CN106276842B - By the method for the LiFePO4 reclaiming in waste and old lithium ion battery - Google Patents
By the method for the LiFePO4 reclaiming in waste and old lithium ion battery Download PDFInfo
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Abstract
The invention belongs to the recycling of waste and old power lithium-ion battery, recycle utilization technology field, more particularly, to a kind of reclaiming method of waste and old power LiFePO4.Described method includes following steps：1) by the waste lithium iron phosphate powder after drying through be added 0.1-5M mixed organic acid based on aqueous solution in handle；It is obtained by filtration containing Li+、Fe2+、PO4 3‑Acid solution；2) it obtains ferric lithium phosphate precursor added with solvent in mother liquor and slightly precipitates；3) ferric lithium phosphate precursor is collected by filtration slightly to precipitate, is scattered in organic dispersing agent high-energy ball milling 0.5-8 hours, obtained slurry is dried and removed into after solvent 600 DEG C -800 DEG C of calcinings 2-8 hours in atmosphere, obtains regeneration lithium iron phosphate positive material；4) filtrate in step 3) is recycled, the mixed organic acid solution in Separation of Organic/dispersing agent and after being concentrated is re-used for the dissolution of LiFePO4 in step 1).
Description
Technical field
The invention belongs to the recycling of waste and old power lithium-ion battery, recycle utilization technology field, more particularly, to a kind of waste and old
The reclaiming method of power LiFePO4.
Background technique
Gradually industrialization and the scale of pure electric automobile, plug-in hybrid-power automobile, it is most important as new-energy automobile
The power battery of one of components will progress into the batch scrap stage in forthcoming years.One side scrap lithium ion battery tool
There is the poisonous and harmful property such as inflammability, Leaching, corrosivity, reactivity, on the other hand with the growth of yield, lithium member in the earth's crust
The market price of lithium ion battery, the industry development of bring new-energy automobile and ring have also been raised in the limitation of plain abundance year by year
Contradiction will be more and more prominent between border, resource.Therefore, the lithium iron phosphate electrode material in simultaneously regenerative power lithium ion battery is recycled
To energy-saving and emission-reduction, sustainable development are realized, it is of great significance.Traditional LiFePO4 regenerative process has usually contained a large amount of nothings
The use of machine acid, to produce a large amount of inorganic waste liquids, environment is caused increased while secondary pollution recycling at
This.Therefore, novel recovery technology how is researched and developed, reduces and even realizes that zero-emission is the green reclaim for developing LiFePO4
Significant challenge.
In view of this, the present invention is specifically proposed.
Summary of the invention
It a kind of is assisted back using organic acid the technical problem to be solved in the present invention is that overcoming the deficiencies of the prior art and provide
Receive and regenerate the environmentally protective processing method of LiFePO4.
In order to solve the above technical problems, the present invention is using the basic conception of technical solution：It will be in waste and old lithium ion battery
LiFePO4 reclaiming method, include the following steps：
1) by the waste lithium iron phosphate powder after drying through be added 0.1-5M mixed organic acid based on aqueous solution in 50-
It is handled at 95 DEG C, and the solid-to-liquid ratio of mixed liquor is 40-200 grams per liter；It is molten that the acidity containing Li+, Fe2+, PO43- is obtained by filtration
Liquid；
2) it is added a certain amount of organic solvent in mother liquor, the volume ratio of organic solvent and mother liquor is 2:1-1:10, obtain phosphorus
Sour iron lithium presoma slightly precipitates；
3) ferric lithium phosphate precursor is collected by filtration slightly to precipitate, it is small is scattered in high-energy ball milling 0.5-8 in a kind of organic dispersing agent
When, it is 1 that wherein ferric lithium phosphate precursor, which is slightly precipitated with the solid-to-liquid ratio of organic dispersing agent,:3-1:1, obtained slurry is dried and removed
After solvent in atmosphere 600 DEG C -800 DEG C of calcinings 5-20 hours, obtain regeneration lithium iron phosphate positive material.Wherein, high-energy ball milling
Process is affected to the electrochemical properties of regeneration lithium iron phosphate positive material, can not omit；
4) filtrate in step 3) is recycled, the mixed organic acid solution in Separation of Organic/dispersing agent and after being concentrated
It is re-used for the dissolution of LiFePO4 in step 1).
As the preferred technical solution of the present invention, between step 1) and step 2), can follow the steps below：B) it depressurizes
Acid filtrate of the heating concentration containing Li+, Fe2+, PO43-, at 45-98 DEG C, pressure is controlled in 0.1-0.5 atmospheric pressure for temperature control,
Cocnentration factor is 0.1-0.9.In this way, the LiFePO4 rate of recovery can be improved, the use of organic solvent is reduced.
As the preferred technical solution of the present invention, between step 1) and step b), follow the steps below：A) contain to above-mentioned
The acid filtrate of Li+, Fe2+, PO43- carry out titration or inductively coupled plasma atomic emission elemental analysis, are tied according to analysis
Appropriate lithium salts and other necessary compounds is added in fruit, and the molar ratio of Li, Fe, P in solution is made to reach 1-1.05:1:1-1.05.
It can be effectively improved the electrochemical properties of regeneration LiFePO4 in this way, and control the reproduction of the LiFePO4 waste material of separate sources
The product quality of object improves the consistency of regeneration lithium iron phosphate positive material.
It is further comprising the steps of between step 2) and step 3) as the preferred technical solution of the present invention：C) in phosphoric acid
Iron lithium presoma wherein adds conductive agent and conductive agent presoma in slightly precipitating, wherein conductive agent adds with conductive agent presoma
Enter amount and LiFePO4 mass ratio is 0-1:20, solid-to-liquid ratio 1:3-1:1.
As the preferred technical solution of the present invention, the conductive agent is acetylene carbon black, graphitic carbon black, the wear-resisting charcoal of high structure
One of black, graphene or carbon nanotube or more than one combination；Conductive agent presoma is glucose, fructose, malt
One of sugar or sucrose or more than one combinations.
As the preferred technical solution of the present invention, the organic acid is formic acid, acetic acid, propionic acid, oxalic acid, citric acid, anti-bad
One or more of hematic acid.
It include ethyl alcohol, hydrogen peroxide, phosphoric acid in the aqueous solution of the organic acid as the preferred technical solution of the present invention
One or more of.
As the preferred technical solution of the present invention, used lithium source be lithium hydroxide, lithium carbonate, lithium nitrate, lithium chloride,
One or more of lithium formate, lithium dihydrogen phosphate, two lithium of phosphoric acid hydrogen or lithium phosphate.
As the preferred technical solution of the present invention, used phosphorus source is phosphoric acid, ammonium dihydrogen phosphate, diammonium hydrogen phosphate, phosphorus
One or more of acid dihydride lithium, two lithium of phosphoric acid hydrogen or lithium phosphate.
As the preferred technical solution of the present invention, the organic solvent be acetonitrile, toluene, n-hexane, hexamethylene, methanol,
One or more of ethyl alcohol or acetone；
As the preferred technical solution of the present invention, the conductive agent is acetylene carbon black, graphitic carbon black, the wear-resisting charcoal of high structure
One of black, graphene or carbon nanotube or more than one combination；Conductive agent presoma is glucose, fructose, malt
One of sugar or sucrose or more than one combinations；
As the preferred technical solution of the present invention, the atmosphere is one of hydrogen, ammonia, nitrogen or argon gas or several
The arbitrary proportion mixing of kind gas.
As the preferred technical solution of the present invention, the separation of the organic solvent/dispersing agent using filtering, vacuum distillation,
The combination of one or more of heating water bath or high-throughput chromatographic isolation means, treatment temperature control are in 45-98 DEG C, time
1-10 hours.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art：Through step of the present invention
It handles obtained regeneration lithium iron phosphate positive material and has brand-new lithium iron phosphate positive material feature, reach iron phosphate lithium positive pole material
The national standard of material can be used as qualified positive electrode and use, and also can according to need design specifically for regeneration ferric phosphate
The formula of lithium anode material can also be used in mixed way with other brand-new lithium iron phosphate positive materials；2) it is mixed used in present invention process
Close organic acid, organic solvent can whole recycling and reusings, do not generate waste liquid, spent acid, therefore environmentally protective, be particluarly suitable for
Densely populated surrounding city is founded the factory；3) using the method for the present invention satisfiable realization lithium iron phosphate positive material production simultaneously
The recycling and reusing of waste material in process effectively reduces the synthesis production cost of lithium ion battery material；4) the method for the present invention
It is low in cost, it is easy to implement, it is suitble to promote.
Detailed description of the invention
Fig. 1 is that 0.1C, 0.5C and the 1C of regeneration lithium iron phosphate positive material obtained by embodiment 1 recycle discharge curve；
Fig. 2 is that 0.1C, 0.5C and the 1C of regeneration lithium iron phosphate positive material obtained by embodiment 2 recycle discharge curve；
Fig. 3 is that 0.1C, 0.5C and the 1C of regeneration lithium iron phosphate positive material obtained by embodiment 3 recycle discharge curve.
Specific embodiment
Explanation is further explained to the present invention below in conjunction with specific embodiments and the drawings.
Embodiment 1：
(1) dry waste and old lithium iron phosphate dynamic battery positive electrode 50g is added to the citric acid and oxalic acid of 1.0L
Mix acid liquor (concentration 1.1mol/L) in, add 10.0mL 30wt% aqueous hydrogen peroxide solution, heating water bath is to close to boiling
Rise, after be cooled to 85 DEG C of maintenances and react 150 minutes.
(2) wait be cooled to room temperature, the ratio of lithium, iron and phosphorus in solution is measured, and suitable lithium dihydrogen phosphate is added, is made molten
The molar ratio of Li, Fe, P in liquid reach 1.05:1:1.05.
(3) (volume ratio with mother liquor is 3 to the mixed solvent of addition ethyl alcohol and propyl alcohol in mother liquor:2) LiFePO4, is obtained
Presoma slightly precipitates.LiFePO4 is slightly precipitated together with sucrose, (sucrose additional amount 7.5wt%, solid-to-liquid ratio are scattered in ethyl alcohol
1:2), according to the electrode material production technology high-energy ball milling of our company 3 hours, by obtained slurries filtration and solvent is dried and removed
700 DEG C calcining 5 hours in nitrogen atmosphere afterwards, obtain regeneration lithium iron phosphate positive material.
Anode sizing agent is made into using regeneration positive electrode obtained by the present embodiment, ingredients by weight ratio is regeneration positive electrode：It leads
Electric agent SP：Binder PVdF：NMP=95:2:3:105, CR2032 button cell is assembled according to test battery production technology process,
The battery discharge curve is as shown in Figure 1.Compared with the button cell of normal positive electrode assembling, it is known that regenerated using the present embodiment
The charging and discharging curve of lithium iron phosphate positive material is consistent, and capacity is excellent with cycle performance, meets the country of ferric phosphate lithium cell
Standard.There is good chemical property with the LiFePO 4 material that the method recycles, be 140mAh/g, charge and discharge in 1C discharge capacity
It is 100.0% that electricity, which recycles 100 capacity retention ratios,.
By the filtrate recycling in step 3, coarse ethanol is recycled by 80 DEG C of heating water baths, remaining mother liquor continues heating and is concentrated into
Volume terminates to be concentrated to get recycling mixed organic acid solution close to 1.0L.
Embodiment 2：
(1) dry waste and old lithium iron phosphate dynamic battery positive electrode 50g is added to the citric acid and oxalic acid of 500mL
Mix acid liquor (concentration 1.1mol/L) in, add 5.0mL 30wt% aqueous hydrogen peroxide solution, heating water bath is to close to boiling
Rise, after be cooled to 85 DEG C of maintenances and react 15 minutes.
(2) ethyl alcohol is added in mother liquor, and (volume ratio with mother liquor is 4:1), ferric lithium phosphate precursor is obtained slightly to precipitate.
(3) LiFePO4 is slightly precipitated together with sucrose, is scattered in ethyl alcohol (sucrose additional amount 5wt%, solid-to-liquid ratio 1:
2), according to the electrode material production technology high-energy ball milling of our company 6 hours, by obtained slurries filtration and after drying and removing solvent
In nitrogen：Hydrogen (95:5) 800 DEG C calcining 10 hours in mixed atmosphere, obtain regeneration lithium iron phosphate positive material.
Anode sizing agent is made into using regeneration positive electrode obtained by the present embodiment, ingredients by weight ratio is regeneration positive electrode：It leads
Electric agent SP：Binder PVdF：NMP=95:2:3:105, CR2032 button cell is assembled according to test battery production technology process,
The battery discharge curve is as shown in Figure 2.Compared with the button cell of normal positive electrode assembling, it is known that regenerated using the present embodiment
The charging and discharging curve of lithium iron phosphate positive material is consistent, and capacity is slightly poor, and cycle performance is excellent, meets the country of ferric phosphate lithium cell
Standard.There is good chemical property with the LiFePO 4 material that the method recycles, be 133mAh/g, charge and discharge in 1C discharge capacity
It is 99.1% that electricity, which recycles 100 capacity retention ratios,.
By the filtrate recycling in step 3, coarse ethanol is recycled by 80 DEG C of heating water baths, remaining mother liquor continues heating and is concentrated into
Volume terminates to be concentrated to get recycling mixed organic acid solution close to 1.0L.
Embodiment 3
(1) dry waste and old lithium iron phosphate dynamic battery positive electrode 50g is added to the citric acid and oxalic acid of 800mL
Mix acid liquor (concentration 1.2mol/L) in, add 5.0mL 30wt% aqueous hydrogen peroxide solution, heating water bath is to close to boiling
It rises, maintains reaction 120 minutes.
(2) wait be cooled to room temperature, the ratio of lithium, iron and phosphorus in solution is measured, and suitable lithium dihydrogen phosphate is added, is made molten
The molar ratio of Li, Fe, P in liquid reach 1.1:1:1.Ethyl alcohol is added in mother liquor, and (volume ratio with mother liquor is 2:1) phosphorus, is obtained
Sour iron lithium presoma slightly precipitates.
(3) LiFePO4 is slightly precipitated together with sucrose, is scattered in ethyl alcohol (sucrose additional amount 2wt%, solid-to-liquid ratio 1:
2).Unlike the first embodiment, according to the electrode material production technology high-energy ball milling of our company 1.5 hours, the slurry that will be obtained
It filters and dries and removes after solvent in argon gas：Hydrogen (90:10) 600 DEG C calcining 20 hours in mixed atmosphere, obtain regeneration phosphoric acid
Iron lithium anode material.
Anode sizing agent is made into using regeneration positive electrode obtained by the present embodiment, ingredients by weight ratio is regeneration positive electrode：It leads
Electric agent SP：Binder PVdF：NMP=95:2:3:105, CR2032 button cell is assembled according to test battery production technology process,
The battery discharge curve is as shown in Figure 3.Compared with the button cell of normal positive electrode assembling, it is known that regenerated using the present embodiment
The charging and discharging curve of lithium iron phosphate positive material is consistent, and capacity is slightly lower, and high rate performance is bad, and cycle performance is good, but still accords with
Close the national standard of ferric phosphate lithium cell.There is good chemical property with the LiFePO 4 material that the method recycles, put in 1C
Capacitance is 120mAh/g, and 100 capacity retention ratios of charge and discharge cycles are 99.6%.
By the filtrate recycling in step 3, coarse ethanol is recycled by 80 DEG C of heating water baths, remaining mother liquor continues heating and is concentrated into
Volume terminates to be concentrated to get recycling mixed organic acid solution close to 1.0L.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (8)
1. by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that include the following steps：
1) the waste lithium iron phosphate powder after drying is added to the aqueous solution based on the mixed organic acid of 0.1-5M at 50-95 DEG C
It is handled, and the solid-to-liquid ratio of mixed liquor is 40-200 grams per liter；It is obtained by filtration containing Li+、Fe2+、PO4 3-Acid solution；
2) it is added organic solvent in mother liquor, the volume ratio of organic solvent and mother liquor is 2:1-1:10, obtain LiFePO4 forerunner
Body slightly precipitates；
3) ferric lithium phosphate precursor is collected by filtration slightly to precipitate, is scattered in organic dispersing agent high-energy ball milling 0.5-8 hours, wherein phosphorus
It is 1 that sour iron lithium presoma, which is slightly precipitated with the solid-to-liquid ratio of organic dispersing agent,:3-1:1, by obtained slurry dry and remove after solvent in
600 DEG C -800 DEG C of calcinings 5-20 hours in atmosphere obtain regeneration lithium iron phosphate positive material；
4) filtrate in step 3) is recycled, based on the mixed organic acid by Separation of Organic/organic dispersing agent and after being concentrated
Aqueous solution be re-used for the dissolution of LiFePO4 in step 1)；
Between step 1) and step 2), follow the steps below：B) heating under reduced pressure concentration contains Li+、Fe2+、PO4 3-Acid solution,
At 45-98 DEG C, pressure is controlled in 0.1-0.5 atmospheric pressure, cocnentration factor 0.1-0.9 for temperature control；
Organic solvent in step 2) is the mixture of ethyl alcohol or ethyl alcohol and propyl alcohol.
2. as described in claim 1 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
Between step 1) and step b), follow the steps below：A) contain Li to above-mentioned+、Fe2+、PO4 3-Acid solution carry out titration or
Appropriate lithium salts and other necessary compounds are added based on the analysis results, makes for inductively coupled plasma atomic emission elemental analysis
The molar ratio of Li, Fe, P in solution reach 1-1.05:1:1-1.05.
3. as described in claim 1 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
The organic acid is one or more of formic acid, acetic acid, propionic acid, oxalic acid, citric acid, ascorbic acid.
4. as described in claim 1 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
It include one or more of ethyl alcohol, hydrogen peroxide, phosphoric acid in aqueous solution based on the mixed organic acid.
5. as described in claim 1 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
The atmosphere is the arbitrary proportion mixing of one or more of hydrogen, ammonia, nitrogen or argon gas gas.
6. as described in claim 1 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
The separation of the organic solvent/organic dispersing agent is using filtering, vacuum distillation, heating water bath or high-throughput chromatographic isolation means
One or more of combination, at 45-98 DEG C, the time is 1-10 hours for treatment temperature control.
7. by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that include the following steps：
1) the waste lithium iron phosphate powder after drying is added to the aqueous solution based on the mixed organic acid of 0.1-5M at 50-95 DEG C
It is handled, and the solid-to-liquid ratio of mixed liquor is 40-200 grams per liter；It is obtained by filtration containing Li+、Fe2+、PO4 3-Acid solution；
2) it is added organic solvent in mother liquor, the volume ratio of organic solvent and mother liquor is 2:1-1:10, obtain LiFePO4 forerunner
Body slightly precipitates；
It is further comprising the steps of between step 2) and step 3)：C) conductive agent is added in ferric lithium phosphate precursor slightly precipitates
Or conductive agent presoma, wherein conductive agent or conductive agent presoma additional amount and LiFePO4 mass ratio are 0-1:20, it is conductive
Agent or conductive agent presoma additional amount and LiFePO4 mass ratio are not 0, solid-to-liquid ratio 1:3-1:1；
3) step c) products therefrom is collected by filtration, is scattered in organic dispersing agent high-energy ball milling 0.5-8 hours, wherein step c) institute
The solid-to-liquid ratio for obtaining product and organic dispersing agent is 1:3-1:1, obtained slurry is dried and removed after solvent 600 DEG C in atmosphere-
800 DEG C calcining 5-20 hours, obtain regeneration lithium iron phosphate positive material；
4) filtrate in step 3) is recycled, based on the mixed organic acid by Separation of Organic/organic dispersing agent and after being concentrated
Aqueous solution be re-used for the dissolution of LiFePO4 in step 1)；
Between step 1) and step 2), follow the steps below：B) heating under reduced pressure concentration contains Li+、Fe2+、PO4 3-Acid solution,
At 45-98 DEG C, pressure is controlled in 0.1-0.5 atmospheric pressure, cocnentration factor 0.1-0.9 for temperature control；
Organic solvent in step 2) is the mixture of ethyl alcohol or ethyl alcohol and propyl alcohol.
8. as claimed in claim 7 by the method for the LiFePO4 reclaiming in waste and old lithium ion battery, which is characterized in that
The conductive agent is one of acetylene carbon black, graphitic carbon black, high structure abrasion resistant carbon black, graphene or carbon nanotube or one kind
Above combination；Conductive agent presoma is one of glucose, fructose, maltose or sucrose or more than one combinations.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106976852A (en) * | 2017-04-26 | 2017-07-25 | 长沙理工大学 | The green reparative regeneration technology of LiFePO 4 material in a kind of old and useless battery |
| CN108400401A (en) * | 2018-02-27 | 2018-08-14 | 四川省有色冶金研究院有限公司 | A method of using the active material of waste and old lithium dynamical battery separation as Material synthesis nickle cobalt lithium manganate |
| CN110649342B (en) * | 2018-06-26 | 2022-08-12 | 中天储能科技有限公司 | Method for recycling positive active material of waste lithium iron phosphate battery |
| CN109485027A (en) * | 2018-11-02 | 2019-03-19 | 新疆舰目摩托车有限公司 | A kind of recovery method of lithium cell anode material of lithium iron phosphate |
| CN112299387B (en) * | 2019-08-02 | 2022-05-13 | 惠州比亚迪实业有限公司 | Regenerated lithium iron phosphate positive electrode material and preparation method thereof |
| CN110620278B (en) * | 2019-09-25 | 2021-07-02 | 深圳清华大学研究院 | Method for recovering anode material of waste lithium iron phosphate battery |
| CN110760874B (en) * | 2019-10-16 | 2022-02-01 | 许昌学院 | Method for preparing iron oxide photo-anode film by using waste lithium iron phosphate battery |
| CN111732089A (en) * | 2020-08-27 | 2020-10-02 | 湖南长远锂科股份有限公司 | Preparation method of lithium iron phosphate |
| CN115784324B (en) * | 2022-11-29 | 2024-04-12 | 四川蜀矿环锂科技有限公司 | Method for recycling and preparing ternary positive electrode material precursor by using waste ternary lithium battery |
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