CN112430744A - Waste lead plaster recovery method - Google Patents
Waste lead plaster recovery method Download PDFInfo
- Publication number
- CN112430744A CN112430744A CN202011072832.6A CN202011072832A CN112430744A CN 112430744 A CN112430744 A CN 112430744A CN 202011072832 A CN202011072832 A CN 202011072832A CN 112430744 A CN112430744 A CN 112430744A
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- China
- Prior art keywords
- lead
- carbonate
- sulfate
- solution
- carbon dioxide
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B13/00—Obtaining lead
- C22B13/02—Obtaining lead by dry processes
- C22B13/025—Recovery from waste materials
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/11—Removing sulfur, phosphorus or arsenic other than by roasting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to a waste lead plaster recovery method, which is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2. The waste lead plaster recovery method provided by the invention has the advantages that the waste lead plaster is recovered to form a circulating system, and the efficiency is high.
Description
Technical Field
The invention relates to the technical field of waste treatment.
Background
The waste lead plaster mainly comprises the following components: the lead sulfate content is about 50% -60%, the lead dioxide content is about 20% -30%, the lead oxide content is about 5% -15%, and the metallic lead content is about 1% -2%. Because the melting point and the decomposition temperature of the lead sulfate are high, the property is stable, the chemical conversion reaction is difficult to occur, and lead dioxide (generally regarded as the anhydride of the original high lead acid or higher lead acid) has strong oxidizing property and is insoluble in oxidizing acid and alkali, the recycling treatment of the waste lead plaster becomes the key point for recycling the waste lead-acid storage battery.
Disclosure of Invention
In order to solve the technical problem, the invention provides a waste lead plaster recovery method, which is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2.
Further, in the step 1, the waste lead plaster is conveyed into a reaction kettle to be mixed with 10% -30% of waste sulfuric acid and subjected to shearing reaction for 1-3 hours at the reaction temperature of 70-100 ℃, so that the lead sulfate lead plaster is obtained.
Further, in the step 2, the lead sulfate and the ammonium carbonate are mixed and subjected to a shearing reaction at normal temperature for 1-2 hours, and a solution of the lead carbonate and the ammonium sulfate is obtained after solid-liquid separation.
Further, in the step 3, adding calcium oxide into the ammonium sulfate solution, mixing, grinding and shearing at normal temperature for 1-3h, and performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution.
Further, in the step 3, the lead carbonate and the coal powder are mixed and smelted at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas, and the crude lead and the carbon dioxide gas are absorbed by ammonia water after surface cooling to prepare an ammonia carbonate solution.
Further, in the step 4, the calcium sulfate and the coal powder are mixed and calcined at the temperature of 600-.
Further, in the step 1, the carbon dioxide which reacts with the ammonia water to prepare the ammonia carbonate solution includes carbon dioxide obtained by melting calcium sulfate and carbon dioxide obtained by melting lead carbonate.
The waste lead plaster recovery method provided by the invention has the advantages that the waste lead plaster is recovered to form a circulating system, and the efficiency is high.
Drawings
FIG. 1 is a flow chart of the waste lead plaster recovery process of the present invention.
Detailed Description
The invention is further described below with reference to the specific drawings.
As shown in fig. 1
Step 1: lead sulfate preparation
And conveying the waste lead plaster into a reaction kettle, mixing and shearing the waste lead plaster with 10-30% of waste sulfuric acid for 1-3 hours at the reaction temperature of 70-100 ℃ to obtain the lead sulfate lead plaster. The reaction formula is as follows:
PbO+H2SO4→PbSO4+H2O
PbO2+Pb+2H2SO4→2PbSO4+2H2O
2PbO2+2H2SO4→2PbSO4+2H2O+O2
step 2: preparation of lead carbonate
And (3) mixing the lead sulfate prepared in the step (1) with ammonia carbonate, carrying out shearing reaction for 1-2h at normal temperature, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonia sulfate. The reaction formula is as follows:
PbSO4+(NH4)2CO3→PbCO3+(NH4)2SO4
and step 3: preparation of ammonia water from ammonia sulfate and smelting of lead carbonate
And (3) adding the ammonium sulfate solution prepared in the step (2) into calcium oxide, mixing, grinding and shearing at normal temperature for 1-3h, and carrying out solid-liquid separation to obtain calcium sulfate and an ammonia water solution. The reaction formula is as follows:
(NH4)2SO4+CaO+H2O→CaSO4+2NH3.H2O
mixing the lead carbonate and the coal powder in the step 2, smelting at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas,
the reaction formula is as follows:
2PbCO3+C→2Pb+3CO2
and (4) cooling the surface of the carbon dioxide, and absorbing the cooled carbon dioxide with ammonia water to prepare an ammonia carbonate solution.
And 4, step 4: calcination of calcium sulfate
Mixing calcium sulfate and coal powder, calcining at the temperature of 600-800 ℃, calcining to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, wherein the calcium oxide is used for preparing ammonia water, the sulfur dioxide is absorbed by hydrogen peroxide to prepare sulfuric acid for recycling, the carbon dioxide and the ammonia water are absorbed to prepare ammonia carbonate solution for recycling, and the carbon dioxide can comprise carbon dioxide formed by mixing and calcining calcium sulfate and coal powder, and lead carbonate and coal powder, and are mixed and smelted to obtain carbon dioxide.
The reaction equation is as follows: 2CaSO4+ C → 2CaO + CO2+2SO2
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (7)
1. A waste lead plaster recovery method is characterized by comprising the following steps: step 1: reacting the waste lead plaster with sulfuric acid to obtain lead sulfate lead plaster; step 2, reacting lead sulfate with ammonium carbonate, and carrying out solid-liquid separation to obtain a solution of lead carbonate and ammonium sulfate; step 3, adding calcium oxide into the ammonium sulfate solution for reaction, performing solid-liquid separation to obtain calcium sulfate and an ammonia water solution, and smelting lead carbonate at high temperature to obtain lead bullion and carbon dioxide gas; and 4, calcium sulfate is smelted at a high temperature to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, the sulfur dioxide is used for preparing sulfuric acid and returns to the step 1 to react with the waste lead paste, the calcium oxide is used for returning and adding the ammonium sulfate solution in the step 3 to prepare ammonia water, and the carbon dioxide and the ammonia water are absorbed to prepare an ammonia carbonate solution which is used for preparing lead carbonate in the step 2.
2. The waste lead plaster recovery method according to claim 1, wherein in the step 1, the waste lead plaster is conveyed into a reaction kettle to be mixed with 10% -30% of waste sulfuric acid for shearing reaction for 1-3h, and the reaction temperature is 70-100 ℃, so that the lead sulfate lead plaster is obtained.
3. The method for recycling the waste lead plaster according to the claim 1, wherein in the step 2, the lead sulfate and the ammonium carbonate are mixed and subjected to a shearing reaction at normal temperature for 1-2h, and a solution of the lead carbonate and the ammonium sulfate is obtained after solid-liquid separation.
4. The waste lead plaster recovery method according to claim 1, wherein in the step 3, calcium oxide is added into the ammonium sulfate solution, mixed at normal temperature, ground and sheared for 1-3 hours, and the calcium sulfate and the ammonia water solution are obtained through solid-liquid separation.
5. The method for recycling waste lead plaster as claimed in claim 1, wherein in the step 3, the lead carbonate and the coal powder are mixed and smelted at the temperature of 700-900 ℃ to obtain crude lead and carbon dioxide gas, and the crude lead and the carbon dioxide gas are absorbed by ammonia water after surface cooling to prepare the ammonia carbonate solution.
6. The method for recycling waste diachylon as claimed in claim 1, wherein in the step 4, the calcium sulfate and the coal powder are mixed and calcined at the temperature of 600-800 ℃ to obtain calcium oxide, sulfur dioxide and carbon dioxide gas, and the sulfur dioxide is absorbed by hydrogen peroxide to prepare sulfuric acid.
7. The method for recycling waste lead plaster as claimed in claim 1, wherein the carbon dioxide for preparing the ammonia carbonate solution by reacting with the ammonia water comprises carbon dioxide obtained by smelting calcium sulfate and carbon dioxide obtained by smelting lead carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011072832.6A CN112430744A (en) | 2020-10-09 | 2020-10-09 | Waste lead plaster recovery method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011072832.6A CN112430744A (en) | 2020-10-09 | 2020-10-09 | Waste lead plaster recovery method |
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| CN112430744A true CN112430744A (en) | 2021-03-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115159467A (en) * | 2021-04-02 | 2022-10-11 | 中冶长天国际工程有限责任公司 | Method for synthesizing catalyst based on ammonia circulation and catalytically recovering elemental sulfur from sulfur dioxide flue gas |
| CN115557530A (en) * | 2022-09-14 | 2023-01-03 | 超威电源集团有限公司 | Method for preparing battery-grade lead oxide from waste lead paste |
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| CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
| CN103030165A (en) * | 2012-11-27 | 2013-04-10 | 刘立文 | Method for treating waste generated in process of producing calcium oxide from calcium sulfate |
| CN103436702A (en) * | 2013-08-30 | 2013-12-11 | 湖北骆驼蓄电池研究院有限公司 | Method for preparing highly oxidized lead powder from waste battery lead plaster |
| CN104263944A (en) * | 2014-09-29 | 2015-01-07 | 湖南江冶机电科技股份有限公司 | Lead paste desulfurization method based on grinding mechanism |
| CN105858716A (en) * | 2016-04-03 | 2016-08-17 | 株洲盈定自动化设备科技有限公司 | Novel method for directly regenerating waste lead-acid battery into lead powders |
| CN109694955A (en) * | 2019-02-20 | 2019-04-30 | 湘潭大学 | A kind of pre- sulfur method of lead plaster based on the double alkali of sodium calcium |
| CN110453077A (en) * | 2019-08-26 | 2019-11-15 | 湘潭大学 | A kind of method that scrap lead cream recycles |
| CN110917852A (en) * | 2019-11-21 | 2020-03-27 | 江苏省沙钢钢铁研究院有限公司 | Resource recovery method and resource recovery system for desulfurized fly ash |
| 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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2020
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Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101608264A (en) * | 2009-06-30 | 2009-12-23 | 张天任 | A kind of waste lead recovering method for lead-acid storage batteries |
| CN103030165A (en) * | 2012-11-27 | 2013-04-10 | 刘立文 | Method for treating waste generated in process of producing calcium oxide from calcium sulfate |
| CN103436702A (en) * | 2013-08-30 | 2013-12-11 | 湖北骆驼蓄电池研究院有限公司 | Method for preparing highly oxidized lead powder from waste battery lead plaster |
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| CN110453077A (en) * | 2019-08-26 | 2019-11-15 | 湘潭大学 | A kind of method that scrap lead cream recycles |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115159467A (en) * | 2021-04-02 | 2022-10-11 | 中冶长天国际工程有限责任公司 | Method for synthesizing catalyst based on ammonia circulation and catalytically recovering elemental sulfur from sulfur dioxide flue gas |
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| CN115557530A (en) * | 2022-09-14 | 2023-01-03 | 超威电源集团有限公司 | Method for preparing battery-grade lead oxide from waste lead paste |
| CN115557530B (en) * | 2022-09-14 | 2023-08-22 | 超威电源集团有限公司 | Method for preparing battery-grade lead oxide from waste lead paste |
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