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Client: Kamdhenu Paints, Gurgaon SPC. M04-101 Dexter Technologies Issued By Pg 1 OF 80 Resin Manual Rev. 0 Date 19/05/2010 Dexter Technologies RESIN MANUAL KAMDHENU PAINTS PROJECT KPJ-101

Resin Manual (Rev0)

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Page 1: Resin Manual (Rev0)

Client: Kamdhenu Paints, Gurgaon SPC. M04-101

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OF 80

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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

of oil Length

On The Basis

of Drying

Characteristics

Short Oil

AlkydMedium Oil

Alkyd

Long Oil

Alkyd

Drying

Semi Drying

Non Drying

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 :-

C

CH2OH CH2OH

CH2OH CH2OH

CH OH

CH2OH

CH2OH

Pentaerythritol Glycerol

HO CH

CH OH

CH2OH

CH OH

CH OH

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.

HO CH

CH OH

CH2OH

CH OH

CH OH

CH2OH

HO CH

CH OH

CH2

CH OH

CH

CH2OH

OAt 210 - 260 deg C

+ H2O

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Polybasic Acids

CO

CO

O

Phthallic Anhydride

COOH

COOH

Isophthallic Anhydride

CH COOH

||

CHCOOH

Maleic Anhydride

COOH

COOH

Terphthallic Anhydride

COOH

Tetrahydrophthallic Anhydride

( Cis - 4 - cyclohexene -

1,2 dicaroxylic Anhydride )

COOH

2

1

3

4

5

6

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

Acid Source

Iodine

Value

Speed of

Drying

Color

Retention

Gloss

Retention

Linseed oil

DCO oil

Soya oil

Castor oil

Coconut oil

189

155

135

85

9

Approx.

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

Rosin

Faster Dry

Better Brushability

Greater hardness

Better mar resistance

Better adhesion

More yellowing

Decreases exterior durability when used in excess

Benzoic Acid

Reduces alkyd functionality ( Chain Terminator ) and acts as a gelation inhibitor

Greater hardness

Higher viscosity

Faster dry

Improved colour and gloss

Improved chemical resistance

Poor solubility

Poor flexibility

Iso cyanates

Better water resistance

Faster dry

Better abrasion resistance

Greater yellowish tone

Toxicity problem ( During raw material handling )

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: -

HO CH

CH OH

CH2OH

CH OH

CH OH

CH2OH

HO CH

CH OH

CH2

CH OH

CH

CH2OH

OAt 210 - 260 deg C

+ H2O

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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

ChargingCharging Powder

Charging

Thinning

( Blender Stage )

Solvent

Charging

Processing

( Reactor Stage )

Filteration Approvel from

QAD

Heating Cooling

(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

ChargingPolyol Charging

Check

for

M.G.

Heating for M.G. Temp

240 - 250 deg C

DNo

M.G.

Cleared

No

Cooling the batch

to 150 - 160 deg C

TPP Charging , Post

M.G. Charging

Heating to 170 -180 degMaintenance for 1 hrs. Heating for poly.

Max. 250 deg

Is dv &

AV ok

Stop heating / reduce

RPM

Cooling of the batch

200 deg CQuenching & temp. Red.Discharging to

Blender

Check

for dv

& AV

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 Removal of WOR

Maintenance of reflux rate

D

Dil.Visc.= 68 - 80 sec

Acid Value = 10 - 16

No

Yes

Batch cooled to 200 deg CTemp. at 180 - 200 deg C

Agitation of blender

Blender should have

some material

Flushing of

Reactor

Clean Reactor

N2 Purging

No. of coil operated

TP Outlet temperature

Heating kept open

Maintain Temp.

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

C

CH2OH CH2OH

CH2OH CH2OH

Pentaerythritol

+

CH2OCOR1

|

CH OCOR2

|

CH2OCOR3

Oil ( Triglycerides)

CH2OH

|

CH OH

|

CH2OCOR3

Monoglyceroides

+

Tri Glyceroides

Diglyceroides

M.G. + Phthallic Anhydride + Pentaerythritol Alkyd

CH2OCOCH2 - C - CH2O

CHOCOR2

CH2OCOCH2

(CH2OH)2

O-- C OCOOH

C - O - CH2 - C - CH2 - 0 - C

CH2OH

CH2OH

O

O - C

O

n

C - O - CH2 - C - CH2 - 0 - C

CH2OH

CH2OH

O

O - C

O O

----------------------------------

PentaPAN

Fatty Acid Fatty Acid Benzoic

Acid

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. (d) Stripping and Thinning Stage :

Strip Xylene till discharging viscosity is achieved.

Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix it in the reactor.

Discharge the batch to a blender containing pre-arranged solvent under stirring.

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Reactor Stage Process map of Alkyd Processing by Acidolysis Process

Castor Oil Charging Heating of Oil Polybasic Acid and

Xylene Charging

Check

forAcid

Value

Heating for Acidolysis

170 - 180 deg C

DNo

A.V.

Attained

No

Cooling the batch

to 100 - 120 deg C Rosin Charging

Heating for poly.

Max. 240 deg

Is dv &

AV ok

Stop heating / reduce

RPM

Cooling of the batch

180 - 200 deg CQuenching & temp. Red.Discharging to

Blender

Check

for dv

& AV

Max. Temp. 240 deg C

DNo

Yes

Batch cooled to 180 - 200 deg CTemp. at 180 - 200 deg C

Agitation of blender

Blender should have

some material

Flushing of

Reactor

Clean Reactor

YesHeating to 140 - 150 Deg C

Sorbitol ChargingCooling to 120 deg

Post Sorbitol Charging

( Polybasic Acid , Polyol ,

Xylene , Antioxidant )

Heating For Dehydration

Dehyd. at temp 260 - 265 deg C

Is MTO

Tol., dv

& AV

Achieved

Check

for dv

& AV

MTO

toleranceKeep Heating on and

Maintain temp. at 260 - 2650

NO

Cooling of the batch to

210 - 220 deg and

Xylene part III addition

Yes

Removal of WOR

N2 Purging

Maintenance of reflux rate

Keeping the Agitation on

Maintain the temp at

170 - 180 deg C

N2 Purging

No. of coil operated

TP Outlet temperature

Charging At Right Rate

at 140 - 150 temp continual

Removal of WOS

Removal of WOR

N2 Purging

Maintenance of reflux rate

References :- ISTM test method :- Viscosity ; %NVM ; Acid value ; MTO tolerance GPI :- General Processing Instruction SPI :- Specific Processing Instructions WI :- Work Instructions

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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. (d) Stripping and Thinning Stage :

Strip Xylene till discharging viscosity is achieved.

Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix it in the reactor.

Discharge the batch to a blender containing pre-arranged solvent under stirring. References :- ISTM test method :- Viscosity ; %NVM ; Acid value MTO tolerance GPI :- General Processing Instruction SPI :- Specific Processing Instructions WI :- Work Instructions

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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 :

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. References :- ISTM test method :- Viscosity ; %NVM ; Acid value GPI :- General Processing Instruction SPI :- Specific Processing Instructions WI :- Work Instructions

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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 to 170 -180 degMaintenance for 1 hrs. Heating for poly.

Max. 240 deg

Is dv &

AV ok

Stop heating / reduce

RPM

Cooling of the batch

200 deg CQuenching & temp. Red.Discharging to

Blender

Check

for dv

& AV

N2 Purging

No. of coil operated

TP Outlet temperature

Temperature at 170-180 deg C

Time of maintaining the temp.

Removal of WOR

Maintenance of reflux rate

Max. Temp. 240 deg C

D

Dil.Visc.as per SPI

Acid Value as per SPI

No

Yes

Temp. at 180 - 200 deg C

Agitation of blender

Blender should have

some material

Flushing of

Reactor

Clean Reactor

Heating kept open

Maintain Temp.

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

Adjust blender to reach reqd.

Viscosity & % NVM

Heat blender to

140 - 150 deg C

Start Filtration

Check

Finish

DCheck

FinishIs Finish

O.K.?

Is Finish

O.K.?

Transfer to tank / Barrel

No

Yes

No

Should be 7

Heat input from Thermopac

Agitation kept on

Dil .Viscosity % NVM , Gardner

Adjusted as per SPI

Yes

Materail at 140 - 150 deg C temp.

Should be 7

References :- ISTM test method :- Viscosity ; %NVM GPI :- General processing instruction SPI :- Specific Process Instruction WI :- Work Instructions

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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

NC - C - N = N - C - CN

CH3

CH3CH3

CH3

H3C - C - O - O - C - CH3

CH3

CH3CH3

C = O

|

O

|

O

|

C = OAIBN DTBP

Di Benzyl

Peroxide

Bet Temp. 20 - 100 deg 80 - 150 Deg 40 - 90 Deg

for Use

B) Monomer :- Examples are as follows :-

CH2 = CH - CO O H CH3

|

CH2 = C - C O O H

CH = CH2

STYRENEMETHACRYLLIC

ACID

ACRYLLIC ACID

ACRYLATES CH2 = CH - C O O R

Methyl acrylates R - > CH 3 ( 8 Deg )

Ethyl acrylates R - > C2H5 ( -22 Deg )

n-Butyl acrylate R - > C4H9 ( - 54 Deg )

METHACRYLATE CH3

|

CH2 = C - C O O R

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

NC - C - N = N - C - CN

CH3

CH3CH3

CH3

NC - C .CH3

2 + N 2

I - I I .2

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 - RI - ( 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. -

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 :

I - ( 2 - CH - R ) n - ( CH 2 - CH - R 2 I ( CH 2 - CH ) n - 2 - CH - 2 -CH- ( 2 -CH ) n -

| | | |

R R R R

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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)

C

// \

N N

| | |

C C

\\ /

NH 2 N NH 2

NH2

H2N - C - NH2

||O

C

// \

N N

| | |

C C

\\ /

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 stageEtherification and

self condensation stage

Solvent stripping stageFiltearion 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

CC

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 .

O Make up

Cold water basin

Air Inlet

Louvers

Over flow connection

Outlet

Connection

Packing

Water

Distribution

System

Inlet

Conn.

Casing of

Shell

Fan

Drift

eliminator

Air Outlet

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

Heat Lost due

to evaporation

Bulk unsaturated air flowing passes drople

Radiant

Heat

Layer of air

at 100 % humidity

and same temp. as water

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 105C, 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

vO

O

OOOO O O

O

O

OOOO O O

O

O

OOOO O O

O

v

v

O

Side Tie Rod

Compression Ring

Central Tie Rod

Compression Cup

OSpacer Cup

Clips

Plate

Screen

Filter Aid

O

OOO

O

OO

OO

O

OO

OO

O

OO O O

O

OOOO

O

OO O O

Formed powder

cake on filteration

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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S.No

Raw Material

Name Harmful Effect PPEs

Work place where

exposure is possible

1

MTO Vapour causes headache confusion

& respiratory distress. Liquid

irritates skin. If ingested can irritate

the entire digestive system & may

injure kidneys. If liquid is taken into

lungs severe pneuomintis results.

Wear respiratory

protection, face shield

and protective clothing

Sampling,

Addition/Charging ,

Filteration , Filter

machine making

2

XYLENE Vapour causes headache, dizziness.

Liquid irritates eyes and skin. If

taken into lungs causes severe

coughing, distress, rapidly

developing pulmonary edema. If

ingested causes nausea, vomiting,

cramps, headache, coma & can be

fatal. Kidney and liver damage

Air supplied mask ,

safety googles/ face

shield. Plastic gloves,

apron and shoes

Sampling,

Addition/Charging ,

Filteration , Filter

machine making

3

SOLV CIX DIST Irritation of eyes and skin if

contacted. If inhaled may cause

damage to respiratory tract, cause

headache and dizziness. In case of

ingestion may cause bronchio

pneumonia.

Safety goggles,

chemical resistant

gloves, safety cloths.

Sampling,

Addition/Charging

4

BUTANOL Inhalation: Causes anesthesia,

nausea, headache, dizzines, irritation

of respiratory passage. Mildly

irritating to skin and eyes. Harmful

if swallowed.

Organic vapour mask,

fully covered safety

goggles/face shield,

hand gloves

Sampling,

Addition/Charging ,

Filteration , Filter

machine making

5

ISO PROP

ALCOHOL

Vapour causes mild irritation to eyes

& upper respiratory tracts. High

conc. may be anesthetic. Liquid

irritates eyes and may cause injury.

Harmless to skin. If ingetsed causes

drunkenness and vomiting.

organic vapour mask,

face shield, rubber

hand gloves, apron and

shoes

Sampling , Lab

cleaning

6

METHANOL Exposure to vapours cause eye

irritation, headache, fatigue,

drowsiness. High concs. can

produce CNS depressions & optic

nerve damage. 50000 ppm will

probably cause death in 1- 2 hrs.

Can absorbed to skin. Swallowing

may cause death or eye damage.

Air supply respirator,

Boots , safety goggles,

protective apron and

rubber gloves

Sample checking

Details of hazardous material in Resin House

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7

HEXANE Causes irritation of respiratory tract,

cough, mild depression, cardiac

arrhythmis. Aspiration causes severe

lung irritation, coughing, Pulmonary

edema, excitement followed by

depression. ingestion causes nausea,

vomiting or swelling of abdomen,

headache

Provide face

shield/safety goggles,

plastic or rubber gloves

Sample checking

8

TDI This material is toxic to human

system and if swallowed is FATAL

Self contained

breathing apparatus,

side covered safety

goggles/face shield

rubber hand gloves,

protective overclothing

and shoes

During charging

9

M M A Inhalation & Ingestion: Irritation of

nose. throat,nausea,vomiting. Skin

& Eyes:Liquid causes severe

irritation

Provide self contained

breathing apparatus,

side covered safety

goggles/face shield ,

rubber han d gloves,

protective over

clothing and shoes.

During charging ,

sample checking

10

STYRENE

MONOMER

Causes moderate irritation of eyes

and skin. High vapor concentration

causes dizziness, drunkenness and

anesthesia. Ingestion: Causes painful

irritation of mouth and stomach

Safety goggles, Face

shield, hand gloves,

shoes , air supplied

mask.

During charging ,

sample checking

11

BUTYL ACRL Harmful if swallowed, inhaled or

absorbed through skin. Vapor is

irritating to the eyes, mucous

membranes and respiratory tract.

Exposure can cause Nausea,

headache and vomiting

Self contained

breathing apparatus,

Rubber gloves, Safety

goggles, Rubber boots

During charging ,

sample checking

12

MALEIC

ANHYD

Inhalation: Causes coughing,

sneezing, throat irritation. Skin:

Contact causes irritation and

redness. Vapors cause severe eye

irritation, photophobia and double

vision may occur

Organic vapor mask,

safety face shield,

rubber gloves, boots

and apron

During charging

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13

PHOSPHORIC

ACID

Causes burns of mouth and lips,

sour acrid taste, severe

gastointestinal irritation, nausea,

vomiting, bloody diarrhea, difficult

swallowing, severe abdominal pain,

thirst, acidemia, difficult breathing,

convulsions, collapse, shock and

death

Face shield, rubber

hand gloves, protective

overclothing and shoes

During charging

14

AMMONIA Causes burning pain in mouth,

throat, stomach,constriction of

throat and coughing, followed by

vomitting of blood, Severe eye and

skin irritant.

Rubber boots, Hand

gloves , apron, safety

goggles. Use of

protective oil will

reduce irritation

During charging

15

2-ETHYL

HEXYL

ACRYLATE

MONOMER

Harmful if swallowed. Inhaled.

Vapor or mist is irritating to the eyes

and respiratory tract

Rubber gloves, Safety

goggles, shoes, self

contained breathing

apparatus

During charging

16

ACETIC ACID :breathing of vapours causes

coughing,chest pain and irritation of

nose and throat.May cause nausea

and vomiting.Skin:contact cause

burns.Eyes:contact cause burns.

Provide PVC hand

gloves, apron,

complete eye

protection and

respiratory protection

During charging

18

LAFFSOLVE-

MEB

Inhalation: Vapors irritate nose and

throat. Ingestion: Causes headche,

nausea, vomiting, dizziness.

Organic respirator, side

covered safety

goggles/face shield,

rubber hand gloves,

body overclothing and

shoes

During charging

19

PHTH ANHYD

ASN

Solid irritates skin and eyes, causing

coughing and sneezing. Liquid

causes severe thermal burns

Rubber apron, Rubber

shoes,, face shield,

approved vapor

respirator, leather or

rubber gloves and

shoes.

During charging

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20

GLYCERINE (

ANHYDROUS )

Mildly Toxic by Ingestion,

Inhalation, Causes Mild headache,

nausea,vomitting. Causes Eye &

Skin Irritation.

Rubber gloves and

goggles

During charging

21

MORPHOLINE Toxic by inhalation and ingestion.

Irritant toskin and get absorb by skin

Wear goggles and

plastic or rubber gloves

During charging

22

2 E H A Causes

aneshtesia,nausea,headache,dizzines

s. Mildly irritating to skin and eyes.

Air pack or organic

cannister, safety

goggles. Rubber

gloves, face shield.

During sample

checking

23

TRIETHYL

AMINE

Vapors irritate nose, throat and

lungs, causing coughing, choking

and difficulty in breathing. Eyes:

Causes severe burns. Skin: Clothing

wet with this chemical causes burns.

Provide self contained

breathing apparatus ,

side covered safety

goggles/ face shield,

rubber gloves,

protective over

clothing shoes

During charging

24

Bisphenol A Dust irritating to respiratory

passages. May cause sneezing.

Protective hand gloves,

protective

overclothing, shoes,

side covered safety

goggles/face shield,

dust mask.

During charging

25

CAUSTIC SODA Inhalation : Causes small burns to

upper respiratory tract and lungs,

mild nose irritation. INGESTION:

cause severe damage to muocus

membrane. Severe scaring or

perforation may occur. Eyes; Severe

damage. Skin: C auses severe burns.

side covered safety

goggles, face shield,

dust type respirator,

rubber shoes and

rubber hand gloves

During cleaning ,

charging

26

NITROGEN (

COMPRESSED )

Inhalation : Can cause asphyxiation,

if atmosphere does not contain

oxygen. Dizziness, unconsciousness,

even death can result. Contact of

liquid with skin and eyes causes

frostbite, burns

Provide self contained

breathing apparatus

where insufficient air is

present. Provide safety

face shield, insulated

gloves, long sleeved

trousers worn outside

boots or overhigh top

shoes to shed the

spilled liquid.

During reactor

processing,

Generation

27

HYDROCHLORI

C ACID

Inhalation of fumes results in

coughing,choking sensation,irritation

to nose and lungs. liquid causes

burns, can burn mouth and the

digestive tract.

Chemical protective

suit with self contained

breathing apparatus, air

line mask, rubber hand

gloves, face shield and

shoes.

Sampling

28

ETHYL

ALCOHOL

Irritation of eyes, nose and throat,

Headache and drowsiness may

occur. Liquid causes intoxication.

The substance affects nervous

system and may damage liver.

Safety goggles, all

purpose cannisters,

protective overcolthing

and shoes.

Sampling

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29

POTASSIUM

HYDROXIDE

Ingestion : causes severe pain in

throat and epigastrium ,

hematemesis, collapse. Eyes & Skin

: causes severe irritation. Inhalation:

Causes severe irritation of the

respiratory tract and may cause

shortness of breath.

Safety goggles/ face

shield , respirator for

dust , long sleeves

cotton jacket, rubber

shoes and rubber

apron.

Sampling

30

FORMALDEHY

DE

Inhalation : Causes coughing, chest

pain, nausea, vomiting and effects

respiratory system, kidney, liver.

Ingestion: causes nausea, vomiting,

abdominal pain and collapse. Skin

contact : causes severe irritation and

dermatitis. Contact with eyes: causes

irritation.

Self contained

breathing apparatus ,

chemical goggles,

protective overclothing

, synthetic rubber or

plastic gloves and

shoes.

During charging

31

CYMEL 1130 Can be harmful if swallowed or

vapors are inhaled. Cause slight skin

irritation and eye irritation.

solvent mask, solvent

resistant gloves, safety

goggles, protective

clothing and safety

shoes

During charging

32

DIETHYLENE

GLYCOL

Ingestion: Causes stupor or coma

may lead to fatal kidney injury.

Inhalation: Dullness and nausea.

safety goggles, hand

gloves, apron, safety

shoes and apron.

During charging

33

LATH Early symptoms of lead

intoxification via inhalation or

ingestion are most commonly

gastrointestinal disorders, colic

constipation, weakness which

goes to paralysis, chiefly of the

exterior muscles of wrists, less

often ankles. Ingestion causes

coma, death in 1-2 days.

Causes irritation to eyes.

Protective hand

gloves, dust mask,

safety goggles/ face

shield, protective

overclothing and

shoes

During charging

34

Pyridine

Chronic exposure cuses kidney

and lever damage. Highly irritant

to skin and body tissues.

Causes headache and laryagits

chemical gloves,

rubber gloves gas

mask and rubber

apron

During charging

35

Potassium

Hydroxide Highly corrosive to organic materials

Chemical gloves,

face shield, rubber

hand gloves,

Rubber apron and

gum boots.

During charging

36

Dimethylamine

Inhalation at high concentration

(>100ppm) causes nose and

throat irritation, Progressing all

the way to pulmonary edema.

Eyes & Skin: causes irritation.

Rubber/ acid

ressistant hand

gloves apron, shoes,

face shield, Self

contained breathing

apparatus

During charging

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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

1 a

1 b

1 c

ORGANIC VAPOUR MASK

DUST MASK

AMMONIA MASK

2 SAFETY GOGGLES

3 a

3 b

3 c

3 d

RUBBER GLOVES

PVC GLOVES

LEATHER GLOVES

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

NEEDING

PROTECTION

HAZARD PPE TO BE USED

Head Exposure to falling and or flying objects ,

striking against obstruction

Exposure to head during powder charging

Safety helmet

Safety caps

Eye Exposure to flying particles e.g. dust and

chips, chemical splash and vapours

Exposure to radiation during gas cutting and

welding operations

During sampling – Hot material Falling

Safety goggles

Welder‟s goggles and helmets

with appropriate shades of

glass

Face protection sheet

Ear Exposure to excessive noise levels Ear plugs, Ear muffs

Hand, Arm Exposure to sharp / rough edges leading to

cuts and abrasion

Exposure to Solvents / Monomers

Exposure to acids and alkalis

Exposure to strong electrical current

Cut Resistant Gloves

PVC hand gloves

Rubber hand gloves

Specified rubber hand gloves

for work on electric installations

Hand

Exposure to hot material / equipment‟s

Exposure to acid during hardener packing

Exposure to hard surfaces

Cotton-Felt hand gloves gloves

Asbestos gloves

Surgical hand gloves

Leather hand gloves

Foot

Exposure to falling objects , chemicals /

striking against obstruction

Exposure to acids and alkalis

Safety shoes

Gum boots

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Body Exposure to moderately hot objects and

chemicals

Exposure to acids and alkalis

Exposure to TDI

Exposure to acid during battery charging

Exposure to monomer

Thick cotton uniform

PVC apron

TDI suit

Apron

Monomer suit

Respiratory Passage Contaminants in vapour form which are

toxic

Self contained breathing

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 light weight non biting edges)

Goggles shall be fitted as close to the eyes 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 drapes around the neck, enabling user to remove and reinsert plugs repeatedly during the workday. 3M ear plugs- 3M-1110

Earplugs shall be properly fitted in the ears before use.

Should be washed with mild detergent and soap.

Should be kept in the area devoid of dust, mist and other contaminants.

Ear Muffs 3 M- 1435- Roomy & durable ear cups provide reliable protection for everyday use.

Should be fitted properly to the ear.

Should be worn at all times of exposure to noise.

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The lightweight design and flexible headband provide an easy fit and comfort to the user.

Should be kept in the area devoid of any kind of contamination. Eg. Dust, vapours, mist etc.

PVC Hand Gloves (Yellow colour)

PVC hand gloves with inside Hosiery cotton lining. Best quality gloves designed to give maximum resistance against acid, alkalis, oils, fats, fuel, printing inks, inorganic salts, organic chemicals steam and grease.

Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified.

The contaminated gloves shall be decontaminated before being disposed off.

Rubber hand gloves (Orange colour)

Orange colour thin gloves made from pure latex rubber.

Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified.

The contaminated gloves shall be decontaminated before being disposed off appropriately.

Surgical Gloves White coloured gloves made from latex rubber.

Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified.

The contaminated gloves shall be decontaminated before being disposed off appropriately

Plastic disposable polythene hand gloves

Light weight and Hygienic. It is transparent and used in Catering.

Should be disposed off after one or two uses.

Nitrile gloves

Easy and firm grip.

Highly effective for Industrial solvents.

Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified.

The contaminated gloves shall be decontaminated before being disposed off 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 which provide electrical safety.

Gloves should be thoroughly checked for cuts and any kind of damage.

Gloves should not be wet before usage.

Safety Shoe Protective footwear shall comply to IS code for following parameters.

Impact

Compression

Clearance

Eg. Bata/ Liberty warrior

Safety shoe should be mandatory requirement for all employees in the plant.

Gumboots should not be used in the areas where there is possibility of impact injuries.

Electrical Safety footwear

All exposed external metal parts should be non-ferrous and the design of the soles and

Personnel working near open electrical circuits shall not use conductive footwear.

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heels is such it provides a path to ground.

Gum Boots Industrial black colour full size rubber gumboots with anti skid soles.

Gumboots shall be used in the outside areas.

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 respirator for the exposures < 10*TLV of given contaminant

One of the first Indian products to, obtain European (EN 1490) approval.

Light weight, economical and durable.

Advanced electret media maximizes user protection, ensures high filtering efficiency and offers low breathing resistance to provide longer period of user comfort.

Negative pressure (air purifying) respirators shall be fit tested before use.

Following checks should be done before usage.

1. Proper chin placement. 2. Proper positioning the face piece on

nose. 3. Comfortable strap tension. 4. Ability to talk while wearing face

piece. 5. Room for safety spectacles. 6. Tendency of face piece to slip.

Daily fit test shall be done by the user before use.

For daily fit test, negative pressure and positive pressure tests shall be done.

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

High protection and comfort provided by the advanced electret media.

Special odour removing carbon filter material gives added protection against

Masks shall be stored to protect them from dust, sunlight, extreme moisture/ cold and damaging chemicals.

Mask should be washed and cleaned as per the manufacturer‟s recommendation.

Mask shall not be stored with folds and creases and should not be hanged by the elastic headband.

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the nuisance level organic vapours.

Masks shall not be stored in toolboxes.

Ammonia mask 3 M -6200 with 6004 replaceable cartridge.

Low maintenance design.

Swept back design of cartridges improves balance and user vision.

Dual cartridge enhances the cartridge life and makes breathing easy.

Spares are easily available.

Easy to adjust head straps.

Mask should be stored in the dust free and contamination free atmosphere.

Masks should not be stored in the toolbox.

Filter should be checked and changed after the expiry of its life.

Apron Denim/Cotton apron for working in the shopfloor.

Apron should be properly kept in the 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