CN103606719A - Method for preparing lithium manganate cathode material by taking waste lithium ion batteries as raw material - Google Patents
Method for preparing lithium manganate cathode material by taking waste lithium ion batteries as raw material Download PDFInfo
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- CN103606719A CN103606719A CN201310630619.6A CN201310630619A CN103606719A CN 103606719 A CN103606719 A CN 103606719A CN 201310630619 A CN201310630619 A CN 201310630619A CN 103606719 A CN103606719 A CN 103606719A
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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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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Complex oxides containing manganese and at least one other metal element
- C01G45/1221—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof
- C01G45/125—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO3)n-, e.g. CaMnO3
- C01G45/1257—Manganates or manganites with trivalent manganese, tetravalent manganese or mixtures thereof of the type (MnO3)n-, e.g. CaMnO3 containing lithium, e.g. Li2MnO3 or Li2(MxMn1-x)O3
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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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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Abstract
本发明公开了一种以废旧锂离子电池为原料制备锰酸锂正极材料的方法。本发明的技术方案要点为：一种以废旧锂离子电池为原料制备锰酸锂正极材料的方法，主要以柠檬酸溶液为浸取剂和凝胶剂，采用溶胶-凝胶的方法制备锰酸锂正极材料，并且公开了具体的制备步骤。本发明避免了传统方法采用无机酸为浸取剂产生的S、N以及氯气等气体的污染，以及金属离子分离过程中的副产物和废水的产生，绿色环保，成本低，制备的锰酸锂正极材料可以直接返厂继续使用。
The invention discloses a method for preparing lithium manganate cathode material by using waste lithium ion batteries as raw materials. The key points of the technical solution of the present invention are: a method for preparing lithium manganate positive electrode material using waste lithium ion batteries as raw materials, mainly using citric acid solution as the leaching agent and gelling agent, and preparing manganic acid by a sol-gel method Lithium cathode material, and discloses specific preparation steps. The invention avoids the pollution of S, N, chlorine and other gases produced by using inorganic acid as the leaching agent in the traditional method, as well as the generation of by-products and waste water in the metal ion separation process, and is environmentally friendly and low in cost. The prepared lithium manganate The positive electrode material can be directly returned to the factory for continued use.
Description
Technical field
The present invention relates to waste and old lithium ion battery reutilization field, be specifically related to a kind ofly take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material.
Background technology
It is high that lithium ion battery has energy density, the good chemical property such as have extended cycle life, various portable electricity consumption facilities have been widely used in now, as mobile phone, notebook computer, video camera etc., simultaneously, in new-energy automobile field, lithium ion battery is also being brought into play vital effect.Along with the development of various electricity consumption facilities and new-energy automobile industry, the market demand of lithium ion battery increases year by year.In waste and old lithium ion battery, contain a large amount of precious metals and some flammable poisonous electrolyte, if waste and old lithium ion battery is not processed, not only can cause the waste of resource, also can cause certain environmental pollution.
But now the recovery research of waste and old lithium ion battery is mainly concentrated on to the recycling to cobalt acid lithium, cobalt is very rare metal material, solid content in waste and old lithium ion battery is even higher than the content of natural mineral reserve, and reclaiming the precious metals such as cobalt nickel has good economic benefit and the value of environmental protection.But because cobalt resource is limited, cause cobalt acid lithium cost more and more higher, occupation rate of market declines, in addition the security performance of cobalt acid lithium particularly high-temperature behavior still allow people worry, in recent years, people have mainly been placed on research energy on LiMn2O4, nickle cobalt lithium manganate and LiFePO 4, wish to prepare high performance chemical power source on the basis reducing costs.LiMn2O4 is as important anode material for lithium-ion batteries, there is cost low, environmental friendliness, the advantages such as security performance is good, at lamp power, electrical source of power field has a wide range of applications, therefore, the waste and old lithium ion battery that the LiMn2O4 of take is positive electrode is also more and more, yet less for the recovery research of this type of lithium ion battery.
Publication number is that the patent of CN102347521A discloses " recovery method of manganese and lithium in a kind of used for electric vehicle power type lithium manganate battery ", wherein mainly take inorganic acid as leachate, adopt respectively electrochemical deposition and carbonate precipitation method to reclaim and obtain manganese dioxide solid and lithium carbonate, although inorganic acid leaching in early stage metal ion leaching rate is high, cost is low, but the exhaust environment producing is seriously polluted, the complexity that the reclaiming respectively of metal ion caused in operation and the intractability of waste water accessory substance.Publication number is that the patent of CN101831548A discloses " a kind of method that reclaims valuable metal in waste lithium manganese oxide battery ", proposes to adopt NaOH precipitate and separate final high temperature calcining preparation MnO
2, carbonate deposition reclaims lithium with the form of lithium carbonate, is still difficult to avoid the negative effect that in traditional recovery method, separation of metal ions produces.
Summary of the invention
The present invention provides a kind of and take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material for overcoming the deficiencies in the prior art, the method had both been avoided the environmental pollution that in traditional recovery method, inorganic acid causes, the use of also having saved gel in material preparation process simultaneously, environmental friendliness, pollution-free, and prepared the manganate cathode material for lithium of high added value.
Technical scheme of the present invention is: a kind ofly take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material, it is characterized in that mainly take that citric acid solution is as leaching agent and gel, adopt the method for sol-gel to prepare manganate cathode material for lithium, specifically comprise the following steps: take after the waste and old lithium ion battery electric discharge that LiMn2O4 is positive electrode (1), disassemble battery, isolate positive plate; (2) positive plate step (1) being obtained is put into high-temperature process in vacuum furnace, decomposes binding agent; (3) process the positive plate after high-temperature vacuum pyrolysis, obtain anode sizing agent; (4) anode sizing agent after high temperature pyrolysis is dissolved in citric acid solution, wherein the ratio of the quality of anode sizing agent and the volume of citric acid solution is 45-75g/L, and the molar concentration of citric acid solution is 0.5-2mol/L; (5) add hydrogenperoxide steam generator, dissolution filter; (6) measure the content that GOLD FROM PLATING SOLUTION belongs to ion, with Li in solubility lithium salts and manganese salt regulator solution
+and Mn
2+mol ratio be 1:2; (7) with the pH of ammoniacal liquor regulator solution, be 5-9, be stirred to gel; (8) ageing is dried to obtain xerogel, after 250-350 ℃ of pre-burning 0.5-5h, in 450-900 ℃ of calcining, obtains manganate cathode material for lithium.
In step of the present invention (4), the ratio of the quality of anode sizing agent and the volume of citric acid solution is 60g/L; The molar concentration of described citric acid solution is 1.0mol/L; In described step (6), solubility lithium salts is lithium nitrate, lithium acetate or lithium sulfate, and soluble manganese salt is manganese nitrate, manganese acetate or manganese sulfate.
It is the pollution of the gases such as the leaching agent S, the N that produce and chlorine that the present invention has avoided conventional method to adopt inorganic acid, and the generation of the accessory substance in separation of metal ions process and waste water, environmental protection, cost is low, and the manganate cathode material for lithium of preparation can directly return factory to be continued to use.
Accompanying drawing explanation
Fig. 1 is that the present invention be take waste and old lithium ion battery and prepared the process chart of manganate cathode material for lithium as raw material, and Fig. 2 is the XRD collection of illustrative plates of the manganate cathode material for lithium that makes of the embodiment of the present invention 1.
Embodiment
By the following examples foregoing of the present invention is described in further details, but this should be interpreted as to the scope of the above-mentioned theme of the present invention only limits to following embodiment, all technology realizing based on foregoing of the present invention all belong to scope of the present invention.
Embodiment 1
(1) take after the waste and old lithium ion battery electric discharge that LiMn2O4 is positive electrode, disassemble battery, isolate positive plate; (2) positive plate step (1) being obtained is put into high-temperature process in vacuum furnace, decomposes binding agent; (3) process the positive plate after high-temperature vacuum pyrolysis, obtain anode sizing agent; (4) anode sizing agent after high temperature pyrolysis is dissolved in citric acid solution, wherein the quality of anode sizing agent and the volume ratio of citric acid solution are 60g/L, and the molar concentration of citric acid solution is 1.0mol/L; (5) add hydrogenperoxide steam generator, dissolution filter; (6) measure the content of the metal ion in solution, with Li in lithium nitrate and manganese nitrate regulator solution
+and Mn
2+mol ratio be 1:2; (7) with the pH=8 of ammoniacal liquor regulator solution, be stirred to gel; (8) ageing is dried to obtain xerogel, and in 350 ℃ of pre-burning 2h, 750 ℃ of calcining 12h obtain manganate cathode material for lithium.Fig. 2 is the XRD collection of illustrative plates of the manganate cathode material for lithium of preparation, consistent with the diffraction maximum of LiMn2O4 standard diagram by the product of the known preparation of collection of illustrative plates, and therefore the product of preparation is manganate cathode material for lithium.
Embodiment 2
(1) take after the waste and old lithium ion battery electric discharge that LiMn2O4 is positive electrode, disassemble battery, isolate positive plate; (2) positive plate step (1) being obtained is put into high-temperature process in vacuum furnace, decomposes binding agent; (3) process the positive plate after high-temperature vacuum pyrolysis, obtain anode sizing agent; (4) anode sizing agent after high temperature pyrolysis is dissolved in citric acid solution, wherein the quality of anode sizing agent and the volume ratio of citric acid solution are 45g/L, and the molar concentration of citric acid solution is 0.5mol/L; (5) add hydrogenperoxide steam generator, dissolution filter; (6) measure the content of the metal ion in solution, with Li in lithium acetate and manganese acetate regulator solution
+and Mn
2+mol ratio be 1:2; (7) with the pH=5 of ammoniacal liquor regulator solution, be stirred to gel; (8) ageing is dried to obtain xerogel, and in 350 ℃ of pre-burning 0.5h, 900 ℃ of calcinings obtain manganate cathode material for lithium.
Embodiment 3
(1) take after the waste and old lithium ion battery electric discharge that LiMn2O4 is positive electrode, disassemble battery, isolate positive plate; (2) positive plate step (1) being obtained is put into high-temperature process in vacuum furnace, decomposes binding agent; (3) process the positive plate after high-temperature vacuum pyrolysis, obtain anode sizing agent; (4) anode sizing agent after high temperature pyrolysis is dissolved in citric acid solution, wherein the quality of anode sizing agent and the volume ratio of citric acid solution are 75g/L, and the molar concentration of citric acid solution is 2mol/L; (5) add hydrogenperoxide steam generator, dissolution filter; (6) measure the content of the metal ion in solution, with Li in lithium sulfate and manganese sulfate regulator solution
+and Mn
2+mol ratio be 1:2; (7) with the pH=9 of ammoniacal liquor regulator solution, be stirred to gel; (8) ageing is dried to obtain xerogel, 250 ℃ of pre-burning 5h, and 450 ℃ of calcinings obtain manganate cathode material for lithium.
Above embodiment has described basic principle of the present invention, principal character and advantage.The technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification, describes just illustrates principle of the present invention; do not departing under the scope of the principle of the invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the scope of protection of the invention.
Claims (4)
1. take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material for one kind, it is characterized in that mainly take that citric acid solution is as leaching agent and gel, adopt the method for sol-gel to prepare manganate cathode material for lithium, specifically comprise the following steps: take after the waste and old lithium ion battery electric discharge that LiMn2O4 is positive electrode (1), disassemble battery, isolate positive plate; (2) positive plate step (1) being obtained is put into high-temperature process in vacuum furnace, decomposes binding agent; (3) process the positive plate after high-temperature vacuum pyrolysis, obtain anode sizing agent; (4) anode sizing agent after high temperature pyrolysis is dissolved in citric acid solution, wherein the ratio of the quality of anode sizing agent and the volume of citric acid solution is 45-75g/L, and the molar concentration of citric acid solution is 0.5-2mol/L; (5) add hydrogenperoxide steam generator, dissolution filter; (6) measure the content that GOLD FROM PLATING SOLUTION belongs to ion, with Li in solubility lithium salts and manganese salt regulator solution
+and Mn
2+mol ratio be 1:2; (7) by the pH value of ammoniacal liquor regulator solution, be 5-9, be stirred to gel; (8) ageing is dried to obtain xerogel, after 250-350 ℃ of pre-burning 0.5-5h, in 450-900 ℃ of calcining, obtains manganate cathode material for lithium.
2. according to claim 1ly take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material, it is characterized in that: in described step (4), the ratio of the quality of anode sizing agent and the volume of citric acid solution is 60g/L.
3. according to claim 1ly take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material, it is characterized in that: the molar concentration of the citric acid solution in described step (4) is 1.0mol/L.
4. according to claim 1ly take waste and old lithium ion battery and prepare the method for manganate cathode material for lithium as raw material, it is characterized in that: in described step (6), solubility lithium salts is lithium nitrate, lithium acetate or lithium sulfate, soluble manganese salt is manganese nitrate, manganese acetate or manganese sulfate.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105865876A (en) * | 2016-05-29 | 2016-08-17 | 合肥国轩高科动力能源有限公司 | A pretreatment method for detecting metal ions in lithium-ion battery cathode materials |
| CN107699692A (en) * | 2017-09-18 | 2018-02-16 | 北京理工大学 | A kind of recovery and the method for regenerating waste used anode material for lithium-ion batteries |
| CN109022793A (en) * | 2017-06-12 | 2018-12-18 | 长沙矿冶研究院有限责任公司 | A method of the Selectively leaching lithium from the anode material waste powder of at least one of the manganese of nickel containing cobalt |
| CN109207725A (en) * | 2018-09-19 | 2019-01-15 | 中国科学院青海盐湖研究所 | A kind of method and system recycling lithium and manganese from waste lithium manganese oxide battery |
| CN109742364A (en) * | 2019-01-09 | 2019-05-10 | 东北师范大学 | A kind of recycling method of waste lithium cobalt oxide positive electrode |
| CN109734068A (en) * | 2019-01-09 | 2019-05-10 | 东北师范大学 | A kind of recycling method of waste lithium manganate positive electrode |
| CN110564978A (en) * | 2019-10-15 | 2019-12-13 | 俞杰 | operation process for recovering nickel and cobalt in ternary battery material by wet method |
| CN111041230A (en) * | 2019-08-16 | 2020-04-21 | 中国科学院过程工程研究所 | Method for recovering metal from waste lithium ion battery |
| CN111530470A (en) * | 2020-05-06 | 2020-08-14 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN114906863A (en) * | 2022-05-31 | 2022-08-16 | 宁波容百新能源科技股份有限公司 | Comprehensive recovery method of waste lithium manganate cathode material |
| CN117142530A (en) * | 2023-07-27 | 2023-12-01 | 焦作伴侣纳米材料工程有限公司 | A method for recycling valuable metals of lithium manganate material and cathode material |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105865876A (en) * | 2016-05-29 | 2016-08-17 | 合肥国轩高科动力能源有限公司 | A pretreatment method for detecting metal ions in lithium-ion battery cathode materials |
| CN109022793A (en) * | 2017-06-12 | 2018-12-18 | 长沙矿冶研究院有限责任公司 | A method of the Selectively leaching lithium from the anode material waste powder of at least one of the manganese of nickel containing cobalt |
| CN107699692A (en) * | 2017-09-18 | 2018-02-16 | 北京理工大学 | A kind of recovery and the method for regenerating waste used anode material for lithium-ion batteries |
| CN109207725A (en) * | 2018-09-19 | 2019-01-15 | 中国科学院青海盐湖研究所 | A kind of method and system recycling lithium and manganese from waste lithium manganese oxide battery |
| CN109742364A (en) * | 2019-01-09 | 2019-05-10 | 东北师范大学 | A kind of recycling method of waste lithium cobalt oxide positive electrode |
| CN109734068A (en) * | 2019-01-09 | 2019-05-10 | 东北师范大学 | A kind of recycling method of waste lithium manganate positive electrode |
| CN111041230A (en) * | 2019-08-16 | 2020-04-21 | 中国科学院过程工程研究所 | Method for recovering metal from waste lithium ion battery |
| CN110564978A (en) * | 2019-10-15 | 2019-12-13 | 俞杰 | operation process for recovering nickel and cobalt in ternary battery material by wet method |
| CN111530470A (en) * | 2020-05-06 | 2020-08-14 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN111530470B (en) * | 2020-05-06 | 2022-03-18 | 合肥工业大学 | The preparation method of manganese dioxide and its composite material and the degradation method of sulfadiazine |
| CN114906863A (en) * | 2022-05-31 | 2022-08-16 | 宁波容百新能源科技股份有限公司 | Comprehensive recovery method of waste lithium manganate cathode material |
| CN114906863B (en) * | 2022-05-31 | 2023-12-15 | 宁波容百新能源科技股份有限公司 | Comprehensive recovery method of waste lithium manganate anode material |
| CN117142530A (en) * | 2023-07-27 | 2023-12-01 | 焦作伴侣纳米材料工程有限公司 | A method for recycling valuable metals of lithium manganate material and cathode material |
| CN117142530B (en) * | 2023-07-27 | 2026-01-30 | 河南钠锂优材科技有限公司 | A method for recycling valuable metals from lithium manganese oxide materials and a cathode material |
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| CN103606719B (en) | 2016-01-27 |
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