CN110085938A - A kind of waste and old lead acid accumulator sulfuric acid circulation utilization method - Google Patents
A kind of waste and old lead acid accumulator sulfuric acid circulation utilization method Download PDFInfo
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- CN110085938A CN110085938A CN201910282886.6A CN201910282886A CN110085938A CN 110085938 A CN110085938 A CN 110085938A CN 201910282886 A CN201910282886 A CN 201910282886A CN 110085938 A CN110085938 A CN 110085938A
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- Prior art keywords
- sulfuric acid
- lead
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- acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
- C01B17/90—Separation; Purification
- C01B17/901—Recovery from spent acids containing metallic ions, e.g. hydrolysis acids, pickling acids
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Secondary Cells (AREA)
Abstract
The invention proposes a kind of waste and old lead acid accumulator sulfuric acid circulation utilization methods, it is characterised in that: successively the following steps are included: a) b) c) lead plaster production d) is melted into for waste recovery processing for old and useless battery dismantling: e) recycling lead f) waste acidity recovery.Compared with the prior art, using new formula solution, the dilution heat of sulfuric acid for improving concentration carries out " chemical conversion ", sulfuric acid solution concentration after " chemical conversion " further increases, it can be according to requiring to be adjusted, concentration Optimal Control is not necessarily to concentration process in 20%-50% so as to the processing and reuse of subsequent dilution heat of sulfuric acid." chemical conversion " solution formula of the invention has the advantages that sulfuric acid concentration is high, conductivity is high, and " chemical conversion " efficiency can be improved, and is conducive to negative material " chemical conversion " conversion and forms the preferable leading crystal of structure, reduces the oxidation of following process.The present invention is directed to the dilute sulfuric acid that " chemical conversion " generates, and develops membrane separation technique, using concentration difference diffusion principle, the objectionable impurities such as the metal ion in useless dilute sulfuric acid is made to obtain separation removal.
Description
[technical field]
The present invention relates to battery recycling recycle utilization technology field, in particular to a kind of waste and old lead acid accumulator sulfuric acid circulation
Utilize method.
[background technique]
Traditional waste and old lead acid accumulator is recycled using pyrometallurgical smelting mode, sulfuric acid therein in battery with
Lead sulfate and free sulfuric acid state exist.
During recycling disposal, there are two types of methods to carry out " desulfurization ", i.e. " preceding desulfurization " and " rear desulfurization "." preceding desulfurization " be by
Leaded, the acid waste products that waste and old lead acid accumulator dismantling is separated are placed in desulfurizer, and desulfurizing agent is added and carries out desulphurization reaction,
With desulfurizing agent will react containing the sulfate radical in the lead sulfate in scrap lead and to form sulfate and enter solution, by evaporative crystallization
Etc. techniques sulphate crystal is come out, as byproduct.Desulfurizing agent generally uses sodium hydroxide, sodium carbonate, ammonium carbonate etc..In the presence of
Desulphurization cost height, by-product sale and disposition are difficult, and sulfuric acid is not recycled." rear desulfurization " is will be leaded, sour
Waste material is directly entered smelting procedure, and in smelting process, sulfuric acid and lead sulfate decompose under the high temperature conditions, generates sulfur dioxide, warp
Gas collection system is crossed, into sulfur dioxide collection system and acid making system, by preparing sulfuric acid by using sulfur dioxide." rear desulfurization " technique
Solve retrieval of sulfuric acid Utilizing question, still, it is undesulfured it is leaded, acid waste products smelting temperature is very high, bring lead skim amount increase,
A large amount of generations of lead fume, energy consumption also increase substantially, meanwhile, sulfur dioxide concentration is low, collection and acid making system investment are larger,
Higher cost." rear desulfurization " brings high pollution risk, high energy consumption, high-cost problem.Urgent need is developed a kind of new method and is solved
State problem.
Hydrometallurgic recovery disposes waste and old lead acid accumulator, becomes new developing direction, a technology is adopted in existing multiple technologies
With traditional storage battery pole plate " chemical conversion " process, negative plate old and useless battery disassembles the lead mud separated, and full-filling is in acidproof afflux
Body, by drying so that lead mud is formed by curing.Negative current collector can with graphite, acid metal for example titanium, titanium alloy, stainless steel,
The materials such as lead are process, and can be may be reused using grid configuration and sheet form etc..Inert electrode is equipped with as just
Pole, merging concentration are to carry out " chemical conversion " in the dilution heat of sulfuric acid of 5%-10%, leaded, sour material are converted to spongy lead, simultaneously
Sulfuric acid is released, sulfuric acid solution concentration is gradually increased to 15% or less.If wanting reuse, it is concentrated, concentrator
Highly-acidproof is needed, it is also desirable to remove the impurity in dilute sulfuric acid, concentration and cost for purification are high, without economic value.Generally
All the dilute sulfuric acid that chemical conversion generates is neutralized using sodium hydroxide, it is therefore an objective to which the lead ion in dilute sulfuric acid sinks
It forms sediment, reaches discharge standard.But neutralize the sodium sulphate of generation, then enter in neutralizer and discharge, this method should consume price
Higher sodium hydroxide, and sulfuric acid is not recycled and the wasting of resources.There is technology using ammonium carbonate as desulfurization
Agent generates the byproduct of ammonium sulfate, it is intended to as chemical fertilizer, still, the doing of ammonium sulfate being extract from lead-acid accumulator the inside
There is heavy metal lead pollution in fertilizer, hardly result in approval.
[summary of the invention]
It is an object of the invention to overcome above-mentioned the deficiencies in the prior art, a kind of waste and old lead acid accumulator sulfuric acid circulation is provided
Using method, aim to solve the problem that there are at high cost, no economic valences for hydrometallurgic recovery disposition waste and old lead acid accumulator in the prior art
Value, the wasting of resources or it is seriously polluted the problems such as
To achieve the above object, the invention proposes a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method, features
Be: successively the following steps are included:
A) old and useless battery is disassembled: old and useless battery being disassembled to obtain scrap lead slag, lead mud and waste plastics.
B) waste recovery is handled: scrap lead slag is recycled after low smelting heat at metal ingot;Waste plastics is matched by plastics
It is recycled after material processing at plastic granulating.
C) lead plaster makes: negative plate old and useless battery disassembles the lead mud separated, and full-filling is in acidproof collector, by drying
It does so that lead mud is formed by curing.
D) it is melted into: lead plaster being equipped in the dilution heat of sulfuric acid of inert electrode merging and reacted, generate spongy lead and give up
Dilute sulfuric acid.
E) lead is recycled: formation reuse lead pig after carrying out briquetting by the spongiform lead that chemical conversion generates, dissolve ingot casting, removal of impurities.
F) waste acidity recovery: useless dilute sulfuric acid is imported into membrane separation device, isolates shape after raffinate is neutralized, precipitated, filtered
At recycle-water;The pure dilute sulfuric acid isolated carries out being back to use pole plate manufacture and battery acid.
Preferably, in the step d) dilution heat of sulfuric acid optimization formula be 0.01~2%Na2SO4,0.1~2%
K2SO4,0.1~2%Mg2SO4,15%~50%H2SO4,0.01~0.3% sodium lignosulfonate etc., remaining is water.
Preferably, the membrane separation device in the step f) includes ion processing film, spent acid enters channel, raffinate flows out
Channel, pure water enter channel, pure dilute sulfuric acid flow pass, and ion processing film side is equipped with spent acid and enters channel and raffinate stream
Channel out, the spent acid enter the lower section that channel is located at raffinate flow pass, and the ion processing film other side is equipped with pure
Water enters channel and pure dilute sulfuric acid flow pass, and the pure water enters the top that channel is located at pure dilute sulfuric acid flow pass.
Preferably, the dilute sulfuric acid concentration of the pure dilute sulfuric acid channel outflow can be controlled in 20%-50%.
Beneficial effects of the present invention: compared with prior art, a kind of waste and old lead acid accumulator sulfuric acid provided by the invention follows
Ring utilizes method, and using new formula solution, the dilution heat of sulfuric acid for improving concentration carries out " chemical conversion ", and the sulfuric acid solution after " chemical conversion " is dense
Degree further increases, can be according to requiring to be adjusted, and concentration Optimal Control is in 20%-50%, so as to subsequent dilution heat of sulfuric acid
Processing and reuse, be not necessarily to concentration process." chemical conversion " solution formula of the invention has the advantages that sulfuric acid concentration is high, conductivity is high,
" chemical conversion " efficiency can be improved, be conducive to negative material " chemical conversion " conversion and form the preferable leading crystal of structure, reduce subsequent add
The oxidation of work.The present invention is directed to the dilute sulfuric acid that " chemical conversion " generates, and exploitation membrane separation technique makes to give up dilute using concentration difference diffusion principle
The objectionable impurities such as the metal ion in sulfuric acid obtain separation removal.
Feature and advantage of the invention will be described in detail by embodiment combination attached drawing.
[Detailed description of the invention]
Fig. 1 is the structural schematic diagram of the membrane separation device of the embodiment of the present invention.
In figure: 1- ion processing film, 2- spent acid enter channel, 3- raffinate flow pass, 4- pure water enter channel, 5- is pure dilute
Sulfuric acid flow pass.
[specific embodiment]
In order to make the objectives, technical solutions and advantages of the present invention clearer, below by accompanying drawings and embodiments, to this
Invention is further elaborated.However, it should be understood that the specific embodiments described herein are merely illustrative of the present invention,
The range being not intended to restrict the invention.In addition, in the following description, descriptions of well-known structures and technologies are omitted, to keep away
Exempt from unnecessarily to obscure idea of the invention.
Refering to fig. 1, the embodiment of the present invention provides a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method, and feature exists
In: successively the following steps are included:
A) old and useless battery is disassembled: old and useless battery being disassembled to obtain scrap lead slag, lead mud and waste plastics.
B) waste recovery is handled: scrap lead slag is recycled after low smelting heat at metal ingot;Waste plastics is matched by plastics
It is recycled after material processing at plastic granulating.
C) lead plaster makes: negative plate old and useless battery disassembles the lead mud separated, and full-filling is in acidproof collector, by drying
It does so that lead mud is formed by curing.
D) it is melted into: lead plaster being equipped with inert electrode and is reacted as anode, in the dilution heat of sulfuric acid of merging, generation sponge
Shape lead and useless dilute sulfuric acid.
E) lead is recycled: formation reuse lead pig after carrying out briquetting by the spongiform lead that chemical conversion generates, dissolve ingot casting, removal of impurities.
F) waste acidity recovery: useless dilute sulfuric acid is imported into membrane separation device, isolates shape after raffinate is neutralized, precipitated, filtered
At recycle-water;The pure dilute sulfuric acid isolated carries out being back to use pole plate manufacture and battery acid.
In the step d) optimization formula of dilution heat of sulfuric acid be 0.01~2%Na2SO4,0.1~2%K2SO4,0.1~
2%Mg2SO4,15%~50%H2SO4,0.01~0.3% sodium lignosulfonate etc., remaining is water.
Membrane separation device in the step f) include ion processing film 1, spent acid enter channel 2, raffinate flow pass 3,
Pure water enters channel 4, pure dilute sulfuric acid flow pass 5, and 1 side of ion processing film is equipped with spent acid and enters channel 2 and raffinate stream
Channel 3 out, the spent acid enter the lower section that channel 2 is located at raffinate flow pass 3, and 1 other side of ion processing film is set
There is pure water to enter channel 4 and pure dilute sulfuric acid flow pass 5, the pure water enters channel 4 and is located at the upper of pure dilute sulfuric acid flow pass 5
Side.
The dilute sulfuric acid concentration that the pure dilute sulfuric acid channel 5 is flowed out can be controlled in 20%-50%.
The course of work of the present invention:
During the work time, old and useless battery is torn open for a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method of the present invention
Solution, waste recovery processing, lead plaster production, chemical conversion, recycling lead and waste acidity recovery, when devil liquor recovery, which enters waste liquid by waste liquid, leads to
Road 2 pours into membrane separation device, after the processing of ion processing film 1, forms raffinate and pure dilute sulfuric acid, wherein raffinate passes through raffinate stream
Channel 3 is discharged out, and pure dilute sulfuric acid is logical from the outflow of pure dilute sulfuric acid after can according to need into the concentration of pure water configuration 20%-50%
Road 5 is discharged, to reasonably recycle the sulfuric acid of waste and old lead acid accumulator.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention
Made any modification, equivalent replacement or improvement etc., should all be included in the protection scope of the present invention within mind and principle.
Claims (4)
1. a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method, it is characterised in that: successively the following steps are included:
A) old and useless battery is disassembled: old and useless battery being disassembled to obtain scrap lead slag, lead mud and waste plastics.
B) waste recovery is handled: scrap lead slag is recycled after low smelting heat at metal ingot;Waste plastics is by doses of plastics
It is recycled after reason at plastic granulating.
C) lead plaster makes: negative plate old and useless battery disassembles the lead mud separated, and full-filling makes in acidproof collector by drying
Lead mud is obtained to be formed by curing.
D) it is melted into: lead plaster being equipped with inert electrode and is reacted as anode, in the dilution heat of sulfuric acid of merging, generation spongy lead
With useless dilute sulfuric acid.
E) lead is recycled: formation reuse lead pig after carrying out briquetting by the spongiform lead that chemical conversion generates, dissolve ingot casting, removal of impurities.
F) waste acidity recovery: by useless dilute sulfuric acid import membrane separation device, isolate raffinate neutralized, precipitated, filter after formed back
Use water;The pure dilute sulfuric acid isolated carries out being back to use pole plate manufacture and battery acid.
2. a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method described in accordance with the claim 1, it is characterised in that: the step
It is rapid d) in dilution heat of sulfuric acid optimization formula be 0.01~2%Na2SO4,0.1~2%K2SO4,0.1~2%Mg2SO4,15%
~50%H2SO4,0.01~0.3% sodium lignosulfonate etc., remaining is water.
3. a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method described in accordance with the claim 1, it is characterised in that: the step
It is rapid f) in membrane separation device include that ion processing film (1), spent acid enter channel (2), raffinate flow pass (3), pure water enter
Channel (4), pure dilute sulfuric acid flow pass (5), ion processing film (1) side are equipped with spent acid and enter channel (2) and raffinate stream
Channel (3) out, the spent acid enter the lower section that channel (2) is located at raffinate flow pass (3), the ion processing film (1)
The other side is equipped with pure water and enters channel (4) and pure dilute sulfuric acid flow pass (5), and the pure water enters channel (4) and is located at pure dilute sulphur
The top of sour flow pass (5).
4. a kind of waste and old lead acid accumulator sulfuric acid circulation utilization method described in accordance with the claim 3, it is characterised in that: described pure
The dilute sulfuric acid concentration of dilute sulfuric acid channel (5) outflow can be controlled in 20%-50%.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112420996A (en) * | 2020-10-29 | 2021-02-26 | 天能电池集团股份有限公司 | Method for preparing power battery by utilizing recycled lead powder, positive plate and power battery |
CN114645299A (en) * | 2022-02-23 | 2022-06-21 | 浙江铅锂智行科技有限公司 | Electrolysis device |
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CN107887575A (en) * | 2017-11-20 | 2018-04-06 | 江苏华富储能新技术股份有限公司 | A kind of polyaniline prepares and the method for modification negative plate of lead storage battery |
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US20030228525A1 (en) * | 2002-05-16 | 2003-12-11 | Akiya Kozawa | Lead-acid battery having an organic polymer additive and process thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN112420996A (en) * | 2020-10-29 | 2021-02-26 | 天能电池集团股份有限公司 | Method for preparing power battery by utilizing recycled lead powder, positive plate and power battery |
CN114645299A (en) * | 2022-02-23 | 2022-06-21 | 浙江铅锂智行科技有限公司 | Electrolysis device |
CN114645299B (en) * | 2022-02-23 | 2023-08-15 | 浙江铅锂智行科技有限公司 | Electrolysis device |
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