CN103449395A - Method for recycling positive material from water-system waste lithium iron phosphate battery - Google Patents
Method for recycling positive material from water-system waste lithium iron phosphate battery Download PDFInfo
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Abstract
The invention discloses a method for recycling a positive material from a water-system waste lithium iron phosphate battery. The method comprises the following steps: elaborately disassembling fully-discharged waste lithium iron phosphate battery to obtain an undamaged positive plate, separating a positive active material from a current collector in a way of immersing through deionized water, and drying and ball-milling the active material to obtain a lithium iron phosphate positive material to be recycled; respectively testing carbon content and ratio of Li, Fe and P elements of the lithium iron phosphate positive material to be recycled, adding a lithium source and an iron source, adjusting a mole ratio of Li to Fe to P to be (1.0-1.1):1:1, further adding the lithium source, the ion source and the phosphate source according to a ratio of 1:1:1 and adjusting C content ratio in the material; and performing ball milling, low-temperature pre-sintering and high-temperature sintering on the material of which ratio of the elements is adjusted to obtain the recycled lithium iron phosphate positive material. The recycled material has the advantages that 0.1C discharging capability can reach up to 156mAh/g, 2C discharging capability can reach up to 120mAh/g, the retention ratio of 0.1C discharging capability after 50 times of recycling is greater than 99% and various electrochemical properties are excellent. The method disclosed by the invention is low in cost and simple in process; the secondary pollution is avoided.
Description
Technical field
The present invention relates to a kind of from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, belong to waste and old lithium ion battery recycling field.
Background technology
Lithium ion battery has that operating voltage is high, energy density is large, have extended cycle life, the excellent specific properties such as self-discharge rate is low, low pollutions, memory-less effect, is the research and development of secondary cell in the world today and applies focus.Along with the lithium ion battery use range is more and more wider, because of the waste and old lithium ion battery that end of life produces also increasing.Electrolytic solution in waste and old lithium ion battery is mostly LiPF
6organosilane ester solution, environment is had to severe contamination.Wherein, LiPF
6the Yi Yushui reaction, in moisture content>=10 * 10
-6environment in can generate HF, LiPF
6can decompose under 60 ℃, generate PF
5, PF
5with HF be hypertoxic gas; The product of a lot of hard degradations of organosilane ester solvent and generation chemical reaction is hazardous and noxious substances often.Lithium ion battery reclaims research and starts from phase early 1990s, and main study subject concentrates on to use maximum take graphite as negative pole, LiCoO
2on portable small-sized lithium ion battery for positive pole, because cobalt acid lithium contains the precious metal cobalt, so its recovery has more economic worth.And, along with the development of high capacity lithium ion battery, the lithium ion battery quantity of the types such as iron lithium phosphate will surmount cobalt acid lithium type cell gradually, occupy main status.From economic angle, large-capacity lithium iron phosphate battery cell energy is high, cost is high, and the salvage value after its end of life is still very considerable, to its reasonable recovery, will bring extra economic benefit.Therefore LiFePO 4 of anode material accounts for battery cost ratio up to 30%, in the ferric phosphate lithium cell removal process, to the recovery of waste lithium iron phosphate positive electrode material, is very important link.
The renovation process of a patent CN102280673A(lithium ion battery anode material lithium iron phosphate waste material), the renovation process of patent CN10139015A(waste lithium ion phosphate positive pole material), the recovery method of a patent CN101359756A(lithium iron phosphate anode material from lithium ionic cell waste), the comprehensive recovering process of the useless sheet of patent CN101383441(iron phosphate lithium positive pole) etc. mainly be applicable to the waste material produced in LiFePO 4 material and ferric phosphate lithium cell production process, the LiFePO 4 material that the chemical constitutions such as useless pole piece and scrap stock are not yet destroyed reclaims, be not suitable for the positive electrode material reclaiming separated from waste lithium iron phosphate battery.
Patent CN102017276A(waste lithium iron phosphate power cell recoverying and utilizing method), the positive plate of disassembling out in old and useless battery directly is used, with again make battery after new negative plate coordinates, the method is applicable to the battery that causes cell container to descend because negative pole is aging fully, whether can continue normal the use for positive plate in old and useless battery is difficult to accurately judge, easily cause again be made into battery after scrap rate high, the waste resource; Patent CN102285673A (a kind of method that reclaims lithium and iron from electric automobile lithium ferric phosphate power cell), special emphasis is that element reclaims but not material regeneration, recovery process is more complicated and economic benefit is not high; The method of a patent 201010253859(preparing iron lithium phosphate by recovering water-system waste lithium-ion power battery), the comprehensive method reclaimed of patent CN101847763A(waste lithium iron phosphate battery), the two has continued to use the broken recovery process of cobalt acid lithium type small battery extensive style, easily in positive active material, introduce metallic impurity, what it adopted in addition is the liquid phase method reclaiming process, introduce a large amount of acid-base reagents in process, can bring secondary pollution.
Patent CN102208707 (a kind of method of waste lithium iron phosphate battery positive electrode material reparative regeneration) and patent CN102208706A (a kind of reclaiming treatment process of waste lithium iron phosphate battery positive electrode material), technology for waste and scrap regeneration, before sintering, adopt the liquid phase ball milled to carry out batch mixing, in the material regeneration process, utilize flotation separation, air classification or calcination method etc. that conductive agent and binding agent are thoroughly removed as impurity, operational path is comparatively complicated.
Summary of the invention
The object of the invention is to: for the problem existed in existing waste lithium iron phosphate battery positive electrode material reclaiming technology, a kind of method that technique is simple, recovering effect is good is provided, to realize waste lithium iron phosphate battery resource utilization recycling, promote the Sustainable development of lithium ion battery industry.
Enforcement of the present invention mainly comprises the following steps:
1, the water-system waste ferric phosphate lithium cell after abundant electric discharge is become more meticulous and disassembled, obtained intact positive plate; Positive plate is soaked in deionized water, realize that positive active material fully separates with the collector aluminium foil, obtain the mixture of positive active material and deionized water after taking out aluminium foil and pouring out supernatant liquid, to after said mixture oven dry 20～30h, ball milling 5～10h, obtaining positive electrode material to be regenerated;
2, adopt carbon and sulfur analytical instrument to treat twice-laid stuff and carry out the carbon content test, adopt inductive coupling plasma emission spectrograph (ICP-AES) to be tested Li, Fe, P element ratio, obtain treating twice-laid stuff composition information table.According to the mentioned component table, it is (1.0～1.1): 1:1 that interpolation lithium source and source of iron are adjusted the Li:Fe:P molar ratio, on this ratio basis, the molar ratio of further pressing 1:1:1 adds lithium source, source of iron and phosphorus source, for adjusting material C content ratio to 1～7wt.%;
3, adopt solid phase method to adjusting the material ball milling 5～10h after element ratio, mend lithium regeneration mechanism and novel material synthesis condition according to the waste lithium iron phosphate material, obtain the lithium iron phosphate positive material of regenerating calcine 10～30h in two stages under inert atmosphere and differing temps after.
Described lithium source comprises Quilonum Retard, lithium hydroxide, lithium oxalate, lithium acetate, lithium chloride or Trilithium phosphate; Described source of iron comprises Ferrox and ferrous acetate; Described phosphorus source comprises ammonium di-hydrogen phosphate, Secondary ammonium phosphate.
The present invention directly adopts solid-phase ball milling method batch mixing, the extra drying process that minimizing brings because of the liquid phase method batch mixing, and when material regeneration, the conductive agent in positive active material and water system binding agent directly are used as carbon source, obtain the twice-laid stuff that capacity is high and high rate performance is excellent when having reduced the recovery process difficulty, there is obvious technical superiority.
Compared with prior art, advantage of the present invention is:
1, mechanical milling process adopts the higher rotation speed of 300～400r/min, with the standing 10～30min of every ball milling 1～2h, the reverse standing 10～30min of ball milling 1～2h subsequently, the integrating sphere time consuming reaches the control strategy of 5～20h, when guaranteeing the ball milling effect, avoids destroying because the mechanical milling process heat production causes material composition.
2, obtain when regenerating positive electrode material, the binding agent and the conductive agent that exist in positive active material are not done to special processing.When material regeneration is calcined, binding agent and conductive agent, together as carbon source, participate in the LiFePO 4 material regenerative response.
3, in the material regeneration process, take full advantage of and treat existing carbon source in twice-laid stuff, adjust molar ratio and the absolute content of the elements such as Li, Fe, P by increasing lithium source, source of iron and phosphorus source, control C, Li, Fe, P ratio to desired value, guaranteed that twice-laid stuff has good high rate performance when having high gram volume.
4, in the material regeneration process, mend lithium regeneration mechanism and novel material synthesis condition according to the waste lithium iron phosphate material, preferably optimum calcinating temperature and soaking time, adopt 300～500 ℃ of pre-burning 3～10h under inert atmosphere, the two stage calcination methods of 10～25h reburn under 650～850 ℃, synchronously carry out the calcining of waste and scrap reparative regeneration and novel material is synthetic, guaranteed that twice-laid stuff has high gram volume and good cycle performance.
5, whole salvage material regenerative process technique is simple, and waste and old positive electrode active material utilization is high, and the twice-laid stuff excellent combination property is conducive to carry out the mass-producing application.
The accompanying drawing explanation
The charging and discharging curve of Fig. 1 waste lithium iron phosphate battery
The regenerate XRD figure spectrum of lithium iron phosphate positive material of Fig. 2
The regenerate first charge-discharge curve of lithium iron phosphate positive material of Fig. 3
The regenerate multiplying power discharging curve of lithium iron phosphate positive material of Fig. 4
The regenerate cycle performance curve of lithium iron phosphate positive material of Fig. 5
Embodiment
Embodiment 1:
By 2 fully electric discharges after the 60Ah water system lithium iron phosphate battery constant volume of 2000 circulations, become more meticulous and disassemble the complete battery core of rear taking-up, positive pole, negative pole and barrier film are separated, obtain intact positive plate.Positive plate is soaked in deionized water to 5min, realize that positive active material fully separates with the collector aluminium foil, obtain the mixture of positive active material and deionized water after taking out aluminium foil and pouring out supernatant liquid; To after the dry 24h of said mixture, carry out ball-milling processing and obtain lithium iron phosphate positive material to be regenerated under 80 ℃, the ball-grinding machine of employing is planetary ball mill, and ratio of grinding media to material is 15:1, and rotational speed of ball-mill is 350r/min.Standing 30min after every ball milling 1h in mechanical milling process, reverse ball milling 1h subsequently, standing 30min, integrating sphere is consumed time to 5h.Adopt the carbon and sulfur analytical instrument test to obtain treating that in twice-laid stuff, carbon content is 7%, adopting inductive coupling plasma emission spectrograph (ICP-AES) test to obtain the Li:Fe:P molar ratio is 0.8:1.0:1.0.
Embodiment 2:
Get in embodiment 1 and treat twice-laid stuff 20g, adding Quilonum Retard adjustment Li:Fe:P molar ratio is 1:1:1, on this ratio basis, the molar ratio of further pressing 1:1:1 adds Quilonum Retard, Ferrox and primary ammonium phosphate, and in the adjustment material, the carbon content ratio is to 3wt.%.Element ratio carries out ball-milling processing to material after adjusting, and ball-grinding machine is planetary ball mill, and ratio of grinding media to material is 15:1, and rotational speed of ball-mill is 350r/min.Material after ball milling, under nitrogen protection, continues calcining 10h under 750 ℃ after 400 ℃ of pre-burning 5h, obtain the lithium iron phosphate positive material of regenerating.Take N-Methyl pyrrolidone as solvent, this iron lithium phosphate sample, conductive agent (SuperP) and binding agent are ground to even form slurry by the mass ratio of 80:15:5, be coated on aluminium foil and make positive plate, be assembled into half-cell with metal lithium sheet, through Land electrochemical property test instrument analytical test, this regeneration LiFePO 4 material 0.1C loading capacity reaches 156mAh/g, 0.5C loading capacity reaches 142mAh/g, the 1C loading capacity reaches 132mAh/g, the 2C loading capacity reaches 120mAh/g, and 50 capacity of 0.1C circulation are undamped.
Embodiment 3:
With embodiment 2 differences, be, treat that twice-laid stuff carbon content ratio is to 2wt.% after the adjustment removal of impurities, all the other conditionally completes are consistent.Through Land electrochemical property test instrument analytical test, this regeneration LiFePO 4 material 0.1C loading capacity is 155mAh/g, and the 0.5C loading capacity reaches 137mAh/g, and the 1C loading capacity reaches 128mAh/g, the 2C loading capacity reaches 116mAh/g, and 50 capacity of 0.1C circulation are undamped.
Embodiment 4:
Be with embodiment 2 differences, after the material ball milling after the adjustment element ratio, after 400 ℃ of lower pre-burning 5h, under 800 ℃, calcine 10h, obtain the LiFePO 4 material of regenerating.Through Land electrochemical property test instrument analytical test, this regeneration LiFePO 4 material 0.1C loading capacity is 151mAh/g, and the 0.5C loading capacity reaches 136mAh/g, and the 1C loading capacity reaches 126mAh/g, the 2C loading capacity reaches 113mAh/g, and 50 capability retentions of 0.1C circulation are 99.3%.
Above-mentioned embodiment is the preferred embodiment of the present invention; can not be limited claim of the present invention; the change of making under the technology contents that any the present invention of utilization discloses, modification, substitute, combination, simplify; all should be equivalent embodiment; and do not break away from technical characterictic content of the present invention; all still belong to the technology of the present invention characteristic range, within being included in protection scope of the present invention.
Claims (6)
1. the method for a reclaiming positive electrode material from the water-system waste ferric phosphate lithium cell is characterized in that recycling step is as follows:
1) the water-system waste ferric phosphate lithium cell after abundant electric discharge is become more meticulous and disassembled, obtained intact positive plate; Positive plate is soaked in deionized water, realize that positive active material fully separates with the collector aluminium foil, obtain the mixture of positive active material and deionized water after removing aluminium foil and pouring out supernatant liquid, to after said mixture oven dry 20～30h, ball milling 5～10h, obtaining positive electrode material to be regenerated;
2) adopt carbon and sulfur analytical instrument to treat twice-laid stuff and carry out the carbon content test, adopt inductive coupling plasma emission spectrograph (ICP-AES) to be tested Li, Fe, P element ratio, obtain treating twice-laid stuff composition information table; According to the mentioned component table, it is (1.0～1.1): 1:1 that interpolation lithium source and source of iron are adjusted the Li:Fe:P molar ratio, on this ratio basis, further in the ratio of 1:1:1, adds lithium source, source of iron and phosphorus source, adjusts C content ratio to 1～7wt.% in material;
3) adopt solid phase method to adjusting the material ball milling 5～10h after element ratio, mend lithium regeneration mechanism and novel material synthesis condition according to the waste lithium iron phosphate material, obtain the lithium iron phosphate positive material of regenerating calcine 10～30h in two stages under inert atmosphere and differing temps after.
According to claim 1 from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, the rotating speed that it is characterized in that mechanical milling process employing 300～400r/min in step 1) and step 3), with the standing 10～30min of every ball milling 1～2h, reverse ball milling 1～2h subsequently, the technique of standing 10～30min, the integrating sphere time consuming reaches the control strategy of 5～10h, when guaranteeing the ball milling effect, avoids destroying because the mechanical milling process heat production causes material composition.
According to claim 1 from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, it is characterized in that step 1) obtains when regenerating positive electrode material, the binding agent and the conductive agent that in positive active material, exist are not done to special processing; When step 3) material regeneration sintering, binding agent and conductive agent, together as carbon source, participate in the LiFePO 4 material regenerative response.
According to claim 1 from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, it is characterized in that in step 3) waste lithium iron phosphate positive electrode material regenerative process, take full advantage of and treat existing carbon source in twice-laid stuff, adjust molar ratio and the absolute content of the elements such as Li, Fe, P by increasing lithium source, source of iron and phosphorus source, control C, Li, Fe, P ratio to desired value, guaranteed that twice-laid stuff has good high rate performance when having high gram volume.
According to claim 1 from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, it is characterized in that in step 3) waste lithium iron phosphate positive electrode material regenerative process, mend lithium regeneration mechanism and novel material synthesis condition according to the waste lithium iron phosphate material, adopt 300～500 ℃ of pre-burning 3～10h under inert atmosphere, the two stage calcination methods of 10～20h reburn under 650～850 ℃, synchronously carry out the calcining of waste and scrap reparative regeneration and novel material is synthetic, guaranteed that twice-laid stuff has high gram volume and good cycle performance.
According to claim 1 from the water-system waste ferric phosphate lithium cell method of reclaiming positive electrode material, it is characterized in that described lithium source comprises Quilonum Retard, lithium hydroxide, lithium oxalate, lithium acetate, lithium chloride or Trilithium phosphate; Described source of iron comprises Ferrox and ferrous acetate; Described phosphorus source comprises ammonium di-hydrogen phosphate, Secondary ammonium phosphate.
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| CN103728290A (en) * | 2013-12-30 | 2014-04-16 | 天津力神电池股份有限公司 | Method for testing content of impurities of lithium battery pole piece |
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