CN110534834A - The recovery method of electrolyte in a kind of waste and old lithium ion battery - Google Patents
The recovery method of electrolyte in a kind of waste and old lithium ion battery Download PDFInfo
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- CN110534834A CN110534834A CN201910855302.XA CN201910855302A CN110534834A CN 110534834 A CN110534834 A CN 110534834A CN 201910855302 A CN201910855302 A CN 201910855302A CN 110534834 A CN110534834 A CN 110534834A
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- electrolyte
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- lithium ion
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- 238000000034 method Methods 0.000 title claims abstract description 63
- 239000003792 electrolyte Substances 0.000 title claims abstract description 56
- 239000002699 waste material Substances 0.000 title claims abstract description 31
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 30
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 238000011084 recovery Methods 0.000 title claims abstract description 18
- 238000004227 thermal cracking Methods 0.000 claims abstract description 22
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011737 fluorine Substances 0.000 claims abstract description 18
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000012545 processing Methods 0.000 claims abstract description 13
- 238000000197 pyrolysis Methods 0.000 claims abstract description 13
- 239000007772 electrode material Substances 0.000 claims abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910052742 iron Inorganic materials 0.000 claims abstract description 8
- 239000007787 solid Substances 0.000 claims abstract description 8
- 239000004411 aluminium Substances 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 239000011162 core material Substances 0.000 claims description 18
- 239000012535 impurity Substances 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 239000002351 wastewater Substances 0.000 claims description 12
- 238000010521 absorption reaction Methods 0.000 claims description 11
- 239000011230 binding agent Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 229910052799 carbon Inorganic materials 0.000 claims description 8
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- 239000007921 spray Substances 0.000 claims description 7
- 229910001290 LiPF6 Inorganic materials 0.000 claims description 6
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical group [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 6
- 239000000292 calcium oxide Substances 0.000 claims description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 6
- 239000001506 calcium phosphate Substances 0.000 claims description 6
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 6
- 235000011010 calcium phosphates Nutrition 0.000 claims description 6
- 159000000007 calcium salts Chemical class 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 6
- 238000005336 cracking Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 6
- 239000010865 sewage Substances 0.000 claims description 5
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 4
- 238000007885 magnetic separation Methods 0.000 claims description 4
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims description 2
- 235000017557 sodium bicarbonate Nutrition 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000007789 gas Substances 0.000 description 28
- 229910052744 lithium Inorganic materials 0.000 description 23
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 22
- 208000028659 discharge Diseases 0.000 description 18
- 238000000926 separation method Methods 0.000 description 11
- 239000000243 solution Substances 0.000 description 10
- 239000005030 aluminium foil Substances 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 239000000428 dust Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 description 4
- 238000009833 condensation Methods 0.000 description 4
- 230000005494 condensation Effects 0.000 description 4
- 238000002309 gasification Methods 0.000 description 4
- 150000007524 organic acids Chemical class 0.000 description 4
- 230000001376 precipitating effect Effects 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 239000002253 acid Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- KFDQGLPGKXUTMZ-UHFFFAOYSA-N [Mn].[Co].[Ni] Chemical compound [Mn].[Co].[Ni] KFDQGLPGKXUTMZ-UHFFFAOYSA-N 0.000 description 2
- 239000011149 active material Substances 0.000 description 2
- 239000010405 anode material Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000007767 bonding agent Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- OVAQODDUFGFVPR-UHFFFAOYSA-N lithium cobalt(2+) dioxido(dioxo)manganese Chemical compound [Li+].[Mn](=O)(=O)([O-])[O-].[Co+2] OVAQODDUFGFVPR-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000007773 negative electrode material Substances 0.000 description 2
- 235000005985 organic acids Nutrition 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 230000001698 pyrogenic effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- QGHDLJAZIIFENW-UHFFFAOYSA-N 4-[1,1,1,3,3,3-hexafluoro-2-(4-hydroxy-3-prop-2-enylphenyl)propan-2-yl]-2-prop-2-enylphenol Chemical group C1=C(CC=C)C(O)=CC=C1C(C(F)(F)F)(C(F)(F)F)C1=CC=C(O)C(CC=C)=C1 QGHDLJAZIIFENW-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- QXZUUHYBWMWJHK-UHFFFAOYSA-N [Co].[Ni] Chemical compound [Co].[Ni] QXZUUHYBWMWJHK-UHFFFAOYSA-N 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- JXAZAUKOWVKTLO-UHFFFAOYSA-L sodium pyrosulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OS([O-])(=O)=O JXAZAUKOWVKTLO-UHFFFAOYSA-L 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
- B09B3/40—Destroying solid waste or transforming solid waste into something useful or harmless involving thermal treatment, e.g. evaporation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B5/00—Operations not covered by a single other subclass or by a single other group in this subclass
-
- 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
- Y02W30/20—Waste processing or separation
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Primary Cells (AREA)
- Secondary Cells (AREA)
Abstract
The invention discloses a kind of recovery methods of electrolyte in waste and old lithium ion battery, including the single battery core of the waste and old lithium ion battery after electric discharge is disassembled, thermal cracking processing is carried out at 300-500 DEG C, pyrolysis time is 0.5-1.5h, and the solid matter after thermal cracking recycles after crushing, sorting and obtains electrode material and iron, aluminium, copper powder；Gas after thermal cracking is first dusted, and is then condensed, and condensed electrolyte is recycled, condensed gas discharges after lye elutes, method of the invention not only recycles electrolyte, and the fluorine content of discharge gas is reduced to discharge standard hereinafter, reaching the requirement of environmental protection treatment.
Description
Technical field
The invention belongs to waste and old lithium ion battery recovery technology fields, and in particular to a kind of waste and old lithium ionic cell electrolyte
Recovery and treatment method.
Background technique
With the fast development of New-energy electric vehicle, the yield of power train in vehicle application lithium battery will be greatly improved.Lithium battery contains
There are various recoverable materials, an electric car averagely uses 50 kilograms of positive electrode, 40 kilograms of negative electrode material, electrolyte
40 kilograms, if 2014-2018 will expedite the emergence of 5000 tons based on 2009-2011 China 100,000 lithium battery electrical automobiles of investment
Positive electrode, 4000 tons of negative electrode materials, 4000 tons of electrolyte.If being put into based on 2,000,000 lithium battery electrical automobiles by the year two thousand twenty,
2025-2027 will expedite the emergence of 100000 tons of anodes, 80000 tons of cathode, 80000 tons of electrolyte, and industry size will be more than 35,000,000,000
Member.China's lithium battery recycle system it is unsound etc. due to, lithium battery recovery utilization rate is lower.The place of waste lithium cell
Reason faces great harm to environmental protection.
At present to waste and old lithium ion battery recycle research be concentrated mainly on waste lithium cell pretreatment and it is subsequent valuable
Metal recovery use aspects, but to electrolyte and the organic matter recycling volatilized in waste lithium cell preprocessing process therein or nothing
The problems such as research of evilization processing is less, and that there are mechanization degrees when large-scale production is low, environmental pollution.
Chinese patent CN201210230857.3 discloses a kind of method, by waste lithium ion cell anode material directly with
The mixing of fluorine-containing aqueous solutions of organic acids, or it is broken after mixed with fluorine-containing aqueous solutions of organic acids, reacted at 40 DEG C -70 DEG C, make it is waste and old just
Active material containing lithium in the material of pole is separated with aluminium foil, solid then carrying out liquid-solid-separation, respectively obtains leachate, containing lithium activity
Substance and aluminium foil.Isolated active material containing lithium is placed in high temperature kiln roasting, removes conductive agent and binder therein,
Then dealuminzation mistake is obtained to remove a small amount of impurity aluminum therein using the positive active material obtained after aqueous slkali dissolution roasting
Imitate positive active material.Then by inorganic acid acidleach, neutralization precipitation method removal of impurities and etc., it is finally prepared to ternary precursor.
The method that this method uses fluorine-containing organic acid soak is unable to reach being kept completely separate for positive electrode and aluminium foil, while impregnating
Cheng Zhong, temperature are 40 DEG C~70 DEG C, and a large amount of fluorine-containing organic acid volatilizees, and generate secondary pollution to environment.
Chinese patent CN201410116605.7 discloses a kind of method, first by waste and old lithium ion battery discharge treatment,
Waste and old lithium ion battery is broken into the sheet of diameter 10-20mm in closed shear crusher, is sprayed when broken, will be given up
Lithium hexafluoro phosphate in old lithium ion battery is dissolved into spray liquid, by the carbon dust of stirring removing copper foil surface, and will electrolysis
Liquid is dissolved into spray liquid, then recycles carbon dust.Obtained board is sent into the hydrogen-oxygen that mass percentage concentration is 0.5-5%
Change in sodium solution, by the cobalt acid lithium powder of the stirring removing aluminium foil surface of mixing plant, obtains cobalt acid lithium powder.This method exists
Spray-absorption is carried out to the fluorine-containing organic exhaust gas that volatilizees in shattering process, cannot achieve the ring of waste gas containing fluoride only with the method for spray
Guarantor's processing.
Chinese patent CN201610251626.9 discloses a kind of method, uses waste and old lithium ion battery for raw material, by it
Positive plate is taken out in dismantling, carries out ultrasound, separating active substances.It is recycled positive electrode material acidleach after aluminium foil is dry again, removes iron, then
The ratio for adjusting nickel cobalt manganese in solution prepares nickel-cobalt-manganese ternary hydroxide.This method is needed only for old and useless battery positive plate
Manually it is sorted with battery cathode, shell, this is not easy to realize in actual production operation, especially heavy industrialization
When can make troubles to production.
104466295 A of Chinese patent CN discloses a kind of method, and used Li ion cell is discharged, disassembles acquisition
Useless positive plate, useless positive plate are fired, water dissolution, filter the useless nickle cobalt lithium manganate powder of acquisition；By useless nickle cobalt lithium manganate powder with
Sodium pyrosulfate roasts after being mixed in a certain ratio, and product of roasting is gone out with water logging, and mistake after sodium carbonate liquor is then added into solution
It filters, its ball milling, compression, roasting is regained into nickel cobalt mangaic acid after the ratio of Li, Ni, Co, Mn in supplement carbonate adjustment filter residue
Lithium anode material.This method belongs to pyrogenic attack, and the method roasted using pyrogenic process cannot achieve the efficient of positive electrode and aluminium foil
Separation, and the exhaust gas being discharged can pollute air, not meet the idea of development of green reclaim.
CN110061320A discloses a kind of method using active powder material in cracking process recycling waste power lithium battery, specifically
It is: waste power lithium battery is charged in the environment of inert gas shielding and is crushed, battery particle, diaphragm and shell are obtained；It will
Obtained battery particle, diaphragm and shell obtains battery particle after sorting, magnetic separation；The battery particle and battery that will be obtained
The electrolyte and bonding agent carried secretly in particle are cracked, and electrolyte and bonding agent volatilization removal, battery particle crack to obtain electricity
Pole powder and copper aluminium foil；Obtained electrode powder and copper aluminium foil are subjected to water cooling sorting, recycle electrode powder；The cracking that will be obtained
Smoke secondary high-temp combustion, obtains carbon dioxide and water.
Patent CN105846004A discloses a kind of technique using organic solvent cleaning electrolyte, but uses organic solvent
The method of cleaning electrolyte can introduce new organic matter, introduce new impurity for subsequent technique.
Patent CN103825065B eliminates the harm of electrolyte using low-temperature freezing, but low-temperature freezing energy consumption it is high,
Operating cost is big.The above existing method is not recycled electrolyte, while also not reaching environmental protection to the processing of fluorine
Standard, the gas of discharge still generate pollution to atmosphere.
Summary of the invention
The present invention provides a kind of recovery and treatment method of electrolyte in waste and old lithium ion battery, this method is not only effectively returned
Electrolyte is received, treated, and exhaust emissions reaches discharge standard, and the content of fluorine is less than 9mg/m in tail gas3。
The recovery method of electrolyte in a kind of waste and old lithium ion battery of the invention, comprising the following steps:
1) single battery core of the waste and old lithium ion battery after electric discharge is disassembled；
2) core material after disassembling carries out thermal cracking processing, and pyrolysis temperature is 300-500 DEG C, pyrolysis time 0.5-
1.5h；
3) solid matter after thermal cracking recycles after crushing, sorting and obtains electrode material and iron, aluminium, copper powder；
4) gas after thermal cracking is first dusted, and is then condensed, and condensed electrolyte, condensed gas are recycled
Body uses lye spray-absorption, the tail gas qualified discharge after spray-absorption；
5) calcium salt removal of impurities is added in the waste water that spray generates, generates calcirm-fluoride, calcium phosphate, the waste water after removal of impurities is sent at sewage
Reason.
The method of aforementioned present invention, dismantling described in step 1) are disassembled using mechanical means, and the interior of battery is destroyed
Portion's structure, the single battery core are selected from soft-package battery, cylindrical battery and rectangular cell；It cracks, was cracking described in step 2)
Electrolyte LiPF6 in journey in electrolyte is converted into fluoride and phosphide, and solvent therein is gasified, and glues in cracking process
Knot agent carbonization is agraphitic carbon to fail；In step 3), smashed material is sheet, powdery and/or graininess, granularity <
20mm, the sorting, mode are screening, selection by winnowing, magnetic separation or/and eddy current separation；In step 4), the condensation, condensation
For temperature less than 90 DEG C, the lye is sodium hydroxide, sodium carbonate or sodium bicarbonate, the fluorine content < 9mg/m in emission3；
Calcium salt described in step 5) is calcium oxide.
In one embodiment, in a kind of waste and old lithium ion battery electrolyte recovery method, include
1) the used Li ion single battery core after electric discharge is mechanically disassembled, destroys the internal structure of battery, just
In conveying, treatment effeciency is improved, risk is avoided.Single battery core includes soft-package battery, cylindrical battery, rectangular cell；
2) core material after disassembling carries out thermal cracking processing, the pollution such as effective solution electrolyte, binder.Electrolyte
In electrolyte LiPF6It is converted into fluoride and phosphide, solvent gasification；Binder carbonization is agraphitic carbon to fail, and is mentioned
The separation rate of high electrode material and collector.Pyrolysis temperature is 300-500 DEG C, pyrolysis time 0.5-1.5h.In pyrolytic process
Logical inert gas shielding；
3) solid matter after thermal cracking obtains electrode material and iron, aluminium, copper powder after crushing, sorting.After crushing
Material be sheet or powdery, granularity < 20mm.Crusher is placed in exhausting system, is focused on after dust collection.Sorting side
Formula is screening, selection by winnowing, magnetic separation, eddy current separation etc.；
4) gas after thermal cracking is first dusted, and is then condensed, and condensed electrolyte is recycled；Condensed gas
Body uses lye spray-absorption, and the lye is sodium hydroxide, sodium carbonate or sodium bicarbonate etc., the tail gas of spray-absorption row up to standard
It puts, fluorine content < 9mg/m3；
5) calcium salt removal of impurities is added in the waste water after spraying, generates the precipitating such as calcirm-fluoride, calcium phosphate, the waste water after removal of impurities send dirt
Water process.Calcium salt is calcium oxide.
Technical effect of the invention: method of the invention uses thermal cracking process, is recycled in waste and old lithium ion battery
Electrolyte can not only recycle organic matter in electrolyte, defluorinate, moreover it is possible to decompose binder, improve point of electrode material and collector
From rate.Electrolyte in method safety of the invention, efficient recycling waste and old lithium ion battery, electrolyte rate of recovery > 90%, row
Fluorine content < 9mg/m3 in deflation body.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Following embodiment be only it is representative, be used to help understand Spirit Essence of the invention, but do not limit in any way
The scope of the present invention processed.
The recovery processing of electrolyte in 1 waste and old lithium ion battery of embodiment
Process flow is as shown in Figure 1.
The specific process is as follows:
1, the used Li ion single battery core after electric discharge is mechanically disassembled, destroys the internal structure of battery, just
In conveying, treatment effeciency is improved, risk is avoided.Single battery core includes soft-package battery, cylindrical battery, rectangular cell.
2, the core material after disassembling carries out thermal cracking processing, the pollution such as effective solution electrolyte, binder.Electrolyte
In electrolyte LiPF6It is converted into fluoride and phosphide, solvent gasification；Binder carbonization is agraphitic carbon to fail, and is mentioned
The separation rate of high electrode material and collector.Pyrolysis temperature is 400 DEG C, and pyrolysis time is about 1.0h, leads to inertia in pyrolytic process
Gas shield.
3, the solid matter after thermal cracking is sheet or powdery or graininess, granularity < by crushing, smashed material
20mm.Crusher is placed in exhausting system, is focused on after dust collection, according to lithium battery at component selections screening, selection by winnowing, magnetic
The sorting mode of choosing, eddy current separation or their combinations sorts comminuting matter to obtain electrode material and iron, aluminium, copper
Powder.
4, the gas after thermal cracking is first dusted, and is then condensed, and condensation temperature recycles condensed less than 90 DEG C
Electrolyte；Condensed gas uses sodium bicarbonate, sodium carbonate or sodium hydroxide or their mixture solution spray-absorption, spray
Drench the tail gas qualified discharge absorbed, fluorine content < 9mg/m3。
5, calcium oxide removal of impurities is added in the waste water after spraying, generates the precipitating such as calcirm-fluoride, calcium phosphate, the waste water after removal of impurities is sent
Sewage treatment.
As a result: above-mentioned technique has recycled electrolyte in waste and old lithium ion battery, and electrolyte rate of recovery > 90% discharges gas
Fluorine content < 9mg/m3 in body.Exhaust gas discharge reaches national emission standard.
The recovery processing of electrolyte in 2 waste and old lithium ion battery of embodiment
Process flow is as shown in Figure 1.
The specific process is as follows:
1, the used Li ion single battery core after electric discharge is mechanically disassembled, destroys the internal structure of battery, just
In conveying, treatment effeciency is improved, risk is avoided.Single battery core includes soft-package battery, cylindrical battery, rectangular cell.
2, the core material after disassembling carries out thermal cracking processing, the pollution such as effective solution electrolyte, binder.Electrolyte
In electrolyte LiPF6It is converted into fluoride and phosphide, solvent gasification；Binder carbonization is agraphitic carbon to fail, and is mentioned
The separation rate of high electrode material and collector.Pyrolysis temperature is 300 DEG C, and pyrolysis time is about 1.5h.Lead to inertia in pyrolytic process
Gas shield.
3, the solid matter after thermal cracking is sheet or powdery or graininess, granularity < by crushing, smashed material
20mm.Crusher is placed in exhausting system, is focused on after dust collection, according to lithium battery at component selections screening, selection by winnowing, magnetic
The sorting mode of choosing, eddy current separation or their combinations sorts comminuting matter to obtain electrode material and iron, aluminium, copper
Powder.
4, the gas after thermal cracking is first dusted, and is then condensed, and condensation temperature recycles condensed less than 90 DEG C
Electrolyte；Condensed gas uses sodium bicarbonate, sodium carbonate or sodium hydroxide or their mixture solution spray-absorption, spray
Drench the tail gas qualified discharge absorbed, fluorine content < 9mg/m3。
5, calcium oxide removal of impurities is added in the waste water after spraying, generates the precipitating such as calcirm-fluoride, calcium phosphate, the waste water after removal of impurities is sent
Sewage treatment.As a result: above-mentioned technique has recycled electrolyte in waste and old lithium ion battery, and electrolyte rate of recovery > 90% discharges gas
Fluorine content < 9mg/m3 in body.Exhaust gas discharge reaches national emission standard.
The recovery processing of electrolyte in 3 waste and old lithium ion battery of embodiment
Process flow is as shown in Figure 1.
The specific process is as follows:
1, the used Li ion single battery core after electric discharge is mechanically disassembled, destroys the internal structure of battery, just
In conveying, treatment effeciency is improved, risk is avoided.Single battery core includes soft-package battery, cylindrical battery, rectangular cell.
2, the core material after disassembling carries out thermal cracking processing, the pollution such as effective solution electrolyte, binder.Electrolyte
In electrolyte LiPF6It is converted into fluoride and phosphide, solvent gasification；Binder carbonization is agraphitic carbon to fail, and is mentioned
The separation rate of high electrode material and collector.Pyrolysis temperature is about 500 DEG C, and pyrolysis time is about 0.5, and inertia is led in pyrolytic process
Gas shield.
3, the solid matter after thermal cracking is sheet or powdery or graininess, granularity < by crushing, smashed material
20mm.Crusher is placed in exhausting system, is focused on after dust collection, according to lithium battery at component selections screening, selection by winnowing, magnetic
The sorting mode of choosing, eddy current separation or their combinations sorts comminuting matter to obtain electrode material and iron, aluminium, copper
Powder.
4, the gas after thermal cracking is first dusted, and is then condensed, and condensed electrolyte is recycled；Condensed gas
Body is up to standard using sodium bicarbonate, sodium carbonate or sodium hydroxide or their mixture solution spray-absorption, the tail gas of spray-absorption
Discharge, fluorine content < 9mg/m3。
5, calcium oxide removal of impurities is added in the waste water after spraying, generates the precipitating such as calcirm-fluoride, calcium phosphate, the waste water after removal of impurities is sent
Sewage treatment.As a result: above-mentioned technique has recycled electrolyte in waste and old lithium ion battery, and electrolyte rate of recovery > 90% discharges gas
Fluorine content < 9mg/m in body3.Exhaust gas discharge reaches national emission standard.
Claims (10)
1. the recovery method of electrolyte in a kind of waste and old lithium ion battery, comprising the following steps:
1) single battery core of the waste and old lithium ion battery after electric discharge is disassembled；
2) core material after disassembling carries out thermal cracking processing, and pyrolysis temperature is 300-500 DEG C, pyrolysis time 0.5-1.5h；
3) solid matter after thermal cracking recycles after crushing, sorting and obtains electrode material and iron, aluminium, copper powder；
4) gas after thermal cracking is first dusted, and is then condensed, and condensed electrolyte is recycled, and condensed gas is adopted
Tail gas qualified discharge with lye spray-absorption, after spray-absorption；
5) calcium salt removal of impurities is added in the waste water that spray generates, generates calcirm-fluoride, calcium phosphate, the waste water after removal of impurities send sewage treatment.
2. the method as described in claim 1, dismantling described in step 1) is disassembled using mechanical means, destroys battery
Internal structure.
3. the method as described in claim 1, single battery core described in step 1) is selected from soft-package battery, cylindrical battery and square electric
Pond.
4. the method as described in claim 1 cracks, the electrolyte in cracking process in electrolyte described in step 2)
LiPF6 is converted into fluoride and phosphide, and solvent therein is gasified.
5. the method as described in claim 1 cracks described in step 2), binder carbonization is agraphitic carbon in cracking process
To fail.
6. the method as described in claim 1, in step 3), smashed material is sheet, powdery and/or graininess, granularity
< 20mm.
7. the method as described in claim 1, in step 3), the sorting, mode is that screening, selection by winnowing, magnetic separation or/and whirlpool are electric
Classification.
8. the method as described in claim 1, in step 4), the lye is sodium hydroxide, sodium carbonate or sodium bicarbonate.
9. the method as described in claim 1, in step 4), the fluorine content < 9mg/m in emission3。
10. the method as described in claim 1, in step 5), the calcium salt is calcium oxide.
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