MBA TECH CHEMICAL

Chemical Processes 1 Report

Chloro-Alkalis
Prabhdeep SinghVirdi
4/26/2010

Roll no 215

This Report contains the various details of Chloro-alkalies, their properties , manufacturing processes, top manufacturers and the economic scenario of the indutry

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Chlor-Alkalies Contents
Introduction.................................................................................................................................................. 2 Properties of Causitic Soda and Chlorine...................................................................................................... 2 Caustic soda .............................................................................................................................................. 2 Chlorine ..................................................................................................................................................... 3 Top Manufacturers and their details ............................................................................................................ 4 REACTIONS ............................................................................................................................................. 5 Comparison of cell technologies ........................................................................................................... 6 Manufacturing process .............................................................................................................................. 7 Mercury cells ................................................................................................................................. 8 Diaphragm cells ................................................................................................................................... 9 Membrane cells ............................................................................................................................. 9 Chlorine processing..................................................................................................................... 10 Hydrogen processing ................................................................................................................... 11 Caustic soda processing ..................................................................................................................... 11 Brine processing ................................................................................................................................. 12 Environmental issues within the chlor/alkali industry ................................................................................ 13 Chlorine bleaching of wood pulp and dioxin emissions to the environment ................................... 13 Ozone layer depletion ......................................................................................................................... 14 Polyvinyl chloride plastic ................................................................................................................... 14 Mercury emissions ............................................................................................................................. 15 Asbestos .............................................................................................................................................. 15 Economic Overview of chloroalkal industry ............................................................................... 16 Major Chemicals .................................................................................................................... 16

Caustic Soda ...................................................................................................................................... 16 Overview .......................................................................................................................................... 16 Industry............................................................................................................................................ 17 Major Players ................................................................................................................................. 17

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Chlorine ................................................................................................................................................ 18 Overview .......................................................................................................................................... 18 Industry............................................................................................................................................ 18 Major Players ................................................................................................................................. 18 References ................................................................................................................................................... 18

Introduction Salt is one of the oldest and most popular condiments. What is relatively unknown, however, is that salt is also the raw material for one of the most potentially profitable chemical industries in the country chlor alkali. This is possibly one of the few industries where supply far exceeds demand, making it a promising candidate for export. So it seems almost surreal that the chlor alkali industry faces a threat from the imported product. The chlor alkali industry in India is around 60 years old. It began with a modest capacity of a few thousand tonnes per annum and has since grown into a 2.24 million tonnes per annum capacity industry

Properties of Causitic Soda and Chlorine

Caustic soda

Specific gravity Odour Melting point (calcination) Boiling point Hygroscopicity Solubility in water
2

2.13 Odourless 320C 1390C Hygroscopic and deliquescent Highly soluble

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Solubility in organic solvents

Soluble in alcohols but insoluble in ether and benzene

Chlorine

Colour Odour Boiling (liquefying) point Freezing (melting) point Density - liquid - dry gas Vapour Pressure Latent heat of vaporisation Liquid - Gas volume relationship Solubility in water

Gas-Greenish Yellow Liquidclear Amber Characteristic, suffocating -34C (1 atm) -101C (1 atm) 1.468 gms/cc at 0C and 3.617 atm 3.209 g/L (0C, 1 atm) 3.617 atm (at 0C) 68.7 cal/gm at -34C One volume of liquid chlorine weighs as much as 457.6 volumes of gas at 0C and 1 atm Slightly soluble

Chemical properties
I - Flammability 1. Neither liquid nor gaseous chlorine is explosive or flammable. II Reactivity than 5% of either component,

1. A mixture of chlorine and hydrogen containing more forms an explosive substance.

2. It reacts with ammonia, alkalies and hydroxides of alkaline earth metals.

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3. It reacts with organic compounds to form chlorinated derivatives and hydrogen chloride. Some of these reactions, particularly those with hydrocarbons, alcohols and ethers may become explosive. Dry Chlorine reacts with several materials.

Top Manufacturers and their details

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REACTIONS Electrochemical and chemical reactions occurring in mercury cells [1] 2Cl- ==> Cl2 + 2e[2] 2Na+ + 2Hg + 2e- ==> 2Na (in Hg) 2Cl- + 2Na+ + 2Hg ==> Cl2 + 2Na (in [3] Hg) [4] 2Na (in Hg) + 2H2O ==> H2 +2NaOH + Hg (anodic reaction) (cathodic reaction) (overall cell reaction) (decomposer reaction) (overall process reaction) (anodic reaction) (cathodic reaction) (overall ionic reaction) Electroche mical and chemical reactions occurring in diaphrag m and membran e cells Reaction [9] will contaminat e the caustic product with chlorate.

[5] 2NaCl + 2H2O ==> Cl2 +2NaOH + H2 [1] 2Cl ==> Cl2 + 2e
-

[6] 2H2O + 2e- ==> 2OH- + H2 [7] 2Cl- + 2H2O ==> Cl2 + H2 + 2OH-

[5] 2NaCl + 2H2O ==> Cl2 +2NaOH + H2 (overall reaction) [8] Cl2 + 2NaOH ==> NaOCl + NaCl + H2O (side reaction) (side reaction)

[9] 3NaOCl ==> NaClO3 + 2NaCl

Chemical reactions occurring in brine processing [10] CaSO4 + Na2CO3 ==> CaCO3 +NaSO4 (CaCO3 precipitates) (Mg(OH)2 precipitates)

[11] MgCl2 + 2NaOH ==> Mg(OH)2 +

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2NaCl

Comparison of cell technologies Mercury Operating current density ( kA/m2) Cell voltage (V) NaOH strength (wt%) Energy consumption ( kWh/MT Cl2) at a current density of (kA/m2) Steam consumption (kWh/MT Cl2) for concentration to 50% NaOH 8 - 13 3.9 - 4.2 50 3360 (10) 0 Diaphragm Membrane 0.9 - 2.6 2.9 - 3.5 12 2720 (1.7) 610 3-5 3.0 - 3.6 33-35 2650 (5) 180

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Manufacturing process The chlor-alkali (also called "chlorine-caustic") industry is one of the largest electrochemical technologies in the world. It is an energy intensive process and is the second largest consumer of electricity (2400 billion kWh) among electrolytic industries. In 2006, about 84% of the total world chlorine capacity of about 59 million metric tons was produced electrolytically using diaphragm and membrane cells, while about 13% was made using mercury cells (Figure 4). Chlorine is produced by the electrolysis of sodium chloride (common table salt) solution, often called "brine." Thus, when sodium chloride is dissolved in water, it dissociates into sodium cations and chloride anions. The chloride ions are oxidized at the anode to form chlorine gas and water molecules are reduced at the cathode to form hydroxyl anions and hydrogen gas. The sodium ions in the solution and the hydroxyl ions produced at the cathode constitute the components of sodium hydroxide formed during the electrolysis of sodium chloride. (The chemical reactions occurring in the cell are shown in the Appendix.) Fig. 4. Chlorine cell technology in the U.S. Chlorine is produced electrolytically using three types of electrolytic cells. The main difference in these technologies lies in the manner by which the chlorine gas and the sodium hydroxide are prevented from mixing with each other to ensure generation of pure products. Thus, in diaphragm cells, brine from the anode compartment flows through the separator to the cathode compartment, the separator material being either asbestos or polymer-modified asbestos composite deposited on a foraminous cathode. In membrane cells, on the other hand, an ionexchange membrane is used as a separator. Anolyte-catholyte separation is

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achieved in the diaphragm and membrane cells using separators and ion-exchange membranes, respectively, whereas mercury cells contain no diaphragm or membrane and the mercury itself acts as a separator. The anode in all technologies is titanium metal coated with an electrocatalytic layer of mixed oxides. All modern cells (since the 1970's) use these so-called dimensionally stable anodes" (DSA). Earlier cells used carbon based anodes. The cathode is typically steel in diaphragm cells, nickel in membrane cells, and mercury in mercury cells. These cell technologies are schematically depicted in Figures 5-7 and are described below. Mercury cells The mercury cell has steel bottoms with rubbercoated steel sides, as well as end boxes for brine and mercury feed and exit streams with a flexible rubber or rubber-coated steel cover. Adjustable metal anodes hang from the top, and mercury (which forms the cathode of the cell) flows on the inclined bottom. The current flows from the

Fig. 5. Schematic of a mercury cell. steel bottom to the flowing mercury.

Saturated brine fed from the end box is electrolyzed at the anode to produce the chlorine gas, which flows from the top portion of the trough and then exits. The sodium ion generated reacts with the mercury to form sodium amalgam (an alloy of mercury and sodium), which flows out of the end box to a vertical cylindrical tank. About 0.25% to 0.5% sodium amalgam is produced in the cell. The sodium amalgam reacts with water in the decomposer, packed with graphite particles and produces caustic soda and hydrogen. Hydrogen, saturated with water vapor, exits from the top along with the mercury vapors. The caustic soda then flows out of the decomposer as 50% caustic. The unreacted brine flows out of the exit end box. Some cells are designed with chlorine and anolyte outlets from the end box, which are separated in the depleted brine tank. The mercury from the decomposer is pumped back to the cell.

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Diaphragm cells The diaphragm cell is a rectangular box with metal anodes supported from the bottom with copper-base plates, which carries a positive current. The cathodes are metal screens or punch plates connected from one end to the other end of the rectangular tank. Asbestos, dispersed as a slurry in a bath, is vacuum Fig. 6. Schematic of a diaphragm cell. deposited onto the cathodes, forming a diaphragm. Saturated brine enters the anode compartment and the chlorine gas liberated at the anode during electrolysis, exits from the anode compartment. It is saturated with water vapor at a partial pressure of water over the anolyte. The sodium ions are transported from the anode compartment to the cathode compartment, by the flow of the solution and by electromigration, where they combine with the hydroxyl ions generated at the cathode during the formation of the hydrogen from the water molecules. The diaphragm resists the back migration of the hydroxyl ions, which would otherwise react with the chlorine in the anode compartment. In the cathode compartment, the concentration of the sodium hydroxide is ~12%, and the salt concentration is ~14%. There is also some sodium chlorate formed in the anode compartment, dependent upon the pH of the anolyte. Membrane cells

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In a membrane cell, an ionexchange membrane separates the anode and cathode compartments. The separator is generally a bi-layer membrane made of perfluorocarboxylic and perfluorosulfonic acidbased films, sandwiched between the anode and the cathode. The saturated brine is fed to the anode compartment where Fig. 7. Schematic of a membrane cell. chlorine is liberated at the anode, and the sodium ion migrates to the cathode compartment. Unlike in the diaphragm cells, only the sodium ions and some water migrate through the membrane. The unreacted sodium chloride and other inert ions remain in the anolyte. About 30-32% caustic soda is fed to the cathode compartment, where sodium ions react with hydroxyl ions produced during the course of the hydrogen gas evolution from the water molecules. This forms caustic, which increases the concentration of caustic solution to ~35%. The hydrogen gas, saturated with water, exits from the catholyte compartment. Only part of the caustic soda product is withdrawn from the cathode compartment. The remaining caustic is diluted to ~32% and returned to the cathode compartment. Thus, all three basic cell technologies generate chlorine at the anode, and hydrogen along with sodium hydroxide (caustic soda) in the cathode compartment (or in a separate reactor for mercury cells, see Figure 5). The distinguishing difference between the technologies lies in the manner by which the anolyte and the catholyte streams are prevented from mixing with each other. Separation is achieved in a diaphragm cell by a separator, and in a membrane cell by an ion-exchange membrane. In mercury cells, the cathode itself acts as a separator by forming an alloy of sodium and mercury (sodium amalgam) which is subsequently reacted with water to form sodium hydroxide and hydrogen in a separate reactor. Chlorine processing The chlorine gas from the anode compartment contains moisture, by-product oxygen, and some back-migrated hydrogen. In addition, if the brine is alkaline, it

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will contain carbon dioxide and some oxygen and nitrogen from the air leakage via the process or pipelines. Chlorine is first cooled to 60oF (16oC) and passed through demisters to remove the water droplets and the particulates of salt and sodium sulfate. The cooled gas goes to sulfuric acid circulating towers, which are operated in series. Commonly, three towers are used for the removal of moisture. The dried chlorine then goes through demisters before it is compressed and liquefied at low temperatures. The noncondensed gas, called snift gas, is used for producing hypochlorite or hydrochloric acid. If there is no market for hydrochloric acid, the snift gas is neutralized with caustic soda or lime (calcium hydroxide) to form hypochlorite. The hypochlorite is either sold as bleach or decomposed to form salt and oxygen. Hydrogen processing The hydrogen gas from the chlor-alkali cells is normally used for the production of hydrochloric acid or used as a fuel to produce steam. Hydrogen from mercury cells is first cooled to remove the mercury, which is then returned to the cells. Occasionally, a secondary treatment is used to remove the trace levels of mercury in the hydrogen via molecular sieve columns. The hydrogen gas is then normally compressed. If a customer needs nearly pure hydrogen containing low amounts of oxygen, some plants will heat the hydrogen over a platinum catalyst (to remove the oxygen by reacting it with the hydrogen to form water), cool, and compress the diaphragm or membrane cell hydrogen, before supplying it to the customer. The heat value in the hydrogen cell gas can be recovered in a heat exchanger via heating the brine feed to the cells. Although only shown for diaphragm cells, the heat recovery from hydrogen is also possible with mercury and membrane cell processes.

Caustic soda processing Caustic soda is marketed as 50%, 73%, or anhydrous (dry) beads or flakes. The mercury cell can produce 50% and 73% caustic directly. The caustic from the decomposer is cooled and passed once or twice through an activated carbon filter to reduce the mercury levels in the caustic. After filtration, the mercury concentration is lowered to the parts-per-million (ppm) levels. Even these low levels of mercury may be unacceptable to some customers, who then have to switch to using membrane grade caustic soda. The mercury cell caustic soda has a

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few ppm salt and <5-ppm sodium chlorate. The mercury cell caustic is the highest purity caustic that can be made electrolytically if trace concentrations of mercury are tolerable in the end use of caustic. The membrane cell caustic is concentrated in a multiple effect falling film evaporator, which increases the caustic soda concentration to 50% with a high steam economy. Caustic soda from membrane cells generally has 30-ppm sodium chloride and 5-10 ppm sodium chlorate. The catholyte from the diaphragm cells contains ~12% sodium hydroxide, ~14% sodium chloride, 0.25%-0.3% sodium sulfate, and 100-500 ppm sodium chlorate. The catholyte is evaporated in a multi-effect evaporator. Most of the salt from the catholyte will precipitate during the concentration of the caustic soda to 50% sodium hydroxide. The 50% caustic soda product will contain about 1% sodium chloride. The 50% caustic also has a high chlorate concentration (~0.1%) compared to the caustic from membrane or mercury cells (~10 ppm). The salt, separated from the caustic during evaporation, is used to re-saturate the brine fed to the cell. An additional single-effect evaporator is needed to produce 73% caustic soda. Anhydrous (dry) caustic soda is produced in a rising film evaporator, operating at 725oF (385oC) and at a few inches (one inch =2.54 cm) of water vacuum. Brine processing Sodium chloride is available in the form of solid salt, mined by excavation or by evaporating seawater. It is also available as a liquid by solution mining the salt domes. The salt has varying concentrations of impurities, which should be removed to operate the electrolytic cells at a high current efficiency. The major impurities are calcium, magnesium, and sulfates. The other minor impurities, which are undesirable, depending upon the type of chlor-alkali process selected, are barium, strontium, manganese, aluminum, silica, iron, vanadium, chromium, molybdenum, titanium, etc. The solution-mined brine or the solid salt dissolved in the salt dissolver is treated in a reactor with sodium carbonate and caustic soda to precipitate calcium carbonate and magnesium hydroxide . These precipitates are settled in a settler. The underflow carries the solid slurry, which is pumped to a filter to remove it as sludge, or sometimes, it is disposed off along with the rest of the liquid effluent from the plant. The calcium carbonate precipitates are heavy, and drag with it the

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hydroxides of aluminum, magnesium, strontium, etc. The overflow from the settler, which carries ~10-50 ppm (parts per million) of suspended solids, is filtered. For the mercury and the diaphragm cell process, this brine is adequate, and can be fed to the electrolyzers. In the all cell processes, the filtered brine is heated and passed through a bed of salt in a saturator in order to increase the salt concentration before feeding it to the electrolyzers. In some plants, the brine feed is acidified to improve the cell current efficiency. The acidification reduces the alkalinity, which would otherwise react with the chlorine in the anolyte compartment forming chlorate. The membrane cell process brine specifications are more stringent than that of the mercury and diaphragm processes, and calls for impurities to be at the parts-perbillion (ppb) level. This is accomplished by filtering the brine in a pre-coat type secondary filter. An ion-exchange resin is used to remove the calcium, magnesium, barium, and iron impurities. It is also possible to remove aluminum by ion exchange. Often, aluminum and silica are removed by adding magnesium chloride in the brine exiting from the salt dissolver. The depleted brine from the membrane and mercury cell processes carries dissolved chlorine. This brine is acidified to reduce the chlorine solubility, and then dechlorinated in a vacuum brine dechlorinator. The dechlorinated brine is returned to the brine wells for solution mining or to the salt dissolver. If the membrane and diaphragm processes coexist at a given location, the dechlorinated brine can be sent to a saturator for resaturation before being sent to the diaphragm cells.

Environmental issues within the chlor/alkali industry There are several environmental concerns that have made a significant impact on the growth of the chlor-alkali industry over the past twenty years and will dictate the future growth as well. These issues are highly debated, and the associated "chemophobia" is likely to adversely affect the chlorine consumption profile in the future. Chlorine bleaching of wood pulp and dioxin emissions to the environment

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Presence of dioxin, at parts per trillion (ppt) levels, in paper and paper based products and chlorinated organics in pulp mill effluents led to decreased chlorine demand. In the U.S., chlorine consumption in the pulp and paper industry, decreased from 15% in 1987 to 7% in 1998. The U.S. Environmental protection agency promulgated "Cluster Rules" in late 1998, mandating the use of elemental chlorine-free bleaching. These rules, which went into effect in April 2001, lowered the chlorine utilization in the North American pulp and paper bleaching operations in favor of sodium chlorate, hydrogen peroxide and oxygen. Ozone layer depletion Because of their contribution to the ozone layer depletion, production of chlorinated fluorocarbons (CFC's), carbon tetrachloride (CCl4), and 1,1,1trichloroethane was banned in 1997 following the Montreal Accord. Chlorinated methanes and ethanes are under great scrutiny due to the environmental and occupational concerns associated with them. Nevertheless, their production will continue because of their use in the manufacture of HCFC-22. HCFC-22 is less harmful than the CFC's towards ozone depletion and is an intermediate in the production of tetrafluoroethylene for use in the production of Teflon and other fluoro polymers. HCFC's are currently substituted for the CFC's, until they are phased out. HFC's containing no chlorine are not subject to this restriction. Polyvinyl chloride plastic In 1987, approximately 38% of all U.S. chlorine production was consumed in vinyl chloride monomer (VCM) production to satisfy the growing polyvinyl chloride (PVC) demand. Through 2010, VCM demand is expected to grow annually because of the demand for PVC in the construction, packaging, and other industries. Nearly 85% of all ethylene dichloride (EDC) manufactured in the United States is used to produce VCM, and another 11% is exported, mostly for foreign VCM production. Even with increasing energy prices in North America, the EDC and VCM capacity is expected to keep growing, by 1.1%, through 2010. However, there are two major environmental issues with PVC, which include their lack of biodegradability and generation of dioxins when they are incinerated for energy recovery and for controlled waste recycling. Hydrochloric acid formation during the thermal decomposition of PVC is another issue that environmentalists are strongly invoking for the substitution of chlorine-free products for PVC.

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Mercury emissions Between 1930 and 1960, several tons of mercury waste was dumped in Minamata Bay in Japan. Thousands of people living around the bay developed methylmercury poisoning through the consumption of contaminated fish. The victims suffered from severe neurological damage, which later became known as Minamata Disease. All told, thousands were afflicted and more than 900 died. As of April 1997, more than 17,000 people had applied to the government to be certified as Minamata victims, 12,615 have been officially recognized. Since then, there was a significant move away from mercury-cell technology to diaphragm and ion-exchange-membrane-cell operations and currently only 35% of the world capacity (mostly in western and center Europe and about 10% of U.S. production) of chlorine is produced using the mercury-cell process. There will be no new construction of mercury-cell plants. Existing plants are focusing on operating their plants at lower than the maximum mercury loss requirements of 1.9 gram/year/metric ton of chlorine as set by the Eurochlor- Best Available Technology. The Eurochlor - BAT plan for mercury emissions became effective in 2007. The goal was to reduce emissions to 1.0g Hg per tonne of Hg cell chlorine capacity. By 2005, the emissions level dropped from 1.09 in 2004 to 1.05g Hg/t chlorine capacity and by 2007 this goal was achieved. Asbestos Asbestos is used as a separator material in diaphragm cells. However, asbestos is a toxic material, causing lung cancer, asbestosis, and mesothelioma. As a result, in 2007, a bill was adopted to ban most uses of asbestos in the United States. ChlorAlkali plants were exempt because few cost effective alternatives exist for this technology. However, the EPA could revoke this exemption if unreasonable risks to health or the environment are found. Some ways that the industry has avoided these risks have included surveillance and monitoring programs for asbestos related diseases and use of proper safety equipment and filtration systems during times of unavoidable exposure. In other countries, the use of asbestos in diaphragm cells had already been banned. Even with all these constraints, the chlor-alkali industry is projected to grow at a rate of 1 to 3% depending on pessimistic or optimistic reasoning. Much of this will be dictated on how effectively the industry responds to the concerns of the environmentalists and the government agencies.

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Economic Overview of chloroalkal industry

Rs. 9,600 crore industry (US $ 2.2 billion) Covers a wide spectrum of products - Soda ash, Caustic soda, Sulphuric acid, Chlorine Calcium Carbonate, Hydrogen Peroxide, Potassium Chlorate, Lead Phosphorus, Titanium Dioxide, Aluminium Fluoride, Carbon Blac Inorganic chemicals are used mainly in the manufacture of detergents, glass industry, soaps, fertilisers, alkalies, etc.

Production Major Chemicals Installed Capacity 1865 1964.5 1031.1 286.2 95 96 96 97 97 98

Products Soda ash Caustic Soda Liquid Chlorine Carbon Black

'000 tonnes 98 99 99 2000*

1552.1 1540 1545.8 1560 1243.1 1250 1309.2 1320 709 715 702.9 715 230

1560 1350 740 240

223.6 250.8 208.3

Caustic Soda Overview

Caustic soda industry saw a sudden surge of activity after liberalisation

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Reasons for capacity additions - a surge in demand for chlorine (by product) There are four processes for making caustic soda diaphragm cell, mercury cell, membrane cell and chemical process technology Membrane cell the most energy efficient process and is being increasingly adopted. In all new plants, it is mandatory to use this technology

Industry

Capacity : 1964,500 tonnes; 98-99 production 1320,000 tonnes Industry characterised by 45 players with turnovers ranging from Rs. 15-20 crores (US $ 3.5 mn - US $ 4.5 mn) Average plant size - 42,000 tpa 5 - 6 large players having an annual turnover of Rs 80 crores (US $ 18 million) dominate the market NaCl, a major raw material, available in Gujarat (60 % of Indias salt production is from Gujarat) NaCl accounts for 15 - 20% of cost of production of caustic soda cost. Many companies have captive salt farms

Major Players

GACL, Bharuch Kanoria Chemicals, Ahmedabad DCM, Kota Tata Chemicals, Jamnagar SIEL, Kota Andhra Sugar, Kovvur

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Chlorine Overview

Chlorine is generated as a co-product with caustic soda It is a toxic, hazardous chemical and is used in the manufacture of PVC, pulp and paper, bleaching powder, etc. Difficult to handle - has to be transported in heavy cylinders freight cost high. Hence sales are restricted to nearby locations. Chlorine consumption likely to improve with increase in production and consumption of PVC / Plastics

Industry

Installed capacity - 1031,000 tonnes 98-99 production - 715,000 tonnes Industry characterised by over 40 players Most manufacturers produce a wide range of chemicals. Chlorine often a co-product of caustic soda Companies located in the Gujarat belt

Major Players

Gujarat Alkalies & Chemicals - Vadodara DCM Sriram - Kota Kanoria Chemicals - Ahmedabad Andhra Sugar - Kovvur Punjab Alkalies - Jallandhar

References
http://en.wikipedia.org/wiki/Chlorine

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http://www.indiamarkets.com/imo/industry/chemicals http://www.moneycontrol.com http://www.adityabirlachemicals.com/ http://www.chemfabalkalis.com/ http://www.gujaratalkalies.com http://www.chemicalweekly.com Drydens outlines of chemical technology

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