CN102351217B - Method of removing lead in by-product sodium sulfate of recovery and processing of waste lead storage batteries - Google Patents
Method of removing lead in by-product sodium sulfate of recovery and processing of waste lead storage batteries Download PDFInfo
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- CN102351217B CN102351217B CN 201110167133 CN201110167133A CN102351217B CN 102351217 B CN102351217 B CN 102351217B CN 201110167133 CN201110167133 CN 201110167133 CN 201110167133 A CN201110167133 A CN 201110167133A CN 102351217 B CN102351217 B CN 102351217B
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- lead
- sodium sulfate
- carbonate
- sodium
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Abstract
Provided is a method of removing lead in the by-product sodium sulfate of recovery and processing of waste lead storage batteries. According to the invention, mother liquor for desulphurization by using crude lead mud and sodium carbonate are fully stirred, and a sodium hydroxide solution is added until the pH value of the mother liquor is 10; a sodium carbonate solution is added drop by drop under the condition of complete stirring until the pH value of the mother liquor is 10.5; lead sulfate is converted into basic lead carbonate which is precipitated; basic lead carbonate precipitate is removed by filtering and is recovered; obtained filtrate is condensed through distillation, and condensed filtrate is cooled to obtain crystals of sodium sulfate decahydrate, wherein, lead content in the crystals of sodium sulfate decahydrate meets quality requirements for industrial products of sodium sulfate. The method provided in the invention is simple and feasible.
Description
Technical field
The present invention relates to waste and old lead storage battery and recycle, specifically, is that waste and old lead storage battery reclaims the method for taking off lead in the processing in the sodium sulfate byproduct.
Background technology
Along with the automotive industry great development, the recovery processing of waste and old lead storage battery is important all the more, the plumbous mud that obtains in the recovery processing of waste and old lead storage battery, adopt the pre-sulfur removal technology of yellow soda ash, the lead sulfate that is about in the plumbous mud transfers lead carbonate to, pre-desulfuration efficiency reaches more than 96%, greatly reduce the sulphur content in the raw materials for metallurgy, reduced the sulphur emissions amount in the flue gas in the fusion process, be converted into low-melting lead carbonate because of high-melting-point lead sulfate in the raw material simultaneously, reduce the smelting reducing temperature, reduced fuel consumption.Fig. 1 is seen in its technical process.
Mainly contain sodium sulfate, yellow soda ash in the pre-desulphurization mother solution, and unconverted lead sulfate (lead content about 0.2% in the sodium sulfate) etc., directly condensing crystal is inevitable leaded in the gained sodium sulfate.
Summary of the invention
The present invention adopts the chemical precipitation technology that pre-desulphurization mother solution is taken off plumbous the processing, and its technical scheme is as follows:
A kind of waste and old lead storage battery reclaims the method for removing lead of by-product sodium sulfate in the processing, and as shown in Figure 2, it comprises the steps:
Step 1. adds lead bullion mud mother liquor hydro-oxidation sodium solution under fully stirring of yellow soda ash desulfurization, to its pH value=10,
Step 2. drips sodium carbonate solution with step 1 gained solution under fully stirring, to its pH=10.5, make lead sulfate be converted into white lead carbonate (Pb
2(OH)
2CO
3), precipitation,
Step 3. removes by filter step 2 gained precipitation white lead carbonate, reclaims,
Step 4. concentrates the filtrate distillation of step 3 gained, and cooling obtains the sal glauberi crystallization, and its lead tolerance reaches the industrial goods specification of quality of sodium sulfate.
Method simple possible of the present invention, the lead of the plumbiferous sodium sulfate mother liquor that waste and old lead storage battery is reclaimed produce in the plumbous sweetening process is produced white lead carbonate and is reclaimed, and the mother liquor behind the deleading concentrates the sal glauberi that obtains meeting sodium sulfate industrial goods specification of quality.
Description of drawings
Fig. 1 is waste and old lead storage battery roughing flow diagram;
Fig. 2 takes off splicer's process flow skeleton diagram for plumbous mud desulphurization mother solution of the present invention.
Embodiment
Embodiment
Get the pre-desulphurization mother solution of 100ml, its sodium sulphate content is 15.3%, and lead content is 500mg/L.Under agitation drip 15% sodium hydroxide solution to pH=10, change into and drip 15% sodium carbonate solution, to pH=10.5, continue to stir 20min, generate a large amount of white cotton-shaped white lead carbonate precipitations, filter, lead concentration is 0.4 mg/L in the filtrate.
Filtrate is concentrated into 50ml, and crystallisation by cooling is separated out colourless sal glauberi crystal 12.6g.Get the 5g sal glauberi and use water dissolution again, survey its lead content, obtaining the sal glauberi lead content is 0.022%, satisfies the specification of quality of industrial goods sodium sulfate.
Claims (1)
1. the method for removing lead of by-product sodium sulfate is characterized in that it comprises the steps: during a waste and old lead storage battery reclaimed and processes
Step 1. adds lead bullion mud mother liquor hydro-oxidation sodium solution under fully stirring of yellow soda ash desulfurization, to its pH value=10,
Step 2. at abundant agitation and dropping sodium carbonate solution, to its pH=10.5, makes lead sulfate be converted into white lead carbonate step 1 gained solution, precipitation,
Step 3. removes by filter step 2 gained precipitation white lead carbonate, reclaims,
Step 4. concentrates the filtrate distillation of step 3 gained, and cooling obtains the sal glauberi crystallization.
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CN 201110167133 CN102351217B (en) | 2011-06-21 | 2011-06-21 | Method of removing lead in by-product sodium sulfate of recovery and processing of waste lead storage batteries |
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CN 201110167133 CN102351217B (en) | 2011-06-21 | 2011-06-21 | Method of removing lead in by-product sodium sulfate of recovery and processing of waste lead storage batteries |
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CN102351217A CN102351217A (en) | 2012-02-15 |
CN102351217B true CN102351217B (en) | 2013-07-31 |
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Families Citing this family (6)
Publication number | Priority date | Publication date | Assignee | Title |
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US9670565B2 (en) | 2014-06-20 | 2017-06-06 | Johnson Controls Technology Company | Systems and methods for the hydrometallurgical recovery of lead from spent lead-acid batteries and the preparation of lead oxide for use in new lead-acid batteries |
US9555386B2 (en) | 2014-06-20 | 2017-01-31 | Johnson Controls Technology Company | Systems and methods for closed-loop recycling of a liquid component of a leaching mixture when recycling lead from spent lead-acid batteries |
US10062933B2 (en) | 2015-12-14 | 2018-08-28 | Johnson Controls Technology Company | Hydrometallurgical electrowinning of lead from spent lead-acid batteries |
CN106337112A (en) * | 2016-08-25 | 2017-01-18 | 安徽华铂再生资源科技有限公司 | Wet low-liquid-solid-ratio desulfurization process for waste lead-acid storage battery lead plaster |
CN107640778B (en) * | 2017-09-04 | 2019-08-27 | 超威电源有限公司 | A method of the low cost recycling sodium sulphate from leaded desulfurization waste liquor |
CN113846223A (en) * | 2021-10-16 | 2021-12-28 | 安徽省华鑫铅业集团有限公司 | Method for desulfurizing, processing and recycling lead slime of waste battery |
Citations (1)
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CN101244831B (en) * | 2008-03-18 | 2010-06-30 | 华中科技大学 | Method and device for recycling anhydrous sodium sulfate from desulfurization lead plaster filter liquor |
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ITMI20041456A1 (en) * | 2004-07-20 | 2004-10-20 | Engitec S R L | PASTEL DESULFORATION PROCESS AND LEAD STORAGE GRIDS + |
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CN101244831B (en) * | 2008-03-18 | 2010-06-30 | 华中科技大学 | Method and device for recycling anhydrous sodium sulfate from desulfurization lead plaster filter liquor |
Non-Patent Citations (2)
Title |
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胡辉等.铅膏脱硫及其滤液中硫酸钠回收利用的影响因素实验研究.《中国环境科学学会学术年会论文集》.2009,725-729. |
铅膏脱硫及其滤液中硫酸钠回收利用的影响因素实验研究;胡辉等;《中国环境科学学会学术年会论文集》;20091231;725-729 * |
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