CN103290225A - Method for recovering lead from lead-containing solid wastes - Google Patents
Method for recovering lead from lead-containing solid wastes Download PDFInfo
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- CN103290225A CN103290225A CN2013102460912A CN201310246091A CN103290225A CN 103290225 A CN103290225 A CN 103290225A CN 2013102460912 A CN2013102460912 A CN 2013102460912A CN 201310246091 A CN201310246091 A CN 201310246091A CN 103290225 A CN103290225 A CN 103290225A
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- lead
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- metal chloride
- leaching
- alkaline earth
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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
Abstract
A method for recovering lead from lead-containing solid wastes comprises the following steps: 1, fragmenting the lead-containing solid wastes, ball-milling, leaching with an alkali chloride-alkaline earth metal chloride solution or an alkaline earth metal chloride solution as a leaching agent, and filtering; 2, adding an NaOH solution or solid NaOH to a filtrate obtained in step 1 for completely converting PbCl2 in the solution at 20-90DEG C for 30-120min to form basic lead chloride, filtering after the reaction completion, and washing to obtain a filtrate and a filter residue which is basic lead chloride; 3, adding basic lead chloride to the NaOH solution for completely converting basic lead chloride into lead hydroxide, filtering after the reaction completion, washing to obtain a filtrate and a filter residue which is lead hydroxide, and carrying out drying dehydration of lead hydroxide to form lead oxide; and 4, recovering or regenerating the leaching agent. The method has the advantages of simple process, simple operation, low processing cost, high lead recovery rate and no pollution to the environment.
Description
Technical field
The present invention relates to a kind of plumbous method that from the lead-contained solid refuse, reclaims, especially relate to and reclaim plumbous method in the lower lead-contained solid refuse of a kind of lead content that from nonferrous metallurgical process, produces.
Background technology
Lead is important non-ferrous metal, along with the increase day by day of demand in the world wide, and the pressure of multiaspect such as the mineral products primary lead is faced with commercial mining reserves scarcity, and the selecting and purchasing smelting technology is seriously polluted.For solving the critical shortage of first resource, also reduce raw material and smelting selection cost simultaneously, plumbous production more and more relies on plumbous secondary resource-secondary lead, contains the main source that lead-contained solid refuses such as lead anode slurry and melting waste slag have become secondary lead.
Lead containing sludge belongs to hazardous solid waste, and the mishandling unordered discharging that will cause leaded acid solution and solid slag causes the severe contamination of ambient air, soil, the face of land and groundwater resource, threatens human body health.Therefore, to the recycling of lead-contained solid refuse, be a resource regeneration problem, the major issue of a containment Lead contamination environment especially.
At present, plumbous recovery technology is divided by production method and roughly can be divided into pyrogenic process, full wet method and do three kinds of wet integrated processs.Secondary lead factory still extensively adopts pyrogenic attack lead-contained solid refuse both at home and abroad, and adopt of modern secondary lead factory done wet integrated process, i.e. wet desulphurization conversion-fire reduction smelting technique more.With respect to pyrogenic attack, lead dust and SO can be fundamentally eliminated in wet processing
2Polluting, is a kind of eco-friendly lead-contained solid waste treatment method.Wet processing process to the lead-contained solid refuse mainly contains both at home and abroad:
1, RSR technology: adopt (NH
4)
2CO
3Or Na
2CO
3Carry out feeding SO after desulfurization transforms as sweetening agent
2Gas or sulphite reduce the PbO in the lead plaster solution
2, the plumbous oxide of generation and lead carbonate precipitate the HBF with 20%
4Or H
2SiF
6Solution leaches and makes electrolytic solution, and electrolysis obtains pure lead powder, and purity is greater than 99.99%, and current efficiency can reach 96%.
2, USBM technology: this technology is that United States Patent (USP) (US, 4769116[P] .1988-9-6.) in 1988 proposes.Compare with RSR technology, its characteristics are exactly PbO
2Reduction reaction adopt lead powder or H
2O
2As reductive agent; Nearest Chinese patents in 2010 (CN 101899576 A) also have identical report.The employing Na of Chinese patent (CN 1664132A) in 2005 proposition
2NO
2As PbO
2Reductive agent.What people such as Wang Duyou proposed uses FeSO under the sulfuric acid existence condition
4Plumbic oxide is reduced to lead sulfate, adds yellow soda ash again lead sulfate is transformed.More than the subsequent disposal of report subsequent processes and RSR technology is basic identical.
3, Placid technology: lead plaster directly adopts the HCl-NaCl solution system of heat to leach, and makes PbSO
4, Pb and PbO
2The soluble PbCl of the system that is converted into
2, purify leach liquor and in having the electrolyzer of cation exchange membrane, carry out electrolytic deposition Pb.
4, Plint technology: this technology is by the Placid technological development, and leaching is identical with Placid technology with scavenging process, unique different be to adopt the lime precipitation step to replace electrolysis with PbCl
2Be converted into Pb (OH)
2, lead hydroxide reduces in reactor with hard coal and obtains metallic lead.
5, other wet treatment methods: CN 101885510A discloses and has a kind ofly prepared the method for lead chloride and calcium sulfate by waste lead accumulator lead plaster wet method, adopts the HCl-NaCl system that lead plaster is leached, can be effectively with the Pb in the lead plaster, PbO, PbO
2And PbSO
4Be converted into the PbCl of solubility
2, obtain lead chloride by crystallisation by cooling again.
At present, full wet method or do the plumbous recovery technology of wet integrated process and be applied to the higher lead-acid accumulator recycling of lead content mostly, and that the one-tenth of low-grade lead-contained solid refuse is grouped into for waste lead acid battery lead cream is more complicated, and difficult recycling.Above-mentioned prior art all can't directly apply to the recycling of complicated low-grade lead-contained solid refuse of composition.
Summary of the invention
Technical problem to be solved by this invention is, provides a kind of and can be directly reclaims plumbous method from the complicated low-grade lead-contained solid refuse of composition.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method that reclaims lead from the lead-contained solid refuse may further comprise the steps:
(1) dense saline solution leaching lead: with the fragmentation of lead-contained solid refuse, below ball milling to 60 order, be that leaching agent carries out lead and leaches with alkali metal chloride-alkaline earth metal chloride solution or alkaline earth metal chloride solution, follow stirring when leaching, leaching temperature is 20-100 ℃ (preferred 70-90 ℃), and leaching time is 30-120 minute; Filter, get filtrate and filter residue;
(2) alkaline solution is heavy plumbous: add NaOH solution or solid sodium hydroxide in step (1) gained filtrate, make the PbCl in the solution
2Be converted into mineral yellow fully, invert point is 20-90 ℃ (preferred 60-80 ℃), and transformation time is 30-120 minute; After question response is complete, filter, washing gets filtrate and filter residue, and filter residue is mineral yellow;
(3) conversion of mineral yellow: step (2) gained mineral yellow is joined in the NaOH solution, make mineral yellow be converted into lead hydroxide fully, temperature of reaction is 50-80 ℃, and the reaction times is 30-160 minute; After question response is complete, filter, washing gets filtrate and filter residue, and filter residue is lead hydroxide, becomes plumbous oxide after the drying dehydration;
(4) recovery of leaching agent or regeneration: step (2) and step (3) gained filtrate are returned leaching system, recycle through concentrated, regulator solution pH to neutrality.
Further, in the step (1), described lead-contained solid refuse can be the melting waste slag of low-grade sulfur-bearing lead plumbates such as electrolytic manganese anode mud, the electrolytic zinc anode sludge, zinc sulfate leaching lead skim.
Further, in the step (1), the concentration of alkali metal chloride is 100-350g/L in described alkali metal chloride-alkaline earth metal chloride solution, and the concentration of alkaline earth metal chloride is 20-100g/L; The concentration of alkaline earth metal chloride is 100-500g/L in the described alkaline earth metal chloride solution.
Further, in the step (1), described alkali metal chloride-alkaline earth metal chloride solution is NaCl-CaCl
2Solution, described alkaline earth metal chloride solution is CaCl
2Solution.
Further, in the step (1), the mass ratio of leaching liquid and lead-contained solid refuse is 2-10:1.
Further, in the step (2), the mass concentration of used NaOH solution is 5-50%.
Further, in the step (3), the mass concentration of used NaOH solution is 5-50%.
When leaching liquid was alkali metal chloride-alkaline earth metal chloride solution, corresponding chemical equation was:
PbSO
4+2NaCl=PbCl
2+Na
2SO
4；
Na
2SO
4+CaCl
2=CaSO
4↓+2NaCl；
PbCl
2+NaOH=?PbOHCl↓+2NaCl；
PbOHCl+NaOH=?Pb(OH)
?2+NaCl。
When leaching liquid was alkaline earth metal chloride solution, corresponding chemical equation was:
PbSO
4+2CaCl
2=PbCl
2+CaSO
4↓；
PbCl
2+NaOH=?PbOHCl↓+2NaCl；
PbOHCl+NaOH=?Pb(OH)
?2+NaCl。
As from the foregoing, the calcium chloride that contains in the leaching liquid and the lead sulfate in the lead skim react, thereby reduce the concentration of sulfate radical in the leaching system, increase plumbous leaching rate; The calcium sulfate precipitation that generates is removed in the lump with leach residue in filtration procedure.
The present invention can carry out lead to lead containing sludge such as electrolytic manganese anode mud lead skims and reclaim, and whole technological process is all carried out in the aqueous solution, can not produce the pollution of lead dust, lead steam and sulfurous gas; The recyclable utilization of leaching liquid; And the formation closed cycle, realize the zero waste water discharging, do not have leaded waste liquid and produce, can not produce secondary pollution; The plumbous oxide purity height that makes can be used as the raw material that metallic lead or lead compound are produced.
In sum, it is simple that the present invention has technology, easy and simple to handle, and processing cost is low, lead recovery height, advantages such as environmentally safe.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
Present embodiment may further comprise the steps:
(1) dense saline solution leaching lead: with the fragmentation of electrolytic manganese anode mud lead skim, below ball milling to 60 order, take by weighing 50g, in sodium-chlor-calcium chloride solution 200ml, leach, the concentration 300g/L of sodium-chlor in the solution, the concentration 20g/L of calcium chloride, following stirring, leaching temperature in the time of leaching is 80 ℃, and leaching time is 2 hours; After the filtration, obtain leaded filtrate;
(2) alkaline solution is heavy plumbous: add 10wt%NaOH solution (2ml) in step (1) gained filtrate, make the PbCl in the solution
2Be converted into mineral yellow fully, invert point is 80 ℃, and transformation time is 32 minutes, reacts completely, and filters, and washing gets filtrate and filter residue, and filter residue is mineral yellow;
(3) conversion of mineral yellow: step (2) gained mineral yellow is joined in the 15wt%NaOH solution, make the mineral yellow in the solution be converted into lead hydroxide fully, temperature of reaction is 55 ℃, reaction times is 60 minutes, reacts completely, and filters, washing, get filtrate and filter residue, filter residue is lead hydroxide, becomes plumbous oxide after the drying dehydration;
(4) recovery of leaching agent or regeneration: step (2) and step (3) gained filtrate are returned leaching system, recycle through concentrated, regulator solution pH to neutrality.
The rate of recovery of present embodiment lead reaches 93.5%.
Embodiment 2
Present embodiment may further comprise the steps:
(1) dense saline solution leaching lead: with the fragmentation of electrolytic manganese anode mud lead skim, below ball milling to 60 order, take by weighing 50g, in sodium-chlor-calcium chloride solution 300ml, leach, the concentration 300g/L of sodium-chlor in the solution, the concentration 40g/L of calcium chloride, following stirring, leaching temperature in the time of leaching is 90 ℃, and leaching time is 1.5 hours; Filter, get filtrate and filter residue;
(2) alkaline solution is heavy plumbous: add 10wt%NaOH solution (3.5ml) in step (1) gained filtrate, make the PbCl in the solution
2Be converted into mineral yellow fully, invert point is 90 ℃, and transformation time is 30 minutes, reacts completely, and filters, and washing gets filtrate and filter residue, and filter residue is mineral yellow;
(3) conversion of mineral yellow: step (2) gained mineral yellow is joined in the 10wt%NaOH solution, make the mineral yellow in the solution be converted into lead hydroxide fully, temperature of reaction is 60 ℃, reaction times is 60 minutes, reacts completely, and filters, washing, get filtrate and filter residue, filter residue is lead hydroxide, becomes plumbous oxide after the drying dehydration;
(4) recovery of leaching agent or regeneration: step (2) and step (3) gained filtrate are returned leaching system, recycle through concentrated, regulator solution pH to neutrality.
The rate of recovery of present embodiment lead reaches 96.70%.
Embodiment 3
Present embodiment may further comprise the steps:
(1) dense saline solution leaching lead: with the fragmentation of electrolytic manganese anode mud lead skim, below ball milling to 60 order, take by weighing 50g, leach in the calcium chloride solution 300ml of concentration 350g/L, leaching temperature is 70 ℃, and leaching time is 1.0 hours; Filter, get filtrate and filter residue;
(2) alkaline solution is heavy plumbous: add 10wt%NaOH solution (3.5ml) in step (1) gained filtrate, make the PbCl in the solution
2Be converted into mineral yellow fully, invert point is 70 ℃, and transformation time is 30 minutes, reacts completely, and filters, and washing gets filtrate and filter residue, and filter residue is mineral yellow;
(3) conversion of mineral yellow: step (2) gained mineral yellow is joined in the 10wt%NaOH solution, make the mineral yellow in the solution be converted into lead hydroxide fully, temperature of reaction is 50 ℃, reaction times is 60 minutes, reacts completely, and filters, washing, get filtrate and filter residue, filter residue is lead hydroxide, becomes plumbous oxide after the drying dehydration;
(4) recovery of leaching agent or regeneration: step (2) and step (3) gained filtrate are returned leaching system, recycle through concentrated, regulator solution pH to neutrality.
The rate of recovery of present embodiment lead reaches 97.20%.
Claims (7)
1. one kind is reclaimed plumbous method from the lead-contained solid refuse, it is characterized in that, may further comprise the steps:
(1) dense saline solution leaching lead: with the fragmentation of lead-contained solid refuse, below ball milling to 60 order, be that leaching agent carries out lead and leaches with alkali metal chloride-alkaline earth metal chloride solution or alkaline earth metal chloride solution, follow stirring when leaching, leaching temperature is 20-100 ℃, and leaching time is 30-120 minute; Filter, get filtrate and filter residue;
(2) alkaline solution is heavy plumbous: add NaOH solution or solid sodium hydroxide in step (1) gained filtrate, make the PbCl in the solution
2Be converted into mineral yellow fully, invert point is 20-90 ℃, and transformation time is 30-120 minute; After question response is complete, filter, washing gets filtrate and filter residue, and filter residue is mineral yellow;
(3) conversion of mineral yellow: step (2) gained mineral yellow is joined in the NaOH solution, make mineral yellow be converted into lead hydroxide fully, temperature of reaction is 50-80 ℃, and the reaction times is 30-160 minute; After question response is complete, filter, washing gets filtrate and filter residue, and filter residue is lead hydroxide, becomes plumbous oxide after the drying dehydration;
(4) recovery of leaching agent or regeneration: step (2) and step (3) gained filtrate are returned leaching system, recycle through concentrated, regulator solution pH to neutrality.
2. according to the described method that reclaims lead from the lead-contained solid refuse of claim 1, it is characterized in that: in the step (1), described lead-contained solid refuse is that electrolytic manganese anode mud, the electrolytic zinc anode sludge or zinc sulfate leach lead skim.
3. according to claim 1 or the 2 described methods that from the lead-contained solid refuse, reclaim lead, it is characterized in that: in the step (1), the concentration of alkali metal chloride is 100-350g/L in described alkali metal chloride-alkaline earth metal chloride solution, and the concentration of alkaline earth metal chloride is 20-100g/L; The concentration of alkaline earth metal chloride is 100-500g/L in the described alkaline earth metal chloride solution.
4. according to claim 1 or the 2 described methods that reclaim lead from the lead-contained solid refuse, it is characterized in that: in the step (1), described alkali metal chloride-alkaline earth metal chloride solution is NaCl-CaCl
2Solution, described alkaline earth metal chloride solution is CaCl
2Solution.
5. according to claim 1 or the 2 described methods that reclaim lead from the lead-contained solid refuse, it is characterized in that: in the step (1), the mass ratio of leaching liquid and lead-contained solid refuse is 2-10:1.
6. according to claim 1 or the 2 described methods that reclaim lead from the lead-contained solid refuse, it is characterized in that: in the step (2), the mass concentration of used NaOH solution is 5-50%.
7. according to claim 1 or the 2 described methods that reclaim lead from the lead-contained solid refuse, it is characterized in that: in the step (3), the mass concentration of used NaOH solution is 5-50%.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104263954A (en) * | 2014-09-19 | 2015-01-07 | 河南金利金铅有限公司 | Comprehensive utilization method of lead-smelting bottom blowing furnace smoke dust |
| CN104619645A (en) * | 2014-02-21 | 2015-05-13 | 超威电源有限公司 | Method for recycling lead oxide-containing waste |
| CN104711637A (en) * | 2013-12-12 | 2015-06-17 | 沈阳有色金属研究院 | Method for recovering metal lead from solid lead oxide |
| CN105331823A (en) * | 2015-12-15 | 2016-02-17 | 安仁县永昌贵金属有限公司 | Lead waste residue recycling method |
| CN105417783A (en) * | 2015-12-09 | 2016-03-23 | 永兴县灿阳贵金属有限责任公司 | Method for recycling lead in lead-containing waste water |
| CN105886766A (en) * | 2014-12-12 | 2016-08-24 | 中国人民解放军63971部队 | Method for preparing high-purity PbO on basis of ion exchange method |
| AU2014201760B2 (en) * | 2013-03-27 | 2016-09-08 | Yunnan Xiangyunfeilong Resources Recycling Technology Co., Ltd. | A Technology of Lead Sulfate Hydrometallurgical Lead Smelting |
| CN106939377A (en) * | 2017-04-27 | 2017-07-11 | 中南大学 | A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled |
| CN107267774A (en) * | 2017-04-27 | 2017-10-20 | 超威电源有限公司 | A kind of method that lead-acid accumulator cast welding lead skim is reclaimed |
| CN107628711A (en) * | 2017-11-07 | 2018-01-26 | 长沙埃比林环保科技有限公司 | A kind of method of caustic soda processing lead waste water |
| CN108441641A (en) * | 2018-04-21 | 2018-08-24 | 四环锌锗科技股份有限公司 | A method of improving tannin germanium slag for comprehensive value |
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN112481507A (en) * | 2020-12-15 | 2021-03-12 | 江苏龙源催化剂有限公司 | Method for recovering metallic lead and thallium components from waste denitration catalyst |
| CN113430389A (en) * | 2021-06-25 | 2021-09-24 | 华南理工大学 | Method for improving lead yield in lead slag |
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| AU2014201760B2 (en) * | 2013-03-27 | 2016-09-08 | Yunnan Xiangyunfeilong Resources Recycling Technology Co., Ltd. | A Technology of Lead Sulfate Hydrometallurgical Lead Smelting |
| CN104711637A (en) * | 2013-12-12 | 2015-06-17 | 沈阳有色金属研究院 | Method for recovering metal lead from solid lead oxide |
| US9828653B2 (en) | 2014-02-21 | 2017-11-28 | Chilwee Power Co. Ltd & Beijing University Of Chemical Technology | Method for recycling lead oxide-containing waste material |
| CN104619645A (en) * | 2014-02-21 | 2015-05-13 | 超威电源有限公司 | Method for recycling lead oxide-containing waste |
| CN104619645B (en) * | 2014-02-21 | 2017-03-01 | 超威电源有限公司 | A kind of recoverying and utilizing method containing oxidation scrap lead |
| CN104263954A (en) * | 2014-09-19 | 2015-01-07 | 河南金利金铅有限公司 | Comprehensive utilization method of lead-smelting bottom blowing furnace smoke dust |
| CN105886766A (en) * | 2014-12-12 | 2016-08-24 | 中国人民解放军63971部队 | Method for preparing high-purity PbO on basis of ion exchange method |
| CN105417783A (en) * | 2015-12-09 | 2016-03-23 | 永兴县灿阳贵金属有限责任公司 | Method for recycling lead in lead-containing waste water |
| CN105331823A (en) * | 2015-12-15 | 2016-02-17 | 安仁县永昌贵金属有限公司 | Lead waste residue recycling method |
| CN106939377A (en) * | 2017-04-27 | 2017-07-11 | 中南大学 | A kind of chlorination of sulfur acid lead materials takes off the method that lead liquid is recycled |
| CN107267774A (en) * | 2017-04-27 | 2017-10-20 | 超威电源有限公司 | A kind of method that lead-acid accumulator cast welding lead skim is reclaimed |
| CN107267774B (en) * | 2017-04-27 | 2019-05-24 | 超威电源有限公司 | A kind of method of lead-acid accumulator cast welding lead skim recycling |
| CN107628711A (en) * | 2017-11-07 | 2018-01-26 | 长沙埃比林环保科技有限公司 | A kind of method of caustic soda processing lead waste water |
| CN108441641A (en) * | 2018-04-21 | 2018-08-24 | 四环锌锗科技股份有限公司 | A method of improving tannin germanium slag for comprehensive value |
| CN110697765A (en) * | 2019-11-26 | 2020-01-17 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN110697765B (en) * | 2019-11-26 | 2022-04-29 | 中原工学院 | Room temperature solid phase synthesis method of basic lead chloride material |
| CN112481507A (en) * | 2020-12-15 | 2021-03-12 | 江苏龙源催化剂有限公司 | Method for recovering metallic lead and thallium components from waste denitration catalyst |
| CN113430389A (en) * | 2021-06-25 | 2021-09-24 | 华南理工大学 | Method for improving lead yield in lead slag |
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Application publication date: 20130911 |