6 INNOVATIVE PROCESS FOR TREATMENT OF SULFURIC ACID WASTE LIQUIDS WITH RECOVERY OF ANHYDROUS SODIUM SULFATE

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1 1 6 INNOVATIVE PROCESS FOR TREATMENT OF SULFURIC ACID WASTE LIQUIDS WITH RECOVERY OF ANHYDROUS SODIUM SULFATE Barry Asano, Project Manager CANVIRO CONSULTANTS A Division of CH2M HILL ENGINEERING LTD. Mississauga, Ontario, Canada L5N 2x7 Dr. Ing. M. Olper, Technical Director Engitec Impianti Tonolli Process Technology Tonolli Canada Limited is a lead recovery and re in the City of Mississauga, Ontario, Canada. Approximately 80% of the feedstock for the plant comes from batteries purchased from scrap dealers and battery manufacturers within 600 km of Mississauga. Electrolyte drained from the batteries is 17 weight percent sulfuric acid. This operation generates approximately 9 million liters per year of sulfuric acid waste liquids. In 1985, Tonolli was requested by the Regional Municipality of Peel to investigate options available for acid recycling or waste treatment to reduce the concentration of soluble sulfate in the discharge to the sewer from the plant. After evaluating a number of options in detail, including lime neutralization, caustic neutralization, waste acid upgrading, and the sale of waste acid without treatment, Tonolli selected the CX Process to satisfy the Region s new waste management request. This process was developed by Tonolli s affiliate company, Engitec Impianti, Milan, Italy. The process, which has been proven in two commercial facilities in Europe, is based on neutralization and reaction of the acid waste with sodium carbonate followed by evaporative crystallization. In addition to overcoming the liquid waste disposal problem, the process has the benefit of recovering detergent-grade sodium sulfate as a byproduct for sale. The process also dramatically reduces the volume of solid waste (slag) that is normally generated in the lead recovery operation. Thus the process has the double benefit of byproduct recovery and waste minimization. Design and construction of this innovative waste management process is underway at Tonolli Canada Limited. ORIGINAL ACID WASTE TREATMENT SYSTEM A schematic flowsheet of the original acid waste treatment system is illustrated in Figure 1. Waste battery acid from the crushing plant, yard washings, and rain water runoff from the yard unloading and slag are% was drained :G three acid pits. Acid pit t! was!mated in the unloading/cr??shing plaa? and received most of the acid from the battery crushing operation. Wastes collected in the acid pits were pumped to two lined lagoons, each covering an area of approximately 1100 m2. The lagoon acid was pumped to the treatment plant where it was neutralized and filtered prior to discharge. The neutralization was performed in three parallel tanks using 50% sodium hydroxide and air as an agitation medium for mixing. Settlement of the precipitate as a batch process was allowed to proceed overnight. An anionic flocculant was added to enhance the settling characteristics of the rticulate matter. After settling, the supernatant was drawn off and the settled sludge was pumped ck to the lagoons. The clarified liquid was discharged directly to the sanitary sewer. The treated J waste liquid composition is shown in Table 1. Activated carbon filters were available as a final treatment stage to ensure compliance with the lead level discharge standards. Sludge from the ponds was trucked away for disposal. As in typical caustic soda neutralization systems, only small amounts of sludge were generated, being limited to the heavy metal precipitate. 43rd Purdue Indus/rru/ H uw Conference Proceedings, Levis Publishers. Inc., Chelsea, Michigan Printed in U.S.A.

2 46 4%~ PURDUE UNIVERSITY INDUSTRIAL WASTE CONFERENCE PROCEEDINGS nagement system. Arsenic

3 BARRY ASANO and ING. M. OLPER 47 EYUmr.W\/ Y, acid treatment system. water tanks while the used wash water fr sent to a filtered water tank. Most of the used wash water is recycled to the process while some is pumped to the crystallizer with filtrate. The wet cake, which is comprised of lead carbonate and a small amount of unconverted lead sulfate is collected and smelted in furnaces to recover the lead product. The filtrate solution is treated in a clarifying filter to remove fine solids and then is pumped to the evaporative crystallizer. The crystallizer is heated by vapor recompression with the cooled condensate being recycled to the process. The magma from the crystallizer is pumped to a centrifugal separator where the solid sodium sulfate product is separated from the mother liquor which is recycled to the evaporator. The sodium sulfate is dried, cooled, and directed to storage in a pneumatically transported system. Depending on the sodium chloride content of the sodium carbonate used for neutralizing, a purge may have to be taken from the crystallizer so that the sodium sulfate product will meet the sodium chloride specification for detergent quality sodium sulfate. Typical specifications required for detergent-grade sodium sulfate are shown in Table 11. The purge from the crystallizer is evaporated in a purge crystallizer. The high sodium chloride content purge product is recovered as a lower grade sodium sulfate. Operating experience in two European plants indicates that 4-5% of the sodium sulfate solution may have to be purged to control the chloride level in the main product. PROCESS DESIGN A summary of the key process design bases is listed in Table 111. The new system is designed to recover 7,100 tons per year of sodium sulfate meeting detergent-grade specifications and an additional 400 tons per year of purge sodium sulfate. --. NEUTRALUAm N.acq +,., + n,o Figure 3. Desulfurizalion and neutralization reactions

4 G.- Na2C03. Insolubles 1.5% 1.O% 0.01 % 5 mg/l 0.1 % TRUCTION APPROACH ases. This was necessary because the y and therefore minimum disruption struction enables full use of funds as ndensate tanks, filter other components of the system, ve crystallizer, centrifugal separator the existing works is s v Table 111. Summary of Process Design Bases Batteries processed Waste acid solution generated 9 million liters per year - Sodium sulfate recovered 7,100 tons Per Year, product meeting detergent grade specification Lead carbonate cake for smelting Metallic lead (gn'ds/poles/connectors) Polypropylene chips Ebonite and polyethylene separators (used for supplemental fuel) Operating basis for chemical process 400 tons Per year, purge product 24,000 tons per year M,000 tons per year 3,000 tons per year 2,000 tons per year 24 hours Per day, 7 days per week, 48 weeks per year

5 BARRY ASANO and ING. M. OLPER 49 Table IV. General Economics Capital cost of new system %6,000,000 Operating & maintenance costs Revenue from sale of sodium sulfate $300,000/yr $ ,000/yr Original waste acid treatment cost $540,000/yr Reduction in solid waste disposal cost $1 50,000/yr GENERAL ECONOMICS General project economics are outlined in Table IV. The revenue from the sale of recovered sodium sulfate will depend on the market price for the product. SUMMARY Tonolli Canada Limited is currently designing and constructing a new acid waste treatment process at its Mississauga plant to satisfy more stringent effluent discharge criteria. This unique process enables recovery of a saleable byproduct, detergent-grade anhydrous sodium sulfate, while at the same time reducing solid waste, air emissions, and worker health and safety risks. The process has been proven in two European facilities and is a cost-effective way to overcome a number of pollution control problems. i ACKNOWLEDGEMENTS The cooperation and assistance of the staff at Tonolli Canada Limited is greatly appreciated. AI1 queries regarding the process technology should be directed to Dr. M. Olper, Engitec Impianti, Viale E. Jenner, 51, Milan, Italy.

6 ll PURDUE ~ ~ UNIVERSITY INDUSTRIAL WASTE CONFERENCE PROCEEDINGS -5% &. REFERENCES Tonolli Canada Ltd., Problems in the Lead-Acid Battery Recycling Industry, Ontario Ministry of the Environment, Education Seminar, (September 1986). U.S. Environmental Protection Agency, Draft Report, Emerging Technology in the Secondary Lad Industry, Office of Research and Development, Cincinnati, Ohio. Regulatory Compliance and Low Lead Prices Create a Crisis for Lead-Acid Batteries, Recyding Today, Volume 25. Number 4, (May 1987). %rap Battery Components Recovery Plant, Engitec Impianti spa Tecnologie Tonolli, Bulletin (1987). 1

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