CN103199320B - Method for recycling nickel-cobalt-manganese ternary anode material - Google Patents
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- CN103199320B CN103199320B CN201310104022.8A CN201310104022A CN103199320B CN 103199320 B CN103199320 B CN 103199320B CN 201310104022 A CN201310104022 A CN 201310104022A CN 103199320 B CN103199320 B CN 103199320B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/006—Compounds containing, besides nickel, two or more other elements, with the exception of oxygen or hydrogen
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention relates to a method for recycling a nickel-cobalt-manganese ternary anode material, belongs to the technical field of recovery of waste cells, and solves the technical problem that a method for recycling the nickel-cobalt-manganese ternary anode material is provided. The method for recycling the nickel-cobalt-manganese ternary anode material comprises a step of removing a binder from the positiveplate of the nickel-cobalt-manganese ternary material by thermal treatment, and the method for removing the binder in the positive plate of the nickel-cobalt-manganese ternary material is thermal treatment of the positive plate of the nickel-cobalt-manganese ternary anode material at 400-1000 DEG C for 0.5-5 hours.
Description
Technical field
The present invention relates to the method that nickel-cobalt-manganternary ternary anode material is recycled, belong to old and useless battery recovery technology field.
Background technology
Nickel-cobalt-manganternary ternary anode material system is developed by binary Ni-Mn sill, and calendar year 2001 OhZuku and Makimura has synthesized the trielement composite material LiNi of nNi:nCo:nMn=1:1:1 first
1/3co
1/3mn
1/3o
2, meanwhile Canadian Dahn etc. have studied the impact of change of component on positive pole material crystal structure, capacity, multiplying power discharging and thermal stability.Although LiNi
1/3co
1/3mn
1/3o
2search time is not long, but because of itself and LiCoO
2there is analog structure, possess good Research foundation, be namely considered to most possibly replace LiCoO once proposition
2, obtain national governments and support energetically.
Tertiary cathode material can be used for digital communication class battery, Notebook Battery, power tool battery, power bicycle/automobile batteries etc.In communication battery, in nearest 3-5 years, the leading position of cobalt acid lithium will weaken gradually, and may occur the phenomenon that cobalt acid lithium and nickel-cobalt-manganternary ternary anode material coexist, after 5 years, may be the epoch that nickel-cobalt-manganese ternary material is dominated exclusively.In field of power tools, nickel-cobalt-manganese ternary material has high energy density, good high rate during charging-discharging, outstanding cycle performance and security performance, likely becomes main positive electrode.
At present, the existing relevant report recycled about nickel-cobalt-manganternary ternary anode material.As: CN200810198972 to application discloses a kind of be the method that nickle cobalt lithium manganate prepared by raw material with waste and old lithium ion battery.Its main feature is: selecting cell positive material to be the waste and old lithium ion battery of nickle cobalt lithium manganate, lithium nickel cobalt dioxide etc. is raw material, through disassembling, sorting, pulverizing, after the preliminary treatment such as screening, adopt high temperature to remove binding agent, NaOH except after the techniques such as aluminium again, obtain nickeliferous, cobalt, manganese inactivation positive electrode; Then adopt that sulfuric acid and hydrogen peroxide system leach, P2O4 abstraction impurity removal, obtain pure nickel, cobalt, manganese solution, allocate suitable manganese sulfate, nickelous sulfate or cobaltous sulfate into, make nickel in solution, cobalt, manganese element mol ratio be 1:1:1; Adopt ammonium carbonate adjust ph subsequently, form nickel cobalt manganese carbonate precursor, then allocate appropriate lithium carbonate into, the activated nickle cobalt lithium manganate battery material of high temperature sintering synthesis tool.And for example: CN200710308154 discloses a kind of from containing the method reclaiming noble metal the battery slag of Co, Ni, Mn, it is for carrying out leaching to comprising the hydrochloric acid solution containing the roughly concentration of more than the lithium cell slag 250g/l of the lithium acid metal salt of Co, Ni and Mn of equivalent, or carry out heating leaching process with the sulfuric acid solution of the concentration of more than 200g/l, with acidic extractant, solvent extraction is carried out to leachate, extract roughly 100% of Mn and Co, generate the solution containing respective metal, from these solution, reclaim this metal.
Said method achieves the recycling of nickel-cobalt-manganternary ternary anode material, but by pulverizing, sieving separating nickel cobalt manganic acid lithium and aluminium foil, separating effect is bad; Adopt carbonate precipitation method to obtain nickel cobalt manganese carbonate precursor, easily cause the segregation of component in preparation process, the homogeneity of each Elemental redistribution of oxide can not be ensured, have impact on positive electrode chemical property; Organic solvent is adopted easily to cause secondary pollution.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method that nickel-cobalt-manganternary ternary anode material is recycled.
The method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled, comprise and remove binding agent step from the heat treatment of cobalt nickel lithium manganate ternary material positive plate, in its removal cobalt nickel lithium manganate ternary material positive plate, binding agent method is: by cobalt nickel lithium manganate ternary material positive plate in 400 ~ 1000 DEG C of heat treatment 0.5 ~ 5h.
Wherein, as preferred technical scheme, the method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled comprises the steps:
A, waste lithium cell remaining capacity to be discharged, then disassemble battery, take out cobalt nickel lithium manganate ternary material positive plate;
B, by cobalt nickel lithium manganate ternary material positive plate in 400 ~ 1000 DEG C of vacuum baking 0.5 ~ 5h, then Ore Leaching is added, leaching process adds a small amount of nickel, cobalt, the manganese that reducing agent is used for being oxidized in reducing roasting process, obtains the mixed solution of nickel salt, cobalt salt, manganese salt, aluminium salt and lithium salts; Wherein, the consumption of reducing agent is that a small amount of nickel of oxidation, cobalt, manganese are reduced, and the reducing agent adopted is preferably at least one in sodium thiosulfate, hydrogen peroxide;
C, adjustment mixed solution pH value 3 ~ 9, preferably regulate mixed solution pH value to 3 ~ 7, make aluminum precipitation in solution, then filter and remove aluminium; Wherein, the conventional alkali lye such as NaOH, potassium hydroxide, lithium hydroxide can be adopted to regulate mixed solution pH value;
D, according to nickel cobalt Fe content in step c gained solution, add appropriate nickel cobalt mn sulphate and regulate nickel in solution, cobalt, manganese mol ratio to be 0.8 ~ 1.2:0.8 ~ 1.2:0.8 ~ 1.2;
E, add NaOH as precipitation reagent, add nickel, cobalt, manganese equal molar amount ammoniacal liquor as compounding ingredient, regulate solution ph to be 10 ~ 12, precipitation obtains nickel-cobalt-manganese ternary material precursor, filter, obtain lithium salt solution, lithium salt solution obtains lithium carbonate through purification precipitation;
F, nickel-cobalt-manganese ternary material precursor and lithium carbonate mixs by weight 2.4 ~ 2.6:1, then in 750 ~ 950 DEG C of calcining 12 ~ 24h, cool, obtain nickle cobalt lithium manganate.
Said method adopts acid+reducing agent system to leach, and NaOH is precipitation reagent synthesis nickle cobalt lithium manganate ternary anode material precursor, avoids generating Mn
3+or Mn (MnOOH)
4+(MnO
2), properties of product are reclaimed in impact, can not cause the segregation of component, ensure that the homogeneity of each Elemental redistribution of oxide, thus guarantee positive electrode stable electrochemical property in preparation process.
Further, the method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled, in its b step, as fruit acid concentration is too high, then nickel, cobalt, manganese are oxidizable; As fruit acid concentration is too low, then the leaching rate of nickel, cobalt, manganese is on the low side, considers above-mentioned situation, preferably adopts that concentration is the sulfuric acid of 10 ~ 15wt%, hydrochloric acid or nitric acid leaches.
Further, in order to improve positive electrode chemical property, the method that above-mentioned nickel-cobalt-manganternary ternary anode material is recycled, in its Step d, preferably regulates the nickel in solution, cobalt, manganese mol ratio to be 1:1:1.
Wherein, the method that above-mentioned nickel-cobalt-manganternary ternary anode material is recycled, in order to make gained ternary material electrical property best, in its step e, when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, preferably also controlling reaction temperature is 40 ~ 90 DEG C.
The present invention has following beneficial effect: the inventive method achieves the recycling of nickle cobalt lithium manganate, eliminate the defect that existing recovery method exists, both be conducive to the sustainable development of industry on long terms, and indirectly reduced again the cost of nickel-cobalt-manganese ternary material, be conducive to popularizing of material.
Embodiment
The method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled, comprise and remove binding agent step from the heat treatment of cobalt nickel lithium manganate ternary material positive plate, in its removal cobalt nickel lithium manganate ternary material positive plate, binding agent method is: by cobalt nickel lithium manganate ternary material positive plate in 400 ~ 1000 DEG C of heat treatment 0.5 ~ 5h.
Wherein, as preferred technical scheme, the method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled comprises the steps:
A, waste lithium cell remaining capacity to be discharged, then disassemble battery, take out cobalt nickel lithium manganate ternary material positive plate;
B, by cobalt nickel lithium manganate ternary material positive plate in 400 ~ 1000 DEG C of vacuum baking 0.5 ~ 5h, then Ore Leaching is added, leaching process adds a small amount of nickel, cobalt, the manganese that reducing agent is used for being oxidized in reducing roasting process, obtains the mixed solution of nickel salt, cobalt salt, manganese salt, aluminium salt and lithium salts; Wherein, the consumption of reducing agent is that a small amount of nickel of oxidation, cobalt, manganese are reduced, and the reducing agent adopted is preferably at least one in sodium thiosulfate, hydrogen peroxide;
C, adjustment mixed solution pH value 3 ~ 9, preferably regulate mixed solution pH value to 3 ~ 7, make aluminum precipitation in solution, then filter and remove aluminium; Wherein, the conventional alkali lye such as NaOH, potassium hydroxide, lithium hydroxide can be adopted to regulate mixed solution pH value;
D, according to nickel cobalt Fe content in step c gained solution, add appropriate nickel cobalt mn sulphate and regulate nickel in solution, cobalt, manganese mol ratio to be 0.8 ~ 1.2:0.8 ~ 1.2:0.8 ~ 1.2;
E, add NaOH as precipitation reagent, add nickel, cobalt, manganese equal molar amount ammoniacal liquor as compounding ingredient, regulate solution ph to be 10 ~ 12, precipitation obtains nickel-cobalt-manganese ternary material precursor, filter, obtain lithium salt solution, lithium salt solution obtains lithium carbonate through purification precipitation;
F, nickel-cobalt-manganese ternary material precursor and lithium carbonate mixs by weight 2.4 ~ 2.6:1, then in 750 ~ 950 DEG C of calcining 12 ~ 24h, cool, obtain nickle cobalt lithium manganate.
Said method adopts acid+reducing agent system to leach, and NaOH is precipitation reagent synthesis nickle cobalt lithium manganate ternary anode material precursor, avoids generating Mn
3+or Mn (MnOOH)
4+(MnO
2), properties of product are reclaimed in impact, can not cause the segregation of component, ensure that the homogeneity of each Elemental redistribution of oxide, thus guarantee positive electrode stable electrochemical property in preparation process.
Further, the method that nickel-cobalt-manganternary ternary anode material of the present invention is recycled, in its b step, as fruit acid concentration is too high, then nickel, cobalt, manganese are oxidizable; As fruit acid concentration is too low, then the leaching rate of nickel, cobalt, manganese is on the low side, considers above-mentioned situation, preferably adopts that concentration is the sulfuric acid of 10 ~ 15wt%, hydrochloric acid or nitric acid leaches.
Further, in order to improve positive electrode chemical property, the method that above-mentioned nickel-cobalt-manganternary ternary anode material is recycled, in its Step d, preferably regulates the nickel in solution, cobalt, manganese mol ratio to be 1:1:1.
Wherein, the method that above-mentioned nickel-cobalt-manganternary ternary anode material is recycled, in order to make gained ternary material electrical property best, in its step e, when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, preferably also controlling reaction temperature is 40 ~ 90 DEG C.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 1000 DEG C of calcining 0.5h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the sulfuric acid leaching of 10wt%, leaching process adds sodium thiosulfate 1kg, obtains nickelous sulfate, cobaltous sulfate, manganese sulfate, aluminum sulfate and lithium sulfate mixed solution after leaching through filtering.Regulate mixed solution pH value 4.5, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickelous sulfate, cobaltous sulfate, manganese sulfate and lithium sulfate mixed solution.Add nickel cobalt mn sulphate in the solution and nickel cobalt manganese mol ratio is adjusted to 1:1:1, then NaOH is added as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 40 DEG C, pH value 12, precipitation obtains nickel-cobalt-manganese ternary material precursor, is separated by filtration, obtains lithium sulfate solution.
Nickel-cobalt-manganese ternary material precursor mixes with 34.7kg lithium carbonate ball milling, and mixture is placed in calciner, and in 750 DEG C of calcinings, constant temperature 12 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 1:
Table 1
Embodiment 2 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 700 DEG C of roasting 3h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the sulfuric acid leaching of 15wt%, leaching process adds sodium thiosulfate 0.8kg, obtains nickelous sulfate, cobaltous sulfate, manganese sulfate, aluminum sulfate and lithium sulfate mixed solution after leaching through filtering.Regulate mixed solution pH value 5, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickelous sulfate, cobaltous sulfate, manganese sulfate and lithium sulfate mixed solution.Add nickel cobalt mn sulphate in the solution and nickel cobalt manganese mol ratio is adjusted to 0.9:1:0.9, then NaOH is added as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 60 DEG C, pH value 10, precipitation obtains nickel-cobalt-manganese ternary material precursor, is separated by filtration, obtains lithium sulfate solution.
Nickel-cobalt-manganese ternary material precursor mixes with 34kg lithium carbonate ball milling, and mixture is placed in calciner, and in 950 DEG C of calcinings, constant temperature 24 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 2:
Table 2
Embodiment 3 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 400 DEG C of roasting 5h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the sulfuric acid leaching of 12wt%, leaching process adds sodium thiosulfate 1.2kg, obtains nickelous sulfate, cobaltous sulfate, manganese sulfate, aluminum sulfate and lithium sulfate mixed solution after leaching through filtering.Regulate mixed solution pH value 6, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickelous sulfate, cobaltous sulfate, manganese sulfate and lithium sulfate mixed solution.Add nickel cobalt mn sulphate in the solution and nickel cobalt manganese mol ratio is adjusted to 1:0.9:1, then NaOH is added as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 45 DEG C, pH value 11, precipitation obtains nickel-cobalt-manganese ternary material precursor, is separated by filtration, obtains lithium sulfate solution.
Nickel-cobalt-manganese ternary material precursor mixes with 35kg lithium carbonate ball milling, and mixture is placed in calciner, and in 850 DEG C of calcinings, constant temperature 15 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 3:
Table 3
Embodiment 4 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 600 DEG C of roasting 4h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the hydrochloric acid leaching of 12wt%, leaching process adds hydrogen peroxide 2.5kg, obtains nickel chloride, cobalt chloride, manganese chloride, aluminium chloride and lithium chloride mixed solution after leaching through filtering.Regulate mixed solution pH value 6, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickel chloride, cobalt chloride, manganese chloride and lithium chloride mixed solution.Add nickel cobalt-manganese salt in the solution and nickel cobalt manganese mol ratio is adjusted to 1:0.9:1, then add NaOH as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 45 DEG C, pH value 11, precipitation obtains nickel-cobalt-manganese ternary material precursor, be separated by filtration, obtain lithium chloride solution.
Nickel-cobalt-manganese ternary material precursor mixes with 35kg lithium carbonate ball milling, and mixture is placed in calciner, and in 850 DEG C of calcinings, constant temperature 15 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 3:
Table 3
Embodiment 5 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 900 DEG C of roasting 1h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the nitric acid leaching of 12wt%, leaching process adds hydrogen peroxide 2.5kg, obtains nickel nitrate, cobalt nitrate, manganese nitrate, aluminum nitrate and lithium nitrate mixed solution after leaching through filtering.Regulate mixed solution pH value 6, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickel nitrate, cobalt nitrate, manganese nitrate and lithium nitrate mixed solution.Add nickel cobalt-manganese salt in the solution and nickel cobalt manganese mol ratio is adjusted to 1:0.9:1, then add NaOH as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 45 DEG C, pH value 11, precipitation obtains nickel-cobalt-manganese ternary material precursor, be separated by filtration, obtain lithium nitrate solution.
Nickel-cobalt-manganese ternary material precursor mixes with 35kg lithium carbonate ball milling, and mixture is placed in calciner, and in 850 DEG C of calcinings, constant temperature 15 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 3:
Table 3
Embodiment 6 adopts the inventive method to recycle nickel-cobalt-manganternary ternary anode material
Discharged by waste nickel cobalt manganic acid lithium battery remaining capacity, disassemble battery, take out positive plate, battery case is pressed the classification such as aluminum hull, box hat, plastics and is reclaimed; By nickle cobalt lithium manganate positive plate through 800 DEG C of roasting 1.5h.
Get the nickle cobalt lithium manganate positive plate 100kg after calcining, adopt the sulfuric acid leaching of 12wt%, leaching process adds hydrogen peroxide 2.5kg, obtains nickelous sulfate, cobaltous sulfate, manganese sulfate, aluminum sulfate and lithium sulfate mixed solution after leaching through filtering.Regulate mixed solution pH value 6, generate aluminum hydroxide precipitation, filter and remove aluminium hydroxide, obtain nickelous sulfate, cobaltous sulfate, manganese sulfate and lithium sulfate mixed solution.Add nickel cobalt mn sulphate in the solution and nickel cobalt manganese mol ratio is adjusted to 1:0.9:1, then NaOH is added as precipitation reagent, add proper ammonia as compounding ingredient, control reaction temperature 45 DEG C, pH value 11, precipitation obtains nickel-cobalt-manganese ternary material precursor, is separated by filtration, obtains lithium sulfate solution.
Nickel-cobalt-manganese ternary material precursor mixes with 35kg lithium carbonate ball milling, and mixture is placed in calciner, and in 850 DEG C of calcinings, constant temperature 15 hours, naturally cools in stove, obtain nickle cobalt lithium manganate tertiary cathode material.Lithium sulfate solution adds sodium carbonate precipitation and obtains lithium carbonate after concentrated.Reclaim obtained nickle cobalt lithium manganate tertiary cathode material chemical property as shown in table 3:
Table 3
Claims (9)
1. the method for nickel-cobalt-manganternary ternary anode material recycling, is characterized in that comprising the steps:
A, waste lithium cell remaining capacity to be discharged, then disassemble battery, take out cobalt nickel lithium manganate ternary material positive plate;
B, by cobalt nickel lithium manganate ternary material positive plate in 400 ~ 1000 DEG C of vacuum baking 0.5 ~ 5h, then Ore Leaching is added, leaching process adds a small amount of nickel, cobalt, the manganese that reducing agent is used for being oxidized in reducing roasting process, obtains the mixed solution of nickel salt, cobalt salt, manganese salt, aluminium salt and lithium salts;
PH value to 3 ~ 9 of c, adjustment mixed solution, make aluminum precipitation in solution, then filter and remove aluminium;
D, according to nickel cobalt Fe content in mixed solution, add appropriate nickel cobalt-manganese salt and regulate nickel in solution, cobalt, manganese mol ratio to be 0.8 ~ 1.2:0.8 ~ 1.2:0.8 ~ 1.2;
E, add NaOH as precipitation reagent, add nickel, cobalt, manganese equal molar amount ammoniacal liquor as compounding ingredient, regulate solution ph to be 10 ~ 12, precipitation obtains nickel-cobalt-manganese ternary material precursor, filter, obtain lithium salt solution, lithium salt solution obtains lithium carbonate through purification precipitation;
F, nickel-cobalt-manganese ternary material precursor and lithium carbonate mixs by weight 2.4 ~ 2.6:1, then in 750 ~ 950 DEG C of calcining 12 ~ 24h, cool, obtain nickle cobalt lithium manganate.
2. the method recycled of nickel-cobalt-manganternary ternary anode material according to claim 1, is characterized in that in b step, adopts that concentration is the sulfuric acid of 10 ~ 15wt%, hydrochloric acid or nitric acid leaches; Described reducing agent is a kind of in sodium thiosulfate or hydrogen peroxide.
3. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 1 and 2, is characterized in that: in step c, regulates pH value to 3 ~ 7 of mixed solution.
4. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 1 and 2, is characterized in that: in Step d, regulates the nickel in solution, cobalt, manganese mol ratio to be 1:1:1.
5. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 3, is characterized in that: in Step d, regulates the nickel in solution, cobalt, manganese mol ratio to be 1:1:1.
6. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 1 and 2, is characterized in that: in step e, and when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, also controlling reaction temperature is 40 ~ 90 DEG C.
7. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 3, is characterized in that: in step e, and when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, also controlling reaction temperature is 40 ~ 90 DEG C.
8. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 4, is characterized in that: in step e, and when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, also controlling reaction temperature is 40 ~ 90 DEG C.
9. the method for nickel-cobalt-manganternary ternary anode material recycling according to claim 5, is characterized in that: in step e, and when coprecipitated nickel hydroxide cobalt-manganese ternary material precursor, also controlling reaction temperature is 40 ~ 90 DEG C.
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| CN201310104022.8A CN103199320B (en) | 2013-03-28 | 2013-03-28 | Method for recycling nickel-cobalt-manganese ternary anode material |
| PCT/CN2014/074157 WO2014154152A1 (en) | 2013-03-28 | 2014-03-27 | Method for recycling nickel-cobalt-manganese ternary anode material |
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| CN103199320B (en) * | 2013-03-28 | 2015-05-27 | 四川天齐锂业股份有限公司 | Method for recycling nickel-cobalt-manganese ternary anode material |
| CN103606651A (en) * | 2013-12-02 | 2014-02-26 | 河南师范大学 | Method for preparing lithium nickelate cobaltate manganate cathode material by taking waste lithium ion batteries as raw material |
| CN104600284B (en) * | 2015-01-15 | 2017-01-11 | 兰州理工大学 | Method for regenerating positive active material in spent lithium manganate lithium ion battery |
| CN104659438B (en) * | 2015-02-11 | 2017-03-01 | 江门市芳源环境科技开发有限公司 | A kind of method that utilization refuse battery prepares ternary anode material precursor |
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