add 100 ml of distilled water ,stir gently to
dissolve the sample ,add 3 drops of 1.0 % solution of phenolphthalein in alcohol and
titrate with KOH solution to faint pink colour .
 The weights of dried phthalate suitable for other normalities of KOH solution are given
in table below
NORMALITY OF SOLUTION WEIGHT OF DRIED PHTHALATE

0.1 0.35 - 0.40 grams
1.0 3.00- 3.50 grams
Calculation:
Weight of Potassium Hydrogen phthalate
Normality of alcoholic KOH solution =-----------------------------------------------------
0.20442 x Titration reading
2. Standardisation of 0.1n Hcl
 Transfer 2-4 gms. Anhydrous Na2CO3 to a petridish or crucible and dry at 120deg C
for four hrs. Cool in a dessicator.
 To standardise against 0.1 N solution Weigh accurately 0.22+-0.01 gms. of dried
Na2CO3, and transfer to 500 ml. conical flask . Add 50 ml. Of water, swirl to dissolve
the carbonate, add drops of 0.1N solution. Of Methyl Red in alcohol. Titrate with Hcl
solution. To first appearance of red colour and boil the solution. Carefully to avoid loss
until the colour is discharged Cool to the room temperature And continue the titration ,
alternating the addition of Hcl solution And the boiling and the cooling to the first
appearance of a faint red colour that is not discharged on further heating.
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The weight of dried Na2CO3 suitable for other normalities of HCl solution are given in the
table-
Normality Vol. Of Hcl to be diluted weight of dried Na2CO3

to one litre (in ml) `to be used (in gms.)
0.22 1.66 0.088 +- 0.001

0.04 3.22 0.176 +- 0.001
0.20 16.6 0.440 +- 0.001
0.25 20.8 0.550 +- 0.01
0.50 41.5 1.10 +- 0.01
1.00 83.0 2.2 +- 0.01
Calculations:
Gms. Of Na2CO3 used

Normality of Hcl solution = ------------------------------------
0.053 X Burette reading
Standardisation of Hydrochloric acid solution can also be done using standard Sodium
Hydroxide solution as per TM.
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COOLING TOWER
Cooling tower is considered to be the main utility in any chemical plant. It is a packed unit
and can be termed as a heat exchanger.
Uses :-
To cool water and circulate the same to plant accessories / equipment as a service fluid for
cooling i.e. :- Mechanical seal of pumps , to condense vapours into liquid ( used in
condensers ) , Reactor gland cooling , Reactor cooling ( Cooling of the batch )
In the cooling tower the cooling process is known as Evaporating cooling
Evaporating Cooling :-
When water changes its state from liquid to vapour or steam an input of heat energy must
take place which is known as the latent heat of evaporation ; this input energy must either
be supplied from fuel as in boiler or be extracted from surroundings , Cooling tower works
on this change of state by creating conditions in which hot water evaporates in the
presence of moving air ; by this heat is extracted from water and transferred to the air and
the process is known as Evaporating cooling.
Main Components of Cooling Tower
 Casing or shell :-The structure enclosing the heat transfer process reinforced as
necessary to carry out the other main items
 Air inlet and air outlet :- The position at which cool air enters , and warmed air leaves
the cooling tower . In natural draught towers the inlet normally protected by drip - proof
louvers and the outlet by a suitable grill . where as induced draught fan is used the
outlet is the fan casing ; with forced draught the fan casing provides the inlet .
 Fan :- Fan size is important for designing a suitable cooling tower
 Drift elimination :- These are positioned in the outlet air stream so as to prevent water
droplets from being carried away from the tower by the air stream .
 Warm water inlet :- The point from which process water ( warm water ) enters in
cooling tower
 Water distribution system :- Water entering in the tower must be spread as evenly as
possible over the cross section of the tower ( Spray nozzles are provided for this
purpose )
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 Packing :- Consists essentially of a system of baffles which slows the progress of the
warm water through the tower and ensures maximum contact between water droplets
and cooling air by maximising surface area and minimising water film thickness.
 Cold water basin ( Tank / Sump ) :- The point at which the cooled water is collected
return to the process.
 Cold water outlet :- The point, which the cooled water, leaves the tower .
Air Outlet
Fan
Drift
Casing of
eliminator
Shell
Inlet
Conn. Water
Distribution
System
Packing
Louvers
Air Inlet
Over flow connection
O Make up
Outlet
Connection
Cold water basin
Figure :- Schematic arrangement of a mechanical draught cooling tower
The factors which influences the performance of the cooling tower can be summarised as:
1. The cooling range

2. The approach ( Design factor )
3. The ambient air wet bulb temperature (humidity)
4. The flow rate of water to be cooled ( Circulation Rate )
5. The rate at which air passed over the water
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6. The temperature level

7. The performance coefficient of the packing to be used
8. The volume of Packing ( i.e. Height multiplied by horizontal cross - section area )
9. Make up water volume ( Level of water present in Basin / bin )
10. Fan of cooling tower is running or not
Point No. 6 is important, because much greater cooling is possible at higher temp as the
total heat or enthalpy of saturated air rises exponentially with temperature
The physical mechanism of cooling tower operations

The mechanism by which the water is cooled is best understood by the figure given below
Convected Heat
Radiant
Heat
Heat Lost due

to evaporation
Layer of air
at 100 % humidity
and same temp. as water
Bulk unsaturated air flowing passes drople

:-
In the given figure illustrated a single droplet of water in the tower . The droplet is
surrounded by a thin film of air, which is saturated and remains almost undisturbed by the
passing air stream . It is throughout his static film of saturated air that the transfer of heat
takes place in three ways i.e. :-
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 By , radiation from the surface of the droplet : this is a very small proportion of the total
amount of heat flow and it is usually neglected.
 By , conduction and convection between water and air ; the amount of heat transferred
will depend on the temperature Of air and water . It is a significant proportion of the
whole , and may be as much as one - quarter of the one - third.
 By , evaporation ; this accounts for the majority of heat transfer and is the reason why
the whole process is termed „ evaporative cooling „ .
The evaporation that occurs when air and water are in contact is caused by the difference
in pressure of water vapour and in the air . These vapour pressure are functions of the
water temperature Sand the degree of saturation of the air , respectively .
Evaporation , will take place throughout the pack .The amount of evaporation depends on
the total surface area as well as the amount of air flow. The greater the air flow more
cooling can be achieved. This is because as the air rate increases , the effect of the water
on its temperature and humidity will become less , and the partial pressure differences
throughout the pack will increased .
Cooling system failure

Indication:
 Cooling water temperature is high.

 Circuit pressure drop.
Reasons:
 Failure of pump- Cooling water pump fails due to electrical or mechanical problem
.Effectiveness of pump also gets reduced due to air lock.
 Poor water supply- This can be due to choking up of on-line strainer, level of water in
basin goes down, air locking
 Leakage in cooling water line
 Due to power failure.
 High humidity.
 Cooling tower fan not working.
 Water distribution on the top of cooling tower not uniform ( due to choking)
Terminology
Saturated Air :-
The maximum amount of water vapour which air can absorb depends on the temperature
of the air and when this maximum is reached the air is said to be saturated air.
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Wet bulb temperature :-

If the bulb of a thermometer is kept constantly wetted and the evaporation of mixture
encouraged by a moving air stream with minimum velocity 5 meters per second , then the
temperature recorded by the thermometer will be depressed until equilibrium is reached .
The temperature, then recorded is known as the wet bulb temperature and has a precise
relationship to the humidity of the air.
Dew Point :-
The temperature at which a mixture of air and water vapour become saturate .
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THERMOPAC
What is thermopac ?
Thermopac is a forced circulation heater using a non - toxic , non - corrosive oil called
thermic fluid as a heating medium . Temperature upto 300 deg C can be obtained at near
atmospheric pressure . Thus eliminating the use of high pressure vessels and piping.
Constructional features
The thermopac is a fully automatic, coil type, oil fired,3 pass, forced drought, packaged
thermic fluid heater. The helical coil fabricated from steel tubes is constructed to form the
combustion chamber & is paced at the centre of two shells, one inside the other. The shell,
which is adjacent to the coil, is called the inner shell & the one outside the inner shell is
called the outer shell. The inner shell & the helical coil are concentric with the outer shell.
Mineral oil called thermic fluid is circulated through the coil.
The fuel burner is situated at the top centre of the helical coil. The burner is down firing
forced draught type with direct electric spark ignition. The combustion air fan & fuel pump
is at the front base of the unit.
Operational features:
The centrifugal type chemical process pump, near the unit circulates the thermic fluid
through the unit & the system. The thermic fluid returning from the user equipment is fed to
the circulating pump through a combined deaerator & expansion tank. Vapours ,gases etc.
are separated from the thermic fluid in this tank. The deaerator tank is connected to the
expansion tank by pipes. The function of the expansion tank is to accommodate the
increased volume of the thermic fluid ,when it is heated. Thermic fluid expands by 7% of its
total volume for every 100 C rise in temperature.
Heat liberated by burning fuel in the combustion chamber is utilised for heating the thermic
fluid in the coil. The products of the combustion after they exchange their heat with the
thermic in the coil are let out of the unit through the flue gas outlet.
Combustion air preheating is achieved by circulation the fresh air for combustion through a
double jacket formed by the inner shell surrounding the combustion chamber. A high
degree of combustion air preheating ensures high thermal efficiency.
After the rotary switch is put in “BURNER ON” position, the burner starts & the
temperature of the thermic fluid goes on increasing to the required degree.
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The return temperature combistat ( & an outlet temperature combistat in case of TP-10 )
keep the thermic fluid temperature under control by making the burner to work either ON-
OFF or on modulation as the case may be.
Thermoapac is basically either oil fired or gas fired . The sequence of operation of oil fired
units are described below:
1. Ensure taps in the pump of cooling tower line opened.
2. When the electric main switch is put on, supply comes to the panel box.
3. After the FO temperature Reaches 90 deg C , the push button switch for fuel circulation
to be kept pressed . Fuel oil preheating starts when the rotary is put on ( applicable to
furnace oil or LDO ) .The fuel oil temperature combistat indicates & controls the fuel oil
temperature. It normally indicates the actual temperature . The set pointer 1 is set to
control the minimum temperature & the set pointer 2 is set to control the maximum
temperature . Normally the set pointer 1 is set at 105 C & the pointer 2 at 120 C ) .The
burner can be fired only when the fuel oil temperature is above 105 C.TP-01 & TP-02
operates only on LDO/HSD. for other units two oil preheating tanks can be provided, one
electrically operated & the other thermic fluid operated.
4.The blower motor (which also drives the fuel pump) starts & the circulation of fuel oil
starts through the fuel oil preheating tank & the burner rod. The fuel oil temperature
increases . Simultaneously the rotary switch for Thermic fluid pump is also put on .
Thermic fluid circulating pump starts & the flow of thermic fluid is established in the coil &
circuit.
5.On observing the pump pressure gauge & circuit pressure gauge is showing steady
pressure & after the fuel oil temperature crosses the minimum temperature mark of 105C,
the rotary switch is put in “ BURNER ON” position.
6. The blower motor starts . The blower pushes air through combustion chamber ,driving
away combustible gases ,if any, from the combustion chamber. This is known as
prepurging. At the same time ,fuel oil pressure is also developed ,as the blower & the fuel
pump are driven simultaneously
7.After prepurging
 Sparking starts
 Burner solenoid valve energises & oil is sprayed into the combustion
chamber.
 Flame is established & sparking stops.
 Heating of thermic fluid starts.
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8. Hot oil is supplied to the user equipment. It exchanges its heat with the material being
processed & returns to the circulating pump through the combined deaerator & expansion
tank.
9. Heat is given to the user equipment & is absorbed in the user equipment . If heat
absorbed from the thermic fluid is less, then the temperature of the thermic fluid returning
from the process increases. When the return temperature of the thermic fluid reaches a
value set on the return temperature combistat, the burner stops firing. The circulating
pumps keeps on circulating the thermic fluid. The burner restarts as soon as the return
temperature of the thermic fluid drops below the set valve. This is known as “ON-OFF”
operation of the unit.
10.In the case of TPA-10,TPA-15 & TPA-20 the return temperature switch controls the
„high flame-low flame‟ operation of the burner. When the return temperature of the thermic
fluid is less than the value set on the return temperature controller, the burner keeps on
firing at high flame & the unit gives full rated heat output. As soon as the return
temperature reaches the set value of PID controller burner goes into low flame. This is
called the “low flame operation” of the burner .Thus in low flame operation ,the unit gives
only 33% of the full rated heat output. The burner goes to high flame again as soon as the
return temperature drops below the value set on the return temperature controller
.Similarly in some of the thermopak outlet temperature controller controls the ON_OFF
operation of the burner.
11.The outlet temperature switch serves as a ultimate safety against overheating of the
thermic fluid. The burner goes to electrical lock out giving alarm when the temperature of
the thermic fluid reaches the valve set on the outlet temperature switch. In such case, the
reason should be sorted out.
Note :-
Modulation Mechanism :-
1. Modulation motor is provided to control air by throttling the side damper and oil by
regulating the opening of ball valve by means of corresponding linkages.
2. Modulation will be from 33 % to 100 % i.e. in low flame output will be 33 % of the rated
output end in high flame it will be 100 % of the rated output.
3. Initially unit will run in low flame and then unit switches over to high flame when the
toggle switch is put “ ON”.
Controls & safeties:

A. On the unit
1. Sequence controller & flame detector

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The sequence controller in conjunction with the flame detector ensures the following:
 Scavenging of the combustion chamber before every fresh firing of the burner.
 No delay in the firing of the fuel & hence no accumulation of fuel inside the combustion
chamber which eliminates the danger of backfiring.
 Flame failure protection :
The controller consisting of a number of relay/contacts controls the sequence of operations

while starting & running the unit. After preparing & ignition, the fuel is let into the
combustion chamber by energising the burner solenoid valve. Flame should be
established within a few seconds from the time fuel is let into the combustion chamber.
Otherwise through the flame detector circuit, the unit goes to electrical lockout shutting of
the entire system giving an alarm. Restarting of the burner requires resetting of the reset
push button. If flame failure occurs , the unit is brought to lockout position giving an alarm.
Thus no accumulation of fuel & hence no backfiring is resulted.
2. Differential pressure switch
Pressure taping are taken across the unit inlet & outlet & fed to the differential
pressure switch. This switch does not allow the unit to function in case the flow of
thermic fluid through the coil of the unit is insufficient. Any attempt in electrical lock-
out sounding an alarm . On a working unit ,if flow of fluid decreases, burner stops
firing & alarm is sounded.
3. Return temperature & outlet temperature switches
The inlet temperature switch indicates & controls the temperature of thermic fluid at
the inlet of the unit. This makes the burner to work ON-OFF in TP-01 to TP-06
models & in case of TPA-10, TPA-15 & TPA-20 it makes the burner to work on
modulation .The outlet temperature switch indicates & controls the temperature of
thermic fluid at the outlet & in case this temperature exceeds the pre-set limit, the
burner goes into electrical lock-out sounding an alarm.
4. Low level switch in deaerator cum expansion tank:
If the level in the deaerator & expansion tank is below the required level of this
switch it makes the burner trip.
5.Stack temperature indicating alarm:
This control shut off the burner & makes the unit to go into electrical lock-out
position in case the stack temperature rises beyond its set value.
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Reasons for stack temperature going high
 In case the TP tube chokes heavily the heat transfer in the TP is affected due to
reduced flow, this increase the stack temperature
 On over firing due to excessive wear out of burner nozzle the stack temp would
increase.
 If a puncture occurs in TF tube in furnace the leaking fluid would catch fire immediately
increasing the stack temperature.
6. Furnace oil temperature switch:
This controls & maintains FO temperature to a pre-set valve by making the electric
heaters to work ON-OFF
This switch shuts off the burner & makes the unit to go into electrical lockout
position in case the level of the thermic fluid goes beyond tolerable limits. When this
switch takes over, the alarm is sounded.
7. Safety valve in the thermic fluid circuit:
The purpose of a safety valve in TF circuit is to maintain a constant flow rate in the
circuit and the unit . The safety valve safeguards reduced flow . If one of the user
equipment is cut off by shutting valves, the total flow in the system will reduce while
the circuit pressure will increase. If circuit pressure increases beyond a pre-set limit,
the safety valve opens and cut circuit partially the supply and return line.
Trouble shooting
Faults:
1. Flame Failure
 Loose electrical connection to burner solenoid

 Carbon deposition on photocell
 Low furnace oil pressure
 Spray not proper
Action to be taken:
Check electrical connection to burner solenoid valve and rectify. Clean photocell with
cotton from both sides. Clean furnace oil strainers and remove air lock. Check furnace oil
pump and pump pressure gauge. Remove and clean burner assembly. Clean burner
nozzle , check burner setting. Adjust air damper on regulator.
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2.Ciruit Pressure High
 Relief valve not functioning

 Non return valve(NRV) not functioning
 Circuit valve not operated properly
 Pressure gauge faulty
Action to be taken:
Get rectified the setting of relief valve. Get rectified NRV. Check all circuit valve and
ensure that they are in required position .[open/closed].Rectify the gauge.
3. White Smoke From Chimney
 Excess air for combustion

 Oil consumption less
 Wrong burner setting
 Leakage in coil
Action to be taken:
Reduce airflow, adjust oil flow. Stop burner firing and check burner setting.
4. Black Smoke From Chimney
 Excess oil/less air for combustion

 Burner setting disturbed
 Excess air leakage from top plate
 Spray not proper
 Pre-heating temperature Low
 Resistance in fluid gas pass
Action to be taken
Adjust oil/air flow. Stop burner firing, check burner setting.

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BOILER (Optional)
The “REVOMAX BOILER” is an oil-fired, coil type steam generators. The three
pass, reverse flue, membrane coil design is a blend of proven techniques in
combustion & heat transfer technology. It is an instant steam generator of water
tube design. It is a fully automatic packaged unit consisting of the boiler & its
accessories mounted on a chassis & enclosed by outer shell .
The boiler consists of a membrane coil fitted in a shell which in turn is enclosed by
an air jacket. The coil forms the combustion chamber (furnace). Burning fuel
generates heat, which produces steam. High pressure supplies water & fuel to the
boiler & air is supplied by a blower fan.
Working principle
Chemical energy in the fuel is released in the form of heat during combustion .The
products of combustion, the flue gases, transfer this heat to the coil carrying water
by radiation & convection. Residual heat in the flue gases is absorbed in the
economiser, where feed water is heated to expel dissolved gases. The blower
supplies air for combustion. Before the fuel is burned it is atomised by passing
through a swirler in the nozzle under pressure. Light Diesel Oil (LDO) has a low
viscosity so that it can easily atomised. While furnace oil or Low Sulphur Heavy
Stock (LSHS) are too viscous at room temperature & have to be heated to reduce
their viscosity .In our plant we use LDO as a fuel in the Boilers.
The Revomax has a reverse flue type furnace. The flame travels down in the
furnace & the flue gases forms an envelope around the flame, so that the flame
does not touch the coil.
Construction
The Boiler is bolted on a bottom chases. Blower control panel & their panels are
also bolted on the chases. The structure is supported by a top chases. Coil is at
the centre of the boiler, enclosed by a pair of concentric shells. Blower is
connected to the boiler by an air duct at the bottom.
A duct joins the economiser to the boiler flue gas outlet. The economiser is a shell
& tube type heat exchanger having a number of vertical steel tubes welded
between two tube plates. The chimney duct is bolted above the economiser.
A heat optimiser is located near the economiser. It is a tube-in-tube heat
exchanger. In RX-04 & RX-06 fuel pump & motor connected by a coupling are
mounted on a common base frame bolted on the module frame. The water pump is
bolted on hinged platform of the module frame. The burner assembly is on the top
plate. Flexible metallic hoses are attached for fuel supply. The control panel
houses the electrical controls, like switches & indicator lamps etc. The control
panel is mounted on its front.
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Sequence of operating for water fuel, air & electrical systems
Water systems
Soft water enters the unit & passes from the shell side of the heat optimiser. It
receives heat from the hot water coming from the economiser. This warm water
then enters the economiser .The hot flue gases passing through economiser tube
bank heat the water. The dissolved gases in the water are released as it is heated
& are vented out through the air vent connection.
Water enters the coil at the bottom evaporates & steam comes out of the top of
coil. Steam pressure & temperature sensing connections are provided on the outlet
header. Steam pressure gauge & the pressure switch (which controls the on-off
operation of the unit )are connected via copper tubes. The steam temperature
indicator cum controller (combistate) senses the steam temperature via its capillary
bulb.
Safety valve ,main steam valve & auxiliary steam valve are mounted on the same
header.
Fuel system:
Fuel from the service tank passes through a filter before entering the fuel pump
in the unit. In RX-04 & RX-06, separate motor drives fuel pump.
The fuel under pressure is filtered again through a fine mesh strainer . A ball valve
is provided for draining off the dirt collected by the strainer. Fuel pressure gauge
indicates the pressure at this point.
When the burner solenoid coil energises, fuel enters the burner rod & is sprayed
through the nozzle. The fuel used in the boiler in our plant is LDO, which is less
viscous hence is directly used instead of passing through the preheater as in the
case of FO.
Air system
The blower drives air into the bottom of the air jacket of the boiler. It is heated as it
passes through the jacket & enters the burner. The flame-cone diffuser plate
combination causes vigorous mixing of air with atomised fuel. The flame is shot
downward in the furnace. Flue gases reverse from the bottom refractory & travel
upward back to the top of the coil. Gases then pass through the gap between coil
& inner shell & enter the economiser from bottom, After passing through
economiser tubes, they are let out of the chimney duct.
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Electrical system: (includes controls & safeties)
The boiler operates on 415 V, 50 Hz, 3 phase, 4 wire electrical supply. The control
circuit voltage is 230 V.
1.Three phase supply is given to blower motor, water pump motor & fuel pump
motor.
2.Single-phase supply is connected to the control circuit through the control fuse.
Neutral is connected to the N.Control circuit works on 230 V AC supplies.
3.When the “fill” switch is put on, water pump motor contactors energised, contact
closes & water pump motor starts.
4.The-safety contactor coil is energised only when all the safeties are in the
healthy condition. Its contact is connected in the burner solenoid valve circuit. If
this contact is open at the time of firing, fuel is not sprayed in the furnace. The unit
goes in electrical lockout giving alarm.
Following safeties are provided in Revomax :-
a) Limit switch for blowdown valve
b)Steam temperature combistat
c)Water level switch
5.When-fire switch is put on, supply reaches fuel pump motor contactor & the
motor starts.
6.After filling up the boiler coil with water, the fire switch may be put on. Supply
reaches terminal 8 of the sequence controller.
7.Burner firing sequence takes place as follows:
 Supply reaches contactor coils of blower, water pump & fuel pump motors
through SC terminal 4 & the motor starts.
 Supply reaches ignition transformer through Sc terminal 3 & sparking starts

between electrode.
 After prepurge period of 6-10 seconds, supply becomes available at Sc terminal

9 & reaches burner solenoid coil. Green light BURNER ON comes on & fuel is
sprayed into the furnace.
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8.When flame is established ,the photoresistor XA senses the light & its electrical
resistance reduces. Ignition stops & the firing sequence is over.
9.When all safeties remain in healthy condition, firing continues till the supply is
available at Sc terminal 8.When steam demand decreases, pressure increases till
pressure controller trips at the pre-set pressure. Supply to SC terminal 8 is then cut
off & firing stops. Green light PRESSURE CONTROL comes on. When pressure
falls pressure controller cut in & burner firing sequence is repeated.
10.The firing sequence may not take place because of any of the following
reasons. This will cause burner trip with alarm.
 Flame has not been established. Photoresistor does not sense light & offers
large resistance to current, hence very small current flows between SC
terminals 1 & 2.
 One or more of the auxiliary contacts of motors are open. No current flows
between SC terminal 1 & 2 .May happen due to tripping of o/l relays of the
motors.
 One or more of the safety devices are not sensing healthy condition.
11.Burner trip with alarm, results in tripping of thermal relay coincide the sequence
controller. Supply reaches SC terminal 7 & hooter starts sounding. Hooter stops
when FIRE Switch is put off. Restarting the unit requires manual resetting.
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SPARKLER FILTER MACHINE

Filtration:
Filtration is an Unit Operation which remove solid particles, gel particles or any other
impurities to separate clear filtrate by means of filter media.
Filtration is carried out using Sparkler filter machine. Filtration of medium is done after
completion of the batch. Medium is pumped into the filter machine by using Gear pump.
Construction:
Filterpress assembly consists of number of horizontal circular plates, which are enclosed,
in a vertical cartridge one above another to make a complete system. The stack of the
plates is completely enclosed within the pressure tight shell.
Each of the circular plate consists of cloth and sieve plate. Material is pumped into the
filterpress by using Gear Pump. Filter media used is either Woven yarn (filter cloth) or
Paper cloth which have pores on the surface. These pores may get clogged with particles
after passing the medium. To prevent this and to increase area of filtration filter aid such
as Dicamol 4254 \ Celite 545 is coated (pre-coat) on each filter cloth. Solvent is used for
precoating.
Model No. and its significance

The first figure of the Model no. Represents the Diameter of filter plates and the last
represents the No. Of plates in the filter.
The middle letter if “ D “ denoted deep plates with larger cake space . While “ S “ denotes
shallow plates with less cake space .
for example :-
18 - S - 11 means 11 plates of 18” diameter ( Shallow Type )filter machine .
Principle of Operation
The liquid enters the filter by way of filter intake and finds its way to the top of several filter
media of the cartridge through the circular opening in the sides of plates. The media arrest
the suspensions and allow the liquid to pass through them and the supporting perforated
screen and then to run down the central vertical channel formed by interposing cups and
go out through the outlet valve.
In model with scavenger features , the bottom bed of the filter is an auxiliary bed used for
scavenging the last part of the liquid remaining in the tank . This bed is connected to
scavenger valve ( an independent valve ). When scavenger is not desired , this bed can be
used for extra capacity.
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Cartridge assembly in A sparkler Filter
Formed powder
cake on filteration
Filter Aid
Screen
Clips
Spacer Cup
O
Plate v
O
O O
O O O
O O O
Central Tie Rod
Compression Ring Compression Cup
O
Side Tie Rod O O

O O O
O O O
O O
O O O
O
O
O O
O
O O
O O
O
O O
O O O
O O
O O O
O
O O O O Ov
O O O
O O O v
Cartridge of plates
Working:
 Clean cartridge and fit it inside the machine.

 Heat the material in blender / reactor to the required temperature.
 For precoating, prepare the slurry of the filter aid in solvent in precoating tub and
circulate through the filter machine by operating appropriate valves. Check clarity of
returned solvent, it should be clear. Drain the solvent used for precoating from filter
machine to tub. Pump the solvent from tub to the empty blender.
 Open the valves from blender / reactor to filter machine header and back to the
blender. Circulate the material (pre heating)
 Open the air vent valve and close the drain valves of filter machine .
 Start feeding the material slowly into the filter machine. When the material starts
coming through the vent line, close the vent line. This indicates that the filter machine is
fully filled with material with out any air trapping.
 Take the material to finish vessel. Circulate the material back into the blender. Check
the finish of the material from finish vessel.
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 If the finish of the material is clear 7+, release the material to tank / barrel. If not
circulate it for some time, check the finish again, still not achieved stop the filter
machine and clean the machine again.
Factor affecting rate of Filtration :

There are various factors which affects the process of filtration. They are
 Cleanliness of the cartridge used for filtration.

 Type and quality of filter media ( cloth and filter aid ) used for filtration.
 Quantity of Filter aid used .
 Temperature of materiel and pressure in the filter machine.
 Viscosity of the material.
 Depends on suction of the pump ( Pumps working and strainer choking).
 Proper filter aid spread on the filter plate (Precoating is done properly or not ).
 In M.G. root batches M.G. tolerance .
 Continuos feed to filter machine
Precautions to be taken during Filtration :
 Ensure that the filter press is clean and ready for use.
 Before starting the filtration, ensure that the auto system is functioning.
 Ensure that strainer on discharge line of blender is cleaned and fitted before starting
the filtration.
 In case of power failure , to prevent medium overflow from the finishing vessel by
closing the valves.
 For ensuring efficient filtration, adjust the pressure of the filter machine below the
maximum permissible pressure.
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Safety
Basic Principal Related to Raw Material Hazardous
Flammability of liquid
Any material presents a fire risk if it will continue to burn in air after the source of ignition has
been removed.
Flammability of vapor
When a flammable liquid is vaporised to form an intimate admixture with air (or o2) and a
source of ignition is subsequently applied, combustion may be propagated with explosion
Flash point and Fire Point

Flash Point of liquid is the lowest temp at which liquid generates enough vapor to form
flammable mix with air. It is roughly the temp. at which vapor conc. Above liquid just
exceeds the lower flammable limit. Vap. Pres of liquid Û liq. Temp. (F1 Pt) Fl. Pt is slightly
below fire point
Highly flammable liquid (HFL)

A liquid is customarily regarded as HFL if its Flash Point lower than surrounding temp (
32°C)
Auto Ignition Temp

At temp very higher than Fl. Pt., flammable liquids or their vapors escaping to atmosphere
will ignite without aid of an external source of ignition.
Vapors of all HFL are denser than air
Occupational Health Hazards

Respiratory system : Due to air borne contaminants
Skin : vulnerable to actions of gaseous, liquid or solid environment. Organis sol. may
cause dermatitis by irritant action
Eyes : Vulnerable to attack by air borne contaminants
Blood : Formation and function of blood may be interfered with chemical agents e.g. Pb &
Benzene
Assessment of hazard
Evaluation of hazard
Safety committees
Good emergency management plan
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Details of hazardous material in Resin House

Raw Material Work place where
S.No Name Harmful Effect PPEs exposure is possible
MTO Vapour causes headache confusion Wear respiratory Sampling,
& respiratory distress. Liquid protection, face shield Addition/Charging ,
irritates skin. If ingested can irritate and protective clothing Filteration , Filter
1 the entire digestive system & may machine making
injure kidneys. If liquid is taken into
lungs severe pneuomintis results.
XYLENE Vapour causes headache, dizziness. Air supplied mask , Sampling,

Liquid irritates eyes and skin. If safety googles/ face Addition/Charging ,
taken into lungs causes severe shield. Plastic gloves, Filteration , Filter
coughing, distress, rapidly apron and shoes machine making
2 developing pulmonary edema. If
ingested causes nausea, vomiting,
cramps, headache, coma & can be
fatal. Kidney and liver damage
SOLV CIX DIST Irritation of eyes and skin if Safety goggles, Sampling,
contacted. If inhaled may cause chemical resistant Addition/Charging
damage to respiratory tract, cause gloves, safety cloths.
3 headache and dizziness. In case of
ingestion may cause bronchio
pneumonia.
BUTANOL Inhalation: Causes anesthesia, Organic vapour mask, Sampling,

nausea, headache, dizzines, irritation fully covered safety Addition/Charging ,
4 of respiratory passage. Mildly goggles/face shield, Filteration , Filter
irritating to skin and eyes. Harmful hand gloves machine making
if swallowed.
ISO PROP Vapour causes mild irritation to eyes organic vapour mask, Sampling , Lab
ALCOHOL & upper respiratory tracts. High face shield, rubber cleaning
conc. may be anesthetic. Liquid hand gloves, apron and
5 irritates eyes and may cause injury. shoes
Harmless to skin. If ingetsed causes
drunkenness and vomiting.
METHANOL Exposure to vapours cause eye Air supply respirator, Sample checking
irritation, headache, fatigue, Boots , safety goggles,
drowsiness. High concs. can protective apron and
produce CNS depressions & optic rubber gloves
6 nerve damage. 50000 ppm will
probably cause death in 1- 2 hrs.
Can absorbed to skin. Swallowing
may cause death or eye damage.
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HEXANE Causes irritation of respiratory tract, Provide face Sample checking

cough, mild depression, cardiac shield/safety goggles,
arrhythmis. Aspiration causes severe plastic or rubber gloves
lung irritation, coughing, Pulmonary
7 edema, excitement followed by
depression. ingestion causes nausea,
vomiting or swelling of abdomen,
headache
TDI This material is toxic to human Self contained During charging

system and if swallowed is FATAL breathing apparatus,
side covered safety
goggles/face shield
8 rubber hand gloves,
protective overclothing
and shoes
MMA Inhalation & Ingestion: Irritation of Provide self contained During charging ,
nose. throat,nausea,vomiting. Skin breathing apparatus, sample checking
& Eyes:Liquid causes severe side covered safety
irritation goggles/face shield ,
9 rubber han d gloves,
protective over
clothing and shoes.
STYRENE Causes moderate irritation of eyes Safety goggles, Face During charging ,
MONOMER and skin. High vapor concentration shield, hand gloves, sample checking
causes dizziness, drunkenness and shoes , air supplied
10 anesthesia. Ingestion: Causes painful mask.
irritation of mouth and stomach
BUTYL ACRL Harmful if swallowed, inhaled or Self contained During charging ,

absorbed through skin. Vapor is breathing apparatus, sample checking
irritating to the eyes, mucous Rubber gloves, Safety
11 membranes and respiratory tract. goggles, Rubber boots
Exposure can cause Nausea,
headache and vomiting
MALEIC Inhalation: Causes coughing, Organic vapor mask, During charging

ANHYD sneezing, throat irritation. Skin: safety face shield,
Contact causes irritation and rubber gloves, boots
12 redness. Vapors cause severe eye and apron
irritation, photophobia and double
vision may occur
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PHOSPHORIC Causes burns of mouth and lips, Face shield, rubber During charging
ACID sour acrid taste, severe hand gloves, protective
gastointestinal irritation, nausea, overclothing and shoes
vomiting, bloody diarrhea, difficult
13 swallowing, severe abdominal pain,
thirst, acidemia, difficult breathing,
convulsions, collapse, shock and
death
AMMONIA Causes burning pain in mouth, Rubber boots, Hand During charging
throat, stomach,constriction of gloves , apron, safety
throat and coughing, followed by goggles. Use of
14
vomitting of blood, Severe eye and protective oil will
skin irritant. reduce irritation
2-ETHYL Harmful if swallowed. Inhaled. Rubber gloves, Safety During charging

HEXYL Vapor or mist is irritating to the eyes goggles, shoes, self
15 ACRYLATE and respiratory tract contained breathing
MONOMER apparatus
ACETIC ACID :breathing of vapours causes Provide PVC hand During charging
coughing,chest pain and irritation of gloves, apron,
nose and throat.May cause nausea complete eye
16
and vomiting.Skin:contact cause protection and
burns.Eyes:contact cause burns. respiratory protection
LAFFSOLVE- Inhalation: Vapors irritate nose and Organic respirator, side During charging
MEB throat. Ingestion: Causes headche, covered safety
nausea, vomiting, dizziness. goggles/face shield,
18 rubber hand gloves,
body overclothing and
shoes
PHTH ANHYD Solid irritates skin and eyes, causing Rubber apron, Rubber During charging
ASN coughing and sneezing. Liquid shoes,, face shield,
causes severe thermal burns approved vapor
19 respirator, leather or
rubber gloves and
shoes.
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GLYCERINE ( Mildly Toxic by Ingestion, Rubber gloves and During charging

ANHYDROUS ) Inhalation, Causes Mild headache, goggles
20 nausea,vomitting. Causes Eye &
Skin Irritation.
MORPHOLINE Toxic by inhalation and ingestion. Wear goggles and During charging
21 Irritant toskin and get absorb by skin plastic or rubber gloves
2EHA Causes Air pack or organic During sample

aneshtesia,nausea,headache,dizzines cannister, safety checking
22 s. Mildly irritating to skin and eyes. goggles. Rubber
gloves, face shield.
TRIETHYL Vapors irritate nose, throat and Provide self contained During charging
AMINE lungs, causing coughing, choking breathing apparatus ,
and difficulty in breathing. Eyes: side covered safety
Causes severe burns. Skin: Clothing goggles/ face shield,
23 wet with this chemical causes burns. rubber gloves,
protective over
clothing shoes
Bisphenol A Dust irritating to respiratory Protective hand gloves, During charging

passages. May cause sneezing. protective
overclothing, shoes,
24
side covered safety
goggles/face shield,
dust mask.
CAUSTIC SODA Inhalation : Causes small burns to side covered safety During cleaning ,
upper respiratory tract and lungs, goggles, face shield, charging
mild nose irritation. INGESTION: dust type respirator,
cause severe damage to muocus rubber shoes and
25 membrane. Severe scaring or rubber hand gloves
perforation may occur. Eyes; Severe
damage. Skin: C auses severe burns.
NITROGEN ( Inhalation : Can cause asphyxiation, Provide self contained During reactor
COMPRESSED ) if atmosphere does not contain breathing apparatus processing,
oxygen. Dizziness, unconsciousness, where insufficient air is Generation
even death can result. Contact of present. Provide safety
liquid with skin and eyes causes face shield, insulated
26 frostbite, burns gloves, long sleeved
trousers worn outside
boots or overhigh top
shoes to shed the
spilled liquid.
HYDROCHLORI Inhalation of fumes results in Chemical protective Sampling

C ACID coughing,choking sensation,irritation suit with self contained
to nose and lungs. liquid causes breathing apparatus, air
27 burns, can burn mouth and the line mask, rubber hand
digestive tract. gloves, face shield and
shoes.
ETHYL Irritation of eyes, nose and throat, Safety goggles, all Sampling
ALCOHOL Headache and drowsiness may purpose cannisters,
occur. Liquid causes intoxication. protective overcolthing
28 The substance affects nervous and shoes.
system and may damage liver.
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POTASSIUM Ingestion : causes severe pain in Safety goggles/ face Sampling

HYDROXIDE throat and epigastrium , shield , respirator for
hematemesis, collapse. Eyes & Skin dust , long sleeves
: causes severe irritation. Inhalation: cotton jacket, rubber
29
Causes severe irritation of the shoes and rubber
respiratory tract and may cause apron.
shortness of breath.
FORMALDEHY Inhalation : Causes coughing, chest Self contained During charging

DE pain, nausea, vomiting and effects breathing apparatus ,
respiratory system, kidney, liver. chemical goggles,
Ingestion: causes nausea, vomiting, protective overclothing
30 abdominal pain and collapse. Skin , synthetic rubber or
contact : causes severe irritation and plastic gloves and
dermatitis. Contact with eyes: causes shoes.
irritation.
CYMEL 1130 Can be harmful if swallowed or solvent mask, solvent During charging
vapors are inhaled. Cause slight skin resistant gloves, safety
31 irritation and eye irritation. goggles, protective
clothing and safety
shoes
DIETHYLENE Ingestion: Causes stupor or coma safety goggles, hand During charging
32 GLYCOL may lead to fatal kidney injury. gloves, apron, safety
Inhalation: Dullness and nausea. shoes and apron.
LATH Early symptoms of lead Protective hand During charging

intoxification via inhalation or gloves, dust mask,
ingestion are most commonly safety goggles/ face
gastrointestinal disorders, colic shield, protective
constipation, weakness which overclothing and
33 goes to paralysis, chiefly of the shoes
exterior muscles of wrists, less
often ankles. Ingestion causes
coma, death in 1-2 days.
Causes irritation to eyes.
Chronic exposure cuses kidney chemical gloves, During charging

and lever damage. Highly irritant rubber gloves gas
34 to skin and body tissues. mask and rubber
Causes headache and laryagits apron
Pyridine
Chemical gloves, During charging
face shield, rubber
35 hand gloves,
Potassium Rubber apron and
Hydroxide gum boots.
Highly corrosive to organic materials
Inhalation at high concentration Rubber/ acid During charging
(>100ppm) causes nose and ressistant hand
throat irritation, Progressing all gloves apron, shoes,
36 the way to pulmonary edema. face shield, Self
Eyes & Skin: causes irritation. contained breathing
apparatus
Dimethylamine
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Good Shop floor Practices
1. Handling of Glassware: Use lubricant while inserting glass tubing into the rubber.
Use suitable hand gloves
2. Handling of Electrical equipment:
 Ensure that exposed wire, open switches and loose wiring are not used.
 Only qualified persons should be allowed to do repairing of electrical equipment.
 Ensure also that earthling and electrical circuit breakers are provided wherever
necessary.
 Handle all electrical equipment with care: do not attempt any repairs while
equipment is on. Keep off from moving parts.
3. Vacuum distillation / distillation: Avoid rapid changes in pressure, which can push
liquid violently out of flask. Use a trap, slow heating rate and release / apply vacuum
carefully in fume cupboard.
4. Compressed gas cylinders:
 Secure cylinders properly.

 Ensure that cylinder trolleys are used for transportation.
 Use Calibrated pressure gauges.
 Keep gas cylinders properly secured with chains.
5. Mechanical problem: Ensure that moving parts are guarded and access to
machinery is easy and safe. Keep instructions for operation of equipment‟s /
instruments at working place wherever necessary. Get defective machinery
repaired.
6. Storage of solvents and other flammables and Gas Cylinders:
 Limit the quantity to be stored. Use suitable containers for storage.
 Do not store large quantities of inflammable / solvent based material in the

Shopfloor.
 Do not store the inflammable / solvent based material near equipment, which may
generate heat or sparks.
 Do not discharge inflammable / solvent based materials in the sink but dispose
them off in the barrel kept for the purpose.
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 Store, handle and dispose various materials in a hazard-free manner.
7. Labelling: Use labels indicating names of chemicals and critical properties on

containers.
8. Housekeeping:
 Avoid loose electrical connections, chemical spillage and disposal of waste by
improper method.
 Ensure that the containers with solvent-based materials are not kept open.
 Turn off all electrical equipment‟s, water taps and other utilities at the end of the
day.
 Shut down procedure (for daily as well as at weekend) to be documented and

followed.
 Operate available exhaust fans periodically or when build up of vapours is

suspected
9. Handling of Shopfloor chemicals :

 Hold solvent and reagent bottle from the bottom and not with the stopper.
 Avoid contact of chemicals and vapours with the skin, eyes, and respiratory
system by prompt use of gloves, goggles and masks.
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PROTECTIVE EQUIPMENTS AND FACILITIES
EQUIPMENT / FACILITY IN SHOPFLOOR
1. Personal Protective Equipment

2. First Aid Facility
3. Fire Extinguishers
4. Eye Wash Bottles / Eye Wash Shower
PPEs:
Introduction: -
Safety products are a positive aid to Safety and contribute in protecting against injuries, or even loss of life.
Certain occupational hazards are present in any normal working environment and employees must be made
aware of the nature of these hazards and should be encouraged to use safety products as a preventive
measure against these hazards.
Personal Protective Equipment (PPE) is such safety product. They are however not a substitute for
engineering, work practice, or administrative controls. Personal protective equipment should be used in
conjunction with these controls to provide for employee safety and health at the work place. Personal
protective equipment includes all clothing and other work accessories designed to create a barrier against
the workplace hazards.
Following pages describe the types of equipment most commonly used for protecting the head, eyes, face,
torso, arms, hands, and feet.
The details of the PPE being used to handle the raw materials in the
section are as under:
PPE CODE Description

1a ORGANIC VAPOUR MASK
1b DUST MASK
1c AMMONIA MASK
2 SAFETY GOGGLES
3a RUBBER GLOVES
3b PVC GLOVES
3c LEATHER GLOVES
3d COTTON GLOVES
4 GUM BOOTS/SAFETY SHOES
5 APRON
6 BREATHING APPARATUS / AIR LINE RESPIRATOR
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Protective equipments including PPE for eyes, face, head, protective clothing, respiratory devices, protective
shields and barriers shall be provided, used and maintained in a reliable condition as required by the
hazards, processes or environment.
The details of hazards and the corresponding PPE required in the

section for protection of various body parts is described as under:
PART OF BODY
HAZARD PPE TO BE USED
NEEDING
PROTECTION
Head Exposure to falling and or flying objects , Safety helmet
striking against obstruction
Exposure to head during powder charging Safety caps
Eye Exposure to flying particles e.g. dust and Safety goggles

chips, chemical splash and vapours
Exposure to radiation during gas cutting and Welder‟s goggles and helmets
welding operations with appropriate shades of
glass
During sampling – Hot material Falling Face protection sheet
Ear Exposure to excessive noise levels Ear plugs, Ear muffs

Hand, Arm Exposure to sharp / rough edges leading to Cut Resistant Gloves
cuts and abrasion
Exposure to Solvents / Monomers PVC hand gloves
Exposure to acids and alkalis Rubber hand gloves
Exposure to strong electrical current Specified rubber hand gloves
for work on electric installations
Hand Exposure to hot material / equipment‟s Cotton-Felt hand gloves gloves
Asbestos gloves
Exposure to acid during hardener packing Surgical hand gloves
Exposure to hard surfaces Leather hand gloves
Foot Exposure to falling objects , chemicals / Safety shoes
striking against obstruction
Exposure to acids and alkalis Gum boots
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Body Exposure to moderately hot objects and Thick cotton uniform

chemicals
Exposure to acids and alkalis PVC apron
Exposure to TDI TDI suit
Exposure to acid during battery charging Apron
Exposure to monomer Monomer suit
Respiratory Passage Contaminants in vapour form which are Self contained breathing
toxic apparatus
3M Organic vapour mask
3M Ammonia mask
Following is the PPE, description and the Do’s and don’t

PPE Description Do’s and Don’t
Safety Helmet IS- 2925  Helmets to be stored in safe and clean
manner.
 Helmet should always be used with the
cradle inside.
 Holes shall not be drilled in the helmet.
 Helmets shall not be painted.
 Helmets shall not be left exposed to sun
when not in use.
 Helmets shall be inspected for cracks.
 Helmets shall be cleaned using mild soap
and detergent.
Safety Goggles  Full view (extremely  Goggles shall be fitted as close to the eyes
light weight non biting edges) as possible to help give widest field of
vision.
 Goggles shall not be cleaned using any kind
of solvents.
 Goggles shall not be used in activities,
which involve toxic, corrosive, and
flammable material.
 Special glasses to be used by welders
during welding and cutting operations.
 Safety goggles should be cleaned using
soap and mildly warm water. The goggles
shall be wiped by tissue paper.
Ear Plugs Foam earplugs with a cord that  Earplugs shall be properly fitted in the ears
drapes around the neck, before use.
enabling user to remove and  Should be washed with mild detergent and
reinsert plugs repeatedly during soap.
the workday. 3M ear plugs- 3M-  Should be kept in the area devoid of dust,
1110 mist and other contaminants.
Ear Muffs 3 M- 1435- Roomy & durable  Should be fitted properly to the ear.
ear cups provide reliable  Should be worn at all times of exposure to
protection for everyday use. noise.
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The lightweight design and  Should be kept in the area devoid of any
flexible headband provide an kind of contamination. Eg. Dust, vapours,
easy fit and comfort to the user. mist etc.
PVC Hand Gloves PVC hand gloves with inside  Gloves contaminated with toxic / infectious
(Yellow colour) Hosiery cotton lining. Best /corrosive material shall not be left
quality gloves designed to give unidentified.
maximum resistance against  The contaminated gloves shall be
acid, alkalis, oils, fats, fuel, decontaminated before being disposed off.
printing inks, inorganic salts,
organic chemicals steam and
grease.
Rubber hand gloves Orange colour thin gloves made  Gloves contaminated with toxic / infectious
(Orange colour) from pure latex rubber. /corrosive material shall not be left
unidentified.
 The contaminated gloves shall be
decontaminated before being disposed off
appropriately.
Surgical Gloves White coloured gloves made  Gloves contaminated with toxic / infectious
from latex rubber. /corrosive material shall not be left
unidentified.
 The contaminated gloves shall be
appropriately
Plastic disposable Light weight and Hygienic. It is
polythene hand gloves transparent and used in  Should be disposed off after one or two
Catering. uses.
 Gloves contaminated with toxic / infectious

Nitrile gloves  Easy and firm grip. /corrosive material shall not be left
 Highly effective for unidentified.
Industrial solvents.  The contaminated gloves shall be
appropriately.
Welding leather gloves  Leather gloves for welding.  Gloves should be cleaned by using soap
and mild detergent.
 Should be checked for worn outs and
replaced if not in usable condition.
Electrical Gloves  Electrical safety gloves  Gloves should be thoroughly checked for
which provide electrical cuts and any kind of damage.
safety.  Gloves should not be wet before usage.
Safety Shoe Protective footwear shall  Safety shoe should be mandatory
comply to IS code for following requirement for all employees in the plant.
parameters.  Gumboots should not be used in the areas
 Impact where there is possibility of impact injuries.
 Compression
 Clearance
 Eg. Bata/ Liberty warrior
Electrical Safety All exposed external metal  Personnel working near open electrical
footwear parts should be non-ferrous and circuits shall not use conductive footwear.
the design of the soles and
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heels is such it provides a path

to ground.
Gum Boots Industrial black colour full size  Gumboots shall be used in the outside
rubber gumboots with anti skid areas.
soles.  Personnel working with corrosive/toxic
liquids should use gumboots.
 Should inspect the inside of the shoe before
usage.
 Should be periodically checked for cuts.
Dust Mask  Use of 3M 8710 IN  Negative pressure (air purifying) respirators
respirator for the exposures shall be fit tested before use.
< 10*TLV of given  Following checks should be done before
contaminant usage.
 One of the first Indian 1. Proper chin placement.
products to, obtain 2. Proper positioning the face piece on
European (EN 1490) nose.
approval. 3. Comfortable strap tension.
 Light weight, economical 4. Ability to talk while wearing face
and durable. piece.
 Advanced electret media 5. Room for safety spectacles.
maximizes user protection, 6. Tendency of face piece to slip.
ensures high filtering  Daily fit test shall be done by the user
efficiency and offers low before use.
breathing resistance to  For daily fit test, negative pressure and
provide longer period of positive pressure tests shall be done.
user comfort.  Negative Pressure test- In this test the
entrance of the respirator is closed with the
help of palm/cloth and inhaling. If the
respirator collapses and no inward leakage
are detected then it indicates that the
respirator has been worn tightly enough.
 Positive Pressure test- It requires the
wearer to close the entrance of the
respirator and exhaling gently into the face
piece. The fit is considered satisfactory if a
slight positive pressure is built up inside the
face piece.
 Dust masks shall be stored to protect them
from dust, sunlight, extreme moisture/ cold
and damaging chemicals.
 Dust mask should be washed and cleaned
as per the manufacturer‟s recommendation.
 Dust mask shall not be stored with folds and
creases and should not be hanged by the
elastic headband.
 Dust masks shall not be stored in toolboxes.
Organic Vapour mask  Use 3M 9913 IN  Masks shall be stored to protect them from
 High protection and comfort dust, sunlight, extreme moisture/ cold and
provided by the advanced damaging chemicals.
electret media.  Mask should be washed and cleaned as per
 Special odour removing the manufacturer‟s recommendation.
carbon filter material gives  Mask shall not be stored with folds and
added protection against creases and should not be hanged by the
elastic headband.
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the nuisance level organic  Masks shall not be stored in toolboxes.

vapours.
Ammonia mask 3 M -6200 with 6004  Mask should be stored in the dust free and
replaceable cartridge. contamination free atmosphere.
 Low maintenance design.  Masks should not be stored in the toolbox.
 Swept back design of  Filter should be checked and changed after
cartridges improves the expiry of its life.
balance and user vision.
 Dual cartridge enhances
the cartridge life and makes
breathing easy.
 Spares are easily available.
 Easy to adjust head straps.
Apron Denim/Cotton apron for working  Apron should be properly kept in the
in the shopfloor. lockers.
 Apron should be washed with soap and mild
detergent.
 Apron should be worn with both the slings
tied up properly.
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SECTIONAL LEVEL PERFORMANCE

INDICATORS
Following are the performance indicators of the section:-
1. OAE : overall asset effectiveness
OAE is the measure of the overall efficiency, capacity ( productiveness) of the Machine /
Equipment under study. It aims at delivering the best out of any machine ( fixed asset ).
OAE is a function of three parameters,
OAE = f n ( Availability, Rate, Acceptance )
OAE = Availability  Rate  Acceptance.
Where,
Total (Actual) Runtime of Asset

Availability ; % Uptime =----------------------------------------------------
Total Available Time
Ideal Batch Cycle Time (BCT)

Rate ; % throughput =----------------------------------------------------
Actual BCT
Acceptance = % Yield or % Fit for use.
One of the ways to measuring the performance / asset utilisation effectiveness has been
RATE INDEX. The procedure to compute the Rate Index is as follows :
Process time available = Total time available for production ( should not exclude
downtimes)  idle times for the want of material  time lost for cleaning between
batches.
Actual rate = Process time available

No. of batches actually made
Rate Index = Benchmark rate

Actual rate
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Benchmark rate for Reactors is :-
Long oil Alkyd Batches 44 Batches per month from a single

reactor
Medium oil Alkyd Batches 25 Batches per month from a single
reactor
Short oil Alkyd Batches 30 Batches per month from a single
reactor
“The Rate Index of 1.0 signifies that the OAE with respect to benchmark rate has been
achieved.”
2. MANDAYS PER TON
Mandays per ton is the measure of Manpower Utilisation in a section. It is the no. of
manpower (operators) used to produce one ton of solid resin.
3. EFFICIENCY
Man power efficiency is a measure of the % Standard shift norms delivered by an

operator in a shift. It reflects the individual performance of operators. Lower the average
efficiency, higher will be the Mandays / Ton.
Efficiency of an operator is computed in the following manner :
Norms delivered
% Efficiency = ------------------------------------ 100
Standard Shift Norms
4. ‘ZERO’ AWD’s and NCP generation.
The Non-Conforming In-Process Batch.
A non-conforming batch or an NCP as it is commonly referred to, is a batch that does not
conform to the specifications . A batch may be deemed non-conforming because it fails the
approval tests at QA or even if it fails critical in-process checks during any stage of
processing of the batch.
Approved With Deviation Batch (AWD)

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It is a batch that does not conform to one (or two) of the specifications and a decision may
be taken to release the batch conditionally.
5. Specific consumption
Specific consumption of following are monitored on sectional wise month wise
a) Filter cloth consumption per ton of solid resins

b) Power consumption per ton of solid resins
c) Water consumption per ton of solid resin
d) Asbestos gloves consumption per ton of solid resin
e) Fuel consumption per ton of solid resin
f) Dicamol consumption per ton of solid resin
6. System Compliance and Audit Performance.
All the sectional work-practices and activities carried out in the section must be in
Compliance to the OCPs (Operational Control Procedures) and Work-Instructions as listed
in the Manuals..
There should be no reportable NORs and NCRs.

( NOR ; Non-compliance observation report , NCR ; Non-compliance report)
7. Housekeeping Standards
Must meet the International Standards of „Kaizen’ and ‘5S’.
8. Safety
No unsafe operations , No dangerous occurrence , No accidents

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Client: Kamdhenu Paints, Gurgaon SPC.

Resin Manual Rev.

Resin Manual Rev.

(1) Alkyd resin.

Resin Manual Rev.

RESIN – CLASSIFICATION IN PAINT INDUSTRY

Alkyd Emulsion Acrylics Epoxy Amino Miscellaneous

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Classification of Alkyd Resins

Short Oil Long Oil Drying Non Drying

On The Basis of oil length

Alkyd Type Oil Contents ( % )

On The Basis of Drying Characteristics

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Resin Manual Rev.

Polyhydric Alcohol (polyols)

CH2OH CH2OH CH2OH CH OH

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CH2OH CH2OH CH2OH CH2 CH2OH

At 210 - 260 deg C

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Fatty Acids and Oils

Oil is made up of glycerides derived from different fatty acids.

The effect of oil on alkyd properties are as follows :-

Triglyceride or Fatty Iodine Speed of Color Gloss

Linseed oil 189

DCO oil 155

Soya oil 135

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Modifier Advantage Disadvantage

Processing Of Alkyd Resin

1. Condensation reaction among alkyd ingredients or alkyd modifiers, including

Examples of Above named reactions during alkyd processing are: -

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A). Esterification and ester exchange: -

The basic reaction involved in an alkyd processing is esterification. This is happening

R1COOH + ROH R1COOR + H2O

R1COO R2 + R3COO R4 R1COO R4 + R3COO R2

2ROH ROR + H2O

At 210 - 260 deg C

Resin Manual Rev.

C) Alcoholysis and Acidolysis

CH2OHCHOHCH2COOR +(CH2OH)2 C(CH2OCOR)2

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Manufacturing of Alkyd Resins

Flow chart of manufacturing of a resin

Oil and Solvent Charging Powder

Heating Processing Cooling

Filteration Approvel from

(A) Alkyd Resin is manufactured by four processes (In Reactor Stage)

(B) Thinning and Filtration Stage (Blender stage)

(1) Alkyds by Mono Glycerolysis:

The systematic processing steps are given below

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(b) Post M.G. Charging:

(c) Esterification Stage:

 Continue N2 purging, heat to esterification temperature. Remove water of reaction

(d) Stripping and Thinning Stage :

 Strip Xylene till discharging viscosity is achieved.

Reactor Stage Process map of Alkyd Processing by M.G. Process

Resin Manual Rev.