CN101359756B - Method for recycling lithium iron phosphate anode material from lithium ionic cell waste - Google Patents
Method for recycling lithium iron phosphate anode material from lithium ionic cell waste Download PDFInfo
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- CN101359756B CN101359756B CN2007101298982A CN200710129898A CN101359756B CN 101359756 B CN101359756 B CN 101359756B CN 2007101298982 A CN2007101298982 A CN 2007101298982A CN 200710129898 A CN200710129898 A CN 200710129898A CN 101359756 B CN101359756 B CN 101359756B
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
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Abstract
The invention relates to a method for recovering a lithium iron phosphate anode material in lithium ion battery scraps, comprising: roasting the scraps in the atmosphere of inert gases at a temperature of between 450 and 600 DEG C for 2 to 5 hours, wherein, the method also includes: adding the powdered products into an ethanol solution of soluble ferric salt for mixing, drying the mixture, then roasting the mixture in the atmosphere of inert gases at a temperature of between 300 and 500 DEG C for 2 to 5 hours, and obtaining the lithium iron phosphate anode material through recovery. The recovery method can be used to obtain the lithium iron phosphate anode material with rather high tap density, so the lithium ion secondary battery made by adopting the anode material has rather high capacity.
Description
Technical field
The present invention relates to the recovery method of lithium iron phosphate positive material in a kind of lithium ion battery waste material.
Background technology
At present, with the LiFePO4 lithium rechargeable battery of positive electrode because characteristics such as cost is low and security performance is good are progressively moved towards market, and begun to be widely used in the electrokinetic cell of notebook computer, electric tool and electric motor car.Along with being the application of the lithium rechargeable battery of positive electrode with the LiFePO4, the output of battery is in quick growth, and meeting produces a large amount of waste slurries and useless pole piece in the process of preparation battery.Therefore, for the recycling material, save cost and protect environment, the LiFePO4 that reclaims in the waste material becomes very necessary.
CN1585180A discloses a kind of recovery method of lithium ion secondary battery positive electrode defective material.The anodal leftover pieces machine relic that this method will be produced in the time of will preparing lithium rechargeable battery is heat-treated, and removes the adhesive between aluminium foil matrix and the positive electrode, adopts mechanical means that aluminium foil matrix and positive electrode are broken away from; Perhaps heat treated anode pole piece is placed in the distilled water, in utilizing methods such as ultrasonic oscillation or mechanical agitation to break away under the uniform temperature attached to positive electrode on the aluminium foil matrix and aluminium foil matrix, again positive electrode is separated, obtained the positive electrode that can directly use after the dried.But the capacity of the lithium rechargeable battery that the positive electrode that adopts this method to reclaim is made is lower.
CN1953269A discloses a kind of recycling waste lithium battery, and described method is that battery is emitted electric weight fully, the positive pole of split cell, negative pole and barrier film; It is characterized in that may further comprise the steps: (1) isolated positive pole is cut into fragment, places N-methyl pyrrolidone solution, stirs 2-5 hour under the 50-100 ℃ of temperature, isolate aluminium foil, after leaching positive electrode active materials, vacuum 100-140 ℃ of drying obtains the thick product of positive electrode active materials; (2) with thick product of the described positive electrode active materials of step (1) and Li
2CO
3Mechanical ball milling mixes, and calcines 10-24 hour in the air or oxygen atmosphere under 700-950 ℃ of temperature, is cooled to room temperature, obtains LiCoO after the grinding
2, thick product of described positive electrode active materials and Li
2CO
3The mass ratio that feeds intake be 3-5: 1.So can reclaim the positive electrode active materials of lithium ion battery.But the capacity of the lithium rechargeable battery that the positive electrode that adopts this method to reclaim is made is still lower.
Summary of the invention
The objective of the invention is to overcome the lower defective of capacity that resultant positive electrode in the recovery method of above-mentioned prior art makes lithium rechargeable battery, a kind of method that can obtain to make lithium iron phosphate positive material in the higher recovery lithium ion battery waste material of lithium ion secondary battery capacity is provided.
The invention provides the recovery method of lithium iron phosphate positive material in the lithium ion battery waste material, this method comprises, described waste material was toasted 2-5 hour down at 450-600 ℃ under inert gas atmosphere, wherein, this method also comprises, the powdered product that baking is obtained adds in the ethanolic solution of soluble ferric iron salt and mixes drying, then under inert gas atmosphere at 300-500 ℃ of following roasting 2-5 hour, reclaim and to obtain lithium iron phosphate positive material.
Adopt recovery method provided by the invention, the tap density of resulting lithium iron phosphate positive material is higher, thereby adopts the capacity of the lithium rechargeable battery that this positive electrode makes higher.Realize the raw-material recycling of LiFePO4, can save cost, and had the benefit of environmental protection.
Description of drawings
Fig. 1 is the XRD diffraction pattern of embodiment 1 resulting lithium iron phosphate positive material;
Fig. 2 is the sem photograph of embodiment 1 resulting lithium iron phosphate positive material.
Embodiment
The recovery method of lithium iron phosphate positive material comprises in the lithium ion battery waste material provided by the invention, described waste material was toasted 2-5 hour down at 450-600 ℃ under inert gas atmosphere, wherein, this method also comprises, the powdered product that baking is obtained adds in the ethanolic solution of soluble ferric iron salt and mixes, drying, then under inert gas atmosphere at 300-500 ℃ of following roasting 2-5 hour, reclaim and to obtain lithium iron phosphate positive material.
According to recovery method provided by the invention, described waste material comprises waste slurry and useless pole piece, waste slurry comprises the various iron phosphate lithium positive pole slurries that prepare in the mode of oil system or water system, and useless pole piece comprises the useless pole piece of disassembling out in useless pole piece, leftover pieces and the waste battery that produces in the production process.When in the waste material that needs reclaim useless pole piece being arranged,, isolate from collector with sieve and to peel off the material that gets off, and sort out collector simultaneously, so also recyclable collector through after the above-mentioned baking.When the waste material that need reclaim is waste slurry,, then need not sieve, directly carry out following step through after the above-mentioned baking.
According to recovery method provided by the invention, in the preferred case, the concentration of soluble ferric iron salt is 0.01-0.2mol/L, is preferably 0.05-0.15mol/L in the ethanolic solution of described soluble ferric iron salt, described soluble ferric iron salt can be ferrous iron and/or ferric various water-soluble salt, for example one or more in sulfate, chloride and the nitrate.
According to recovery method provided by the invention, in the preferred case, described method also comprises, resulting lithium iron phosphate positive material is mixed with lithium source and/or phosphorus source, oven dry, 550-750 ℃ of following roasting, the time of roasting is 3-10 hour under inert gas atmosphere.In the preferred case, adopt ball milling to mix resulting lithium iron phosphate positive material and mixing of lithium source and/or phosphorus source, the medium that ball milling mixes can be the various media that well known to a person skilled in the art, for example one or more in absolute ethyl alcohol, acetone and the deionized water.
According to recovery method provided by the invention, in the preferred case, the molal quantity in employed lithium source or phosphorus source is the 0.1-3% of the molal quantity of the described LiFePO4 that obtains, is preferably 0.5-2.0%.
According to recovery method provided by the invention, described lithium source can be the various lithium sources that are used for the solid phase synthesis LiFePO4 that well known to a person skilled in the art, for example one or more in lithium carbonate, lithium hydroxide, lithium oxalate, lithium acetate, lithium fluoride, lithium bromide, lithium iodide and the lithium dihydrogen phosphate; Described phosphorus source can be the various phosphorus sources that are used for the solid phase synthesis LiFePO4 that well known to a person skilled in the art, for example one or more in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate and the lithium dihydrogen phosphate.
According to recovery method provided by the invention, in the preferred case, this method also comprises, the described lithium iron phosphate positive material that obtains is mixed with carbon source, and oven dry, 550-750 ℃ of following roasting, the time of roasting is 3-10 hour under inert gas atmosphere.
According to recovery method provided by the invention, in the preferred case, this method also comprises, before oven dry and roasting, carbon source is mixed with the mixture of the described lithium iron phosphate positive material that obtains with lithium source and/or phosphorus source.
According to recovery method provided by the invention, in the preferred case, the molal quantity of the carbon source of using is the 0.1-3% of the molal quantity of the described LiFePO4 that obtains, and described carbon source is one or more in carbon black, acetylene black, graphite and the carbohydrate.Carry out the lithium iron phosphate positive material that carbon coats like this, can improve the conductivity of lithium iron phosphate positive material.
According to recovery method provided by the invention, described inert gas is for well known to a person skilled in the art various inert gases, for example one or more in nitrogen, helium, neon, argon gas, krypton gas, xenon and the radon gas.
According to of the present invention preferred embodiment various, relatively poor at the electrical property of LiFePO4 own, the shortcoming that density is lower, the various shortcomings of LiFePO4 in removal process, have been solved targetedly, thereby reach every standard of utilizing again, can directly be used as the positive electrode active materials of lithium rechargeable battery.
Adopt the mode of embodiment to describe the present invention in more detail below.
Embodiment 1
Getting 10kg iron phosphate lithium positive pole waste slurry, in the charging tray of packing into, put into the high temperature resistance furnace under the nitrogen atmosphere, is 450 ℃ of baking 5h down in furnace temperature, cools off with stove then.The concentration that the material of cooling is joined ferric nitrate is to stir in the ethanolic solution of ferric nitrate of 0.15mol/L, treat that ethanol is evaporated completely after, the charging tray of packing into, be placed in the high temperature resistance furnace under the nitrogen atmosphere, in furnace temperature is 350 ℃ of baking 5h down, with the stove cooling, obtains lithium iron phosphate positive material then.
Adopt the X-ray diffractometer of Japanese D/MAX2200PC type of science to test to this product, resulting diffraction pattern as shown in Figure 1, as can be seen from the figure, the diffraction maximum of the standard LiFePO4 of diffraction maximum that top is tested and bottom is basic identical, and the main peak peak is higher by force, half-peak breadth (the B value is 0.178) is narrower, illustrates that its crystal is very complete.Adopt ESEM (the KYKY2800 type that Beijing instrument plant of the Chinese Academy of Sciences produces) to observe to this product, resulting sem photograph as shown in Figure 2, as can be seen from the figure, particle is more even, the surface is more smooth, and individual particle is dense.
Getting 10kg LiFePO4 waste slurry, in the charging tray of packing into, put into the high temperature resistance furnace under the nitrogen atmosphere, is 450 ℃ of baking 5h down in furnace temperature, cools off with stove then.The concentration that the material of cooling is joined ferric nitrate is to stir in the ethanolic solution of ferric nitrate of 0.2mol/L, treat that ethanol is evaporated completely after, the charging tray of packing into is placed in the high temperature resistance furnace nitrogen atmosphere under, is 350 ℃ in furnace temperature and toasts 5h down, cools off with stove then.
Then the resulting material of 5kg is joined in the ball grinder, take by weighing lithium carbonate 70.6g and ammonium di-hydrogen phosphate 109.4g respectively by 3% of 5kg LiFePO4 molal quantity, all join in the ball grinder, add alcohol and pick ball again, take out the material that mixes behind the ball milling 2h, 60 ℃ of oven dry down.The material that to dry is put in the high temperature resistance furnace under the nitrogen atmosphere at last, and the roasting temperature 10h at 650 ℃ cools to room temperature then with the furnace, promptly obtains lithium iron phosphate positive material.
Use respectively and with embodiment 1 employed identical X-ray diffractometer and ESEM resulting lithium iron phosphate positive material is tested, resulting XRD diffraction pattern is similar substantially to Fig. 1, and resulting sem photograph is to similar substantially as Fig. 2.The diffraction maximum of the XRD diffraction pattern of being tested is the LiFePO4 diffraction maximum, and its peak is by force all more than 1340, and half-peak breadth B value illustrates that below 0.18 crystalline form is all very complete.From sem photograph as can be seen, resulting lithium iron phosphate positive material pattern surface is more smooth, uniform particles, and individual particle is fine and close.
Embodiment 3
Getting the iron phosphate lithium positive pole sheet of scrapping in the 10kg production, in the charging tray of packing into, put into the high temperature resistance furnace under the nitrogen atmosphere, is 550 ℃ of baking 4h down in furnace temperature, cools off with stove then.Pole piece after the baking is put on the screen cloth that mesh is 5mm, rubs pole piece, and rock sieve frequently, material is thoroughly separated with collector.The concentration that the powder that obtains is joined ferric nitrate is to stir in the ethanolic solution of ferric nitrate of 0.1mol/L, treat that ethanol is evaporated completely after, the charging tray of packing into is placed in the high temperature resistance furnace under the nitrogen atmosphere, is 400 ℃ of baking 4h down in furnace temperature, cools off with stove then.
Then the resulting material of 5kg is joined in the ball grinder, take by weighing Lithium hydroxide monohydrate 26g respectively by 2% of 5kg LiFePO4 molal quantity, diammonium hydrogen phosphate 84.3g and acetylene black 7.6g, all join in the ball grinder, add alcohol and pick ball again, take out the material that mixes behind the ball milling 2h, 60 ℃ of oven dry down.The material that to dry is put in the high temperature resistance furnace under the nitrogen atmosphere at last, and the roasting temperature 6h at 750 ℃ cools to room temperature then with the furnace, promptly obtains lithium iron phosphate positive material.
Use respectively and with embodiment 1 employed identical X-ray diffractometer and ESEM resulting lithium iron phosphate positive material is tested, resulting XRD diffraction pattern is similar substantially to Fig. 1, and resulting sem photograph is to similar substantially as Fig. 2.The diffraction maximum of the XRD diffraction pattern of being tested is the LiFePO4 diffraction maximum, and its peak is by force all more than 1340, and half-peak breadth B value illustrates that below 0.18 crystalline form is all very complete.From sem photograph as can be seen, resulting lithium iron phosphate positive material pattern surface is more smooth, uniform particles, and individual particle is fine and close.
Embodiment 4
Getting the iron phosphate lithium positive pole sheet of scrapping in the 10kg production, in the charging tray of packing into, put into the high temperature resistance furnace under the nitrogen atmosphere, is 600 ℃ of baking 2h down in furnace temperature, cools off with stove then.Pole piece after the baking is put on the screen cloth that mesh is 5mm, rubs pole piece, and rock sieve frequently, the material on the collector is thoroughly separated with collector.The concentration that the powder that obtains is joined iron chloride is to stir in the ethanolic solution of iron chloride of 0.05mol/L, treat that ethanol is evaporated completely after, the charging tray of packing into is put into the high temperature resistance furnace under the nitrogen atmosphere, is 500 ℃ of baking 4h down in furnace temperature, cools off with stove then.
Then the resulting material of 5kg is joined in the ball grinder, take by weighing lithium dihydrogen phosphate 32.94g, join in the ball grinder, add alcohol and pick ball, take out the material that mixes behind the ball milling 2h, 60 ℃ of oven dry down by 1% of 5kg LiFePO4 molal quantity.The material that to dry is put in the high temperature resistance furnace under the nitrogen atmosphere at last, and the roasting temperature 4h at 600 ℃ cools to room temperature then with the furnace, promptly obtains lithium iron phosphate positive material.
Use respectively and with embodiment 1 employed identical X-ray diffractometer and ESEM resulting lithium iron phosphate positive material is tested, resulting XRD diffraction pattern is similar substantially to Fig. 1, and resulting sem photograph is to similar substantially as Fig. 2.The diffraction maximum of the XRD diffraction pattern of being tested is the LiFePO4 diffraction maximum, and its peak is by force all more than 1340, and half-peak breadth B value illustrates that below 0.18 crystalline form is all very complete.From sem photograph as can be seen, resulting lithium iron phosphate positive material pattern surface is more smooth, uniform particles, and individual particle is fine and close.
Comparative Examples 1
Getting 10kg LiFePO4 waste slurry, in the charging tray of packing into, put into the high temperature resistance furnace under the nitrogen atmosphere, is 450 ℃ of baking 5h down in furnace temperature, cools off with stove then.Then the resulting material of 5kg is joined in the ball grinder, take by weighing Lithium hydroxide monohydrate 26g respectively by 2% of 5kg LiFePO4 molal quantity, diammonium hydrogen phosphate 84.3g, acetylene black 7.6g all joins in the ball grinder, add alcohol and pick ball again, take out the material that mixes behind the ball milling 2h, in following 60 ℃ of oven dry.The material that to dry is put in the high temperature resistance furnace under the nitrogen atmosphere at last, and the roasting temperature 10h at 650 ℃ cools to room temperature then with the furnace, promptly obtains lithium iron phosphate positive material.
Performance test
1, test density
Adopt the tap density of homemade stainless steel tap density tester specimen.The cylindrical shell of tester is divided into test cylindrical shell and auxiliary cylindrical shell two parts, and the volume of wherein testing cylindrical shell is 50cm
3, quality is 165.2g.
During test, sample is packed in the cylindrical shell in the tester, whole cylindrical shell is lifted vertically upward the height of 30cm, allow it freely fall then, and repeat 40 times, take off the auxiliary cylindrical shell that is enclosed within on the test cylindrical shell then, be put in horizontal level, wipe unnecessary material on the test cylindrical shell with scraper sideling off with miter angle, and remove all in appearance powders of cylindrical shell, and it is weighed, deduct the cylindrical shell sole mass then, promptly obtain the mass M of powder, tap density is M/50 (g/cm
3), each sample test three times is averaged.
To embodiment 1-4 and the Comparative Examples 1 lithium iron phosphate positive material test density that obtains that reclaims, the results are shown in Table 1 for gained according to the method described above.
Table 1
| (g/cm for the first time 3) | (g/cm for the second time 3) | (g/cm for the third time 3) | Mean value (g/cm 3) | |
| Embodiment 1 | 1.62 | 1.61 | 1.62 | 1.62 |
| |
1.60 | 1.61 | 1.62 | 1.61 |
| Embodiment 3 | 1.66 | 1.68 | 1.68 | 1.67 |
| Embodiment 4 | 1.64 | 1.65 | 1.64 | 1.64 |
| Comparative Examples 1 | 1.09 | 1.08 | 1.08 | 1.08 |
2, test battery capacity
Respectively with embodiment 1-4 and Comparative Examples 1 prepared lithium iron phosphate positive material be to mix at 80: 15: 5 as conductive agent acetylene black with as 60% ptfe emulsion of binding agent by mass ratio.As dispersant, supersonic oscillations 15 minutes mix them with absolute ethyl alcohol, make the about 1cm of area
2, thickness is less than the disk of 1mm, and it is pressed on the collector aluminium foil constitutes positive plate, at 120 ℃ of following vacuumize 8h.
Be negative pole again with the metal lithium sheet, microporous polypropylene membrane (2300) is a barrier film, electrolyte is the mixed solution of lithium hexafluoro phosphate ethylene carbonate+diethyl carbonate+dimethyl carbonate (volume ratio is 1: 1: 1), wherein the concentration of lithium hexafluoro phosphate is 1mol/L, be mounted to 2032 type button cells in the glove box of applying argon gas, every kind of positive electrode is made ten button cells.Be 0.05 to carry out charge-discharge test with charge-discharge magnification respectively, voltage range is 2.5-3.8v.
Test the average specific discharge capacity and the average first charge-discharge efficiency of the button cell of being made by the positive electrode of embodiment 1-4 and Comparative Examples 1 respectively, the results are shown in Table 2 for gained.
Table 2
| Positive electrode | Average specific discharge capacity (mAh/g) | Average first charge-discharge efficiency (%) |
| Embodiment 1 | 147.9 | 90.2 |
| |
150.6 | 92.7 |
| Embodiment 3 | 153.8 | 94.9 |
| Embodiment 4 | 149.2 | 93.1 |
| Comparative Examples 1 | 119.9 | 87.5 |
The specific discharge capacity computing formula is:
The quality (g) of specific discharge capacity=discharge capacity (mA)/sample
The computing formula of first charge-discharge efficiency is:
First charge-discharge efficiency=discharge capacity (mA)/charging capacity (mA) * 100%
By the data of table 1 as can be seen, the density of the resulting lithium iron phosphate positive material of embodiment 1-4 is bigger than the density of Comparative Examples 1 resulting lithium iron phosphate positive material.
From the data of table 2 as can be seen, the resulting lithium iron phosphate positive material of embodiment 1-4 makes Capacity Ratio Comparative Examples 1 big a lot of of lithium rechargeable battery.
Therefore, adopt the density of the resulting lithium iron phosphate positive material of recovery method of the present invention very big, thus also very big by the capacity of the resulting lithium rechargeable battery of this positive electrode, and can directly make lithium rechargeable battery as positive electrode.
Claims (9)
1. the recovery method of lithium iron phosphate positive material in the lithium ion battery waste material, this method comprises, with described waste material at nitrogen, helium, neon, argon gas, krypton gas, toasted 2-5 hour down at 450-600 ℃ under the atmosphere of one or more in xenon and the radon gas, it is characterized in that, this method also comprises, the powdered product that baking is obtained adds in the ethanolic solution of soluble ferric iron salt and mixes, dry, then at nitrogen, helium, neon, argon gas, krypton gas, under the atmosphere of one or more in xenon and the radon gas at 300-500 ℃ of following roasting 2-5 hour, recovery obtains lithium iron phosphate positive material, and described waste material is the useless pole piece of LiFePO4 waste slurry and/or LiFePO4.
2. method according to claim 1, wherein, the concentration of soluble ferric iron salt is 0.01-0.2mol/L in the ethanolic solution of described soluble ferric iron salt, and described soluble ferric iron salt is one or more in ferrous iron and/or ferric sulfate, chloride and the nitrate.
3. method according to claim 2, wherein, the concentration of soluble ferric iron salt is 0.05-0.15mol/L in the ethanolic solution of described soluble ferric iron salt.
4. method according to claim 1, wherein, described method also comprises, resulting lithium iron phosphate positive material is mixed with lithium source and/or phosphorus source, the oven dry, under the atmosphere of one or more in nitrogen, helium, neon, argon gas, krypton gas, xenon and radon gas 550-750 ℃ of following roasting.
5. method according to claim 4, wherein, the molal quantity in employed lithium source or phosphorus source is the 0.1-3% of the molal quantity of the described LiFePO4 that obtains.
6. method according to claim 5, wherein, the molal quantity in described lithium source or phosphorus source is the 0.5-2.0% of the molal quantity of the described LiFePO4 that obtains.
7. according to claim 4,5 or 6 described methods, wherein, described lithium source is one or more in lithium carbonate, lithium hydroxide, lithium oxalate, lithium acetate, lithium fluoride, lithium bromide, lithium iodide and the lithium dihydrogen phosphate; Described phosphorus source is one or more in ammonium phosphate, diammonium hydrogen phosphate, ammonium dihydrogen phosphate and the lithium dihydrogen phosphate.
8. method according to claim 1, wherein, this method also comprises, the described lithium iron phosphate positive material that obtains is mixed with carbon source, the oven dry, under the atmosphere of one or more in nitrogen, helium, neon, argon gas, krypton gas, xenon and radon gas 550-750 ℃ of following roasting; The molal quantity of the carbon source of using is the 0.1-3% of the molal quantity of the described LiFePO4 that obtains, and described carbon source is one or more in carbon black, acetylene black, graphite and the carbohydrate.
9. method according to claim 4, wherein, this method also comprises, before oven dry and roasting, carbon source is mixed with the mixture of the described lithium iron phosphate positive material that obtains with lithium source and/or phosphorus source, the molal quantity of the carbon source of using is the 0.1-3% of the molal quantity of the described LiFePO4 that obtains, and described carbon source is one or more in carbon black, acetylene black, graphite and the carbohydrate.
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| CN101916889B (en) * | 2010-08-16 | 2012-05-30 | 长春劲能锂电池科技有限公司 | Method for preparing iron lithium phosphate by recovering water-system waste lithium-ion power battery |
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