Resin Manual (Rev0)

Client: Kamdhenu Paints, Gurgaon

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Dexter Technologies RESIN MANUAL

KAMDHENU PAINTS PROJECT KPJ-101

80 Date

19/05/2010


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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 pro vides 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 i n 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 Resins are the condensation / addition polymers which form by reacting monomer units. It is the film forming material of the paint and provides pro vides 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 i n 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 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 Drying Characteristics

On The Basis of oil Length

Short Oil Alkyd

Long Oil Alkyd

Drying

Medium Oil Alkyd

Non Drying Semi 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 Short Oil Alkyd Medium Oil Alkyd Long Oil Alkyd

Oil Contents ( % ) 35 - 45 % 46 - 55 % 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 i odine value( more than 160) .It has higher unsaturation, unsaturation, which in the presence presence of oxygen 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 Isophthalic Acid Maleic Anhydride Tetra hydro phthalic anhydride

Ajelaic Acid Succinic Acid Adipic Acid` Fumaric Acid

Oils Linseed Oil Soya Oil Castor Oil Tung Oil

Sunflower Oil Cotton seed Oil Dehydrated Castor Oil (DCO) Coconut Oil

Polyhydric Alcohol Glycerine Pentaerythritol Ethylene glycol Trimethylol prophthalice Neopentyl glycol

Sorbitol Propylene glycol Trimethylol ethane Di propylene glycol Di ethylene glycol

Monobasic Acids Fatty Acids obtained from oils Benzoic Acids

Synthetic saturated fatty acids


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Monoglycerolysis Catalyst Lead Acetate Trihydrate ( LATH ) Cerium Octoate 6% Calcium Oxide / hydroxide Di-butyl tin oxide ( DBTO)

Litharge Lithium Stearate Sodium Naphthalene Sodium Hydroxide

Anti Oxidant Hypophosphorous Acid ( HPA )

Triphenyl phosphite ( TPP )

Solvents Xylene C - IX

M.T.O.

Polyhydric Alcohol (polyols) The 3 predominant Polyhydric alcohol used in alkyd resins are :CH2OH CH2OH

CH2OH

CH2OH CH OH

C

CH2OH

CH OH

CH2OH

CH2OH

HO CH

CH OH CH OH

Pentaerythritol

Glycerol CH2OH Sorbitol

The high functionality of Pentaerythritol makes it of wide interest as the polyol for long oil alkyds containing 60 % or more fatty acid, because of its high functionality, Pentaerythritol is often blended with either glycerol or glycol in alkyds containing less than 60 % fatty acids. Pentaerythritol containing alkyd tends to have higher viscosity and molecular weights, dry more rapidly and give coatings of greater hardness with lower flexibility, better gloss and gloss retention, better heat and yellowing resistance better chemical resistance, better water resistance and better exterior durability than glycerol based alkyds of comparable oil contents. In paints, Pentaerythritol types also shows antisagging at equal brushing, brushability and flow.

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The higher functionality of pentaerythritol over glycerol is the main reason for many of above mentioned advantages. Our major quantity of the polyol used is pentaerythritol. We get three types pentaerythritol. They are named as Penta - 88, Penta -98(Penta nitration grade) and Penta technical (Kanoria Penta). The differences between these are based on the purity. Penta exists as mono penta and dipenta. Penta 98/nitration grade contains 98% of monopenta and 2% of dipenta. Penta 88 contains 88% of mono penta and 12% of dipenta and penta technical/ penta Kanoria contains 96% of mono penta and 4% dipenta.

CH2OH C CH2OH

CH2OH CH2OH

CH2OH C CH2OH

mono penta

CH2

C

CH2

CH2OH CH2OH

di penta

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

CH2

CH OH

CH OH At 210 - 260 deg C

HO CH

HO CH

CH OH

CH OH

CH OH

CH

CH2OH

CH2OH

O

+

H2O

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Polybasic Acids COOH

COOH

3

CO 4

COOH CH COOH || CHCOOH

2

O 1

5

CO Phthallic Anhydride

COOH Isophthallic Anhydride

COOH Terphthallic Anhydride

6

COOH

Maleic Anhydride

Tetrahydrophthallic Anhydride ( Cis - 4 - cyclohexene 1,2 dicaroxylic Anhydride )

Phthalic anhydride is the most extensively used polybasic acid in Alkyd resins because of its low cost and the excellent properties it imparts to Alkyd resin products. In recent years Isophthalic acid has been more extensively used in place of phthalic anhydride. Isophthalic acid compared to orthophthalic acids are claimed to have higher molecular weight and higher viscosity, to have better drying characteristics and to give hard and more durable films with better heat and chemical stability. Isophthalic acid is more reactive than phthalic anhydride. The reason is intermolecular cyclization in phthalic anhydride makes it less reactive than Isophthalic acid. The para isomer of phthalic acid, terphthalic acid has very poor solubility in alkyd ingredients It also has very high melting point (436 deg C), has made processing of terphthalic acid based alkyds very difficult. Other dibasic acids used in alkyds in limited amount includes THPA (Tetrahydro phthalic anhydride), Maleic anhydride etc. Maleic acid / anhydride often used to replace part (upto 10 % max on a molar basis) of the phthalic anhydride in the alkyd resin. It reacts with the unsaturation in fatty acids, Its effect is to increase the total functionality of the alkyd system, viscosity and polymer molecular weights. When Maleic anhydride is used in small amounts in phthalic anhydride alkyds they dry more rapidly and give harder films with improved colour, better alkali resistance, better exterior durability because of improved water resistance .

Catalyst Alkyds are manufactured through different routes. One of the routes is through Monoglycerolysis. Here a catalyst is required to convert oil (triglyceride) into monoglyceride. E.g. Lead acetate Trihydrate (LATH), Di butyl tin oxide (DBTO), Cerium Octoate 6%, Liocat etc.


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Fatty Acids and Oils Chemically oils are carboxylic esters derived from the single alcohol (glycerol HOCH2CHOHCH2OH ) and are known as glycerides . More specifically, they are triglycerols. O || H2C-O-C-R | H C-O-CO-R' | H2C-O-C-R" || O A Triglycerol (A glyceride) {here R, R', R'' are fatt y 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 Approx.

Linseed oil

189

DCO oil

155

Soya oil

135

Castor oil

85

Coconut oil

9

Speed of Drying

Color Retention

Gloss Retention

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 fi t 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 Rosin

Benzoic Acid

Iso cyanates

Advantage Disadvantage   Faster Dry More yellowing   Better Brushability Decreases exterior durability when used in  Greater hardness excess  Better mar resistance  Better adhesion  Reduces alkyd  Poor solubility functionality ( Chain  Poor flexibility Terminator ) and acts as a gelation inhibitor  Greater hardness  Higher viscosity  Faster dry  Improved colour and gloss  Improved chemical resistance   Better water resistance Greater yellowish tone   Faster dry Toxicity problem ( During raw material handling )  Better abrasion resistance

Processing Of Alkyd Resin Chemical Reactions involved in Alkyd Processing

The chemical reaction occurs during the alkyd processing are as follows: 1. Condensation reaction among alkyd ingredients or alkyd modifiers, including esterification; ester, alcohol, or acid exchange; and etherification. 2. Addition reaction of the unsaturated hydrocarbon portions of the monobasic fatty acids, including free - radical or Diels - Alder reactions with other alkyd ingredients, modifiers or oxygen. 3. Addition reactions, especially free- radical types with other unsaturated alkyd ingredients. 4. Side reactions such as decarboxylation. Examples of Above named reactions during alkyd processing are: -

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A). Esterification and ester exchange: -

The basic reaction involved in an alkyd processing is esterification. This is happening during the reaction of an alcohol with an acid. It is a reversible reaction (In all alkyd preparation we have polyhydric alcohols and polybasic acids). The reaction is: -

R1COOH + ROH

R1COOR + H2O

Ester exchange or tranesterification reaction is: -

R1COO R2 + R3COO R4

R1COO R4 + R3COO R2

As this reaction can occur in any two-ester molecules, it is of important in alkyd preparations, especially for its effect on the molecular weight distribution in the final product.

B) Etherification: -

At the alkyd processing temp (210 deg to 250 deg C) etherification reaction can occur in alcohols: -

2ROH

ROR + H2O

In an observation made by a scientist, he found that at 240 deg C temp with glycerol 7-8 % esterification can be possible. He reported lesser etherification (Approximately negligible) with pentaerythritol. While sorbitol is found to be more prone to etherification than glycerol because it is capable of internal etherification: CH2OH

CH2

CH OH

CH OH At 210 - 260 deg C

HO CH

HO CH

CH OH

CH OH

CH OH

CH

CH2OH

CH2OH

O

+

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 Charging

Charging

Powder Charging

Heating

Processing ( Reactor Stage )

Cooling

Solvent Charging

Thinning ( Blender Stage ) Filteration

Approvel from QAD

(A) Alkyd Resin is manufactured by four processes (In Reactor Stage) (1) Mono Glycerolysis Process or M.G. Process (2) Acidolysis Process or Half Ester Process (3) Homogeneity Process (4) Fatty Acid Process (B) Thinning and Filtration Stage (Blender stage)

(1) Alkyds by Mono Glycerolysis: In M.G. Process, Oil, which is triglyceride, is first converted into monoglyceride by reacting it with polyol. The resulting mixture is reacted with polybasic acid for further polymerisation reaction. The systematic processing steps are given below (a) Charging:  General Checks  Charge Oil to the reactor.  Maintain appropriate water level in separator.  Start heating as per SPI, stirring and pass N 2 through the batch at approximate 200 litres/hr.


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Charge the Catalyst and stir for 5-10 minutes and then charge Polyol (Part-1) Raise to M.G. temperature as specified in SPI. Maintain the temperature till the desired tolerance for M.G. with specified alcohol is obtained. If the tolerance for M.G. is not in range, proceed further only after passing phthalic anhydride compatibility test. Cool the batch to 1800C or below and stop N2 purging.

(b) Post M.G. Charging:   

Charge Polyol (Part-2), Polybasic Acid, Monobasic Acid, antioxidant & Xylene in sequence. Start heating and N2 purging. Heat and maintain at 170+-5 for 1hr.

(c) Esterification Stage: 



Continue N2 purging, heat to esterification temperature. Remove water of reaction azeotropically. Check acid value and viscosity periodically. After attaining desired viscosity and acid value stop heating and start stripping if specified in the SPI.

(d) Stripping and Thinning Stage :   

Strip Xylene till discharging viscosity is achieved. Cooling to 180-2000C. Thin it partially with solvent and thoroughly mix in the reactor. Discharge the batch to a blender containing pre-arranged solvent under stirring.

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

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Catalyst Charging

Heating of Oil

Date 19/05/2010

Polyol Charging

Temp of Oil 70 to 100 oc

Temp of Oil 100 - 120 deg C

80

Temp of Oil 100 to 160oc

N 2 Purging No. of coil operated TP Outlet temperature

TPP Charging , Post M.G. Charging

Cooling the batch to 150 - 160 deg C

Check for M.G.

M.G. Cleared

Heating for M.G. Temp 240 - 250 deg C

No No

D Heating kept open Maintain Temp.

N 2 Purging No. of coil operated TP Outlet temperature

D

Removal of WOR Maintenance of reflux rate

Heating to 170 -180 deg

Maintenance for 1 hrs.

Heating for poly. Max. 250 deg

No

Check for dv & AV

Dil.Visc.= 68 - 80 sec

Is dv & Acid Value = 10 - 16 AV ok

Yes

Agitation of blender Blender should have some material

Flushing of Reactor



Discharging to Blender

Clean Reactor

References :-

Quenching & temp. Red.

Cooling of the batch 200 deg C

Temp. at 180 - 200 deg C

Batch cooled to 200 deg C

ISTM test method :GPI SPI WI

Stop heating / reduce RPM

M.G. tolerance checking phthalic compatibility ; Viscosity ; %NVM ; Acid value :General Processing Instruction :Specific Processing Instructions :Work Instructions

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Chemistry involved in above-mentioned process is :Alkyd preparation by M.G.Process CH2OH

CH2OH

+

C

CH2OH

CH2OCOR1 | CH OCOR2 | CH2OCOR3

CH2OH | CH OH | CH2OCOR3

Oil ( Triglycerides)

Monoglyceroides

Tri Glyceroides + Diglyceroides

CH2OH

Pentaerythritol

Alkyd

M.G. + Phthallic Anhydride + Pentaerythritol

O

(CH2OH)2 CH2OCOCH2 - C - CH2O

O-- C

O

O-C

O

CH2OH

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

COOH CH2OH CHOCOR2

n

CH2OCOCH2

O ----------------- O - C

O

CH2OH

O

C - O - CH2 - C - CH2 - 0 - C ----------------CH2OH

Fatty Acid

Fatty Acid Penta

PAN

Alkyd

Benzoic Acid


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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. 


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 N 2 Purging No. of coil operated TP Outlet temperature

Castor Oil Charging

Heating of Oil

Heating for Acidolysis 170 - 180 deg C

Polybasic Acid and Xylene Charging

Keeping the Agitation on

Heating to 140 - 150 Deg C

Cooling the batch to 100 - 120 deg C

Rosin Charging

Yes

No

Charging At Right Rate at 140 - 150 temp continual Removal of WOS

No Post Sorbitol Charging ( Polybasic Acid , Polyol , Xylene , Antioxidant )

Cooling to 120 deg

Sorbitol Charging

Is MTO Tol., dv & AV Achieved NO Keep Heating on and Maintain temp. at 260 - 2650

Yes

Check forAcid Value

A.V. Attained

Check for dv & AV MTO tolerance

D

Maintain the temp at 170 - 180 deg C

Removal of WOR Heating For Dehydration N 2 Purging Dehyd. at temp 260 - 265 deg C Maintenance of reflux rate

Removal of WOR N 2 Purging Maintenance of reflux rate

Cooling of the batch to 210 - 220 deg and Xylene part III addition


D Check for dv & AV

No

Is dv & AV ok

Max. Temp. 240 deg C

Yes


Flushing of Reactor Clean Reactor

References :-


Quenching & temp. Red. Temp. at 180 - 200 deg C

Cooling of the batch 180 - 200 deg C Batch cooled to 180 - 200 deg C

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 100-125 0C, 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.


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 GPI :SPI :WI :-

:Viscosity ; %NVM ; Acid value General Processing Instruction Specific Processing Instructions 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 kept open Maintain Temp. N 2 Purging No. of coil operated TP Outlet temperature Time of maintaining the temp.

Heating to 170 -180 deg

Maintenance for 1 hrs.

Temperature at 170-180 deg C

D

Removal of WOR Maintenance of reflux rate


Check for dv & AV

Clean Reactor


Dil.Visc.as per SPI as per SPI

Is dv & Acid Value AV ok

Max. Temp. 240 deg C

Yes


Flushing of Reactor

No

Quenching & temp. Red.

Cooling of the batch 200 deg C


Temp. at 180 - 200 deg C

Note :- General Checks :- It involves following Activities    

Checking the reactor hygiene Check the Reactor Bottom valve getting closed / not bypassing Check and ensure that no line is open to reactor . Check and ensure that the all RMs are available in sufficient qty. at shop floor before starting the batch


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(B) Thinning and Filtration stage

Adjust blender to reach reqd. Viscosity & % NVM

Heat input from Thermopac Agitation kept on

Heat blender to 140 - 150 deg C

Dil .Viscosity % NVM , Gardner Adjusted as per SPI

Materail at 140 - 150 deg C temp.

Start Filtration

Check Finish No

No

Is Finish O.K.? Should be 7

D

Check Finish

Is Finish O.K.? Should be 7

Yes

Transfer to tank / Barrel

References :-

ISTM test method GPI :SPI :WI :-

:Viscosity ; %NVM General processing instruction Specific Process Instruction Work Instructions

80

Yes


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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 Lower Higher

Dehydration rate Higher Lower

Further reaction Higher pick up Stagnancy

Final properties High AV 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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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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M04-101 Pg 27 OF 0

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ACRYLIC RESIN Acrylic resins are the homopolymers or copolymers based on acrylic acid and their esters . However polymers based on styrene are also classified as acrylic resins . Thus acrylic resins are structurally macromolecules of saturated C-C chain obtained by addition of the individual monomer units across the vinyl group. Raw Materials :-

A) Initiators :Initiates free radical Reaction. E.g. di tertiary butyl peroxide(DTBP), AIBN and Di benzyl peroxide. CH3

CH3

CH3

-

NC C - N = N - C - CN CH3

H3C

CH3

- C - O - O - C - CH3 CH3

AIBN Bet Temp. for Use

CH3

CH3

DTBP

20 - 100 deg

80 - 150 Deg

C =O | O Di Benzyl | Peroxide O | C =O 40 - 90 Deg

B) Monomer :Examples are as follows :-

CH = CH 2

CH2 = CH - CO O H

ACRYLLIC ACID

CH 3 | CH2 = C - C O O H METHACRYLLIC ACID

ACRYLATES Methyl acrylates Ethyl acrylates n-Butyl acrylate

CH2 = CH - C O O R R - > CH 3 ( 8 Deg ) R - > C2H5 ( -22 Deg ) R - > C4H9 ( - 54 Deg )

METHACRYLATE

CH3 | CH2 = C - C O O R

STYRENE

MMA EMA HEMA

R - > CH3 ( 105 Deg ) R - > C2H5 ( 65 Deg ) 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 stagesa) Initiation: initiator splits to give the free radical CH3 NC

CH3

CH3

- C - N = N - C - CN CH3

2

CH3

NC

-C

.

+

N2

CH3

I-I

2

I

.

b)Propagation: Initiator free radical attacks the monomer molecule to propagate the reaction.

I

.

+

I - CH2 - CH - R

CH2 = CH - R

+

CH2 = CH - R

.

I - CH2 - CH - R

.

I - ( CH2 - CH - R ) n - ( CH2 - CH - R )


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C) Termination: This takes place when reactive sites on the polymer chain have rendered inactive. 2

I -(

2-

CH - R ) n - ( CH2 - CH - R

I ( CH 2 - CH ) n | R

2-

CH | R

2-CH-

| R

(

2-CH

)n-

| R

Free radical polymerisation of acrylic monomer may be carried out in any of four basic polymerisation system. Bulk Absence of any solvent. Solution Polymerisation carried out in presence of solvent. Suspension Polymerisation carried out in the presence of non solvent. Emulsion Polymerisation carried out in the presence of non solvent , usually water but with water soluble initiator. Controlling of molecular weight during process 

Rate of addition : Degree of polymerisation depends on the rate of addition . Faster rate of addition will tend to increase the monomer concentration resulting in higher molecular weight resin . On the other hand slower addition rate will give low molecular weight resin .



Initiator Concentration: As initiator concentration increases molecular weight decreases.



Type of initiator : AIBN gives lower molecular weight than DTBP



Processing Solids- High processing solid polymerisation reduces chain transfer activity of solvents resulting in higher molecular weight system.

Viscosity or molecular weight is proportional monomer concentration and inversely proportional to initiator concentration. Precautions to be taken during processing of acrylic resins

a) Temperature: Since the molecular weight is highly sensitive to temperature, proper temperature maintenance is necessary. b)Proper weighing of monomers and initiator :


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


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AMINO RESIN Amino resins are produced as a result of condensation reactions between amino compounds and formaldehyde . The most common amino compounds used are urea , melamine , hexamethoxymethyl melamine and benzoguanamine. Commonly used raw materials in amino resin processing are :(a) Paraform (b) Melamine / Urea / Benzoguanamie (compound containing -NH2 group.) (c) Alcohol (methanol / butanol) A.

Formaldehyde and paraform

Preparation of formaldehyde Ag/Cu catalyst

CH3OH

HCHO +H2 -20kcal.

CH3OH +1/2 O2

HCHO+H2O+38 kcal.

Product gases absorbed in water , and gives formaldehyde solution which contain mixture of CH2(OH)2 and H(CH2O)2 where n=2-3.Paraform is obtained by vacuum concentration of solution. Paraform - HO(CH2O)n where n =8-100 =93-99% formaldehyde content In paraform due to moisture formaldehyde contents drops to 91% or lower. B.

Melamine/Urea/Benzoguanamine (-NH2 group containing compounds) NH2

C // N | C \\ NH 2

\ N || C / N

Melamine

C

O || H2N - C - NH2

NH 2

// N | C \\ NH 2

Urea

\ N || C / N

NH 2

Benzoguanamine


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C. Alcohol‟s

Methanol Butanol Isobutanol

Processing of amino resins

Alcoform formation stage

Methylalation stage

Filtearion stage

Etherification and self condensation stage

Solvent stripping stage

80 Date

19/05/2010


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EPOXY RESINS These are the condensation product of Bis phenol (Bis A) and epichlorohydrin(ECH). Alkali is used as condensing agent [lye= NaOH in DM water]  

Chemically epoxy means a compound containing 3 members cyclic ring of “oxirane”

O C

C TYPE OF EPOXY RESINS

Solid epoxy

Liquid epoxy

Less EPCL Higher soft point High M.Wt. n>2 Better chemical resistance

More EPCL Low soft point Low M.Wt. n=2 Inferior chemical 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 -----------------------> (low mol.wt.) Bis A

highly polymer products


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TAFFY PROCESS

ADVANCEMENT PROCESS

1. Side reactions 2. By products 3. No control over material 4. Long PCT 5. Branching 6. Low cost

No side reactions No by products Better control over mat. Less PCT No Branching 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

:-

80 Date

19/05/2010


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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. 2. 3. 4. 5. 6. 7.

Water tolerance test for water reducible resin MT tolerance Non volatile matter of hydrocarbon resin solution Determination of acid value Test for monoglycerolysis (MG) and phthalic compatibility Viscosity of resins by ford viscosity cup 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 120 o 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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Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 44 OF 0

80 Date

19/05/2010

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 0.1 1.0 Calculation:

WEIGHT OF DRIED PHTHALATE 0.35 - 0.40 grams 3.00- 3.50 grams 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.


SPC. Issued By

M04-101 Pg 45 OF

Rev.

Resin Manual

Dexter Technologies

0

80 Date

19/05/2010

The weight of dried Na 2CO3 suitable for other normalities of HCl solution are given in the tableNormality

Vol. Of Hcl to be diluted to one litre (in ml)

weight of dried Na2CO3 `to be used (in gms.)

0.22 0.04 0.20 0.25 0.50 1.00

1.66 3.22 16.6 20.8 41.5 83.0

0.088 +- 0.001 0.176 +- 0.001 0.440 +- 0.001 0.550 +- 0.01 1.10 +- 0.01 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.


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 46 OF 0

80 Date

19/05/2010

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 )


SPC.

M04-101 Pg 47 OF

Issued By

Resin Manual

Rev.

0

Dexter Technologies

80 Date

19/05/2010



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 ) return to the process.



Cold water outlet :- The point, which the cooled water, leaves the tower .

:- The point at which the cooled water is collected

Air Outlet Fan Drift eliminator

Casing of Shell

Inlet Conn.

Water Distribution System

Packing Louvers

Air Inlet Over flow connection

Outlet Connection

O

Make up

Cold water basin

Figure :- Schematic arrangement of a mechanical draught cooling tower

The factors which influences the performance of the cooling tower can be summarised as: 1. 2. 3. 4. 5.

The cooling range The approach ( Design factor ) The ambient air wet bulb temperature (humidity) The flow rate of water to be cooled ( Circulation Rate ) The rate at which air passed over the water


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 48 OF 0

80 Date

19/05/2010

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

The mechanism by which the water is cooled is best understood by the figure given below

Convected Heat

Radiant Heat

Heat Lost due to evaporation Layer of air at 100 % humidity and same temp. as water

:-

Bulk unsaturated air flowing passes drople

In the given figure illustrated a single droplet of water in the tower . The droplet is surrounded by a thin film of air, which is saturated and remains almost undisturbed by the passing air stream . It is throughout his static film of saturated air that the transfer of heat takes place in three ways i.e. :-


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 49 OF 0

80 Date

19/05/2010



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.


SPC. Issued By

Resin Manual

Dexter Technologies Wet bulb temperature

Rev.

M04-101 Pg 50 OF 0

:-

80 Date

19/05/2010

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 .


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 51 OF 0

80 Date

19/05/2010

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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 52 OF 0

80 Date

19/05/2010

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 ONOFF 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 combistat indicates & controls controls the fuel oil 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 switch for Thermic fluid pump is also put on . Thermic fluid circulating pump starts & the flow of thermic fluid is established in the coil & circuit. 5.On observing the pump pressure gauge & circuit pressure gauge is showing steady pressure & after the fuel oil temperature crosses the minimum temperature mark of 105C, the rotary switch is put in “ BURNER ON” position.

6. The blower motor starts . The blower pushes air through combustion chamber ,driving away combustible gases ,if any, from the combustion chamber. This is known as prepurging. At the same time ,fuel oil pressure is also developed ,as the blower & the fuel pump are driven simultaneously 7.After prepurging    

Sparking starts Burner solenoid valve energises & oil is sprayed into the chamber. Flame is established & sparking stops. Heating of thermic fluid starts.

combustion


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 53 OF 0

80 Date

19/05/2010

8. Hot oil is supplied supplied to the user equipment. equipment. It exchanges exchanges its heat with 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


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 54 OF 0

80 Date

19/05/2010

The sequence controller in conjunction with the flame detector ensures t he 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 lockout 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 outlet & in case this temperature temperature exceeds the pre-set pre-set limit, the burner goes into electrical lock-out sounding an alarm. 4. Low level switch iin n 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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 55 OF 0

80 Date

19/05/2010

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 W hen this switch takes over, the alarm is i s 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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 56 OF 0

Date 19/05/2010

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.

80


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 57 OF 0

80 Date

19/05/2010

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.


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 58 OF 0

80 Date

19/05/2010

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:

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. Fuel from the service tank

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.


SPC. Issued By

Resin Manual

Dexter Technologies Electrical system:

Rev.

M04-101 Pg 59 OF 0

80 Date

19/05/2010

(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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 60 OF 0

80 Date

19/05/2010

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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 61 OF 0

80 Date

19/05/2010

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.


SPC. Issued By

Resin Manual

Rev.

M04-101 Pg 62 OF 0

Dexter Technologies

80 Date

19/05/2010

Cartridge assembly in A sparkler Filter

Formed powder cake on filteration Filter Aid Screen Clips Spacer Cup

O Plate

v O O

O O

O

O

O

O

O

Central Tie Rod

Compression Ring

Compression Cup O

Side Tie Rod

O

O O O

O

O

O

O O

O O

O O

O

O

O

O

O O O

O

O

O

O

O

O

O

O

O

O

O

O

O

O

O

O

O O

O

O

O O Ov O v

O

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 ma chine 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.


SPC. Issued By

Resin Manual


Rev.

M04-101 Pg 63 OF 0

80 Date

19/05/2010

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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 64 OF 0

80 Date

19/05/2010

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


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 65 OF 0

80 Date

19/05/2010

Details of hazardous material in Resin House Raw Material S.No Name MTO

1

XYLEN E

Air supplied mask , safety googles/ face shield. Plastic gloves, apron and shoes

Sampling, Addition/Charging , Filteration , Filter machine making

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 b ronchio pneumonia.

Safety goggles, chemical resistant gloves, safety cloths.

Sampling, Addition/Charging

BU TAN OL

Inhalation: Causes anesthesia, nausea, h eadache, dizzines, irritation of respiratory passage. Mildly irritating to skin and eyes. Har mful if swallowed.

Organic vapour mask, fully covered safety goggles/face shield, hand gloves

Sampling, Addition/Charging , Filteration , Filter machine making

ISO PROP ALCOHOL

Vapour causes m ild irritation to eyes & upper respiratory tracts. High conc. may be anesthetic. Liquid irritates eyes and m ay cause injury. Harmless to skin. If ingetsed causes drunkenness and vomiting.

organic vapour mask, Sampling , Lab face shield, rubber cleaning hand gloves, apron and shoes

METHANOL

Exposure to vapours cause eye irritation, headach e, 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, Sample checking Boots , safety goggles, protective apron and rubber gloves

2

3

4

5

6

Harmful Effect Vapour causes headache confusion & respiratory distress. Liquid irritates skin. If ingested can irritate the entire d igestive system & may injure kidneys. If liquid is taken into lungs severe pneuomintis results. V apour causes headache, dizziness. Liquid irritates eyes and skin. If taken into lungs causes severe coughing, distress, rap idly developing pulmonary edema. If ingested causes nausea, vomiting, cramps, headache, coma & can be fatal. Kidney and liver damage

Work place where PPEs exposure is possible Wear respiratory Sampling, protection, face shield Addition/Charging , and protective clothing Filteration , Filter machine making


SPC. Issued By

Resin Manual

Dexter Technologies

0

80 Date

19/05/2010

HEXANE

Causes irritation of respiratory tract, Provide face Sample checking cough, mild depression, cardiac shield/safety goggles, arrhythmis. Aspiration causes severe plastic or rubber gloves lung irritation, coughing, Pulmonary edema, excitement followed by depression. ingestion causes nausea, vomiting or swelling of abdomen, headache

TDI

This material is toxic to human system and if swallowed is FATAL

Self contained During charging breathing apparatus, side covered safety goggles/face shield rubber hand gloves, protective overclothing and shoes

MMA

Inhalation & Ingestion: Irritation of nose. throat,nausea,vomiting. Skin & Eyes:Liquid causes severe irritation

Provide self contained During charging , breathing apparatus, sample checking side covered safety goggles/face shield , rubber han d gloves, protective over clothing and shoes.

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.

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 During charging , breathing apparatus, sample checking Rubber gloves, Safety goggles, Rubber boots

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

7

8

9

10

11

12

Rev.

M04-101 Pg 66 OF

During charging , sample checking

During charging


SPC. Issued By

Resin Manual

Dexter Technologies

Date 19/05/2010

Causes burns of mouth and lips, Face shield, rubber During charging sour acrid taste, severe hand gloves, protective gastointestinal irritation, nausea, overclothing and shoes vomiting, bloody diarrhea, difficult swallowing, severe abdominal pain, thirst, acidemia, difficult breathing, convulsions, collapse, shock and death

AM MO NIA

Causes burning pain in mouth, throat, stomach,constriction of throat and coughing, followed by vomitting of blood, Severe eye and skin irritant.

2-ETHYL HEXYL ACRYLATE MONOMER

Harmful if swallowed. Inhaled. Rubber gloves, Safety During charging Vapor or mist is irritating to the eyes goggles, shoes, self and respiratory tract contained breathing apparatus

ACETIC ACID

:breathing of vapours causes coughing,chest pain and irritation of nose and throat.M ay cause nausea and vomiting.Skin:contact cause burns.Eyes:contact cause burns.

Provide PVC hand gloves, apron, complete eye protection and respiratory protection

LAFFSOLVEMEB

Inhalation: Vapors irritate nose and throat. Ingestion: Causes headche, nausea, vomiting, dizziness.

Organic respirator, side During charging covered safety goggles/face shield, rubber hand gloves, body overclothing and shoes

PHTH ANHYD ASN

Solid irritates skin and eyes, causing Rubber apron, Rubber During charging coughing and sneezing. Liquid shoes,, face shield, causes severe thermal burns approved vapor respirator, leather or rubber gloves and shoes.

14

16

18

19

0

80

PHOSPHORIC ACID

13

15

Rev.

M04-101 Pg 67 OF

Rubber boots, Hand gloves , apron, safety goggles. Use of protective o il will reduce irritation

During charging

During charging


SPC. Issued By

Resin Manual

Dexter Technologies

Toxic by inhalation and ingestion. Wear goggles and During charging Irritant toskin and get absorb by skin plastic or rubber gloves

2EHA

Causes Air pack or organic aneshtesia,nausea,headache,dizzines cannister, safety s. Mildly irritating to skin and eyes. goggles. Rubber gloves, face shield.

During sample checking

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

Bisphenol A

Dust irritating to respiratory passages. May cause sneezing.

Protective hand gloves, During charging protective overclothing, shoes, side covered safety goggles/face shield, dust mask.

23

24

27

28

19/05/2010

MORPHOLINE

22

Rubber gloves and goggles

Date

Mildly Toxic by Ingestion, Inhalation, Causes Mild headache, nausea,vomitting. Causes Eye & Skin Irritation.

21

26

0

80

GLYCERINE ( ANHYDROUS ) 20

25

Rev.

M04-101 Pg 68 OF

During charging

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

NITROGEN ( Inhalation : Can cause asphyxiation, COMPRESSED ) 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 During reactor breathing apparatus processing, where insufficient air is Generation present. Provide safety face shield, insulated gloves, long sleeved trousers worn outside boots or overhigh top shoes to shed the spilled liquid.

HYDROCHLORI Inhalation of fumes results in C ACID coughing,choking sensation,irritation to nose and lungs. liquid causes burns, can burn mouth and the digestive tract.

Chemical protective Sampling suit with self contained breathing apparatus, air line mask, rubber hand gloves, face shield and shoes.

ETHYL ALCOHOL

Safety goggles, all Sampling purpose cannisters, protective overcolthing and shoes.

Irritation of eyes, nose and throat, Headache and drowsiness may occur. Liquid causes intoxication. The substance affects nervous system and may damage liver.

During cleaning , charging


SPC. Issued By

Resin Manual

M04-101 Pg 69 OF

Rev.

Dexter Technologies

Date 19/05/2010

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.

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 During charging breathing apparatus , chemical goggles, protective overclothing , synthetic rubber or plastic gloves and shoes.

CYMEL 1130

Can be harmful if swallowed or solvent mask, solvent During charging vapors are inhaled. Cause slight skin resistant gloves, safety irritation and eye irritation. goggles, protective clothing and safety shoes

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.

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 During charging gloves, dust mask, safety goggles/ face shield, protective overclothing and shoes

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

29

30

31

32

0

80

33

34

Sampling

During charging

During charging

Pyridine

35 Potassium Hydroxide

36

Dimethylamine

Chemical gloves, During charging face shield, rubber hand gloves, Rubber apron and Hi ghl y corrosive to organic materi gum boots. Inhalation at high concentration Rubber/ acid During charging (>100ppm) causes nose and ressistant hand throat irritation, Progressing all gloves apron, shoes, the way to pulmonary edema. face shield, Self Eyes & Skin: causes irritation. contained breathing apparatus


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 70 OF 0

80 Date

19/05/2010

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. Ke ep 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.


SPC. Issued By

Resin Manual


Rev.

M04-101 Pg 71 OF 0

80 Date

19/05/2010

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



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

day.

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.


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 72 OF 0

80 Date

19/05/2010

PROTECTIVE EQUIPMENTS AND FACILITIES EQUIPMENT / FACILITY IN SHOPFLOOR

1. 2. 3. 4.

Personal Protective Equipment First Aid Facility Fire Extinguishers Eye Wash Bottles / Eye Wash Shower

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

The details of the PPE being used to handle the raw materials in the section are as under:

PPE CODE

Description

1a

ORGANIC VAPOUR MASK

1b

DUST MASK

1c

AMMONIA MASK

2

SAFETY GOGGLES

3a

RUBBER GLOVES

3b

PVC GLOVES

3c

LEATHER GLOVES

3d

COTTON GLOVES

4

GUM BOOTS/SAFETY SHOES

5

APRON

6

BREATHING APPARATUS / AIR LINE RESPIRATOR


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 73 OF 0

80 Date

19/05/2010

Protective equipments including PPE for eyes, face, head, protective clothing, respiratory devices, protective shields and barriers shall be provided, used and maintained in a reliable condition as required by the hazards, processes or environment.

The details of hazards and the corresponding PPE required in the section for protection of various body parts is described as under: PART OF BODY

HAZARD

PPE TO BE USED

NEEDING PROTECTION

Head

Exposure to falling and or flying objects , Safety helmet striking against obstruction Exposure to head during powder charging

Eye

Safety caps

Exposure to flying particles e.g. dust and Safety goggles chips, chemical splash and vapours Exposure to radiation during gas cutting and Welder‟s goggles and helmets welding operations

with appropriate shades of glass

During sampling – Hot material Falling

Face protection sheet

Ear

Exposure to excessive noise levels

Ear plugs, Ear muffs

Hand, Arm

Exposure to sharp / rough edges leading to Cut Resistant Gloves cuts and abrasion Exposure to Solvents / Monomers

PVC hand gloves

Exposure to acids and alkalis

Rubber hand gloves

Exposure to strong electrical current

Specified rubber hand gloves for work on electric installations

Hand

Exposure to hot material / equipment‟s

Cotton-Felt hand gloves gloves Asbestos gloves

Foot

Exposure to acid during hardener packing

Surgical hand gloves

Exposure to hard surfaces

Leather hand gloves

Exposure to falling objects , chemicals / Safety shoes striking against obstruction Exposure to acids and alkalis

Gum boots


SPC.

M04-101 Pg 74 OF

Issued By Rev.

Resin Manual

0

Dexter Technologies Body

80 Date

19/05/2010

Exposure to moderately hot objects and Thick cotton uniform chemicals

Respiratory Passage

Exposure to acids and alkalis

PVC apron

Exposure to TDI

TDI suit

Exposure to acid during battery charging

Apron

Exposure to monomer

Monomer suit

Contaminants in vapour form which are Self toxic

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

      

Safety Goggles

Full view (extremely light weight non biting edges)





 

 

Ear Plugs

Ear Muffs

Foam earplugs with a cord that drapes around the neck, enabling user to remove and reinsert plugs repeatedly during the workday. 3M ear plugs- 3M1110 3 M- 1435- Roomy & durable ear cups provide reliable protection for everyday use.

  

 

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. 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. 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. Should be fitted properly to the ear. Should be worn at all times of exposure to noise.


SPC. Issued By

Resin Manual

Dexter Technologies

PVC Hand Gloves (Yellow colour)

Rubber hand gloves (Orange colour)

The lightweight design and flexible headband provide an easy fit and comfort to the user. 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. Orange colour thin gloves made from pure latex rubber.











Surgical Gloves

White coloured gloves made from latex rubber.





Plastic disposable polythene hand gloves

Nitrile gloves

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

Welding leather gloves



Easy and firm grip. Highly effective for Industrial solvents.

Leather gloves for welding.







 

Electrical Gloves Safety Shoe

Electrical Safety footwear

Electrical safety gloves which provide electrical safety. Protective footwear shall comply to IS code for following parameters. Impact  Compression  Clearance  Eg. Bata/ Liberty warrior  All exposed external metal parts should be non-ferrous and the design of the soles and 

   



Rev.

M04-101 Pg 75 OF 0

80 Date

19/05/2010

Should be kept in the area devoid of any kind of contamination. Eg. Dust, vapours, mist etc. Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified. The contaminated gloves shall be decontaminated before being disposed off.

Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified. The contaminated gloves shall be decontaminated before being disposed off appropriately. Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified. The contaminated gloves shall be decontaminated before being disposed off appropriately Should be disposed off after one or two uses. Gloves contaminated with toxic / infectious /corrosive material shall not be left unidentified. The contaminated gloves shall be decontaminated before being disposed off appropriately. Gloves should be cleaned by using soap and mild detergent. Should be checked for worn outs and replaced if not in usable condition. Gloves should be thoroughly checked for cuts and any kind of damage. Gloves should not be wet before usage. 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.

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


SPC. Issued By

Resin Manual

Dexter Technologies

Gum Boots

heels is such it provides a path to ground. Industrial black colour full size rubber gumboots with anti skid soles.

  

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.

 

  







Rev.

M04-101 Pg 76 OF 0

80 Date

19/05/2010

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. 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.



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





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. 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.


SPC. Issued By

Resin Manual

Dexter Technologies

Ammonia mask

Apron

the nuisance level organic vapours. 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.  Denim/Cotton apron for working in the shopfloor.

Rev.

M04-101 Pg 77 OF 0

80 Date

19/05/2010



Masks shall not be stored in toolboxes.



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 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.


SPC. Issued By

Resin Manual

Dexter Technologies

Rev.

M04-101 Pg 78 OF 0

80 Date

19/05/2010

SECTIONAL LEVEL PERFORMANCE INDICATORS Following are the performance indicators of the section:1. OAE : overall asset effectiveness

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

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 = Rate Index =

Process time available No. of batches actually made Benchmark rate Actual rate


SPC. Issued By

Resin Manual

Rev.

Dexter Technologies

M04-101 Pg 79 OF 0

80 Date

19/05/2010

Benchmark rate for Reactors is :Long oil Alkyd Batches Medium oil Alkyd Batches Short oil Alkyd Batches

44 Batches per month from a single reactor 25 Batches per month from a single reactor 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

is the measure of Manpower Utilisation in a section. It is the no. of manpower (operators) used to produce one ton of solid resin. Mandays per ton

3. 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. Man power efficiency

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)

Resin Manual (Rev0)

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