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Internship Report

Caustic Soda Plant


Sitara Chemical Industries Limited (SCIL)
Training Period (21st June 2010 - 18th July, 2011) (Duration: 4 weeks)

By: MUHAMMAD SAJID 4th Semester (2009-CH-309) B.Sc. Chemical Engineering

University of Engineering and Technology Lahore ( FSD Campus ).

Internship Report

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Acknowledgments
I am thankful to the Institute of University of engineering and technology Lahore ( FSD campus ) and Sitara Chemical Industries Limited for providing us such a marvelous and informative professional training program. I am thankful to Mr. Muhammad Yousaf (DM Prod. Area-I) for his kindness and complete guidance throughout our training period. It will also be our pleasure to say thanks to Mr. Adnan Masood (Tr. Engineer), Mr. Asad Niazi (Tr. Engineer), Mr. Zeeshan Jamil (Tr. Engineer), Mr. Hassan (Tr. Engineer), and Mr. Adnan waheed (Tr. Engineer) and Mr. Tayyab (Tr. Engineer) for their friendly behavior and time to time guidance. And at the end, special thanks to Mr. Ramzan (Senior Superindent) and all plant operators for their help and cooperation.

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TABLE OF CONTENTS Company Profile Introduction Companys Mission statement Achievements Safety & Environment Management Corporate social responsibilities Caustic soda plant Primary brine section PFD of Primary brine section Secondary brine section PFD of secondary brine section Cell room PFD of cell room Dechlorination Evaporation unit PFD of evaporation Caustic solidification plant (CSP) Block diagram of CSP Utilities and protective equipments Utilities Personal protective equipments (PPEs) Product Details Ammonium chloride Carbon dioxide gas Bleaching powder Calcium chloride Liquid Caustic soda (33%) Liquid Caustic soda (50%) Caustic soda flakes Summary

PAGE NO. 4 4 4 4 5 5 7 8 12 18 23 24 28 29 32 34(b) 35 39 40 40 41 42 42 42 43 44 45 46 47 48

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About Company: Sitara Group of Industries is one of the renowned industrial groups of Pakistan. This group started its industrial activity with textile weaving sector in 1956. Sitara Group by now is in textile cloth finishing and processing, textile spinning, chlor alkali industries and power plant. It is situated at 32 km, sheikhupura road, Faisalabad. Its capacity is now 617 metric ton per day. Besides manufacturing Caustic Soda and various allied chemicals, the company has been able to set up independent plants of some more gases i.e. Oxygen (O2), Nitrogen (N2), Carbon Dioxide (CO2), Nitrous Oxide (N2O) in the same premises, during last one and half year. Companys objective:We believe in stimulating and challenging team oriented work environment that encourages, develops and rewards excellence and diligently serve communities, maintaining high standards of moral and ethical values. We strive to develop and employ innovative technological solutions to add value to business with progressive and proactive approach. As well as work hard for continuing growth and diversification for bottom line results with risks well contained.

Vision
Strive to develop and employ innovative technological solutions to add value to business with progressive and proactive approach.

Mission
Continuing growth and diversification for bottom line results with risks well contained.

Code of Ethics and Business Practices


We believe in stimulating and challenging team oriented work environment that encourages, develops and rewards excellence and diligently serve communities, maintaining high standards of moral and ethical values.

Company Values
Integrity and Honesty Open, Respectful and Supportive Prepared to take challenges and see them through Deep regards for Customers, Business partners and employees Self-critical and accountable Quality in products and dealings

Safety & Environment Management:SCIL is a very much responsible organization. It cares greatly for the environment as well satisfaction of its customers. For this reason they have adapted almost all national and international quality and environment safety policies.

QUALITY POLICY :
Sitara Chemical Industries Ltd. is committed to remain alert and advance, to continuously grow as a Quality Symbol for its products and in meeting industrial and consumer requirements, through training, team work, and procedures, on time, every time.

ENVIRONMENTAL POLICY:
Sitara Chemical Industries Ltd. is committed to continual improvement of its Environmental Management System (EMS) by adoption of appropriate pollution prevention measures and complying with all relevant training, teamwork and procedures as implemented from time to time. In actual words, SCIL has well developed and recognized Quality Management Systems as well as Environmental Management Systems. SCIL has following certifications in QMS and EMS from SGS under the authority of UKAS Quality Management. ISO 9001:2008 ISO 14001:2004

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Human Development Center:SCIL has introduced numerous ways to train, upgrade their people. In this context, a Human Development Center has been established at Sitara Chemical Industries Ltd where internal training sessions are held regularly. The renowned trainers are also called at the center to impart training in the fields of technical, supervisory and management skills.

Caustic Soda Plant


SCIL is manufacturing many important chemicals such as Ammonium Chloride (NH4Cl), Bleaching Powder (Ca(OCl) 2), Chelated Iron, Clorinated Parafin Oil, Hydrochloric acid (HCl), Ferric Chloride (FeCl3), Ferric Sulphate (Fe2(SO4)3) etc. But their main product is Caustic Soda (NaOH) chemically known as Sodium Hydroxide. SCIL is selling caustic Soda in three forms: (1) 32% liquid Caustic Soda, (2) 50 % liquid Caustic Soda and

(3) 98.5 % caustic flakes Sitara Chemical Industries is manufacturing caustic soda (NaOH) by electrolysis of brine solution. Process is carried out in membrane cells equipped with latest technology. At time, SCIL has four caustic manufacturing plants in working, named as BMR, M-II ,M-III and M-IV. Overall caustic production of SCIL is 617 MTD. Since, our internship program was conducted at BMR; therefore in the following lines we will have detailed discussion of all unit operations and unit processes taking place in the cycle of production of Caustic Soda. The production cycle of NaOH goes through the following series of steps.

Primary Brine Section


This section involves saturation of brine solution, its purification by settling after treatment with certain regents and primary filtration by pressure filters.

Secondary Brine Section


In this section, brine coming from primary brine section is filtered by resins to remove any remaining impurities which may cause damage to membranes of the electrolyzer.

De-chlorination Unit
Here de-chlorination and other preliminary treatments of depleted brine coming from cell room are carried out beforesending it to primary brine section.

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Evaporation Unit
Caustic soda obtained from cell room has a concentration of 32 % w/w. in unit; this concentration is raised to 50 %. evaporation

Caustic Solidification Plant( CSP)


In this section, caustic soda from evaporation unit is concentrated upto 98.5% and solidified for packing in bags and drums.

PRIMARY BRINE SECTION


INTRODUCTION Primary brine section involves three types of activities Brine saturation

Brine purification and sedimentation Brine filtration Our main objective of the brine processing is to resaturate the depleted brine coming from the electrolyzer by adding the salt. The impurities which has been introduced in the brine together with the salt are to be removed first by settling and then by chemical treatment and settling. The suspended impurities are removed by filtration 2.1.2 Process Description:In this section de-chlorinated depleted brine coming from cell room after electrolysis is concentrated and purified by sedimentation and filtration. After electrolysis, concentration of brine decreases to 180-200 g/l. so it is sent to saturators (DS-5010 A/B) where it is concentrated to 300-310 g/l. The flow rate of the depleted brine is 100m3/hr. Two saturators are present at A-I one in process and one at standby. Saturators are made of concrete, reinforced with steel and internally epoxy lined. Depleted brine is introduced with the help of five nozzles installed at the bottom of each saturator. Saturator is filled with lumps of Rock Salt with the help of tractor blades from salt yard. Water percolates through the salt lumps dissolving the salt in it and over flows in separate overflow line. Makeup de-mineralized water is also fed through a pipeline to cover water losses and maintain the required flow rate. The level of the salt in the brine saturator is kept as constant as possible by feeding salt in the saturator at required rate. The raw salt impurities such as Ca and magnesium salt are dissolved in the depleted brine faster as compared to sodium chloride, so that if excessive amount of salt is loaded into the saturator, the impurities content in the saturated brine would be higher than the normal. 3

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Follow rate is maintained so that the desired concentration is obtained. If concentration is much higher, salt may crystallize in pipelines, reactors or tanks in cold seasons. When saturator is exhausted (filled with sludge), flow is shifted to second saturator and first one is subjected to cleaning. After concentration brine many suspended and dissolved impurities which are necessary to be remove. Approximate composition of Rock Salt and impurities associated with it are as given below:

NaCl Ca+2 Mg+2 SO4 K


+

97% w/w 021%w/w 0.06%w/w 0.9%w/w 0.17% w/w 0.17% w/w

Sr

SiO2 Al Fe Mn Ni I F Cr, Mo, VInsolubles

1.0ppm 5.0ppm 0.2ppm 0.5ppm 0.05 ppm 0.5ppm 1.0ppm 0.5ppm 0.69%w/w

So in order to remove these impurities, brine is treated with Calcium Chloride CaCl 2. For this purpose brine coming out of saturator is collected in Brine Collecting Tank (D-510) from where almost 40% of it is sent to CaCl2 pits while 60% overflows from tank to the Settling Pits (D-5610 A/B) . Settling pits are working alternatively i.e. one in process and one at standby.

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Insoluble and suspended impurities are settled down settling pits and brine overflows to the next pit known as Common Pit (D5620). In CaCl2 pits , CaCl2 in the form of solution is infused to maintain 30004500 ppm of Ca++ in excess. The CaCl2 pit is made ready twice in a day and transferred in the common pit D-5620. CaCl2 pit is made ready to transfer in 6-8 hrs .CaCl2 which is infused has sp. Gravity 1.1-1.2 and pH in range of 6-9. From the settling pit, the brine over flows into the common pit D-5620 where it is mixed with the brine coming from the CaCl2 pit. From common pit brine is pumped to the first Reactor (R5020 A). The flow rate is 105110m3/hr. In this reactor brine is treated with 8% Barium Carbonate solution to remove any leftover sulphates. After reactor, brine flows to the first Settler (TH- 5010 A) This settler has a capacity of 1800 m 3 and its material of construction is RLS (rubber lined steel). Suspended impurities settle down at the bottom of settler and are removed through a drain valve and screw pump by a slow moving rack. Rack rotates at a speed of 0.1 RPH. Nalco solution prepared in tank D-5310A/B is dosed at controlled rate. The amount of flocculants, Nalco, is maintained at 1-2 ppm. Brine over flows from the settler and is collected in a Tank D-515. From D-515, brine is pumped to the second Reactor (R5020 B) where it is treated with 8% solution of Soda Ash (Na2CO3) and Caustic Soda in order to remove Ca+2 and Mg+2. Both reactors are equipped with agitators for intimate mixing to facilitate reaction and to

avoid settling of insoluble compounds formed, within the reactor instead of settler. After second reactor, brine solution flows by gravity to the second Settler (TH-5010 B). This settler has a capacity of 2630 m3. Flocculent (Nalco) is also added in the settler. This settler is also equipped with a slow moving rake at the bottom to drain settled sludge through a drain valve. This sludge is collected in two Brine Recovery Pits (D-5710 A/B) where any brine which was drained previously with sludge and is sent to Common Pit. From second settler brine overflows to the Pre-filtered storage tanks (D-5060 A/B). From tanks D-5060 A/B, brine solution is fed to six Pressure Leaf Filters (F-5070 A-F) in parallel manner. Brine filters are required to remove the suspended solids overflowing with the brine from the settler TH-5010B. There are six leaf filters F5070A-F operating in parallel, five normally in operation and one in standby. Brine from tank D-5060 A/B is pumped and distributed to each filter through individual manual valves, before proceeding to the filtration the filters must be pre-coated. For pre-coating, the pre-coat slurry is prepared in the tank D-5100. The pre-coat material Arbocel is thoroughly dispersed in the filtered brine. The end of the filtering cycle is indicated by the pressure drop in the filter .When the filter reaches the maximum operating pressure, the filter must be cleaned. The pressure across the filter should not exceed 3 bars. Filters contain 17 leaves each and total filtering surface of each filter is 38.2 m2. Casings of all filters are made HRLS (hard rubber lined steel) and filtering cloth is of FRP (fiber reinforced plastic).

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Filtered brine comes out of each filter at a flow rate of 18-20 m 3/hr and is fed to two Guard Filters (F-5080 A/B) which stops the Arbocel fibers eventually released by pressure leaf filters. These guard filters are of basket type with a total filtering of 2.78 m 2 for each filter. Casing of the filters is made of HRLS (hard rubber lined steel) and filtering cloth is of PP (Polypropylene). one filters in process and one is at standby. From these guard filters, brine is sent to two Storage Tanks (D-5070 A/B) Reactions Involved in Primary Section:Sulphates These are precipitated as barium sulphate by reaction with barium carbonate in 1 st reactor R5020 A. Na2SO4 Calcium + BaCO3 BaSO4 + Na2CO3

This is precipitated as calcium carbonate by reaction with sodium carbonate in 2 5020 B. CaCl2 + Na2CO3 Magnesium This is precipitated as magnesium hydroxide by reaction with caustic soda in 2 5020 B. MgCl2 + 2NaOH Strontium, This is precipitated mainly as strontium carbonate Mg(OH)2 + 2NaCl CaCO3 + 2NaCl

nd

reactor R-

nd

reactor R-

Sr++ + CO3--

SrCO3

At the end of Primary section, brine has following proportion of impurities in it.

Ca+2 Mg+2 Sulphates (SO4)

8 ppm (maximum) 1.92-2 ppm (maximum) 10 g/l

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Most of the sulphates in the brine are being removed by treating with calcium chloride.Hence the consumption of barium carbonate is controlled. BaCO3 is an imported commodity and is very costly, where as calcium chloride is a waste produced in HCl neutralization pits. Another advantage is that Calcium sulphate, which is precipitated out, is a good fertilizer where as barium sulphate is dangerous to water bodies and soil.
From storage tanks, brine is pumped to Secondary Brine section after raising its temperature to 55 C by using a plate type Heat Exchanger (E-5070). Material of construction of the heat exchanger is of titanium and its heat duty is 905.0 k Cal/hr. Here low pressure steam and cooling water connections are provided to allow the brine heating or cooling in order to control the temperature of the brine at 50-60 oC.

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SECONDARY BRINE
Nature of Ion Exchange Resin:Ion exchange resins are based on solid insoluble polymers supplied in the form of beads, which have fixed active ionic groups. Mobile ions of opposite charge can be exchanged reversibly and stoichiometercally for ions of the same charge present in the solution. The resin being used TP-260 has Na ions as mobile ions and exchange with Ca ++ & Mg++ present in the brine. When most of the Na+ has been exchanged with Ca ++ &Mg ++, the bed is exhausted and needs to be regenerated. The exhausted column is taken out of the stream and the other two are remained in operation. TP-260 has weak acidic chelating amino methyl phosphonic acid

groups which form stable complexes with a number of transition metals and main group elements. Process Description:Before feeding brine to electolyzers it is passed through ion exchange resin towers C5040 A/B/C placed in series in order to absorb Ca++, Mg++ and Sr++ contained in brine. The brine feeding to the resin tower has following typical specifications

NaCl Na2SO4 NaClO3 Ca++ Mg++ Sr++ SiO2 Cl2 Suspended solids Temperature PH

290-310g/l 7-8g/l 15g/l 4-6ppm 1-2ppm 1 ppm max 5 ppm max Nil 0.5ppm 50-6 oC 9-10

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The resin bed in the tower stayed on a grid plate. The spargers are fitted on this plate. The purified brine from tank D-5070 is fed in the tower through P-5070A/B at a flow rate of 105-110 m3/hr. As the towers are connected in series, so the brine is fed in the first tower in the series and ultra purified brine is collected from the discharge of the third tower and collected in Ultra Pure Brine Tank (D-5160). From D-5160 brine is pumped to Brine Head Tank (06D-001). Then it is sent to the cell room after controlling its temperature through two Heat Exchangers (06E-001) and (06E-002). 2.2.3 Regeneration of the Resin Bed:The chemical nature of the resin functional group is suitable to form complex compounds with a lot of metal ions. The resin at the beginning of the operating cycle is in the sodic form. During the operation it fixes Ca++ & Mg++ to which it has a high affinity, and releases Na+. When the resin is exhausted, means when it has absorb max. Ca & Mg ions, it must be reconverted in the sodic form. This process is referred to as resin regeneration. The regeneration process requires a sequence of different operations. The most significant of which are a treatment with diluted HCl which displaces the metal ions previously fixed by the resin functional groups followed by a treatment with diluted NaOH solution which makes the resin to change form the acidic form to the sodic form i-e H+ replaced with Na+

STEPS INVOLVE IN THE REGENERATION PROCESS 1. Brine drainage (half empty) 2. Washing with demi water 3. Counter washing with demi water 4. Drainage 5. Washing with 4% HCl solution 6. Drainage 7. Washing with demi water 8. Drainage 9. Counter washing with 5% NaOH solution 10. Drainage 11. Washing with demi water 12. Drainage 13. Water replacement with brine 14. Filling with brine After regeneration resetting is done almost in 60 minutes and brine is circulated between resin towers and brine tanks D-5070. The circulation of brine remains on till the required results of Ca & Mg are achieved.

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Points to be noted : Resin washing with water has the purpose of removing the brine from the tower and counter washing is done to remove the brine trapped in the resin bed. Brine must be removed completely because the chlorates possibly present in the brine could decompose during the acid washing and give free chlorine, which oxidizes the resin with an increase in resin consumption. During washing with HCl real regeneration of the resin bed is occurred. The metal ions attached by the resin are displaced and the resin is converted into the acidic form. After washing with HCl, the bed is again washed with water in order to reduce the consumption of the caustic soda and to fully remove HCl in the column. The more important is to avoid the possible damage of the resin particles due to heat evolved in the reaction between acid and caustic soda. During the washing with caustic soda, the resin is converted from the acidic form to the sodic form. i.e. H+ replaced with Na+ Before filling brine in the regenerated column it is emptied so that the conc. of the brine remained within the range, otherwise it may be lowered.

Chemical Reaction Involved:Chemical reactions involved in secondary purification and regeneration of resin towers are as given below. BRINE PURIFICATION Na2(Resin) + Ca++ Na2(Resin) + Mg++ RESIN REGENERATION Ca(Resin) + HCl Mg(Resin) + HCl H2(Resin) + NaOH H2(Resin) + Ca++ H2(Resin) + Mg++ Na2(Resin) + H2O (Washing by HCl) (Washing by HCl) (Washing by NaOH) Ca(Resin) + 2 Na+ Mg(Resin) + 2 Na+

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CELL ROOM
Electrolyzer:The equipment used to carry the process of electrolysis is called electrolyzer. The cell room comprises of three electrolyzers A/B/C placed in parallel fashion. Each electrolyzer has capacity of 164 cells. Each element consists of anode and cathode compartments separated by a membrane. Anodic side is made of titanium while cathodic side is made of nickel. The ion exchange membrane is clamped between the half shells with interposed PTFE gaskets. The half shells are bolted together at the flange, thus constituting a cell element. The ion exchange membrane is made by an organic polymeric matrix incorporating fixed ionic groups neutralized by mobile ions of opposite charge. Fixed group are sulphonic type or carboxylic type, while mobile counter ion is sodium ion. Only the cation exchange selectivity of the membrane can prevent migration of OH-. The flow of Cl - across the membrane is about negligible, because membrane selectivity and electric field across the membrane opposes the chloride ions transport. The raw material feeding to the electrolyzer is brine. The brine nearly saturated, is introduced into the anode compartment of the cell. The aqueous solution in this compartment is called anolyte. The membrane separates the anolyte from the catholyte compartment. 32% caustic soda from catholyte tank plus Demineralized water to make a 29-30% caustic solution is admitted to catholyte compartment where sodium hydroxide is formed by the combination of hydroxyl ions and sodium ions, which migrate through the membrane to the cathode. Chlorine gas, usually called cell gas, is formed at the anode while Hydrogen gas and sodium hydroxide are formed at the cathode.

2.3.2 Process Description:Ultra pure brine is stored in tank D-5160 and pumped via P-5160A/B into over head feed brine tank. 06D001. Brine enters in the overhead tank from the top and over flows by gravity from the top side back in D-5160 . The outlet is from the bottom of the tank and leads to cell room by gravity. The brine is heated in the way before entering cell room through heat exchanger 06E001 to raise its temperature up to 65-75 C. It is a plate type heat exchanger. Heat exchanger is provided with steam as well as cooling water connections. There is also a stand by heat exchanger 06E002 which is either used to fill a single electrolyzer or in case of emergency. In the cell room main feed brine line has three connections to feed each of the three electrolyzers. These supply lines are underneath of each electrolyzer. Brine is fed in the anodic compartment of each cell. Catholyte (33% NaOH) is stored in the storage tank 31D002. Its temperature is about 8085 C. It is cooled in 31E001 before transferred in overhead tank 31D001.A temperature of 7075C is usually required to feed in cells.

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31E001is a plate type heat exchanger which is provided steam as well as cooling water connections. There is also a stand by heat exchanger/cooler 31E003 which is used in case of emergency or for single electrolyzer filling. This heat exchanger can be used only for cooling purpose as there is no steam connections associated with it. Catholyte enters into catholyte overhead tank 31D001 from the top and over flows from top side. Outlet is from the bottom and leads to cell room by gravity. In the cell room three electrolyzers are arranged in parallel. In each electrolyzer 164 elements are placed in series. At present Electrolyzer A has 162 ELZ-B has 161 and ELZ-C has162 elements. Brine is introduced in the anodic compartment of the cell while caustic soda is introduced in cathodic compartment of the cell. When current is introduced, electrolysis takes place. As a result of it caustic soda is produced in the cathodic compartment together with hydrogen gas where as chlorine gas is produced in the anodic compartment.

Electric Supply Circuit:11KV power is supplied from grid station. It is passed through transformer to step it down to 440 V. Then it is passed through rectifiers to convert it into DC which is then supplied to electrolyzers via bus bars and flexibles. There are 2 bus bars and 9 flexibles associated with each electrolyzer.

Reactions:Following reactions takes place in the cells Sodium chloride and water are dissociated in the brine solution according to the equations NaCl H2 O Na+ H+ + + ClOH-

The principal anode reaction involves the oxidation of the anion Cl- to produce chlorine gas 2ClCl2 + 2e-

The primary cathode reaction is the reduction of the cation H+ to produce hydrogen gas 2H+ + 2eH2

The sodium cation Na+ then combines with the OH- ions to form third overall product NaOH Na+ + OHThe overall cell reaction is 2NaCl + 2H2O 14 2NaOH + Cl2 + H2 NaOH

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Side Reactions:The predominant side reactions in the anodic compartment of the cell are 4OH2OH- + Cl2 6ClO- + 3H2O 3ClOO2 + 2H2O + 4eClO- + Cl- + H2O 2ClO3- + 4Cl- + 3/2 O2 + 6H+ + 6eClO3- + 2Cl-

The source of the OH - ions in these reactions is the migration of OH - ions through the membrane from the catholyte solution, caused by attraction to the positively charged anode.

Products Handling:31.5-32.5% caustic soda is produced in cathodic compartment of the cell and is collected in the catholyte header along with hydrogen gas. It leaves the catholyte header by gravity in the main caustic soda header and passes through hydrogen gas separator 31F002.Then it is stored in the catholyte storage tank 31D002 to maintain its level about 50% for circulation through the cells. The excess caustic is transferred in the caustic buffer tank D2000 from where it is fed to evaporators for concentration. It is also transferred to storage tanks as such 32% caustic soda as finished product. The stream leaving the cells, composed of depleted brine and chlorine gas, is discharged in the anolyte header and termed as anolyte. The depleted brine leaves the anolyte header by gravity in the depleted brine header and chlorine gas is separated in the vertical gas header which is connected to main chlorine gas header. The depleted brine is passed through the chlorine gas separator in order to remove maximum chlorine gas contents carried with it. The depleted brine is acidified in the acidification pot 07D005 and then stored in the depleted brine storage tank 07D001U. In the anodic compartment of the cell chlorine gas is produced as a result of electrolysis. It is separated from depleted brine in the vertical gas header as well as in the gas separator 07F001 and is collected in the main chlorine gas header. Hydrogen gas is produced together with caustic soda in the cathodic compartment of the cells and discharged in the catholyte header. It is disengaged from caustic soda in the vertical gas header as well as in the hydrogen gas separator 31F002 and is collected in the main hydrogen gas header Hydrogen gas is also cooled before it is transferred to furnaces for HCl production through heat exchanger E2310Aand B.

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DECHLORINATION
Introduction:Depleted brine from electrolyzer usually contains 0.3 g/lit dissolved chlorine at a pH about 3.5-4.0 and 1.0 g/lit as available chlorine in the form of hypochlorite ions. Depleted brine also carries 2000-2500 ppm of free chlorine. The process of removal of chlorine from the depleted brine is termed as Dechlorination Chlorine must be removed from brine because of the following facts. The removal of impurities in the primary brine purification becomes difficult. In the presence of high contents of chlorine, the impurities in the rock salt are more easily dissolved during brine saturation. Chlorine oxidizes ion exchange resins, hence increasing its consumption. The

chlorates are necessary to remove because It decreases the sodium chloride solubility resulting in decreased efficiency, possible salt precipitation and potentially adverse chlorate conc. in the caustic soda product.

Chlorates have a strong oxidizing effect which is more evident at high concentrations. Chlorates are formed in the anodic compartment of the cell of electrolyzer via chemical or electrochemical reactions as mentioned before. Chlorates removal rate is a function of the chlorate concentration so that it is convenient to operate at a relatively high chlorate concentration in the feed brine. High temperature also favors the chlorates removal, so a temperature of 85- 90C is recommended. The third parameter affecting chlorates removal is pH. A low pH less than 2.0 is favorable.

2.4.2 Process Description:Dechlorination is carried out in three successive steps By vacuum stripping By Sodium Sulphite treatment With activated carbon Depleted brine leaving the electrolyzers flows into the acidification pot 07D005 where it is mixed with acidified stream of brine from reactor R-5050. Then it is collected in depleted brine

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storage tank 07D001, from here the brine is pumped through 07P001A/B. The discharge of the pump is divided into two streams, one leads to vacuum stripper C-5010 and second leads to acid mixing drum DM-5050. Normally 70 to 75% material goes to C-5010 and 25-30% in DM-5050 for decomposition of chlorates. In DM-5050, 33% HCl is added to lower down its pH almost zero, after acidification the brine flows down by gravity into the reactor R-5050 where it is mixed with chlorinated steam coming from the vacuum stripper C-5010. In R-5050 at low pH and high temperature, chlorates are decomposed, producing free chlorine which is vented in the chlorine sniff line. The over flow of R-5050 entered in the acidification pot and lower the pH of the depleted brine ranging 1.5-2.0 NaClO3 + 6HCl NaCl + 3Cl2 + 3H2O

a) By Vacuum Striping
Brine containing absorbed chlorine enters from the upper part of the packed tower C5010 where vacuum is generated by means of steam ejector J-5600 . In such condition brine leaving the tower has 20-50ppm of chlorine. The wet chlorine stripped from the brine leaves the tower and is cooled in the shell and tube type heat exchanger E-5010. The condensed chlorinated water is returned in the depleted brine tank 07D001 while the chlorinated steam is sent to reactor R-5050. The brine flows down by gravity in the dechlorinated brine tank D-5020. The tank is vented to chlorine sniff line.

b) By Sodium Sulphite Treatment:


Sodium sulphite is added to the depleted brine leaving the tank D-5020 by means of an in line injection on suction of the pump P-5020A/B. Sodium sulphite solution is prepared in the tank D-5250B by absorbing of SO2 in sodium carbonate solution and sent in D-5300 by means of pump P-5250A/B. Sulphur dioxide (SO2) is prepared by burning sulphur mud in the sulphur furnace which is sucked through an absorber by a suction fan. The gas is entered from the bottom of the absorber and left from the top. The sodium carbonate solution is fed from the upper side of the absorber and flows down back to the same tank. When the solution is ready it is transferred in tank 5250A. During chlorates decomposition following reaction takes place Na2SO3 + Cl2 + H2O Na2SO4 + 2HCl

c) With Activated Carbon


After treatment with sodium sulphite, brine is passed through an activated carbon bed in tower C-5020. Care must be taken that the carbon should work with acidic brine pH less than 2 and chlorine less than 50ppm. High chlorine contents in brine feeding the tower causes to violent reaction with the carbon, relatively high pH in the feed brine to tower causes carbon degradation in the form of fine particles which can plug the tower. The brine passing out of the tower is made alkaline by the addition of dilute caustic effluent from tank D-5150B. The pH is raised up to 6.09.0 before it is transferred in primary brine section. 18

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When the carbon is packed down it is necessary to counter wash the carbon bed tower. When the pressure drop across the carbon bed became more frequent, then it is packed with fresh activated carbon. Normally this situation occurs after 40-45 days.

2.5 EVAPORATION UNIT


2.5.1 Introduction:The plant is designed for continuous concentration of caustic soda 31-32% to 50%. The concentration is improved by evaporation in a triple effect counter flow falling film evaporator. The plant consists of three falling film evaporators. At first there was only one unit of capacity 120mt/day, with the passage of time capacity of caustic soda plant was enhanced so another evaporation unit of capacity 250 MT/day was designed to meet industrial and consumers needs. Falling film evaporator is a tube bundle heat exchanger with a separator at the bottom. In the separator vapors and thick liquor are separated. The feed liquor is uniformly distributed in the tubes by a distribution device, thus the liquid moves down forming a thin film along inside wall of the tube. That is why it is called a falling film evaporator.

2.5.2 Process Description:The caustic is fed to the first evaporator EV-201 by a pump P-2000A/B installed at the discharge of caustic buffer tank D-2000. On product side the first evaporator is operated under a vacuum. the caustic leaves the first evaporator effect Ev-201at a concentration of 36-37%. The first evaporator is heated with vapors formed in the second evaporator EV202. The shell of the evaporator EV-201 is also under vacuum about 250-270mmHg. The condensate of the EV-201 collected in the same tank. This vacuum is produced by connecting the condenser 201,duct D201and shell condensate lines of EV-201 to TK-201. The vapors of EV-201 are condensed in E201. The cooling water is fed in the shell and the vapors are condensed in the tubes. The condensate is collected in the tank TK-201.The vacuum in E-201 is produced through steam ejectors. After the EV201, pump 201A/B pumped the caustic soda to the second evaporator EV202 via heat exchangers E-202 & E-203. The discharge of the pump P- 201 is divided into two streams; one admitted to the shell of E-202 and second is admitted in the tubes of the E-203. These two streams rejoined before entering the EV-202. This evaporator effect is heated with the vapors from EV-203.the pressure in the shell of EV-202is about 1.9-2.0.The caustic soda enters EV-202 at conc. range 36-37%, and temp. range110 -115C and leaves at conc. 42-43% and temp.120-125C.This caustic soda is fed to the third evaporator EV203 through pump P-202 via E-204 & E205. The condensate is collected in condensate tank TK-202 and then transferred in TK-201 from where it is transferred in D-5150B. The discharge of pump P-202 is again divided into two streams; one admitted to the shell of E-204 and second is admitted in the tubes of the E-205. These two streams rejoined before entering the EV203. This evaporator effect is heated with the steam at a pressure of about 14bars.The caustic side is under a pressure of 2 bars. The vapors produced here are used to heat the second evaporator and the condensate is collected in the tank TK-203.The caustic leaves this evaporator at 50% conc. at temp. of 175185C.

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Now it is to be cooled before storage. For this purpose it is first passed through tube side of E-204. Here its temp. is reduced to 155-160C. Then it is pumped via P-203 through the tube side of the E-202 and E-206, the final temp is about 55-65C. The condensate of the evaporator EV-203 also bears a sufficient amount of heat, which is recovered by passing it through the shells

of E-205 & E-203.The steam condensate at a temp about 97-98C is returned to boiler section.

Equipment Detail:EVAPORATION PLANT Equipmen t EV-201 EV-202 EV-203 E-201 E-202 E-203 E-204 E-205 E-206 No. of Length tubes 139 116 81 405 48*3=144 20*2=40 48*3=144 24*3=72 26*3=78 (mm) 6000 6000 6000 6000 6000 6000 6000 6000 6000 Diameter Thickness (mm) (mm) 48.3 1.65 48.3 1.65 48.3 1.65 25.0 1.00 26.7 1.65 26.7 1.65 26.7 1.65 26.7 1.65 26.7 1.65 Material of Construction SS.904L Ni-201 Ni-201 SS.904L Ni-201 Ni-201 Ni-201 Ni-201 Ni-201

2.5.4 Normal Operating Data:Plant capacity Feed flow rate Steam pressure Pressure in duct 203 Vacuum in E-201 Vacuum in D-201 Vacuum in EV-201 Vacuum in TK-201 250 ton/day 15-25 m3/h 14-15 bar 1.9-2.0 bar (safety blows at 2.1bar) 600-650 mm Hg 550-570 mm Hg 260-280 mm Hg 0.70-0.75 bar

HEAT EXCHANGERS

E-201(surface condenser) Vacuum 600-650 mmHg Condensate temp. 58-60 oC Cooling water flow rate 250-280 m3/h Cooling water temp. 28-32 oC Cooling water pressure 1.2 bar Parameter Tubes Shell Material flow 35-36 % Caustic cooling water Inlet temperature 75-80 oC 28-32 oC o Outlet temperature 55-60 C 35-40 oC

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CAUSTIC SOLIDIFICATION PLANT


Introduction:Caustic solidification plant is designed in order to concentrate 50 % caustic soda to 9798% caustic soda in solid form. For this purpose a single effete tube bundle falling film evaporator is used as pre-concentrator. 50% NaOH is concentrated up to 60% NaOH using vapors produced in the final concentrator for heating in this equipment. In the final concentrator the concentration is improved up to 97-98% using outside heating media. Due to increasing demand of the solidified caustic soda three CSP units are designed on same pattern named as CSP-I capacity, CSP-II and CSP-III. Another plant named as CSP-IV is under construction yet.

2.6.2 Process Description a) Pre-Concentrator:50% caustic soda stored in caustic buffer tank is pumped via PBT-1&2 to feed into pre-concentrator. The flow of the feed is controlled by LCV-9.11. There are temperature and pressure gauges to indicate the feed temperature and pressure respectively. Pre-concentrator is heated with vapors formed in final concentrator. The pre-concentrator is designed as tube bundle falling film evaporator. Above the tubes there are vertical slits through which caustic soda feed flows evenly into the tubes and form an unbroken film along the inner wall of the tube. The pre-concentrator works at 0.93 bar vacuum on the product side. This vacuum is created in the system by steam ejector. A two stage ejector, 14 bar steam, is used for this purpose. The vapors produced in the pre-concentrator are removed by steam ejector and are condensed in a condenser. Vapors are introduced in the shell side of the condenser while cooling water is introduced in the tubes. Vapors condensed in the condenser are collected in the condensate tank. The condensate of the preconcentrator also goes into condensate tank by gravity. From condensate tank it may transfer in M-II plant under level control where it is stored it the D-5150B. The condensate may be overflow into the drain. This condensate is also used for sugar solution preparation and for heating the seal of 60% caustic pump A/B.

b) Final Concentrator:60% caustic soda obtained from pre concentrator is pumped via P8.11A/B to feed it into final concentrator. The feed rate is controlled by FIC-9.09. The final concentrator is basically consisting of 6 individual concentrator tubes and the vapor separator. The caustic soda feed is evaporated in the falling film concentrator at atmospheric pressure by means of heat applied by salt heating medium. The feed liquor is uniformly distributed to each concentrator element. It flows evenly with the inner wall of the tubes from top to bottom. The heat transfer medium moves counter currently from bottom to top inside the heating jackets surrounding the concentrator tubes. 21

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The vapor produced in the course of the concentration process reached the horizontal collecting channel together with concentrated caustic side. The collecting channel is provided with conic baffle which separate vapors and molten caustic side. The vapors leads to the separator which retains caustic droplets contained in the vapor. These vapors leave the separator from the top and are used to heat the pre concentrator. The molten caustic soda leaves the separator through its lower part and is directed by the distributing device to the flaker and/or drum filling device.

The heating medium is a mixture of following salts in a following composition. KNO3 NaNO2 NaNO3 c) Sucrose System:All the equipment and piping in contact with caustic melt is made of pure nickel are low carbon nickel because of corrosive resistant of nickel. Oxygen acts corrosively, particularly when combines with high temperature and form nickel oxide which would contaminate the product i.e. caustic melt, so it is very important to prevent the penetration of atmospheric oxygen into the equipment. For this purpose system is blanketed with nitrogen or steam. In addition by adding 0.15 Kg sugar solution into the system just after the feeding valve to pre concentrator, the nickel pickup of the caustic soda melt is reduced to 2 ppm approximately. 5% aqueous solution of sugar is prepared by using food grade sugar in the water/vapor condensate in the sugar tanks and dosed into the caustic system by pumping via sugar pump at a rate of 3 - 5 lit/hr. Flow rate of sugar dose is very important, low flow may cause increasing nickel ppm and excessive flow may leads to blackish particles in the caustic melt.

53% 40% 7%

d) Flaker:The flaker consists of a rotating drum/cylinder which dips in the vat containing caustic melt. The cylinder is cooled to 60-55 oC by showering cooling water on its inner walls thus a thin film of caustic melt is formed over the drum surface which is scrapped by a sharp blade/scrapper. The flakes thus formed are directly made to fall into the duct which conveys them to the filling hopper where it is provided with an automated weighing and then filling in PPW bags lined with polyethylene bags which is tied with cable ties and then stacked inserting tag cards in the stitching.

e) Dust Collector:For purpose of operational safety and to facilitate the operator working at filling station, a dust collection system is provided. The system consists of a suction fan .It sucks dry air from the flaker, passed through the duct, weighing system and also from the bags. The suction pipe is dipped into a water tank where the caustic soda is precipitated in water in seal pot when its concentration is about 5 to 10%, it is replaced by another water filling.

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2.6.3 Normal Operating Conditions:PRECONCENTRATOR Caustic feed concentration Caustic feed flow rate Caustic feed temperature Caustic feed pressure Temperature in the separator Vapor inlet temperature Vapor outlet temperature Vacuum Caustic outlet temperature Caustic outlet concentration Sugar dose flow rate CONDENSOR Cooling water inlet temperature Cooling water outlet temperature Cooling water flow rate STEAM EJECTOR Steam pressure Water flow rate BURNER Fuel gas flow rate Salt inlet temperature Salt outlet temperature Salt coil temperature Flue gas temperature FINAL CONCENTRATOTR Caustic feed concentration Caustic feed flow rate Caustic feed temperature Caustic temperature in distributor Caustic temperature in vat Salt inlet temperature Salt outlet temperature Vapor outlet temperature FLAKER DRUM Cooling water inlet temperature Cooling water outlet temperature Cooling water flow rate Cooling water pressure Air pressure 50% 1.0-1.25 m3/hr 60-65 oC 6.4-6.5 bar 90-110 oC 350-360 oC shell side 160-165 oC product side 0.9-0.95 bar 68-72 oC 60-61 % 3-5 lit/hr 30-32 oC 35-40 oC 150-200 m3/hr 13-14 bar 900-1000 lit/h 190-210 Nm3/hr 390-405 oC 420-430 oC 420-435 oC 475-500 oC 60-61 % 1.0-1.25 m3/hr 68-70 oC 360-380 oC 325-330 oC 420-430 oC 390-405 oC 360-370 oC 30-32 oC 35-40 oC 50 m3/hr 1.3-1.5 bar 1 bar

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Product Details
Besides producing Caustic Soda, SCIL manufactures many important chemicals. A brief detail on quality and specifications of some of the products is given in the following lines. Ammonium Chloride:Installed Annual Production Capacity Technology Developed by Specifications Physical Appearance Quality Moisture General Product Information Evolves ammonia when reacting with alkali. Exhibits endothermic nature in aqueous media. Absorbs water & moisture when exposed to atmosphere. Shelf Life: Long life is expected in airtight bags. Product Handling and Safety Instruction It is supplied in the packing of 25 kg Polypropylene bags, having polyethylene liner in bags. Must be stored in well-ventilated and covered area. Do not store it along with caustic soda and other alkaline materials If ammonium chloride contacts the eyes, then eyes must be irrigated immediately with plenty of water for at least 15 minutes. Carbon dioxide Gas:Specifications Appearance/ Colour Normal/Colorless gas. Purity 99.9 % min Taste None Odor None/Characteristics Uses Large quantities of solid carbon dioxide (i.e. in the form of dry ice) are used in processes requiring large scale refrigeration. Carbon dioxide is also used in fire extinguishers as a desirable alternative to water for most fires. It is a constituent of medical gases as it promotes exhalation. It is also used in carbonated drinks. White Crystals 99.7 0.2% 0.1 % max. 3,000 MT Mannesmann (Germany)

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Internship Report (SCIL) Product Handling & Safety Instructions Dry carbon dioxide can be handled in most common structural materials. Moist carbon dioxide is generally corrosive by its formation of carbonic acid. Ferrous Nickel alloys are slightly susceptible to corrosion. At normal temperatures carbon dioxide is compatible with most plastics and elastomers. Use local exhaust to prevent accumulation of high concentrations so as to reduce the oxygen level in the air to less than 19.5% and the carbon dioxide concentration below the exposure limit. Protective gloves of any material appropriate for the job. Positive pressure air line with full-face mask and escape bottle or self-contained breathing apparatus should be available for emergency use. Bleaching Powder:Installed annual production capacity Technology Developed by Specifications Physical Appearance Available Chlorine Moisture Stability White fine Powder 30 % 1 0.50 % max. On heating at 100 2 C it does not lose more than 1/15th of the available chlorine. 4,500 MT Davy mc-kee (Germany)

General Product Information Stable below 0.5 % moisture contents. Produces chlorine odor or HOCl in case of high moisture contents and start decomposing. Decomposes by absorption of CO2 from air. Decomposition by oxygen separation with low water contents, which is accelerated in the presence of heavy metals (Fe+3, Ni and Co etc). Shelf Life: One year in airtight drums; 03 months in airtight bags, if stored at room temperature and dry place Product Handling and Safety Instruction It is supplied in 25 kg Polypropylene bags having polyethylene liner in bags. Airtight packing protects decomposition of bleaching powder due to carbon dioxide from air. Must be stored separately in well-ventilated and covered area. Avoid contact with other chemicals especially from all acids. It catches fire on exposure to naked flame and high temperature.

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Calcium Chloride Purity Physical Appearance Specifications Calcium Chloride Magnesium Chloride Calcium Hydroxide Calcium Sulfate Alkali Chloride Water Insoluble pH (5% w/v solution) Arsenic As Lead Pb Iron Fe Barium Ba Sodium Na Principal Application Minimum 77%w/w White granules /powder

77% Min 2.0% Max 0.3% Max 0.3% Max 0.5% Max 0.5% Max 4.5-9.2 3.0 ppm (max) 10.0 ppm(max) 20.0 ppm(max) 10.0 ppm(max) 20000.00 ppm(max)

Additive to oil well completion. Drying petroleum fractions. Beverages for removing Sodium ion. Mining as dust proofing and freezing resisting ore & coal. Drying air and gases, remove moisture by Hygroscopicity. Fungicides as oxidizing agent. Pharmaceutical as drying and desiccating agent. Water Treatment. Material Handling Must be store in well-ventilated, covered and dry area. Long life is expected in airtight bags. If calcium chloride contacts the eyes, then eyes must be irrigated immediately with plenty of water for at least 15 minutes. Packing Supplied in packing of 25 kg PP Laminated bags having polyethylene line

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Caustic Soda Liquid (33%) Installed Annual Production Capacity Technology Developed by Grade Specifications NaOH Na2CO3 NaCl NaClO3 Na2SO4 Iron Silica Hg General Product Information Caustic attacks body tissue upon contact. The degree of injury depends upon the extent and duration of contact, temperature and concentration of the caustic. Its corrosive action on tissues causes burns and frequently deep ulcerations. Its contact with the eyes rapidly causes severe damage. Caustic solution is detectable by a slippery feeling like soapy water. Toxic limits are TLV = 2 mg. / cubic meter of air. Shelf Life: Long life if protected from air & contamination. Product Handling and Safety Instruction Immediately remove all contaminated clothing and equipment effected by the Caustic, Flush the exposed area thoroughly with a lot of water, followed by washing with a solution of 5 % ammonium chloride in water. If caustic contacts the eyes, they should be irrigated immediately with plenty of water for at least 15 minutes. Hold the eyelids opened during irrigation. The eyes should be then washed with a dilute boric acid solution and wash the eye with water for an additional 15 minutes. A physician should be seen immediately after the eye is thoroughly washed. For personal protection, use face shields, gloves, gum-boots and protective suites. Use safety shower and wash with plenty of water for at least 15 minutes. Caustic soda (liquid) is transported in Mild Steel tanks. 50 + 0.5 % 0.5 % max 0.02 % max 0.01 % max 0.01 % max 10 ppm max 10 ppm max free 129,500 MT Denora(Italy),AKCC(Japan) Commercial

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Caustic Soda Liquid (50%) Installed annual production capacity Technology Developed by Grade Specifications NaOH Na2CO3 NaCl NaClO3 Na2SO4 Iron Silica General Product Information Caustic attacks body tissue upon contact. The degree of injury depends upon the extent and duration of contact, temperature and concentration of the caustic. Its corrosive action on tissues causes burns and frequently deep ulcerations. Its contact with the eyes rapidly causes severe damage. Caustic solution is detectable by a slippery feeling like soapy water. Toxic limits are TLV = 2 mg. / cubic meter of air. Shelf Life: Long life if protected from air & contamination. Product Handling and Safety Instruction Immediately remove all contaminated clothing and equipment effected by the Caustic, Flush the exposed area thoroughly with a lot of water, followed by washing with a solution of 5 % ammonium chloride in water. If caustic contacts the eyes, they should be irrigated immediately with plenty of water for at least 15 minutes. Hold the eyelids opened during irrigation. The eyes should be then washed with a dilute boric acid solution and wash the eye with water for an additional 15 minutes. A physician should be seen immediately after the eye is thoroughly washed. For personal protection, use face shields, gloves, gum-boots and protective suites. Use safety shower and wash with plenty of water for at least 15 minutes. Caustic soda (liquid) is transported in Mild Steel tanks 50 + 0.5 % 0.5 % max. 0.02 % max. 0.01 % max. 0.01 % max. 10 ppm max. 20 ppm max. 129,500 MT Denora(Italy),AKCC(Japan) Commercial

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4.7 Caustic Soda Flakes Installed Annual Production Capacity Technology Developed by Grade Specifications NaOH Na2CO3 NaCl NaClO3 Na2SO4 Iron Silica General Product Information Caustic attacks any body tissue upon contact. The degree of injury depends upon the extent and duration of contact and the temperature and concentration of the caustic. Its corrosive action on tissues causes burns and deep ulcerations. Its contact with the eyes rapidly causes severe damage. Caustic solution is detectable by a slippery feeling like soapy water Toxic limits are TLV = 2 mg. / cubic meter of air. Shelf Life: Long life if protected from air & moisture. Product Handling and Safety Instruction Immediately remove all contaminated clothing and equipment effected by the Caustic. Flush the exposed area thoroughly with a lot of water, followed by washing with a solution of 5 % ammonium chloride in water. If caustic contacts the eyes, they should be irrigated immediately with plenty of water for at least 15 minutes. Hold the eyelids opened during irrigation. The eyes should then be washed with a dilute boric acid solution and wash the eye with water for an additional 15 minutes. A physician should be seen immediately after the eye is thoroughly washed. For personal protection, use face shields, gloves, gum-boots and protective suites. Caustic soda (Flakes) is packed in 25 kg polypropylene bag having polyethylene liner in it. 97.0 1 % 1.0 % max. 0.04 % max. 0.02 % max. 0.01 % max. 20 ppm 20 ppm 129,500 MT Denora(Italy),AKCC(Japan) Commercial

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Summary
Sitara chemical industries is a well known and famous chemicals manufacturer of Pakistan. It is an organization of very responsible and well trained professionals. At the same time SCIL has well developed and well managed Environment Management System and Quality Management System which have been certified and audited by SGS under the authority of UKAS. They produced Caustic Soda along with many other chemicals. SCIL produces Caustic Soda in form of either 33% Caustic solution or as 50% Caustic solution or Caustic flakes of 98.5% purity. Four Caustic Soda manufacturing plants are working at SCIL. The Caustic production cycle goes through many steps. These sections include primary brine section, where depleted brine is saturated and purified by settling, chemical treatment and filtration through pressure leaf filters. After primary treatment brine is ultra purified in secondary section by passing through ion exchange resin beds. When brine meets the required degree of purification and concentration, it is fed to electrolyzers in cell room. In cell room, a current of almost 12.5kA is passed through the brine solution in special type of cells called as membrane cells. Chlorine and Hydrogen are also produced as by products along with Caustic in cell room. They are separated from Caustic and depleted brine and are sent to HCl furnace after necessary treatments. Caustic, thus produced is 33%. It is concentrated up to 50% in three effect, backward feed, falling film, evaporation unit. This 50% caustic is then sent to Caustic Solidification Plant (CSP) to convert it into 98.5% Caustic which is then packed in drums or as flakes in PP bags. Some side reactions also occur in cell room resulting, the formation of chlorates. Therefore brine coming out of cell room contains chlorine and chlorates in it. This brine is sent to the dechlorination section where these contaminates are removed by stripping, treatment with HCl and sodium sulphite and by passing through carbon tower. This dechlorinated brine is then recycled in primary section for saturation. Different utilities such as water, electricity, instrument air and nitrogen for purging H2 and Cl2 lines are also used.

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