CN107611515A - The active substance of lithium ion battery anode molten and its circulation utilization method of acid and equipment - Google Patents

The active substance of lithium ion battery anode molten and its circulation utilization method of acid and equipment Download PDF

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Publication number
CN107611515A
CN107611515A CN201710985506.6A CN201710985506A CN107611515A CN 107611515 A CN107611515 A CN 107611515A CN 201710985506 A CN201710985506 A CN 201710985506A CN 107611515 A CN107611515 A CN 107611515A
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acid
pump
solution
stillpot
sour
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CN201710985506.6A
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Inventor
刘元龙
刘道坦
夏诗忠
邓凯
刘长来
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Camel Group Wuhan Optics Valley R & D Center Co Ltd
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Camel Group Wuhan Optics Valley R & D Center Co Ltd
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Priority to CN201710985506.6A priority Critical patent/CN107611515A/en
Publication of CN107611515A publication Critical patent/CN107611515A/en
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/84Recycling of batteries or fuel cells

Abstract

A kind of sour molten and its circulation utilization method of active substance of lithium ion battery anode and equipment, the transfer box for containing positive active material is immersed into sour fluid bowl, dissolves positive active material;Pump adds sodium hydroxide solution, precipitate phosphoric acid iron into stillpot to stillpot;Adjust Ni in material:Co:The ratio between Mn amount of substance;Material is added into sodium hydrate aqueous solution, ammoniacal liquor, carries out coprecipitation reaction, by filter press press filtration, obtains nickel-cobalt-manganese ternary hydroxide presoma and sodium salt solution respectively, sodium salt solution pump to adjustment tank is standby after supplement sodium hydroxide into adjustment tank.The acid solution JUMPS Automated Supplemental System of the pH value of the infusion solution of monitoring in real time of the invention, reduces acid solution volatilization harm to caused by the health of environment and producers, positive active material is fully dissolved while ensure that dissolved efficiency is maintained in higher level;The technique recycled to inorganic acid excessive in filtrate, realize few discharge of acidleach process, or even zero-emission.

Description

The active substance of lithium ion battery anode molten and its circulation utilization method of acid and equipment
Technical field
The present invention relates to the technical field of energy-conserving and environment-protective, more particularly to a kind of processing method of used Li ion cell and Equipment.
Background technology
Lithium ion battery is widely used in various consumer electronics product and electric automobile fields, causes the metals such as lithium and cobalt Resources requirement increase sharply, explore rational recovery method, realize to waste and old lithium ion battery reclaim and recycle be slow Resource anxiety is solved, eliminates the effective ways of environmental pollution.
After having carried out discharging to used Li ion cell, the pretreatment such as disassemble, according to the master employed in removal process Key technology is wanted, the recycling treatment process of useless lithium battery can be divided into pyrogenic process and wet method this two major class.
Pyrogenic process, i.e., plastic casing and metal shell are directly abolished using the method for high-temperature process, then using flotation, precipitation The methods of obtain metallic compound.The method technique is relatively easy, but higher there is also energy consumption is heat-treated, in electrolyte and electrode Other compositions are changed into the gases such as carbon dioxide and other harmful components by burning(Such as phosphorus pentoxide), can cause secondary Pollution.
Wet method, i.e., plastics, metal shell first are abolished using mechanical means, powder is then obtained using the process such as crushing and screening Shape or granular lithium ion battery waste material, reuse Ore Leaching, make the valuable metals such as lithium contained therein, nickel, cobalt, manganese, iron first Element is dissolved in solution and metal salt solution corresponding to obtaining, and metal compound is obtained by the methods of precipitation, ion exchange, absorption Thing, the method is higher to recovery rate of valuable metals, and operating condition is gentle, and environmental pollution is smaller, turns at present both at home and abroad The widely used method of researcher.Waste and old lithium ion battery leaching agent used when leaching is typically inorganic acid, such as HCl, HNO3 And H2SO4.With the continuous dissolving of positive active material during hydrometallurgic recovery, mineral acid content is constantly reducing in solution, if Acid solution can not obtain appropriate supplement, make the rate of dissolution of positive active material gradually reduce.In addition in precipitation separation process The hydrometallurgic recovery technology of middle waste and old lithium ion battery is all to focus on the separation and recovery of valuable metal salt, have ignored excess therein Inorganic acid solution recycling in technical process, causes the secondary pollution of environment and the waste of resource.
Contestabile M. are in article within 2001《A laboratory-scale lithium-ion battery recycling process》It is middle to propose using HCl dissolvings LiCoO2, but do not propose the circulation profit of excessive sodium salt cleaner liquid Use method.
Castillo S. are in article within 2002《Advances in the recovering of spent lithium battery compounds》It is middle to use HNO3Leach Li+、Fe3+、Ni2+、Co2+And Mn3+Ion, removal process is not also to sodium Salt cleaner liquid is recycled.
Zhang Yongxiang in 2013 et al. patent《A kind of method that lithium is separated and recovered from waste and old lithium ion battery》Middle use Sulfuric acid and hydrogen peroxide dissolving crush after lithium ion battery cell, it is right after the obtained adjusted pH value precipitation of metal salts of solution Obtained filtrate patent is without reference to circulation utilization method.
Above prior art existing automaticity in lithium ion battery hydrometallurgic recovery is not high, contains sodium salt filtering The problems such as liquid can not be utilized rationally, acid solution volatilization endangers to caused by the health of environment and producers.
The content of the invention
The purpose of the present invention is in order to solve the above-mentioned deficiency of prior art, there is provided one kind can improve positive active material The sour molten and its circulation utilization method of active substance of lithium ion battery anode of hour dissolution rate, this method monitor infusion solution in real time PH value acid solution JUMPS Automated Supplemental System, reduce acid solution volatilization to caused by the health of environment and producers harm, Positive active material is fully dissolved while ensure that dissolved efficiency is maintained in higher level;Additionally establish precipitation metal Filtrate after salt is transmitted back to pickling tank by the road, the technique recycled to inorganic acid excessive in filtrate, realizes acidleach Few discharge of journey, or even zero-emission.
The present invention also provides above-mentioned active substance of lithium ion battery anode acid molten and its circulation utilization method special equipment.
Technical scheme step is as follows:Step 1)The transfer box for containing positive active material is immersed equipped with acid The sour fluid bowl of solution, positive active material being dissolved, the acid solutions are 1-3 mol/L, and solution temperature is 50-70 DEG C, Gu Liquor ratio 1g:5-15 mL;
Step 2)The material of positive active material will be dissolved in sour fluid bowl, through acid pump pump to stillpot, added into stillpot Enter sodium hydroxide solution, precipitate phosphoric acid iron, complete iron removal, described concentration of sodium hydroxide solution is 5-7 mol/L, described Ferric phosphate precipitation pH value is 2-4;
Step 3)By the product pump after iron removaling into storage tank, Ni in acid dissoluting liquid is analyzed:Co:The ratio between Mn amount of substance, dissolved to acid NiSO is added in liquid4·6H2O、CoSO4·H2O、MnSO4·H2O or NiCl2·6H2O、CoCl2·6H2O, MnCl2·4H2O or Ni(NO3)2·6H2O、Co(NO3)2·6H2O、Ni(NO3)2·6H2The ratio between O adjustment three's amount of substance ratio needed for;
Step 4)By the material of step 3 and add the sodium hydrate aqueous solution that naoh concentration is 5-7mol/L, Yi Jizhi The mass ratio of the concentrated ammonia liquor and water of measuring concentration 25% is 1:0.5-1.5 ammoniacal liquor, is pumped into reactor with peristaltic pump and is co-precipitated Reaction, obtain nickel-cobalt-manganese ternary hydroxide presoma precipitation;
Step 5)By material of the filter press press filtration from step 4, obtain respectively nickel-cobalt-manganese ternary hydroxide presoma and Sodium salt solution, sodium salt solution pump to adjustment tank, after supplementing sodium hydroxide into adjustment tank, standby step 2 uses.
Acid solution described in step 1 of the present invention is the aqueous solution of sulfuric acid, hydrochloric acid or nitric acid.
Ni described in step 3 of the present invention:Co:The ratio between Mn amount of substance can be adjusted to 1:1:1,8:1:1,5:2:One in 3 Kind.
The condition of coprecipitation reaction described in the present invention rapid four is:Mixing speed 230-250rpm, reaction temperature 40- The addition of 60 DEG C, pH value 10-12, sodium hydrate aqueous solution described in coprecipitation reaction and ammoniacal liquor is controlled with pH value in reaction.
Sodium salt solution described in step 5 of the present invention supplements sodium hydroxide, and the mixed alkali liquor concentration after supplement is 5-7 mol/ L。
Positive active material described in step 1 of the present invention is lithium-containing transition metal oxide, as cobalt acid lithium, LiMn2O4, One kind or wherein several mixtures in nickle cobalt lithium manganate and LiFePO4.
Transfer box material described in step 1 of the present invention is plastics, such as:One in polyethylene, polyvinyl chloride and polypropylene Kind.
The present invention is used for molten and its circulation utilization method the equipment of active substance of lithium ion battery anode acid:Sour fluid bowl warp First acid pump is connected with acid solution tank, and the first magnetic valve is housed on the discharging pipeline of the first acid pump;Cleaner liquid containing sodium salt Groove is connected through the first lye pump with stillpot, and second solenoid valve is housed on the first lye pump discharging pipeline;Stillpot discharging opening It is connected through the second lye pump with the first filter press;Also include the nickel-cobalt-manganese ternary hydroxide forerunner of first filter press of reception The adjustment tank of body and the cleaner liquid containing sodium salt;Adjustment tank is connected through the 3rd acid pump with holding tank;Holding tank is through the 4th acid pump Stillpot is connected together, and co-precipitation kettle discharging opening connects the second filter press;Receive the cleaner liquid containing sodium salt from the second filter press The liquid bath of filtering containing sodium salt be connected through the 3rd lye pump with alkali liquid tank;Sour fluid bowl is equipped with acid concentration electrode, acid concentration electrode with Acid concentration sensor electrically couples;Sour fluid bowl is equipped with temperature sensor, electrothermal tube, relay;Stillpot is equipped with pH meter, pH meter with PH sensors electrically couple;Co-precipitation kettle is equipped with pH meter, and pH meter is electrically connected with pH sensors;Kettle is co-precipitated also to wriggle through first Pump is connected with alkali liquid tank, and is connected through the second peristaltic pump with ammoniacal liquor tank;
The equipment of the present invention also includes one and receives acid concentration electrode and the sour fluid bowl alkali concn signal of acid concentration sensor collection Acid concentration progress to sour fluid bowl accurately controls, received temperature of the sour fluid bowl temperature signal to sour fluid bowl of temperature sensor collection The stillpot acid concentration signal accurately control, reception pH meter gathers with pH sensors is accurately controlled to the pH value of stillpot The single-chip microcomputer of system, the break-make for the instruction control magnetic valve that a reception single-chip microcomputer is sent is so that acid concentration, the precipitation of sour fluid bowl The acid concentration of groove is controlled in setting range, the break-make of control relay so that the temperature control of sour fluid bowl in setting range Output control circuit;Output control circuit electrically couples with each magnetic valve, relay.
The concentration control of acid solution uses acid strength on-line checking and automatic acid supply system in the technological process of the present invention, temperature Degree control uses solution temperature on-line checking and automatic heating system, and the addition of sodium hydroxide solution is joined using pH meter and lye pump Dynamic control, the system are fed intake by scientific measurement, accurate measurement, are advantageous to improve technological effect, are reduced and draw because excess feeds intake The environmental improvement burden risen;The system automation degree is high, is advantageous to improve operating efficiency, reduces operating personnel exposed to strong The health hazard that acid, strong alkali environment are brought.In addition, the sodium salt cleaner liquid in the present invention is transmitted back to alkali lye adjustment tank by the road, it is right Excessive aqueous slkali, which is realized, in filtrate recycles, and the process improves raw material availability by rational technological design, reduced The discharge of ferric phosphate precipitation process.
Beneficial effects of the present invention are as follows:
First, accurate measurement of the present invention feeds intake, and is advantageous to improve technological effect, reduces the environmental improvement caused by excess feeds intake and bear Load.Positive active material hour dissolution rate is 99%.
2nd, automaticity of the present invention is high, is advantageous to improve operating efficiency, reduces operating personnel exposed to strong acid, strong The health hazard that alkali environment is brought.
3rd, present invention process improves raw material availability, reduces the discharge of ferric phosphate precipitation process.
Brief description of the drawings
Fig. 1 is the process chart of the present invention.
Fig. 2 is the device structure schematic diagram of the present invention.
Fig. 3 is temperature online detection and automatic heating circuit block diagram.
Fig. 4 acid, alkali concn on-line checking and automatic alkali adding circuit block diagram.
Embodiment
Technical solution of the present invention is not limited to act embodiment set forth below, in addition between each embodiment Any combination.
Embodiment 1
Technological process as shown in Figure 1:
First, in removal process, the polypropylene transfer box of nickel-cobalt-manganese ternary positive pole and iron phosphate lithium positive pole active material will be contained Sulfuric acid concentration 1mol/L acid fluid bowls are immersed, adjustment solution temperature is 50 DEG C, the g of solid-to-liquid ratio 1:5 mL, dissolve positive active material; The positive active material is lithium-containing transition metal oxide, in cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and LiFePO4 Several mixtures.
2nd, the material of positive active material will have been dissolved in sour fluid bowl, through acid pump pump to stillpot, has been added into stillpot It is 5mol/L sodium hydroxide solutions to enter concentration, and adjustment material pH value is 2, precipitate phosphoric acid iron, completes iron removal;
3rd, by the product pump after iron removaling into storage tank, Ni in acid dissoluting liquid is analyzed:Co:The ratio between Mn amount of substance, add NiSO4· 6H2O、CoSO4·H2O、MnSO4·H2The ratio between O adjustment three's amount of substance is 8:1:1;
4th, by material and 5mol/L sodium hydroxide solutions and 1:0.5 ammoniacal liquor, it is pumped into co-precipitation kettle, is being stirred with peristaltic pump Mix speed 230rpm, reaction temperature be 40 DEG C, pH value coprecipitation reaction is carried out under conditions of 10, obtain nickel-cobalt-manganese ternary hydrogen-oxygen Compound presoma precipitates.
5th, by filter press press filtration, nickel-cobalt-manganese ternary hydroxide presoma and sodium salt solution, sodium salt solution are obtained respectively Pump is to adjustment tank, and it is 5 mol/L to supplement sodium hydroxide to concentration of lye into adjustment tank, and standby step 2 uses.
Described transfer box material is vinyon.
The equipment of the present invention is as shown in Figure 2.Sour fluid bowl 1 is connected through the first acid pump with acid solution tank, in the first acid pump Discharging pipeline on the first magnetic valve is housed;The liquid bath of filtering containing sodium salt 8 is connected through the first lye pump 22 with stillpot 2, and first Second solenoid valve 24 is housed on the discharging pipeline of lye pump 22;The discharging opening of stillpot 2 connects through the second lye pump 21 and the first filter press 3 Connect;Also include the adjustment tank of a nickel-cobalt-manganese ternary hydroxide presoma for receiving the first filter press 3 and the cleaner liquid containing sodium salt 4;Adjustment tank 4 is connected through the 3rd acid pump 41 with holding tank 5;Through the 4th acid pump 51, stillpot 6 is connected holding tank 5 together Connect, the co-precipitation discharging opening of kettle 6 connects the second filter press 7;Receive the filtering containing sodium salt of the cleaner liquid containing sodium salt from the second filter press 7 Liquid bath 8 is connected through the 3rd lye pump 81 with alkali liquid tank 82, and sour fluid bowl 1 is equipped with acid concentration electrode 13, acid concentration electrode 13 and acid Concentration sensor 14 electrically couples;Sour fluid bowl 1 equipped with temperature sensor 15, electrothermal tube 16 and with both above-mentioned relays for being connected 17;Stillpot 2 is equipped with pH meter 25, and pH meter 25 electrically couples with pH sensors 26;Co-precipitation kettle 6 be equipped with pH meter 61, pH meter 61 and PH sensors 64 are electrically connected with;Co-precipitation kettle 6 is also connected through the first peristaltic pump 62 with alkali liquid tank 82, and through the second peristaltic pump 63 It is connected with ammoniacal liquor tank 65.11 pump between stillpot and sour fluid bowl in figure, 12 be valve.
In Fig. 3, external temperature sensor 15 is electrically connected with testing temperature bridge circuit 16, testing temperature bridge circuit 16 and list Piece machine 9 is electrically connected with, single-chip microcomputer 9 and input through keyboard circuit, addressed memory, LED display circuit, relay output control circuit 18 are electrically connected with.
In Fig. 4, external acid concentration sensor 14 is electrically connected with surveying concentration bridge circuit, surveys concentration bridge circuit and monolithic Machine 9 is electrically connected with, single-chip microcomputer 9 and input through keyboard circuit, addressed memory, LED display circuit, magnetic valve output control circuit 19 It is electrically connected with.Magnetic valve output control circuit 19 controls each magnetic valve.
Density control of acid liquor uses acid strength on-line checking and automatic acid supply system in the step 1, when in sour fluid bowl After acid solution consumption, acid concentration electrode, acid concentration sensor 14 in sour fluid bowl acid solution provide signal to single-chip microcomputer 9, start electromagnetism Valve, the first acid pump 11, to sour fluid bowl enriching acid solution, ensure that solution is well mixed by the stirring motor in sour fluid bowl;When acid is molten Acid strength reaches established standardses in groove, and the acid concentration electrode, acid concentration sensor 14 in sour fluid bowl acid solution provide to single-chip microcomputer 9 Signal, magnetic valve make the first acid pump 11 be stopped.
Solution temperature on-line checking and automatic heating system are used in the step 1 in sour fluid bowl, works as positive active material When reaction temperature in acid solution is less than established standardses, signal is provided from temperature sensor 15 to single-chip microcomputer 9, starts relay Device, the electrified regulation acid solution of electrothermal tube 16 into sour fluid bowl, ensures that solution temperature is uniform by the stirring motor in sour fluid bowl;When Acid solution temperature in sour fluid bowl reaches established standardses, and temperature sensor 15 provides signal, relay power-off, electricity to single-chip microcomputer 9 Heat pipe 16 stops heating.
Ferric phosphate settling system in the step 2, when entering new acid dissoluting liquid in stillpot, pH value will be less than 2, sink PH meter 25 provides signal to single-chip microcomputer 9 in shallow lake groove 2, starts magnetic valve, starts lye pump 22, to stillpot enriching alkali lye, by sinking Stirring motor in the groove of shallow lake ensures that solution is well mixed;When solution ph is higher than 4 in stillpot, pH meter provides to single-chip microcomputer 9 Signal, magnetic valve make alkali lye delivery pump be stopped.
Embodiment 2
First, in removal process, the polypropylene transfer box for containing lithium cobaltate cathode and iron phosphate lithium positive pole active material is immersed Concentration of hydrochloric acid 3mol/L acid fluid bowls, adjustment solution temperature is 70 DEG C, the g of solid-to-liquid ratio 1:15 mL, dissolve positive active material;Institute It is lithium-containing transition metal oxide to state positive active material, as several in cobalt acid lithium, LiMn2O4, nickle cobalt lithium manganate and LiFePO4 The mixture of kind.
2nd, the acid solution of positive active material will have been dissolved in sour fluid bowl, through acid pump pump to stillpot, into stillpot Addition concentration is 7mol/L sodium hydroxide solutions, and adjustment acid solution pH value is 4, precipitate phosphoric acid iron, completes iron removal;
3rd, by the acid solution pump after iron removaling into storage tank, Ni in acid dissoluting liquid is analyzed:Co:The ratio between Mn amount of substance, add NiCl2·6H2O、CoCl2·6H2O, MnCl2·4H2The ratio between O adjustment three's amount of substance is 5:2:3;
4th, by acid solution and 7mol/L sodium hydroxide solutions and 1:1.5 ammoniacal liquor, is pumped into reactor with peristaltic pump, is being stirred Mix speed 250rpm, reaction temperature be 60 DEG C, pH value coprecipitation reaction is carried out under conditions of 12, obtain nickel-cobalt-manganese ternary hydrogen-oxygen Compound presoma precipitates.
5th, by filter press press filtration, nickel-cobalt-manganese ternary hydroxide presoma and sodium salt cleaner liquid, sodium salt filter are obtained respectively Clear liquid pump is to adjustment tank, and it is 7 mol/L to supplement sodium hydroxide to concentration of lye into adjustment tank, and standby step 2 uses.
Described transfer box material is polypropylene plastics.
The special equipment of the present embodiment is the same as embodiment 1.

Claims (7)

1. the sour molten and its circulation utilization method of a kind of active substance of lithium ion battery anode, it is characterised in that step is as follows:Step One)The transfer box for containing positive active material is immersed into the sour fluid bowl equipped with acid solution, dissolves positive active material, the acid is molten Liquid concentration is 1-3 mol/L, and solution temperature is 50-70 DEG C, solid-to-liquid ratio 1g:5-15 mL;
Step 2)The material of positive active material will be dissolved in sour fluid bowl, through acid pump pump to stillpot, added into stillpot Enter sodium hydroxide solution, precipitate phosphoric acid iron, complete iron removal, described concentration of sodium hydroxide solution is 5-7 mol/L, described Ferric phosphate precipitation pH value is 2-4;
Step 3)By the product pump after iron removaling into storage tank, Ni in material is analyzed:Co:The ratio between Mn amount of substance, is added into material NiSO4·6H2O、CoSO4·H2O、MnSO4·H2O or NiCl2·6H2O、CoCl2·6H2O, MnCl2·4H2O or Ni (NO3)2· 6H2O、Co(NO3)2·6H2O、Ni(NO3)2·6H2The ratio between O adjustment three's amount of substance ratio needed for;
Step 4)By the material of step 3 and add the sodium hydrate aqueous solution that naoh concentration is 5-7mol/L, Yi Jizhi The mass ratio of the concentrated ammonia liquor and water of measuring concentration 25% is 1:0.5-1.5 ammoniacal liquor, is pumped into reactor with peristaltic pump and is co-precipitated Reaction, obtain nickel-cobalt-manganese ternary hydroxide presoma precipitation;
Step 5)By material of the filter press press filtration from step 4, obtain respectively nickel-cobalt-manganese ternary hydroxide presoma and Sodium salt solution, sodium salt solution pump to adjustment tank, after supplementing sodium hydroxide into adjustment tank, standby step 2 uses.
2. the sour molten and its circulation utilization method of active substance of lithium ion battery anode according to claim 1, it is characterised in that Acid solution described in step 1 is the aqueous solution of sulfuric acid, hydrochloric acid or nitric acid.
3. the sour molten and its circulation utilization method of active substance of lithium ion battery anode according to claim 1, it is characterised in that Ni described in step 3:Co:The ratio between Mn amount of substance can be adjusted to 1:1:1,8:1:1,5:2:One kind in 3.
4. the sour molten and its circulation utilization method of active substance of lithium ion battery anode according to claim 1, it is characterised in that The condition of coprecipitation reaction described in step 4 is:Mixing speed 230-250rpm, reaction temperature are 40-60 DEG C, pH value The addition of 10-12, sodium hydrate aqueous solution described in coprecipitation reaction and ammoniacal liquor is controlled with pH value in reaction.
5. the sour molten and its circulation utilization method of active substance of lithium ion battery anode according to claim 1, it is characterised in that Sodium salt cleaner liquid described in step 5 supplements sodium hydroxide, and the mixed alkali liquor concentration after supplement is 5-7 mol/L.
6. the sour molten and its circulation utilization method of active substance of lithium ion battery anode according to claim 1, it is characterised in that Transfer box material described in step 1 is plastics, such as:One kind in polyethylene, polyvinyl chloride and polypropylene.
7. a kind of be used for molten and its circulation utilization method the equipment of active substance of lithium ion battery anode acid, it is characterised in that:Acid Fluid bowl(1)It is connected through the first acid pump with acid solution tank, the first magnetic valve is housed on the discharging pipeline of the first acid pump;Containing sodium Salt filtering liquid bath(8)Through the first lye pump(22)With stillpot(2)It is connected, the first lye pump(22)Discharge on pipeline equipped with the Two magnetic valves(24);Stillpot(2)Discharging opening is through the second lye pump(21)With the first filter press(3)Connection;Also connect including one Receive the first filter press(3)Nickel-cobalt-manganese ternary hydroxide presoma and the cleaner liquid containing sodium salt adjustment tank(4);Adjustment tank(4) Through the 3rd acid pump(41)With holding tank(5)It is connected;Holding tank(5)Through the 4th acid pump(51)Stillpot together(6)It is connected Connect, be co-precipitated kettle(6)Discharging opening connects the second filter press(7);Reception comes from the second filter press(7)The cleaner liquid containing sodium salt contain sodium Salt filtering liquid bath(8)Through the 3rd lye pump(81)With alkali liquid tank(82)It is connected;Sour fluid bowl(1)Equipped with acid concentration electrode(13), Acid concentration electrode(13)With acid concentration sensor(14)Electrically connection;Sour fluid bowl(1)Equipped with temperature sensor(15), electrothermal tube (16), relay(17);Stillpot(2)Equipped with pH meter(25), pH meter(25)With pH sensors(26)Electrically connection;It is co-precipitated kettle (6)Equipped with pH meter(61), pH meter(61)With pH sensors(64)It is electrically connected with;Also through the first peristaltic pump(62)With alkali liquid tank(82) Connection, and through the second peristaltic pump(63)With ammoniacal liquor tank(65)Connection;
Also include a reception acid concentration electrode(13)With acid concentration sensor(14)The sour fluid bowl alkali concn signal of collection is to acid The acid concentration of fluid bowl accurately control, receives temperature sensor(15)Temperature of the sour fluid bowl temperature signal of collection to sour fluid bowl Accurately control, receive pH meter(25)With pH sensors(26)The stillpot of collection(2)PH of the acid concentration signal to stillpot The single-chip microcomputer that value is accurately controlled(9), a reception single-chip microcomputer(9)The break-make of the instruction control magnetic valve sent is so that acid Acid concentration, the acid concentration of stillpot of fluid bowl are controlled in setting range, and the break-make of control relay is so that the temperature of sour fluid bowl Output control circuit of the degree control in setting range;Output control circuit electrically couples with each magnetic valve, relay.
CN201710985506.6A 2017-10-20 2017-10-20 The active substance of lithium ion battery anode molten and its circulation utilization method of acid and equipment Pending CN107611515A (en)

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Publication number Priority date Publication date Assignee Title
CN108303588A (en) * 2018-04-09 2018-07-20 骆驼集团武汉光谷研发中心有限公司 A kind of Insulation Inspection Device for Direct-Current System based on nonequilibrium bridge
CN108303588B (en) * 2018-04-09 2023-09-01 骆驼集团武汉光谷研发中心有限公司 DC system insulation monitoring device based on unbalanced bridge
CN109037673A (en) * 2018-10-18 2018-12-18 珠海嘉志科技咨询有限公司 A kind of environmentally friendly, efficiently preparation nickel-cobalt-manganternary ternary anode material presoma method

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