CN108110358A - The recovery method of waste and old lithium ion battery binding agent - Google Patents
The recovery method of waste and old lithium ion battery binding agent Download PDFInfo
- Publication number
- CN108110358A CN108110358A CN201711355281.2A CN201711355281A CN108110358A CN 108110358 A CN108110358 A CN 108110358A CN 201711355281 A CN201711355281 A CN 201711355281A CN 108110358 A CN108110358 A CN 108110358A
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- China
- Prior art keywords
- lithium ion
- ion battery
- waste
- binding agent
- old lithium
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Classifications
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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
-
- 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
Abstract
The invention belongs to lithium ion battery recycling fields, and in particular to a kind of recovery method of waste and old lithium ion battery binding agent.Waste and old lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity；Battery after immersion is roasted, is disassembled after being then cooled to room temperature, releases electrolyte, obtain electrode plates and membrane；The electrode plates isolated using organic solvent are dissolved, filter to isolate electrode material and collector；Ethyl alcohol washing is added in gained filtrate, filters to isolate adhesive；Ethyl alcohol and organic solvent are isolated in obtained filtrate heating.Present invention process is easy to operate, at low cost, and reaction condition is mildly loose, can realize recycling for adhesive in waste and old lithium ion battery, avoid environmental pollution, the rate of recovery of adhesive is more than 95%.
Description
Technical field
The invention belongs to lithium ion battery recycling fields, and in particular to a kind of recycling side of waste and old lithium ion battery binding agent
Method.
Background technology
Lithium ion battery is since nineteen ninety comes out, and development is rapidly.The exposure for the lithium ion battery through a long time scrapped
Accumulation, safety device destruction make the huge sum of moneys such as the phosphorous electrolyte of inside battery cobalt, copper, nickel that gradually leakage and inside battery contain
Belong to the hidden danger that element causes environmental pollution.Lithium ion has anode at present, and nickel-cobalt-manganternary ternary anode material, nickel cobalt aluminium ternary is just
Pole, cobalt acid lithium, LiMn2O4 etc., cathode is made of negative electrode active material carbon materials, the acetylene black conductor of 4-5%, 6% 1
7% binding agent uniformly after mixing, is coated in thick about copper foil current collector.Diaphragm material is porous polyethylene or polypropylene.Electricity
Solution liquid is made of electrolyte and organic solvent, and electrolyte is generally lithium salts organic solvent.Binding agent main component is polyvinylidene fluoride
Alkene (PVDF).Therefore the main material of composition lithium ion battery has metal, plastics, metal oxide, organic solvent, inorganic conductive
Salt.
Patent " a kind of roasting direct processing waste and old lithium ion battery and the method for recycling valuable metal
(CN200910130828.) " organic barrier film material and electrode material in 500~850 DEG C of roasting temperatures remove battery are proposed
Organic binder bond on material will be mixed and sized mixing with sodium sulphate (or potassium sulfate), the concentrated sulfuric acid after the battery material of roasting crushes,
Secondary heat treatment is carried out at a temperature of 350~600 DEG C in electric furnace, turns the metals such as cobalt, copper and lithium in waste and old lithium ion battery
Become sulfate soluble easily in water, extracted respectively from leachate after water or dilution heat of sulfuric acid leaching, then with organic extractant
Cobalt, copper, and obtain copper and cobalt product.It is mentioned in paper " lithium and cobalt oxides are recycled from used Li ion cell with floatation " in horse
Electrode material is not heat-treated in stove at a temperature of 773K, then separate lithium and cobalt oxides and graphite with floatation this is because
At a temperature of 773K, organic binder bond volatilization removing, lithium and cobalt oxides surface becomes hydrophily from hydrophobicity.
After paper " integrated conduct method of used Li ion cell " proposes recycling refuse battery, discharge treatment is carried out, is removed outer
Shell recycles outer cover metal material.Battery core with coke, lime stone is mixed, puts into reduction roasting in roaster.Organic compound combustion point
It solves as carbon dioxide and other gases, cobalt acid lithium is reduced to metallic cobalt and lithia, and fluorine and phosphorus are fixed by sediment, and aluminium is aoxidized
For clinker, after most of lithia escapes in vapour form, it is absorbed with water, metallic copper, cobalt etc. form phosphorus-containing alloy.
Although above method can effectively remove binding agent, and cause LiCoO2, acetylene black be desorbed from aluminium foil, but be calcined
Processing mode energy consumption it is big, aluminium foil is oxidized into aluminium oxide, and value is caused to reduce and collect difficult.Paper
" laboratoryscale lithium-ion battery recycling process " is proposed with organic matter NMP (N- first
Base pyrrolidones) dissolving PVDF separation aluminium cobalt films, although being successfully allowed to separate, the too expensive about 30,000 yuan/t of NMP, in actual production
In less be applicable in.
The content of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of recycling sides of waste and old lithium ion battery binding agent
Method, technological operation is simple, at low cost, and reaction condition is mildly loose, can realize the cycling of adhesive in waste and old lithium ion battery
It utilizes, avoids environmental pollution, the rate of recovery of adhesive is more than 95%.
The recovery method of waste and old lithium ion battery binding agent of the present invention, includes the following steps：
(1) waste and old lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity；
(2) battery after being impregnated in step (1) is roasted, is disassembled after being then cooled to room temperature, release electrolyte, obtained
Electrode plates and membrane；
(3) electrode plates isolated in step (2) using organic solvent are dissolved, filters to isolate electrode material sum aggregate
Fluid；
(4) ethyl alcohol washing will be added in gained filtrate in step (3), filters to isolate adhesive；
(5) ethyl alcohol and organic solvent are isolated into the filtrate obtained in step (4) heating.
Wherein：
The temperature impregnated in step (1) is room temperature, time 30-180min.
It is roasted in step (2) and is roasted in muffle furnace, calcination temperature is 50-100 DEG C, time 30-120min, roasting
It softens, modification, is conducive to remove battery case.
Organic solvent is NMP in step (3), and solution temperature is 20-80 DEG C.
It is separated by filtration in step (3) to pull electrode material and collector out from organic solvent using strainer, collector is
The collectors such as copper foil aluminium foil.
The volume ratio of ethyl alcohol and filtrate is 1-3 in step (4):1, washing times are 3-5 times.
It is separated by filtration in step (4) to be filtered using vacuum pump, filter cake is washed 3-5 times with ethyl alcohol.
Heating is 80-200 DEG C to be warming up to temperature in step (5).
Adhesive is PVDF.
The membrane obtained in step (2) can recycle aluminium therein through following technique：Membrane is placed in muffle furnace and is roasted,
Remove remaining binding agent；Ceramic diaphragm after roasting with lye is dissolved out, solution is obtained, is passed through carbon dioxide gas in the solution
Body, generation precipitation；Filtering, obtained precipitation obtain α or γ type alumina powders through calcining.
Preferably, membrane is placed in muffle furnace and roasted, calcination temperature is 150-300 DEG C, removes remaining binding agent；It will
Ceramic diaphragm after roasting is dissolved out with lye, lye be sodium hydroxide solution or potassium hydroxide solution, concentration 150-240g/L,
Leaching temperature is 150-240 DEG C, when the time is 1.5-3 small, obtains solution, is passed through carbon dioxide, titanium dioxide in the solution
The concentration of carbon gas is 20w%-100w%, is passed through the time as 30-180min, generation precipitation；Filtering, obtained precipitation is through calcining
Obtain α or γ type alumina powders.
Calcining heat obtains γ type alumina powders at 100-150 DEG C, and calcining heat obtains the oxidation of α types at 900-1200 DEG C
Aluminium powder, according to product it needs to be determined that calcining heat.
Adhesive recycling principle of the present invention is as follows：
PVDF is a kind of organic solvent, according to the similar principle that mixes, is dissolved readily in organic solvent, NMP and DMF
It is preferably to select, but DMF thermal stability is relatively poor to be easy to oxidant reaction, and also steam toxicity is big, so of the invention
Select solvents of the NMP as dissolving adhesive.It is washed using ethyl alcohol, ethyl alcohol is soluble in NMP, and solubility is non-in ethanol by PVDF
Often small, PVDF will be precipitated.And the boiling point difference of ethyl alcohol and PVDF are larger, it is i.e. separable using the way of distillation.
Compared with prior art, the present invention has the following advantages：
The recovery method of waste and old lithium ion battery binding agent of the present invention, technological operation is simple, at low cost, reacts item
Part is mildly loose, can realize recycling for adhesive in waste and old lithium ion battery, avoids environmental pollution, and adhesive returns
Yield is more than 95%.
Description of the drawings
Fig. 1 is the process flow chart of the recovery method of waste and old lithium ion battery binding agent of the present invention.
Specific embodiment
With reference to embodiment, the present invention will be further described.
Embodiment 1
Lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity.Soaking temperature is room temperature, the time
60min.Battery after immersion in muffle furnace is roasted, is softened, modification is conducive to remove battery case.Calcination temperature is
100 DEG C, time 30min.It is disassembled by hand after being cooled to room temperature, releases electrolyte.The electrode plates isolated, which are utilized, to be had
Solvent dissolves, and filters to isolate the collectors such as electrode material and copper foil aluminium foil.Organic solvent is NMP, and temperature is 30 DEG C, filtering
Mode pulls the collectors such as electrode material and copper foil aluminium foil out using strainer from solvent.Ethyl alcohol washing is added in filtrate, filters and divides
Separate out adhesive (PVDF).The volume ratio of alcohol and filtrate is 1:1, washing times are 3 times.Organic filtrate is warming up to 100 DEG C of separation
Ethyl alcohol and organic solvent.The rate of recovery of adhesive is up to 98%.
Embodiment 2
Lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity.Soaking temperature is room temperature, the time
30min.Battery after immersion in muffle furnace is roasted, is softened, modification is conducive to remove battery case.Calcination temperature is
50 DEG C, time 60min.It is disassembled by hand after being cooled to room temperature, releases electrolyte.The electrode plates isolated are utilized organic
Solvent dissolves, and filters to isolate the collectors such as electrode material and copper foil aluminium foil.Organic solvent is NMP, and temperature is 50 DEG C, filtering side
Formula pulls the collectors such as electrode material and copper foil aluminium foil out using strainer from solvent.Ethyl alcohol washing is added in filtrate, filters separation
Go out adhesive (PVDF).The volume ratio of alcohol and filtrate is 2:1, washing times are 5 times.Organic filtrate is warming up to 120 DEG C of separation second
Alcohol and organic solvent.The rate of recovery of adhesive is up to 99%.
Embodiment 3
Lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity.Soaking temperature is room temperature, the time
100min.Battery after immersion in muffle furnace is roasted, is softened, modification is conducive to remove battery case.Calcination temperature is
60 DEG C, time 80min.It is disassembled by hand after being cooled to room temperature, releases electrolyte.The electrode plates isolated are utilized organic
Solvent dissolves, and filters to isolate the collectors such as electrode material and copper foil aluminium foil.Organic solvent is NMP, and temperature is 40 DEG C, filtering side
Formula pulls the collectors such as electrode material and copper foil aluminium foil out using strainer from solvent.Ethyl alcohol washing is added in filtrate, filters separation
Go out adhesive (PVDF).The volume ratio of alcohol and filtrate is 3:1, washing times are 4 times.Organic filtrate is warming up to 180 DEG C of separation second
Alcohol and organic solvent.The rate of recovery of adhesive is up to 95%.
Embodiment 4
Lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity.Soaking temperature is room temperature, the time
30min.Battery after immersion in muffle furnace is roasted, is softened, modification is conducive to remove battery case.Calcination temperature is
70 DEG C, time 30min.It is disassembled by hand after being cooled to room temperature, releases electrolyte.The electrode plates isolated are utilized organic
Solvent dissolves, and filters to isolate the collectors such as electrode material and copper foil aluminium foil.Organic solvent is NMP, and temperature is 20 DEG C, filtering side
Formula pulls the collectors such as electrode material and copper foil aluminium foil out using strainer from solvent.Ethyl alcohol washing is added in filtrate, filters separation
Go out adhesive (PVDF).The volume ratio of alcohol and filtrate is 1:1, washing times are 5 times.Organic filtrate is warming up to 150 DEG C of separation second
Alcohol and organic solvent.The rate of recovery of adhesive is up to 96%.
Claims (10)
1. a kind of recovery method of waste and old lithium ion battery binding agent, it is characterised in that：Include the following steps：
(1) waste and old lithium ion battery is impregnated in deionized water, battery is made to discharge remaining electricity；
(2) battery after being impregnated in step (1) is roasted, is disassembled after being then cooled to room temperature, release electrolyte, obtain electrode
Pole piece and membrane；
(3) electrode plates isolated in step (2) using organic solvent are dissolved, filters to isolate electrode material and afflux
Body；
(4) ethyl alcohol washing will be added in gained filtrate in step (3), filters to isolate adhesive；
(5) ethyl alcohol and organic solvent are isolated into the filtrate obtained in step (4) heating.
2. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (1)
The temperature of immersion be room temperature, time 30-180min.
3. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (2)
It is roasted to and is roasted in muffle furnace, calcination temperature is 50-100 DEG C, time 30-120min.
4. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (3)
Organic solvent is NMP, and solution temperature is 20-80 DEG C.
5. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (3)
It is separated by filtration to pull electrode material and collector out from organic solvent using strainer.
6. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (4)
The volume ratio of ethyl alcohol and filtrate is 1-3:1, washing times are 3-5 times.
7. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：Adhesive is
PVDF。
8. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (4)
It is separated by filtration to be filtered using vacuum pump, filter cake is washed 3-5 times with ethyl alcohol.
9. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (5)
It is 80-200 DEG C to heat up to be warming up to temperature.
10. the recovery method of waste and old lithium ion battery binding agent according to claim 1, it is characterised in that：In step (2)
Obtained membrane recycles aluminium therein through following technique：Membrane is placed in muffle furnace and is roasted, removes remaining binding agent；It will roasting
Ceramic diaphragm after burning is dissolved out with lye, obtains solution, is passed through carbon dioxide, generation precipitation in the solution；Filtering, obtains
Precipitation through calcining obtain α or γ type alumina powders.
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| CN201711355281.2A CN108110358A (en) | 2017-12-16 | 2017-12-16 | The recovery method of waste and old lithium ion battery binding agent |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109103535A (en) * | 2018-08-09 | 2018-12-28 | 深圳市伟创源科技有限公司 | A kind of disassembling method of automobile elevator primary cell mould group |
| CN109309266A (en) * | 2018-09-20 | 2019-02-05 | 广东工业大学 | A kind of method and regeneration positive electrode of recycling waste lithium ion cell anode material |
| CN110120560A (en) * | 2019-04-16 | 2019-08-13 | 福建常青新能源科技有限公司 | A kind of waste and old ternary lithium battery recycling sorting process |
| CN110661055A (en) * | 2019-10-14 | 2020-01-07 | 赣州有色冶金研究所 | Method for efficiently stripping waste lithium ion battery material |
| CN111180820A (en) * | 2020-01-04 | 2020-05-19 | 浙江大学 | Method for recovering lithium ion battery original material and regenerating battery |
| CN111203172A (en) * | 2020-01-08 | 2020-05-29 | 山东建筑大学 | Method for preparing heavy metal adsorbent by recycling waste lithium ion battery anode material |
| CN111710932A (en) * | 2020-08-11 | 2020-09-25 | 湖南省正源储能材料与器件研究所 | Method for recovering binder of retired lithium ion battery anode |
| CN112687974A (en) * | 2021-03-16 | 2021-04-20 | 嘉兴模度新能源有限公司 | Chemical disassembling method applied to battery adhesive module |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109103535A (en) * | 2018-08-09 | 2018-12-28 | 深圳市伟创源科技有限公司 | A kind of disassembling method of automobile elevator primary cell mould group |
| CN109309266A (en) * | 2018-09-20 | 2019-02-05 | 广东工业大学 | A kind of method and regeneration positive electrode of recycling waste lithium ion cell anode material |
| CN110120560A (en) * | 2019-04-16 | 2019-08-13 | 福建常青新能源科技有限公司 | A kind of waste and old ternary lithium battery recycling sorting process |
| CN110661055A (en) * | 2019-10-14 | 2020-01-07 | 赣州有色冶金研究所 | Method for efficiently stripping waste lithium ion battery material |
| CN110661055B (en) * | 2019-10-14 | 2021-04-02 | 赣州有色冶金研究所 | Method for efficiently stripping waste lithium ion battery material |
| CN111180820A (en) * | 2020-01-04 | 2020-05-19 | 浙江大学 | Method for recovering lithium ion battery original material and regenerating battery |
| CN111180820B (en) * | 2020-01-04 | 2021-10-12 | 浙江大学 | Method for recovering lithium ion battery original material and regenerating battery |
| CN111203172A (en) * | 2020-01-08 | 2020-05-29 | 山东建筑大学 | Method for preparing heavy metal adsorbent by recycling waste lithium ion battery anode material |
| CN111203172B (en) * | 2020-01-08 | 2023-05-19 | 山东建筑大学 | Method for preparing heavy metal adsorbent by recycling waste lithium ion battery anode material |
| CN111710932A (en) * | 2020-08-11 | 2020-09-25 | 湖南省正源储能材料与器件研究所 | Method for recovering binder of retired lithium ion battery anode |
| CN112687974A (en) * | 2021-03-16 | 2021-04-20 | 嘉兴模度新能源有限公司 | Chemical disassembling method applied to battery adhesive module |
| CN112687974B (en) * | 2021-03-16 | 2021-06-18 | 嘉兴模度新能源有限公司 | Chemical disassembling method applied to battery adhesive module |
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Application publication date: 20180601 |