CN105428745A - Method for comprehensive harmless recovery and utilization of waste lithium ion power battery - Google Patents
Method for comprehensive harmless recovery and utilization of waste lithium ion power battery Download PDFInfo
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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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- 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
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion 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
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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
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- Y02W30/84—Recycling of batteries or fuel cells
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Abstract
The present invention relates to a method for comprehensive harmless recovery and utilization of a waste lithium ion power battery. The method comprises the following steps: disassembling a waste battery pack, and measuring and collecting good battery cells to re-combine the good batteries for gradient utilization; sufficiently discharging defective waste lithium ion power battery cells, and disassembling the power battery cells in an oxygen-isolated environment; performing heat treatment on a fetched core pack in a heating furnace, and collecting a distilled solvent by means of condensation; disassembling the core pack from which the solvent is distilled off to obtain a membrane material, a positive electrode plate and a negative electrode plate; placing the positive electrode plate and the negative electrode plate in a rotary kiln of 200-600 DEG C to be subjected to heat treatment; sorting electrode plates, which have been subjected to the heat treatment, by using a pulverizer and a powder sorter separately, so as to obtain an aluminum powder, a copper powder, a waste positive electrode powder and a waste negative electrode powder; and repairing the positive electrode powder and the negative electrode powder separately. According to the method provided by the present invention, a fully-dry closed-circuit recovery process is adopted, thereby achieving the harmless recovery and utilization of the waste lithium ion power battery.
Description
Technical field
The invention belongs to the recovery technology field of lithium-ion-power cell, the gradient especially relating to applying waste lithium ionic electrokinetic cell utilizes and innoxious synthetical recovery process.
Background technology
Along with energy problem highlights day by day, environmental problem more and more comes into one's own, and ev industry adapts to historical development trend, expands rapidly in the mode of advancing by leaps and bounds.Lithium ion battery is because its energy density is high, and security performance is good, and memory-less effect is subject to extensive concern, wherein particularly using LiFePO 4 as the lithium ion battery of positive electrode, because of stable discharge platform, higher security performance, use amount grows with each passing day in electrokinetic cell field.Electric automobile is a Main way of Chinese automobile future development, estimate according to " electric automobile development in science and technology " 12 " ad hoc planning ", Electric Cars in China recoverable amount in 2015 plan reaches 500,000, and electrokinetic cell production capacity about reaches 10,000,000,000 watt-hours (about 3,000,000,000 ampere-hour); 2020 reach 5,000,000, and its development prospect is boundless.
Also bring thinking on the other hand to us while electric automobile develop rapidly, the battery on electric automobile has started to update, and will there is the propagation process of a normalization over a period to come.Waste and old electrokinetic cell voltage reaches hundreds of kilograms and even upper ton up to hundreds of volt, capacity ampere-hour up to ten thousand, weight, unavoidably there is potential safety hazard and environmental protection hidden danger in it, the innoxious synthetical recovery of therefore how economy, safety, environmental protection is the difficult problem of pendulum in face of us.Current a lot of document and patent report reclaim the method adopting batch electrical discharge machine pulverizing high-temperature calcination to purify again to lithium ion battery, this is more convenient to small-scale lithium ion cell, but also there is the secondary pollution such as organic solvent, electrolytic salt.But for applying waste lithium ionic electrokinetic cell bag (assembly), after power brick is waste and old, wherein still there is a considerable amount of cell to have good performance, also there is good value; If all carry out metallurgy to disassemble, the wasting of resources certainly will be caused.Therefore the technical matters comprehensive reutilization of lithium-ion-power cell being proposed to architectonical is also needed.
The method of the waste and old ferrous phosphate lithium battery synthetical recovery of patent CN101847763A(mono-kind), patent CN102738539A(reclaims the method and apparatus of ferrousphosphate lithium material from waste and old ferrous phosphate lithium battery anode sheet), the recovery repair process method of a patent CN102208706A(waste and old ferrous phosphate lithium battery anode material), the method that the waste and old lithium iron phosphate cathode material reparation of patent CN102208707A(mono-kind is repaired), patent CN102403554A(waste and old ferrous phosphate lithium ion battery positive electrode circulation utilization method), the recovery method of the waste and old ferrous phosphate lithium battery of patent CN102664294A(), patent CN102751548A(mono-kind reclaims the method preparing LiFePO 4 from LiFePO 4 old and useless battery), patent CN103449395A(mono-kind reclaims and repairs the method for positive electrode from water-system waste ferrous phosphate lithium battery) etc. mainly by wet process, positive electrode is peeled off, again using the positive electrode peeled off as raw material, Fe source is added by proportioning, P source or Li source, mix rear high temperature sintering synthesizing lithium ferrous phosphate more in some way, all there is wet method stripping process in these methods, there is the consumption of various reagent or solvent, and the electrolyte in electrokinetic cell, electrolyte will enter solution to be difficult to reclaim, water pollutions may be caused.
The recoverying and utilizing method of the waste and old ferrous phosphate lithium dynamical battery of patent CN102017276A() positive plate in old and useless battery is directly used and again makes battery, the method seems that technique is simple, but be difficult to the useful life of positive plate judge, heavy freshly prepd battery qualification rate will be caused low, cause the huge waste of resource; Patent CN102956936A(mono-kind processes the method for junked-auto dynamic lithium battery lithium iron phosphate cathode material) by hydrometallurgical processes, positive electrode is leached, finally obtain ferric phosphate, iron hydroxide and aluminum hydroxide precipitation, the method complex technical process, acid and alkali consumption is comparatively large, pollution is large, cost intensive, the added value of final products is low, considers that this method does not possess feasibility from the angle of cost; Exemplary process method is reclaimed in the waste and old power ferrous phosphate lithium battery environmental protection of patent CN103825064A(mono-kind) displacement liquid is injected inside battery and again displacement liquid is extracted out and carry out distillation and process; always by innoxious for inside battery electrolyte extraction; the method has feasibility in theory; but in practical operation; inside battery space is very little; and a small amount of solvent injected is difficult to immerse core bag inside completely, and the extraction of solvent is also a stubborn problem.
The problems such as the utilization of resources existed for the existing method of applying waste lithium ionic electrokinetic cell recycling is thorough, treatment process process contamination is large, long flow path, electrolyte cannot reclaim, the present invention proposes the innoxious comprehensive reutilization method of applying waste lithium ionic electrokinetic cell, solving in applying waste lithium ionic electrokinetic cell removal process has valency monomer to utilize, avoid the problem such as secondary pollution, electrolyte recovery, makes whole comprehensive reutilization process obtain good economic benefit and social benefit.
Summary of the invention
The object of the invention is to: for Problems existing in existing applying waste lithium ionic electrokinetic cell recycling process, a kind of method that process route is simply clear, cost recovery is cheap, recovery is complete, recovering effect is good, good in economic efficiency is provided, realize the comprehensive reutilization of applying waste lithium ionic electrokinetic cell, promote the sustainable development of new forms of energy industry.
Enforcement of the present invention mainly comprises the following steps:
1. the innoxious comprehensive reutilization method of applying waste lithium ionic electrokinetic cell, is characterized in that, comprise the following steps:
(1) waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the charging and discharging curve registration rule combo again that is greater than 95%, carry out cascade utilization;
(2) (1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
(3) in oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
(4) heat-treat in the heating furnace core bag of taking-up being placed in 80 ~ 200 DEG C, and the organic solvent of volatilization is driven out of by a kind of gas passed in air, nitrogen, argon gas, or by the mode of vacuum, the gas of volatilization is extracted out;
(5) the organic mixed solvent evaporated effectively reclaims by the method adopting condensation to reclaim, and remaining tail gas adopts adsorbent, eliminates environmental impact;
(6) the core bag that step (4) obtains to be made by hand or anti-up-coiler carries out unreel, isolate positive plate, negative plate and plastic diaphragms;
(7) barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
(8) positive/negative plate that obtains of step (6) respectively in rotary furnace in air atmosphere or under inert atmosphere through 200-600 DEG C of high-temperature process, bonding agent was lost efficacy, is conducive to lower step and is separated;
(9) positive/negative plate after heat treatment is placed in crusher for crushing respectively, fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, recovery negative material powder respectively and reclaims positive electrode powder;
(10) the recovery negative electrode powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use;
(11) the recovery positive powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use.
2. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, is characterized in that: described lithium-ion-power cell comprises ferrous lithium phosphate cathode lithium ion battery, ternary material positive pole lithium ion battery, manganate cathode material for lithium lithium ion battery, lithium titanate material negative electrode lithium ion battery, silicon carbon material negative electrode lithium ion battery, carbon material negative pole lithium ion battery.
3. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that: will add a kind of in 0.5 ~ 8% pitch, phenolic resins or their mixture in the recovery negative electrode powder obtained in step (9), the prior dispersing and dissolving of pitch, phenolic resins forms solution in ethanol, cyclohexanol or its mixed solvent; High-speed stirred makes formation slurry in 1 ~ 6 hour, is warming up to 100 DEG C of solvent flashings, and at 900 ~ 1200 DEG C of carbonization 1 ~ 5h, crushing and classification obtains the negative material repaired.
4. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that: the recovery positive powder obtained in step (9) is carried out elementary analysis, according to analysis result, allocate the component lacked into, then the mode of ball milling or stirring is taked to mix, 600 ~ 1000 DEG C of sintering 3 ~ 12h under suitable atmosphere, crushing and classification obtains the positive electrode repaired.
5. the solution that formed in ethanol, cyclohexanol or its mixed solvent of pitch according to claim 3, the prior dispersing and dissolving of phenolic resins, it is characterized in that: more optimal method adds in this solution by the nano silica fume of 0.5 ~ 10%, to improve the capacity of negative material further.
6. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that, the adsorbent described in step (5) is one or both and above combination in active carbon, activated alumina, molecular sieve, active silica, NaOH solution, sodium bicarbonate solution, sodium carbonate liquor.
7. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, is characterized in that, the adjustment of granularity described in step (10), (11) processing method is the one of ball milling, air-flow crushing, classification.
Compared with prior art, advantage of the present invention is:
1. propose method accurately, to the cell combo utilization again having value in old and useless battery bag, the residual value of old and useless battery bag is utilized and maximizes, decrease the wasting of resources, improve the economic benefit in whole technological procedure.
2. adopt the mode of cutting under the environment of oxygen barrier to achieve being separated of core bag and housing, safe operation process is reliable, the burning that other cutting modes can be avoided to produce or blast; Aluminium alloy, aluminum plastic film and Stainless Steel Shell can be made to be retained preferably, produce and be better worth, the taking-up that core bag also can be complete, is conducive to the classification process of follow-up various types of materials simultaneously.
3. the core bag obtained directly is placed in stove heating evaporation solvent and condensation is reclaimed, solvent can be obtained maximized recycling (directly takes core bag apart on the one hand, solvent will volatilize totally at short notice), on the other hand because directly core bag is evaporated after disassembling aluminum hull, decrease the volatilization that process solvent disassembled by core bag, reduce the harm to human body in subsequent processes, be conducive to the improvement of shopwork environment; It also avoid additive method simultaneously and do not reclaim the secondary pollution to water body, air that electrolyte causes.
4. lithium hexafluoro phosphate fast decoupled in the situation of being heated, the fluoro-gas produced is run out of along with solvent vapo(u)r, by tail gas adsorption agent as the absorption such as active carbon, dilute alkaline soln, avoid the pollution of fluoro-gas to environment, really achieve the harmless treatment of old and useless battery material.
5. the method that Reuse of materials process adopts machinery to be separated, the conductive black in material is preserved preferably, and this reclaims the actual addition of carbon black in positive electrode use procedure by reducing, decrease the dust pollution of carbon black to environment.
6. positive/negative plate pulverizing-sieve-gravity treatment-pulse dust removal technical maturity is reliable, for pure physical process, there is not the consumption of soda acid and the consumption of solvent, dust in simultaneously producing can effectively be reclaimed and be controlled, and avoids in additive method and adopts water, acid, alkali to carry out processing the pollution brought.
7. whole material recovery process is simple, and with low cost, take the full closed cycle of dry method, three waste discharge is zero substantially, and the waste and scrap rate of recovery is high, reclaims positive and negative pole material better performances, good in economic efficiency, is conducive to large-scale application.
Accompanying drawing explanation
The SEM collection of illustrative plates of the lithium iron phosphate cathode material that Fig. 1 repairs
The XRD collection of illustrative plates of the lithium iron phosphate cathode material that Fig. 2 repairs
The grain size analysis collection of illustrative plates of the lithium iron phosphate cathode material that Fig. 3 repairs
The first charge-discharge curve of the lithium iron phosphate cathode material that Fig. 4 repairs
The cycle performance curve of the lithium iron phosphate cathode material that Fig. 5 repairs
Embodiment
Below by embodiment, the present invention is described in detail, example below just meets several examples of the technology of the present invention content, do not illustrate that the present invention is only limitted to the content described in following example, the technical staff in the industry all belongs to content of the present invention according to the product of the claims in the present invention item manufacture.
embodiment 1
(1) the used for electric vehicle waste and old ferrous phosphate lithium ion electrokinetic cell bag (graphite cathode) of one group of 320V60Ah is got, waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the rule that charging and discharging curve registration is greater than 95% is made into the battery pack of 72V100Ah again, the battery of combo is used for low-speed electronic car again;
(2) (1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
(3) in oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
(4) heat-treat in the heating furnace core bag of taking-up being placed in 80 DEG C, and pass into air organic solvent and drive out of;
(5) the organic mixed solvent evaporated effectively reclaims by the method adopting the cooling medium of-10 DEG C to reclaim, and remaining tail gas adopts charcoal absorption;
(6) the core bag that step (4) obtains is made to carry out unreel by hand, isolate positive plate, negative plate and plastic diaphragms;
(7) barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
(8) positive/negative plate that obtains of step (6) respectively in rotary furnace in air atmosphere through 200 DEG C of heat treatments, bonding agent was lost efficacy;
(9) positive/negative plate after heat treatment is placed in crusher for crushing respectively, fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, graphite cathode powder and LiFePO 4 lithium positive powder respectively;
(10) 0.5% pitch is added in the recovery negative electrode powder that step (9) obtains, the prior dispersing and dissolving of pitch forms the solution (containing the nano silica fume of 0.5% in this solution) of 20% in ethanol, high-speed stirred makes formation slurry in 1 hour, be warming up to 100 DEG C of solvent flashings, at 900 DEG C of carbonization 1h, then ball mill grinding obtains the negative material of reparation;
(11) the recovery positive powder that step (9) obtains carries out elementary analysis, according to analysis result, allocates the NH of lack 5% into
4h
2pO4, then takes ball milling method to mix, under an argon atmosphere 600 DEG C of sintering 12h, and crushing and classification obtains the positive electrode repaired.Fig. 1 is the SEM collection of illustrative plates of the lithium iron phosphate cathode material repaired, and Fig. 2 is the XRD collection of illustrative plates of the lithium iron phosphate cathode material repaired, and Fig. 3 is the grain size analysis collection of illustrative plates of the lithium iron phosphate cathode material repaired;
(12) positive and negative pole material obtained in (10), (11) traditionally lithium ion battery manufacture process is made into lithium ion battery and evaluates and tests, and its half-cell positive electrode capacity reaches the full battery capacity 120mAh/g of 132mAh/g(), capacity of negative plates reaches 381mAh/g.Fig. 4 is the first charge-discharge curve of the lithium iron phosphate cathode material repaired, and Fig. 5 is the cycle performance curve of the lithium iron phosphate cathode material repaired.
embodiment 2
(1) the used for electric vehicle waste and old ternary lithium-ion-power cell bag (lithium titanate anode) of one group of 370V100Ah is got, waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the rule that charging and discharging curve registration is greater than 95% is made into the battery pack of 74V160Ah again, the battery of combo is used for low-speed electronic car again;
(2) (1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
(3) in oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
(4) heat-treat in the heating furnace core bag of taking-up being placed in 150 DEG C, and pass into nitrogen the organic solvent of volatilization is driven out of;
(5) the organic mixed solvent evaporated effectively reclaims by the method adopting-20 DEG C of condensations to reclaim, and remaining tail gas by 5% sodium hydroxide solution, then passes through 5A type molecular sieve adsorption;
(6) use anti-up-coiler to carry out unreel the core bag that step (4) obtains, isolate positive plate, negative plate and plastic diaphragms;
(7) barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
(8) positive/negative plate that obtains of step (6) respectively in rotary furnace under argon gas through 400 DEG C of high-temperature process, bonding agent was lost efficacy, is conducive to lower step and is separated;
(9) positive/negative plate after heat treatment is placed in crusher for crushing respectively, fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, recovery negative material powder respectively and reclaims positive electrode powder;
(10) the recovery negative electrode powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use;
(11) the recovery positive powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use.
embodiment 3
(1) the waste lithium manganese oxide electrokinetic cell bag (graphite cathode) used for electric vehicle of one group of 370V100Ah is got, waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the rule that charging and discharging curve registration is greater than 95% is made into the battery pack of 74V160Ah again, the battery of combo is used for low-speed electronic car again;
(2) (1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
(3) in oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
(4) heat-treat in the heating furnace core bag of taking-up being placed in 200 DEG C, and by the mode of vacuum, the gas of volatilization is extracted out;
(5) the organic mixed solvent evaporated effectively reclaims by the method adopting-10 DEG C of condensations to reclaim, and remaining tail gas is first adsorbed by sodium bicarbonate solution, then is adsorbed by activated alumina;
(6) the core bag that step (4) obtains is made to carry out unreel by hand, isolate positive plate, negative plate and plastic diaphragms;
(7) barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
(8) positive/negative plate that obtains of step (6) respectively in rotary furnace under an argon atmosphere through 600 DEG C of high-temperature process, bonding agent was lost efficacy, is conducive to lower step and is separated;
(9) positive/negative plate after heat treatment is placed in crusher for crushing respectively, fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, recovery negative material powder respectively and reclaims positive electrode powder;
(10) 8% phenolic resins is added in the recovery negative electrode powder that step (9) obtains, the prior dispersing and dissolving of phenolic resins forms the solution (containing the nano silica fume of 10% in this solution) of 20% in the mixed solvent of ethanol and ring ethanol 1:1, high-speed stirred makes formation slurry in 6 hours, be warming up to 100 DEG C of solvent flashings, at 1200 DEG C of carbonization 5h, then air-flow crushing obtains the negative material of reparation;
(11) the recovery positive powder that step (9) obtains carries out elementary analysis, according to analysis result, allocates the MnO of lack 6% into
2, then take agitating mode to mix, in air atmosphere 800 DEG C of sintering 8h, ball mill grinding, classification obtain the positive electrode repaired.
embodiment 4
(1) the used for electric vehicle waste and old ternary electrokinetic cell bag (silicon-carbon cathode) of one group of 300V100Ah is got, waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the rule that charging and discharging curve registration is greater than 95% is made into the battery pack of 72V160Ah again, the battery of combo is used for low-speed electronic car again;
(2) (1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
(3) in oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
(4) heat-treat in the heating furnace core bag of taking-up being placed in 200 DEG C, and pass into argon gas the organic solvent of volatilization is driven out of;
(5) the organic mixed solvent evaporated effectively reclaims by the method adopting-10 DEG C of condensations to reclaim, and remaining tail gas is first adsorbed by sodium carbonate liquor, then is adsorbed by active silica;
(6) the core bag that step (4) obtains is made to carry out unreel by hand, isolate positive plate, negative plate and plastic diaphragms;
(7) barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
(8) positive/negative plate that obtains of step (6) respectively in rotary furnace in a nitrogen atmosphere through 300 DEG C of high-temperature process, bonding agent was lost efficacy, is conducive to lower step and is separated;
(9) positive/negative plate after heat treatment is placed in crusher for crushing respectively, fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, recovery negative material powder respectively and reclaims positive electrode powder;
(10) 3% phenolic resins is added in the recovery negative electrode powder that step (9) obtains, the prior dispersing and dissolving of phenolic resins forms the solution (containing the nano silica fume of 3% in this solution) of 10% in alcohol solvent, high-speed stirred makes formation slurry in 4 hours, be warming up to 100 DEG C of solvent flashings, at 1000 DEG C of carbonization 3h, then air-flow crushing obtains the negative material of reparation;
(11) the recovery positive powder that step (9) obtains carries out elementary analysis, according to analysis result, allocates the MnO of lack 3% into
2, then take ball milling method to mix, in air atmosphere 1000 DEG C of sintering 3h, ball mill grinding, classification obtain the positive electrode repaired.
Claims (7)
1. the innoxious comprehensive reutilization method of applying waste lithium ionic electrokinetic cell, is characterized in that, comprise the following steps:
Waste and old electrokinetic cell bag is disassembled, measure each battery performance, capacity is at former nominal capacity more than 60% and internal resistance is no more than the cell of former nominal value 3 times, according within volume error ± 2%, within internal resistance error ± 30%, within leakage current error ± 20% and the charging and discharging curve registration rule combo again that is greater than 95%, carry out cascade utilization;
(1) is eliminated the waste and old electrokinetic cell got off and carry out discharge process, be discharged to voltage < 0.5V;
In oxygen barrier environment, adopt the mode of cutting to be cut along battery top by battery, cut off the connection of core bag and terminal, open battery and take out core bag;
Heat-treat in the heating furnace core bag of taking-up being placed in 80 ~ 200 DEG C, and the organic solvent of volatilization is driven out of by a kind of gas passed in air, nitrogen, argon gas, or by the mode of vacuum, the gas of volatilization is extracted out;
The organic mixed solvent evaporated effectively reclaims by the method adopting condensation to reclaim, and remaining tail gas adopts adsorbent, eliminates environmental impact;
The core bag that step (4) obtains to be made by hand or anti-up-coiler carries out unreel, isolate positive plate, negative plate and plastic diaphragms;
The barrier film that step (6) obtains carries out briquetting, fusing, granulation process, obtains plastic grain;
The positive/negative plate that step (6) obtains respectively in rotary furnace in air atmosphere or under inert atmosphere through 200-600 DEG C of high-temperature process, bonding agent was lost efficacy, is conducive to lower step and is separated;
Positive/negative plate after heat treatment is placed in crusher for crushing respectively, and fluidization sorting bed carries out gravity separation, and tail gas is collected by pulsed dedusting, obtains copper powder, aluminium powder, recovery negative material powder respectively and reclaims positive electrode powder;
The recovery negative electrode powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use;
The recovery positive powder that step (9) obtains returns after carrying out granularity adjustment process and does battery use.
2. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, is characterized in that: described lithium-ion-power cell comprises ferrous lithium phosphate cathode lithium ion battery, ternary material positive pole lithium ion battery, manganate cathode material for lithium lithium ion battery, lithium titanate material negative electrode lithium ion battery, silicon carbon material negative electrode lithium ion battery, carbon material negative pole lithium ion battery.
3. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that: will add a kind of in 0.5 ~ 8% pitch, phenolic resins or their mixture in the recovery negative electrode powder obtained in step (9), the prior dispersing and dissolving of pitch, phenolic resins forms solution in ethanol, cyclohexanol or its mixed solvent; High-speed stirred makes formation slurry in 1 ~ 6 hour, is warming up to 100 DEG C of solvent flashings, and at 900 ~ 1200 DEG C of carbonization 1 ~ 5h, crushing and classification obtains the negative material repaired.
4. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that: the recovery positive powder obtained in step (9) is carried out elementary analysis, according to analysis result, allocate the component lacked into, then the mode of ball milling or stirring is taked to mix, 600 ~ 1000 DEG C of sintering 3 ~ 12h under suitable atmosphere, crushing and classification obtains the positive electrode repaired.
5. the solution that formed in ethanol, cyclohexanol or its mixed solvent of pitch according to claim 3, the prior dispersing and dissolving of phenolic resins, it is characterized in that: more optimal method adds in this solution by the nano silica fume of 0.5 ~ 10%, to improve the capacity of negative material further.
6. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, it is characterized in that, the adsorbent described in step (5) is one or both and above combination in active carbon, activated alumina, molecular sieve, active silica, NaOH solution, sodium bicarbonate solution, sodium carbonate liquor.
7. the innoxious comprehensive reutilization method of a kind of applying waste lithium ionic electrokinetic cell according to claim 1, is characterized in that, the adjustment of granularity described in step (10), (11) processing method is the one of ball milling, air-flow crushing, classification.
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