CN103000968A - Lead plaster desulfurization transforming method for waste lead-acid storage batteries - Google Patents
Lead plaster desulfurization transforming method for waste lead-acid storage batteries Download PDFInfo
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- CN103000968A CN103000968A CN2012104243056A CN201210424305A CN103000968A CN 103000968 A CN103000968 A CN 103000968A CN 2012104243056 A CN2012104243056 A CN 2012104243056A CN 201210424305 A CN201210424305 A CN 201210424305A CN 103000968 A CN103000968 A CN 103000968A
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- lead
- desulfurization
- lead plaster
- waste
- conversion fluid
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The invention discloses a lead plaster desulfurization transforming method for waste lead-acid storage batteries, which belongs to the field of waste battery disposal. The method comprises the following steps: (1) the preparation of a lead plaster original sample: carrying out decomposition on waste lead-acid storage batteries, taking out a grid alloy, taking out lead plaster from a grid, removing impurities in the lead plaster, drying the lead plaster in an environment at a temperature of 80-90 DEG C, and grinding the lead plaster in a grinding machine for 10-30 min so as to obtain the lead plaster original sample with a particle size of 50-300 mu m; (2) the configuration of a desulfurization transforming agent: preparing a desulfurization transforming agent into transforming liquid, and heating the desulfurization transforming liquid to 20-90 DEG C by using a constant-temperature water bath bed; (3) full reaction: adding weighted lead plaster into the transforming liquid obtained in step (2), and stirring the obtained mixture, so that the mixture is fully reacted; and (4) after the transforming is completed, cooling and filtering the obtained product, and carrying out repeated washing and residue filtering on the obtained product for many times by using distilled water. According to the method, the desulfurization transforming process parameters of lead plaster in waste lead-acid storage batteries are determined, PbSO4 is effectively transformed into easily-decomposed PbCO3, the energy consumption is lowered, and the environmental pollution is reduced.
Description
Technical field
The invention belongs to the old and useless battery treatment field, more particularly, relate to a kind of waste lead acid battery lead cream desulfurization and transformation method.
Background technology
In recent years, along with the continuous increase of the day by day exhausted of lead ore resource and the plumbous amount of lead acid accumulator consumption, reclaiming lead becomes the important channel of realizing the lead resource sustainable development from lead-acid accumulator.Yet in China, because technology is immature, in the process of plumbous regeneration plurality of heavy metal or SO are arranged
2Be discharged in the environment, pollute.The plumbous amount of the consumption of China's lead acid accumulator occupies about 70% of total value at present, but recycling waste lead batteries rate less than 90%, and developed country's general warranty 100%; In addition, the lead recovery in China's secondary lead smelting process is generally about 80%, and Foreign Advanced Lerel can reach more than 98%.Therefore annual China has the waste lead accumulator about 30,000 tons to fail to be recycled utilization approximately; cause China to have approximately every year lead and lead compound about 4.5 ten thousand tons to flow in air, the soil and water because the rate of recovery is low simultaneously; cause the serious wasting of resources and environmental pollution (Li Jinhui etc.; China's recycling waste lead batteries is utilized present situation and management game; environmental protection, (2000) No.4:40-42).In this simultaneously, according to the literature, according to the reserve-production ratio of having verified at present the lead ore resource, lead ore is only enough exploited 25-30.Along with the mouth benefit of lead ore resource is exhausted, the recycling and reuse of lead metal has become the only way of realizing the plumbing sustainable development.The also direct relation development of China's plumbing of the research of carrying out the plumbous regenerative process of pollution-free or light pollution.
Lead metal mainly consumes in the production of storage battery at present, and therefore plumbous regenerative process mainly is the lead plaster slag mud in the lead-acid accumulator to be reduced transform to obtain the process of lead and lead alloy.The difficult point of this process is the smelting of lead plaster, its method can be divided at present pyrogenic process, wet method and do wet combination method (Xiao Yongqing. market business opportunity unlimited [J] is produced in automobile-used waste lead acid battery reclaiming. the metal world, 2004 (2): 11-13; Hu Tao, Han Hong, Zhu Bin waits recovery [J] plumbous in the waste lead acid battery. battery, 2007,37 (6): 472-473; Straight China. pollution-free pyrogenic process is smelted reviver and alloy [J] from used and scrapped battery. Shanghai non-ferrous metal, 2002,23 (4): 156-163).Pyrometallurgical smelting exists that metal recovery rate is low, energy consumption is high and seriously polluted three large problems.Do wet combination method and generally take wet desulphurization, pyrometallurgical smelting, namely waste lead accumulator is carried out cracking and sorting, comprehensively reclaims, after the lead plaster desulfurization transforms, carries out melting with rotary kiln or reverberatory furnace again.This method has significantly reduced SO than pure pyrometallurgical smelting
2Discharge capacity, but therefore high-temperature service has still been adopted in the later stage melting, can't can cause lead dust pollution with avoiding.The wet treatment of waste lead accumulator can be divided three classes: (1) lead plaster desulfurization transforms one and leaches an electrodeposition method; (2) lead plaster directly leaches an electrodeposition method; (3) lead plaster direct electrowinning method.From the angle of environmental protection, the plumbous regeneration techniques of wet method is to eliminate SO
2With the important method of lead dust pollution, but since hydrometallurgy for the solids in the scrap battery not the bonus point selection of land to mix smelting mixing, cause having approximately every year 10000 tons of lead to run off in vain.
Summary of the invention
The technical problem that solves
For the problem that the lead-acid accumulator recovery utilization rate is low, seriously polluted and lead plaster pyrometallurgical smelting cost is high that exists in the prior art, the invention provides a kind of waste lead acid battery lead cream desulfurization and transformation method, it has determined the technological parameter that the lead plaster desulfurization transforms in the lead-acid accumulator, effectively with PbSO
4The PbCO of conversion in order to be easy to decompose
3, after the desulfurization pyrometallurgical smelting temperature of lead plaster than its desulfurization before smelting temperature low more than 150 ℃, reduced energy consumption, alleviated environmental pollution.
Technical scheme
Purpose of the present invention is achieved through the following technical solutions.
A kind of waste lead acid battery lead cream desulfurization and transformation method of the present invention the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 80 ~ 90 ℃ environment, grinds the lead plaster former state that 10 ~ 30min gets granularity 50 ~ 300 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, with the water bath with thermostatic control bed desulfurization conversion fluid is heated to 20 ~ 90 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted;
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
Preferably, the desulfurization transforming agent in the described step (2) is Na
2CO
3, NH
4HCO
3And K
2CO
3Mixture, and Na
2CO
3: NH
4HCO
3: K
2CO
3=1:2 ~ 6:1(mass ratio).
Preferably, in the described step (2), the temperature of conversion fluid is 60 ~ 70 ℃.
Preferably, in the described step (2), the pH value of conversion fluid is 6 ~ 9.5.
Further, in the described step (2), the pH value of conversion fluid is 7.
Preferably, in the described step (2), the CO in the conversion fluid
3 2-Concentration be 0.5 ~ 1.5mol/L.
Preferably, in the described step (3), the stir speed (S.S.) of conversion fluid is 700 ~ 1300r/min.
Preferably, the granularity of lead plaster former state is 100 ~ 125 μ m in the described step (1).
Beneficial effect
Than prior art, the invention has the advantages that:
(1) in the method for the invention, control granularity size and certain conditions such as temperature, time and mixing speed so that lead plaster fully reacts with the desulfurization transforming agent, generate sulfate, PbCO in agitating device
3Or PbO etc.For pyrometallurgical smelting, lead plaster is after the desulfurization preliminary treatment, and plumbous grade gets a promotion, and has reduced the inventory of advancing stove, and the lead metal rate of recovery effectively improves.Because PbCO
3At about 340 ℃ of lower PbO that just can be decomposed into, therefore lead plaster can carry out pyrometallurgical smelting under lower temperature after desulfurization is processed, and after the desulfurization pyrometallurgical smelting temperature of lead plaster than its desulfurization before smelting temperature low more than 150 ℃, thereby reduced energy consumption, alleviated environmental pollution.The experiment structure shows, adopts this technology that the sulfur content of furnace charge is reduced more than 90%, has greatly reduced and has smelted required flux amount and SO
2Discharge capacity; With compare before the desulfurization, lead plaster smelting ability has improved 30%, the metallic lead rate of recovery reaches more than 90%, Energy Intensity Reduction surpasses 10%, smelts discarded object and reduces 75%;
(2) because pH value affects the final form of converted product, so need in the course of reaction to keep pH value in 6 ~ 9.5 scope, under these circumstances, PbSO
4Conversion ratio can reach more than 80%.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
A kind of waste lead acid battery lead cream desulfurization and transformation method of the present invention the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 80 ~ 90 ℃ environment, grinds the lead plaster former state that 10 ~ 30min gets granularity 50 ~ 300 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, with the water bath with thermostatic control bed desulfurization conversion fluid is heated to 20 ~ 90 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted;
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
Embodiment 1
A kind of waste lead acid battery lead cream desulfurization and transformation method of present embodiment 1 the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 80 ℃ environment, grinds the lead plaster former state that 10min gets granularity 50 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, and the desulfurization transforming agent is Na
2CO
3, NH
4HCO
3And K
2CO
3Mixture, and Na
2CO
3: NH
4HCO
3: K
2CO
3=1:2 ~ 3:1(mass ratio).The pH value of conversion fluid is 6.CO in the conversion fluid
3 2-Concentration be 0.5mol/L, with the water bath with thermostatic control bed desulfurization conversion fluid is heated to 20 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted; The stir speed (S.S.) of conversion fluid is 700r/min.
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
Embodiment 2
A kind of waste lead acid battery lead cream desulfurization and transformation method of present embodiment 2 the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 85 ℃ environment, grinds the lead plaster former state that 20min gets granularity 100 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, and the desulfurization transforming agent is Na
2CO
3, NH
4HCO
3And K
2CO
3Mixture, and Na
2CO
3: NH
4HCO
3: K
2CO
3=1:3 ~ 4:1(mass ratio).CO in the conversion fluid
3 2-Concentration be 1.0mol/L, the pH value of conversion fluid is 7.With the water bath with thermostatic control bed desulfurization conversion fluid is heated to 70 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted; The stir speed (S.S.) of conversion fluid is 1000r/min.
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
Embodiment 3
A kind of waste lead acid battery lead cream desulfurization and transformation method of present embodiment 3 the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 90 ℃ environment, grinds the lead plaster former state that 30min gets granularity 300 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, and the desulfurization transforming agent is Na
2CO
3, NH
4HCO
3And K
2CO
3Mixture, and Na
2CO
3: NH
4HCO
3: K
2CO
3=1:5 ~ 6:1(mass ratio).CO in the conversion fluid
3 2-Concentration be 1.5mol/L, the pH value of conversion fluid is 9.5, with the water bath with thermostatic control bed desulfurization conversion fluid is heated to 90 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted; The stir speed (S.S.) of conversion fluid is 1300r/min.
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
Below schematically the invention and execution mode thereof are described, this description does not have restricted.So, if those of ordinary skill in the art is enlightened by it, in the situation that does not break away from this creation aim, without the creationary technical scheme similar to this technical scheme and the embodiment of designing, all should belong to the protection range of this patent.
Claims (8)
1. a waste lead acid battery lead cream desulfurization and transformation method the steps include:
(1) lead plaster former state preparation
The lead-acid accumulator resolution process is taken out grid alloy, take off lead plaster from grid, impurities removing is dried in 80 ~ 90 ℃ environment, grinds the lead plaster former state that 10 ~ 30min gets granularity 50 ~ 300 μ m in grinder;
(2) configuration desulfurization transforming agent
The desulfurization transforming agent is mixed with conversion fluid, with the water bath with thermostatic control bed desulfurization conversion fluid is heated to 20 ~ 90 ℃;
(3) fully reaction
Load weighted lead plaster is added in the conversion fluid that step (2) makes, and stir it is fully reacted;
(4) complete rear cooling to be transformed is filtered, and repeatedly washes filter residue repeatedly with distilled water.
2. waste lead acid battery lead cream desulfurization and transformation method according to claim 1 is characterized in that, the desulfurization transforming agent in the described step (2) is Na
2CO
3, NH
4HCO
3And K
2CO
3Mixture, and Na
2CO
3: NH
4HCO
3: K
2CO
3=1:2 ~ 6:1(mass ratio).
3. waste lead acid battery lead cream desulfurization and transformation method according to claim 2 is characterized in that, in the described step (2), the temperature of conversion fluid is 60 ~ 70 ℃.
4. according to claim 2 or 3 described waste lead acid battery lead cream desulfurization and transformation methods, it is characterized in that in the described step (2), the pH value of conversion fluid is 6 ~ 9.5.
5. waste lead acid battery lead cream desulfurization and transformation method according to claim 1 and 2 is characterized in that, in the described step (2), the pH value of conversion fluid is 7.
6. waste lead acid battery lead cream desulfurization and transformation method according to claim 5 is characterized in that, in the described step (2), and the CO in the conversion fluid
3 2-Concentration be 0.5 ~ 1.5mol/L.
7. waste lead acid battery lead cream desulfurization and transformation method according to claim 3 is characterized in that, in the described step (3), the stir speed (S.S.) of conversion fluid is 700 ~ 1300r/min.
8. according to claim 1 or 7 described waste lead acid battery lead cream desulfurization and transformation methods, it is characterized in that the granularity of lead plaster former state is 100 ~ 125 μ m in the described step (1).
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| CN201210424305.6A CN103000968B (en) | 2012-10-31 | 2012-10-31 | A kind of waste lead acid battery lead cream desulfurization and transformation method |
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|---|---|---|---|
| CN201210424305.6A CN103000968B (en) | 2012-10-31 | 2012-10-31 | A kind of waste lead acid battery lead cream desulfurization and transformation method |
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| CN103000968B CN103000968B (en) | 2015-10-07 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468970A (en) * | 2013-09-03 | 2013-12-25 | 四川景星环境科技有限公司 | Lead plaster desulfurizer and desulphurization method for secondary lead industry |
| CN103540741A (en) * | 2013-11-05 | 2014-01-29 | 湖南江冶机电科技股份有限公司 | Forcible wet desulphurization process for lead plaster |
| WO2016049994A1 (en) * | 2014-09-29 | 2016-04-07 | 湖南江冶机电科技股份有限公司 | Lead paste desulfurization method based on grinding mechanism |
| CN105950872A (en) * | 2016-06-30 | 2016-09-21 | 中南大学 | Waste lead-acid battery diachylon hydrothermal reduction dual conversion method |
| CN106816662A (en) * | 2016-12-24 | 2017-06-09 | 骆驼集团蓄电池研究院有限公司 | A kind of waste diachylon high-efficiency desulfurization technique |
| CN111170351A (en) * | 2018-11-13 | 2020-05-19 | 湖南省金翼有色金属综合回收有限公司 | Lead sulfate waste material desulfurization device and process thereof |
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2012
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103468970A (en) * | 2013-09-03 | 2013-12-25 | 四川景星环境科技有限公司 | Lead plaster desulfurizer and desulphurization method for secondary lead industry |
| CN103540741A (en) * | 2013-11-05 | 2014-01-29 | 湖南江冶机电科技股份有限公司 | Forcible wet desulphurization process for lead plaster |
| CN103540741B (en) * | 2013-11-05 | 2015-11-04 | 湖南江冶机电科技股份有限公司 | A kind of lead plaster wet method forces sulfur removal technology |
| WO2016049994A1 (en) * | 2014-09-29 | 2016-04-07 | 湖南江冶机电科技股份有限公司 | Lead paste desulfurization method based on grinding mechanism |
| CN105950872A (en) * | 2016-06-30 | 2016-09-21 | 中南大学 | Waste lead-acid battery diachylon hydrothermal reduction dual conversion method |
| CN105950872B (en) * | 2016-06-30 | 2017-12-12 | 中南大学 | A kind of method of waste lead acid battery lead cream hydrothermal reduction dual conversion |
| CN106816662A (en) * | 2016-12-24 | 2017-06-09 | 骆驼集团蓄电池研究院有限公司 | A kind of waste diachylon high-efficiency desulfurization technique |
| CN111170351A (en) * | 2018-11-13 | 2020-05-19 | 湖南省金翼有色金属综合回收有限公司 | Lead sulfate waste material desulfurization device and process thereof |
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