CN101383441B - Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell - Google Patents
Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell Download PDFInfo
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- CN101383441B CN101383441B CN2007100768904A CN200710076890A CN101383441B CN 101383441 B CN101383441 B CN 101383441B CN 2007100768904 A CN2007100768904 A CN 2007100768904A CN 200710076890 A CN200710076890 A CN 200710076890A CN 101383441 B CN101383441 B CN 101383441B
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- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000002699 waste material Substances 0.000 title claims abstract description 15
- 229910052744 lithium Inorganic materials 0.000 title claims description 24
- 239000005955 Ferric phosphate Substances 0.000 title claims description 15
- 229940032958 ferric phosphate Drugs 0.000 title claims description 15
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 title claims description 15
- 229910000399 iron(III) phosphate Inorganic materials 0.000 title claims description 15
- 239000000463 material Substances 0.000 claims abstract description 37
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 22
- 238000004519 manufacturing process Methods 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims abstract description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- 239000012634 fragment Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 5
- 239000006258 conductive agent Substances 0.000 claims description 18
- 239000000853 adhesive Substances 0.000 claims description 17
- 230000001070 adhesive effect Effects 0.000 claims description 17
- 239000005030 aluminium foil Substances 0.000 claims description 17
- 238000013467 fragmentation Methods 0.000 claims description 15
- 238000006062 fragmentation reaction Methods 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000012216 screening Methods 0.000 claims description 6
- 239000000428 dust Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 239000004411 aluminium Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000011363 dried mixture Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 235000013312 flour Nutrition 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 abstract description 9
- 239000010405 anode material Substances 0.000 abstract description 8
- 230000000694 effects Effects 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 4
- 230000009514 concussion Effects 0.000 abstract 1
- 239000011888 foil Substances 0.000 abstract 1
- 239000007789 gas Substances 0.000 abstract 1
- 239000011261 inert gas Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 238000003466 welding Methods 0.000 abstract 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 9
- 230000004087 circulation Effects 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- 238000010586 diagram Methods 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 7
- 239000002994 raw material Substances 0.000 description 5
- 229910052493 LiFePO4 Inorganic materials 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 239000002033 PVDF binder Substances 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- ZSYNKHJUSDFTCQ-UHFFFAOYSA-N [Li].[Fe].P(O)(O)(O)=O Chemical compound [Li].[Fe].P(O)(O)(O)=O ZSYNKHJUSDFTCQ-UHFFFAOYSA-N 0.000 description 2
- 239000010941 cobalt Substances 0.000 description 2
- 229910017052 cobalt Inorganic materials 0.000 description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910012851 LiCoO 2 Inorganic materials 0.000 description 1
- 229910015645 LiMn Inorganic materials 0.000 description 1
- 229910014689 LiMnO Inorganic materials 0.000 description 1
- 229910013290 LiNiO 2 Inorganic materials 0.000 description 1
- 229910018095 Ni-MH Inorganic materials 0.000 description 1
- 229910018477 Ni—MH Inorganic materials 0.000 description 1
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OJIJEKBXJYRIBZ-UHFFFAOYSA-N cadmium nickel Chemical compound [Ni].[Cd] OJIJEKBXJYRIBZ-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000001473 noxious effect Effects 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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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
-
- 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
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/84—Recycling of batteries or fuel cells
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- Battery Electrode And Active Subsutance (AREA)
- Secondary Cells (AREA)
Abstract
The invention relates to a synthesized recovery method for waste positive plates of iron phosphate lithium batteries. The method comprises the following steps: collected waste positive plate material is mechanically crashed into fragments; the fragments are positioned in a welding furnace which is protected by vacuum atmosphere, inert gases and/or reducing gases and/or nitrogen and are heat processed in the temperature of 150-750 DEG C; aluminum foil basal bodies are separated from the fragments after heat process by adopting mechanical separation or ultrasonic concussion to obtain a mixture of iron phosphate lithium positive material, conduction agent and caking agent giblets; the mixture of iron phosphate lithium anode material, conduction agent and caking agent giblets is roasted for 8-24 hrs in 80-150 DRG C; the mixture after roasting is classified to control the grain diameter of the powder material to be not more than 20 microns, and the D50 is controlled to be 3-10 microns so as to obtain iron phosphate lithium positive recovery material. The method has simple technique, takes effect fast and reduces the material consumption and production cost of a manufacturer.
Description
[technical field]
The present invention relates to a kind of recovery method of battery material, relate in particular to a kind of comprehensive recovering process of positive pole waste tablet from ferric phosphate lithium cell.
[background technology]
The fast development of electronic technology makes and also is used widely day by day for various portable type electronic products provide the lithium battery of power supply, and lithium battery has replaced the main flow that nickel-cadmium cell and Ni-MH battery become commercial secondary cell in the small-sized secondary batteries field at present.Sustainable growth along with the lithium battery consumption, leftover bits that produce in lithium battery manufacturing process and relic are also more and more, a lot of lithium battery manufacturers and waste disposal unit are to the processing of this class industrial waste, also only rest at present and carry out simple soda acid processing with on the recovery section lithium salts, this processing mode not only can't obtain resource regeneration to greatest extent, the economic benefit that also can cause certain environmental pollution simultaneously and reduce producer.
Present most lithium ion battery all adopts LiCoO
2, LiNiO
2, LiMn
2O
4, LiMnO
2Deng as positive electrode, developed corresponding useless sheet recovery method at the positive electrode of these types in the industry, disclose the recovery method that is fit to this type of anode material waste sheet as Chinese patent literature CN1206765 and CN1585180 etc.Yet the positive electrode of dissimilar lithium ions has the characteristic of himself, and disclosed method is not the recovery that is applicable to the anode material waste sheet of all types lithium ion in the above-mentioned document.
Lithium iron phosphate positive material owing to have extra long life, fast charging and discharging, high temperature resistant, big capacity, characteristics such as memoryless, safe in utilization become the most good anode material of lithium battery in current market, have become to make the first-selection of lithium battery.In the manufacture process of ferric phosphate lithium cell, usually can or cut in the coating of lithium iron phosphate positive material and the compressing tablet process and produce a large amount of leftover pieces and useless sheet because of test piece, broken belt, the loss late of material can reach 3-6% in the whole process for making.These useless sheets not only cause the wasting of resources, increase the cost pressure of battery producer, can cause environmental pollution if it is dealt with improperly also, and known method and be not suitable for the recycling of this type of anode material waste sheet at present.
[summary of the invention]
At at present ferric phosphate lithium cell anode material waste sheet being lacked a kind of this present situation of effective recovery and treatment method, the invention provides that a kind of technology is simple, production cost is low, the comprehensive recovering process of environment amenable positive pole waste tablet from ferric phosphate lithium cell.
For achieving the above object, the invention provides a kind of comprehensive recovering process of positive pole waste tablet from ferric phosphate lithium cell, comprise following steps:
Use disintegrating machine to carry out fragmentation the useless sheet of the positive pole of collecting in the ferric phosphate lithium cell production, broken pole piece granular size after the fragmentation is controlled at 4-8cm, anodal fragment after the fragmentation is placed Muffle furnace heat treatment 6hrs under 400 ℃ temperature of nitrogen protection, make the adhesive failure in the pole piece; Adopt vibrating screen to sieving through the useless sheet of heat treated positive pole, screenings promptly is the mixture of lithium iron phosphate positive material, conductive agent and adhesive residue thing, and oversize is aluminium foil, anodal material block and attached to the anodal material of aluminium foil surface.
Above-mentioned gained oversize is immersed among 45 ℃ the NMP, and keeps stirring 1h, realize that lithium iron phosphate positive material, conductive agent and adhesive residue thing peel off from aluminium foil, isolated aluminium foil send the smelter to reclaim metallic aluminium; Continue to stir 1h, make the dispersion of fully loosening of block cathode mixture; Lithium iron phosphate positive material, conductive agent and adhesive residue thing toast 10hrs after filtering under 150 temperature; With flour mill dried mixture is carried out classification behind the abrasive dust 2hrs, the particle diameter of controlling qualified powder is not more than 20 μ m, D
50Be controlled at 3～10 μ m.
The beneficial effect that comprehensive recovering process brought of positive pole waste tablet from ferric phosphate lithium cell provided by the invention is, realized the comprehensive reutilization of the useless sheet of lithium iron phosphate positive material, avoided the noxious waste pollution that may cause, also do not caused secondary pollution in useless sheet recycling process; Iron phosphate lithium positive pole reclaimed materials and the regular burden(ing) of handling gained through the inventive method have close chemical property; Realized the recovery of aluminium foil matrix simultaneously; This method technology is simple, production cost is low, instant effect, has reduced the material consumption of ferric phosphate lithium cell manufacturer and the production cost of battery, has realized that economic benefit combines with the harmony of environment social benefit.
[description of drawings]
Shown in Figure 1 is the X-ray diffractogram of iron lithium phosphate raw material;
Shown in Figure 2 is the scanning electron microscope diagram of iron lithium phosphate raw material;
Shown in Figure 3 is the X-ray diffractogram of isolated phosphoric acid iron lithium anode material mixture in the first embodiment of the invention;
Shown in Figure 4 is the scanning electron microscope diagram of isolated phosphoric acid iron lithium anode material mixture in the first embodiment of the invention;
Shown in Figure 5 is 350 circulation volume conservation rate schematic diagrames that adopt the battery of non-salvage material production;
Shown in Figure 6 is 350 circulation volume conservation rate schematic diagrames that adopt the battery that the salvage material of first embodiment of the invention gained produces;
Shown in Figure 7 is 350 circulation volume conservation rate schematic diagrames that adopt the battery that the salvage material of second embodiment of the invention gained produces;
Shown in Figure 8 is 350 circulation volume conservation rate schematic diagrames that adopt the battery that the salvage material of third embodiment of the invention gained produces.
[embodiment]
Embodiment 1:
Use disintegrating machine to carry out fragmentation the useless sheet of the positive pole of collecting in the ferric phosphate lithium cell production, the broken pole piece granular size after the fragmentation is controlled at 0.5-3cm.Anodal fragment after the fragmentation is placed the Muffle furnace of nitrogen protection, and heat treatment 8hrs under 600 ℃ temperature decomposes the adhesive failure in the pole piece.Use vibrating screen to sieving through the useless sheet of heat treated positive pole, screenings promptly is the mixture of lithium iron phosphate positive material, conductive agent, adhesive residue thing, and oversize is that aluminium foil, anodal material block are reaching still the anodal material that is attached to aluminium foil surface.XRD figure of screenings (X-ray diffractogram) and SEM figure (scanning electron microscope diagram) are as shown in Figure 3 and Figure 4, scheme (Fig. 2) more as can be known with the XRD figure (Fig. 1) and the SEM of LiFePO4 raw material, the position at both X-ray diffraction peaks and feature basically identical, but sieve down the diffraction peak intensity of mixture than the LiFePO4 raw material a little less than, illustrate that sieve contains more its class materials in the mixture down, is mainly conductive agent and small amount of binder residue; From SEM figure as can be seen sieve down in the mixture the circumgranular conductive agent of LiFePO4 obviously many than the carbon content in the LiFePO4 raw material.
Above-mentioned gained screenings is carried out the abrasive dust classification, and the particle diameter of controlling qualified powder is not more than 20 μ m, and D50 is controlled at 1-10 μ m.Press qualified powder: binding agent: NMP=100: 4: 100 mass ratio, with addition of PVDF binding agent and solvent, by the production technology production of preparing burden, the 1C cycle performance of obtained battery as shown in Figure 6, after 350 circulations, capability retention is 95.2%, and 350 circulation volume conservation rates of ordinary production battery are 96.4% (see figure 5), both are more or less the same, and all have excellent cycle performance.
Embodiment 2:
Use disintegrating machine to carry out fragmentation the useless sheet of the positive pole of collecting in the ferric phosphate lithium cell production, the broken pole piece granular size after the fragmentation is controlled at 4-8cm.Anodal fragment after the fragmentation is placed Muffle furnace heat treatment 6hrs under 400 ℃ temperature of nitrogen protection, make the adhesive failure in the pole piece.Adopt vibrating screen to sieving through the useless sheet of heat treated positive pole, screenings promptly is the mixture of lithium iron phosphate positive material, conductive agent, adhesive residue thing, and oversize is aluminium foil, anodal material block and attached to the anodal material of aluminium foil surface.
Above-mentioned gained oversize is immersed among 45 ℃ the NMP, and keeps stirring 1h, can realize that lithium iron phosphate positive material, conductive agent and adhesive residue thing peel off from aluminium foil, isolated aluminium foil send the smelter to reclaim metallic aluminium.Continue to stir 1h, make the dispersion of fully loosening of block cathode mixture.Lithium iron phosphate positive material, conductive agent and adhesive residue thing toast 10hrs after filtering under 150 temperature.With flour mill dried mixture is carried out classification behind the abrasive dust 2hrs, the particle diameter of controlling qualified powder is not more than 20 μ m, and D50 is controlled at 3～10 μ m.Press qualified powder: conductive agent: binding agent: NMP=100: 1: 4: 100 mass ratio, with addition of conductive agent V7, PVDF binding agent and solvent, by the production technology production of preparing burden, the 1C cycle performance of obtained battery as shown in Figure 7, after 350 circulations, capability retention is 92.7%, though that its cycle performance is more normally produced cycle performance of battery is poor, with the cobalt acid lithium battery that is far superior to the current production rate maximum.
Embodiment 3:
Use disintegrating machine to carry out fragmentation the useless sheet of the positive pole of collecting in the ferric phosphate lithium cell production, the broken pole piece granular size after the fragmentation is controlled at 4-8cm.Anodal fragment after the fragmentation is placed the Muffle furnace of nitrogen protection, and heat treatment 5hrs under 500 ℃ temperature makes the adhesive failure in the pole piece.
Useless pole piece after the heat treatment is immersed among 60 ℃ the NMP, and keeps stirring 0.5h, can realize that lithium iron phosphate positive material, conductive agent and adhesive residue thing peel off from aluminium foil, isolated aluminium foil send the smelter to reclaim metallic aluminium.Continue to stir 2hrs, make the dispersion of fully loosening of block cathode mixture.Lithium iron phosphate positive material, conductive agent and adhesive residue thing toast 20hrs after filtering under 120 temperature.With flour mill dried mixture is carried out classification behind the abrasive dust 2hrs, the particle diameter of controlling qualified powder is not more than 20 μ m, and D50 is controlled at 3-10 μ m.Press qualified powder: conductive agent: binding agent: NMP=100: 1: 4: 100 mass ratio, with addition of conductive agent V7, PVDF binding agent and solvent, by the production technology production of preparing burden, the 1C cycle performance of obtained battery as shown in Figure 8, after 350 circulations, capability retention is 92.1%, and cycle performance obviously is better than the cobalt acid lithium battery of current production rate maximum, realizes effectively comprehensively reclaiming of anodal useless sheet.
The above embodiment has only expressed several execution mode of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that for the person of ordinary skill of the art without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection range of patent of the present invention should be as the criterion with claims.
Claims (1)
1. the comprehensive recovering process of a positive pole waste tablet from ferric phosphate lithium cell is characterized in that, comprises following steps:
Use disintegrating machine to carry out fragmentation the useless sheet of the positive pole of collecting in the ferric phosphate lithium cell production, broken pole piece granular size after the fragmentation is controlled at 4-8cm, anodal fragment after the fragmentation is placed Muffle furnace heat treatment 6hrs under 400 ℃ temperature of nitrogen protection, make the adhesive failure in the pole piece; Adopt vibrating screen to sieving through the useless sheet of heat treated positive pole, screenings promptly is the mixture of lithium iron phosphate positive material, conductive agent and adhesive residue thing, and oversize is aluminium foil, anodal material block and attached to the anodal material of aluminium foil surface;
Above-mentioned gained oversize is immersed among 45 ℃ the NMP, and keeps stirring 1h, realize that lithium iron phosphate positive material, conductive agent and adhesive residue thing peel off from aluminium foil, isolated aluminium foil send the smelter to reclaim metallic aluminium; Continue to stir 1h, make the dispersion of fully loosening of block cathode mixture; Lithium iron phosphate positive material, conductive agent and adhesive residue thing toast 10hrs after filtering under 150 temperature; With flour mill dried mixture is carried out classification behind the abrasive dust 2hrs, the particle diameter of controlling qualified powder is not more than 20 μ m, D
50Be controlled at 3～10 μ m.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100768904A CN101383441B (en) | 2007-09-06 | 2007-09-06 | Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007100768904A CN101383441B (en) | 2007-09-06 | 2007-09-06 | Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell |
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| Publication Number | Publication Date |
|---|---|
| CN101383441A CN101383441A (en) | 2009-03-11 |
| CN101383441B true CN101383441B (en) | 2011-10-26 |
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