CN110137469A - A kind of waste and old lithium ion battery graphite cathode material regeneration method - Google Patents
A kind of waste and old lithium ion battery graphite cathode material regeneration method Download PDFInfo
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- CN110137469A CN110137469A CN201910406291.7A CN201910406291A CN110137469A CN 110137469 A CN110137469 A CN 110137469A CN 201910406291 A CN201910406291 A CN 201910406291A CN 110137469 A CN110137469 A CN 110137469A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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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Abstract
The invention discloses a kind of waste and old lithium ion battery graphite cathode material regeneration method, include the following steps: 1) by waste and old graphite cathode material under protective atmosphere sintering processes, to remove conductive agent, binder, thickener；2) by sintered waste and old graphite cathode material and inorganic acid fluid hybrid reaction, graphite powder is obtained after filtration, washing and drying；3) by graphite powder, inorganic ti sources and urea and/or ammonium hydroxide hybrid reaction, under protective atmosphere, reactant obtains the graphite cathode material that titanium dioxide uniformly coats after calcining.The present invention makes coated by titanium dioxide waste and old lithium ion battery graphite cathode material using sluggish precipitation, solves dendrite problems accumulated in battery use；Simultaneously in repair process, the structure change of embedding de- lithium process is small, cycle performance and service life after being obviously improved graphite cathode material regeneration.
Description
Technical field
The invention belongs to lithium ion battery negative material regeneration field, specially a kind of waste and old lithium ion battery graphite cathode
The method of material regeneration.
Background technique
Waste lithium ion processing mode focuses primarily upon positive precious metal material at present, and negative electrode material is as battery structure
Cheng Si great raw material, the research processing recycled at present to it is still insufficient, this not only wastes a large amount of carbon resources, if but also subsequent
It handles and mishandling will cause serious secondary pollution.The graphite cathode material isolated in waste lithium cell is asked there are following
Topic: graphite cathode easily forms irregular Li dendrite in cyclic process, while graphite cathode and organic electrolyte generation are irreversible
Reaction, causes irreversible capacity loss, so that cycle performance decline is serious, these problems are that waste and old lithium ion battery graphite is negative
Pole material recovery regenerates the significant problem faced.
Summary of the invention
In order to solve the problems in the existing technology, the object of the present invention is to provide a kind of waste and old lithium ion batteries
Graphite cathode material regeneration method makes coated by titanium dioxide waste and old lithium ion battery graphite cathode material using sluggish precipitation
Material solves dendrite problems accumulated in battery use；Simultaneously in repair process, the structure change of embedding de- lithium process is small, significantly
Cycle performance and service life after promoting graphite cathode material regeneration.
To achieve the goals above, the present invention provides a kind of regenerated sides of waste and old lithium ion battery graphite cathode material
Method includes the following steps:
1) by waste and old graphite cathode material under protective atmosphere sintering processes, to remove conductive agent, binder, thickening
Agent；
2) it by sintered waste and old graphite cathode material and inorganic acid fluid hybrid reaction, obtains after filtration, washing and drying
Graphite powder；
3) by graphite powder, inorganic ti sources and urea and/or ammonium hydroxide hybrid reaction, under protective atmosphere, reactant is after calcining
Obtain the graphite cathode material that titanium dioxide uniformly coats.
Preferably, in step 2), the solid-to-liquid ratio of the waste and old graphite cathode material and inorganic acid fluid is 1:3~4.5, reaction
80~100 DEG C of temperature, 1~3h of time.
Preferably, in step 2), the inorganic acid is sulfuric acid, nitric acid or hydrochloric acid.
Preferably, in step 3), the inorganic ti sources are titanium sulfate or titanyl sulfate.
Preferably, in step 3), the inorganic ti sources are 1:2~3 with the mass ratio of urea and/or ammonium hydroxide.
Preferably, in step 3), the concentration of the urea or ammonium hydroxide is 2~3mol/L.
Preferably, in step 3), the reaction temperature is 60~80 DEG C, 2~4h of time.
Preferably, in step 3), the calcination temperature is 700~900 DEG C, 1~2h of time.
The present invention coats waste and old lithium ion battery graphite cathode material using titanium dioxide, TiO2It is stored up in nature
Amount is big, environmentally friendly, and the de- Li current potential of embedding Li is higher (about 1.75V), can effectively avoid the formation of Li dendrite, promotes lithium-ion electric
The safety in pond, while also inhibiting the continuous of SEI film in cyclic process and being formed and fallen off, reduce the loss of capacity.Open
Crystal structure and the flexible electronic structure of titanium ion, make TiO2The electronics of acceptable foreign ion.In order to keep electroneutral, electronics
It can be along with Li+Common insertion TiO2In lattice.It can thus equation indicate are as follows: Li++TiO2+xe-=LixTiO2.Thus charge and discharge
Volume change is small in the process, for the cation (Li of insertion+、H+And Na+Deng) vacancy is provided, after promoting graphite cathode material regeneration
Cycle performance and service life.
The present invention makes coated by titanium dioxide graphite lithium ion battery negative electrode material using sluggish precipitation, so that precipitating crystal form
It slowly grows, controls the speed for generating precipitating reagent, that is, can avoid uneven concentration phenomenon, make degree of supersaturation control appropriate
In range, precipitating reagent is evenly distributed in entire solution, and controls the speed of growth of particle, is obtained epigranular, densification, is convenient for
Washing, nanoparticle with high purity.
Due to urea decomposition rate by heating temperature and urea concentration control, can make urea decomposition speed keep compared with
Low-level, to obtain the uniform nano-TiO of particle diameter distribution2.The decomposition product CO of urea2And NH3, after reaction or calcination
It is volatile for gas, will not purity to product and quality impact.NH3·H2O is in TiOSO4It is evenly distributed, makes in solution
It obtains sediment TiO (OH)2Uniformly generate:
CO(NH2)2+3H2O=2NH3·H2O+CO2
TiOSO4+2NH3·H2O=TiO (OH)2+(NH4)2SO4
TiO(OH)2Calcination obtains TiO2:TiO(OH)2=TiO2+H2O
The present invention uses waste and old lithium ion battery graphite cathode material for raw material, using protective atmosphere sintering, inorganic acidleach
Treatment process removes no-bonder, thickener, metal impurities, then uses titanyl sulfate basic hydrolysis pre-coated, protective atmosphere calcining
The graphite material of final obtained coated by titanium dioxide, can solve dendrite problems accumulated in battery use；Repair process simultaneously
In, the structure change of embedding de- lithium process is small, cycle performance and service life after promoting negative electrode material regeneration.Present invention process letter
Single, at low cost, the rate of recovery is high, is easy to large-scale industrial production.
Detailed description of the invention
Fig. 1 is the SEM figure of the graphite cathode material of coated by titanium dioxide made from embodiment 1；
Fig. 2 is the circulation first charge-discharge efficiency figure of the graphite cathode material of coated by titanium dioxide made from embodiment 1.
Specific embodiment
Embodiment 1
It takes graphite cathode powder to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in inert atmosphere furnace, to remove no-bonder
Equal impurity.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution is mixed with graphite material, permanent
Warm water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
By 300g graphite powder after wet-treating and 650ml 0.9mol/L TiOSO4Solution mixing, promoted water temperature to 80 DEG C,
Urea 65g is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2The graphite of pre-coated
Powder；The lower 800 DEG C of calcinings of inert atmosphere protection, obtain TiO2Coated graphite negative electrode material, covering amount 3.50wt%.Sample SEM
Figure is as shown in Figure 1, the graphite particle surface after cladding has preferable smoothness, and particle is more close and regular, covered effect
Well.
Gram volume test condition: standing 2h, and multiplying power discharging is gradually down to 0.02C by 0.1C, and being discharged to voltage is 0V；It stands
0.5h, then 0.1C multiplying power charges to voltage greater than 2V；Charge and discharge 5 circulations.
Embodiment 2
It takes graphite cathode powder to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in inert atmosphere furnace, to remove no-bonder
Equal impurity.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution is mixed with graphite material, permanent
Warm water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
By 300g graphite powder after wet-treating and 700ml 0.8mol/L TiOSO4Solution mixing, promoted water temperature to 80 DEG C,
Urea 70g is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2The graphite of pre-coated
Powder, the lower 800 DEG C of calcinings of inert atmosphere protection, obtains TiO2Coated graphite negative electrode material, covering amount 3.77wt%.
Embodiment 3
It takes graphite cathode powder 300g to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in nitrogen atmosphere stove, it is viscous to remove
Tie the impurity such as agent.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution and graphite material are mixed
It closes, thermostat water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
By 300g graphite powder after wet-treating and 500ml 0.6mol/L TiOSO4Solution mixing, promoted water temperature to 75 DEG C,
2.0mol/L ammonium hydroxide 330ml is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2In advance
The graphite powder of cladding, the lower 800 DEG C of calcinings of inert atmosphere protection, obtains TiO2Coated graphite negative electrode material, covering amount are
3.29wt%.
Embodiment 4
It takes graphite cathode powder 300g to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in nitrogen atmosphere stove, it is viscous to remove
Tie the impurity such as agent.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution and graphite material are mixed
It closes, thermostat water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
300g graphite powder after wet-treating is mixed with 100ml 0.9mol/L titanium sulfate solution, promoted water temperature to 75 DEG C,
Urea 58g is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2The graphite of pre-coated
Powder, the lower 800 DEG C of calcinings of inert atmosphere protection, obtains TiO2Coated graphite negative electrode material.
Comparative example 1
It takes graphite cathode powder 300g to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in nitrogen atmosphere stove, it is viscous to remove
Tie the impurity such as agent.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution and graphite material are mixed
It closes, thermostat water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
By 300g graphite powder after wet-treating and 180ml 0.5mol/L TiOSO4Solution mixing, promoted water temperature to 75 DEG C,
1.5mol/L ammonium hydroxide 110ml is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2In advance
The graphite powder of cladding, the lower 800 DEG C of calcinings of inert atmosphere protection, obtains TiO2Coated graphite negative electrode material.
Comparative example 2
It takes graphite cathode powder 300g to be processed in porcelain boat, is put into 450 DEG C of sintering 4h in nitrogen atmosphere stove, it is viscous to remove
Tie the impurity such as agent.Powder after being sintered is taken out, weighing takes 2L 0.5mol/L H by 1:4 solid-to-liquid ratio2SO4Solution and graphite material are mixed
It closes, thermostat water bath reacts 2h, and water temperature controls 90 DEG C.Graphite after will be purified is placed in baking oven, 105 DEG C of drying 12h.
By 300g graphite powder after wet-treating and 180ml 0.5mol/L TiOSO4Solution mixing, promoted water temperature to 80 DEG C,
3.5mol/L ammonium hydroxide 270ml is added, stirring makes it completely dissolved, and reaction 1.5h is filtered, and washes several times, obtains TiO (OH)2In advance
The graphite powder of cladding, the lower 800 DEG C of calcinings of inert atmosphere protection, obtains TiO2Coated graphite negative electrode material.
As shown in table 1, sample physical properties index made from Examples 1 to 4 is ideal.In comparative example 1,2,
If urea or ammonia concn are too small, precipitating will lead to not exclusively, yield reduces；If urea or ammonia concn are excessive, can cause to urinate
The reduction of element or ammonium hydroxide hydrolysis rate, crystal grain become smaller.
The physical and chemical performance index of sample made from 1 Examples 1 to 4 of table and comparative example 1-2
Claims (8)
1. a kind of waste and old lithium ion battery graphite cathode material regeneration method, characterized by the following steps:
1) by waste and old graphite cathode material under protective atmosphere sintering processes, to remove conductive agent, binder, thickener；
2) by sintered waste and old graphite cathode material and inorganic acid fluid hybrid reaction, graphite is obtained after filtration, washing and drying
Powder；
3) by graphite powder, inorganic ti sources and urea and/or ammonium hydroxide hybrid reaction, under protective atmosphere, reactant obtains after calcining
The graphite cathode material that titanium dioxide uniformly coats.
2. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 2), the solid-to-liquid ratio of the waste and old graphite cathode material and inorganic acid fluid is 1:3~4.5,80~100 DEG C of reaction temperature,
1~3h of time.
3. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 2), the inorganic acid is sulfuric acid, nitric acid or hydrochloric acid.
4. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 3), the inorganic ti sources are titanium sulfate or titanyl sulfate.
5. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 3), the inorganic ti sources are 1:2~3 with the mass ratio of urea and/or ammonium hydroxide.
6. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 3), the concentration of the urea or ammonium hydroxide is 2~3mol/L.
7. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 3), the reaction temperature is 60~80 DEG C.
8. a kind of waste and old lithium ion battery graphite cathode material regeneration method according to claim 1, it is characterised in that:
In step 3), the calcination temperature is 700~900 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| CN112803024A (en) * | 2021-01-18 | 2021-05-14 | 山东玉皇新能源科技有限公司 | Regeneration method and application of waste lithium ion battery negative electrode graphite material |
| CN114242966A (en) * | 2021-11-12 | 2022-03-25 | 惠州锂威新能源科技有限公司 | Negative electrode composite material, preparation method thereof, negative electrode plate and secondary battery |
| CN114309452A (en) * | 2021-11-15 | 2022-04-12 | 北京仁创砂业铸造材料有限公司 | Precoated sand additive, precoated sand and preparation method thereof |
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| CN108083270A (en) * | 2017-12-21 | 2018-05-29 | 天津理工大学 | A kind of reparative regeneration method of graphite cathode waste material |
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| KR20160031782A (en) * | 2014-09-15 | 2016-03-23 | (주)포스코켐텍 | Negative electrode active material for rechargable lithium battery, method for manufacturing the same, and rechargable lithium battery including the same |
| CN105789574A (en) * | 2016-03-04 | 2016-07-20 | 深圳市翔丰华科技有限公司 | Preparation method of high-temperature graphite anode material for lithium-ion battery |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| CN112803024A (en) * | 2021-01-18 | 2021-05-14 | 山东玉皇新能源科技有限公司 | Regeneration method and application of waste lithium ion battery negative electrode graphite material |
| CN114242966A (en) * | 2021-11-12 | 2022-03-25 | 惠州锂威新能源科技有限公司 | Negative electrode composite material, preparation method thereof, negative electrode plate and secondary battery |
| CN114309452A (en) * | 2021-11-15 | 2022-04-12 | 北京仁创砂业铸造材料有限公司 | Precoated sand additive, precoated sand and preparation method thereof |
| CN114309452B (en) * | 2021-11-15 | 2023-07-25 | 北京仁创砂业铸造材料有限公司 | Precoated sand additive, precoated sand and preparation method thereof |
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Application publication date: 20190816 |