CN114400393A - A kind of method that utilizes heat treatment to separate positive and negative electrode powder to recover lithium iron phosphate - Google Patents
A kind of method that utilizes heat treatment to separate positive and negative electrode powder to recover lithium iron phosphate Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 52
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000010438 heat treatment Methods 0.000 title claims abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 15
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000011261 inert gas Substances 0.000 claims abstract description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 6
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- 230000008929 regeneration Effects 0.000 claims description 10
- 238000011069 regeneration method Methods 0.000 claims description 10
- 239000002699 waste material Substances 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- 230000008439 repair process Effects 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- 238000011084 recovery Methods 0.000 claims description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims description 4
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 4
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 229910003002 lithium salt Inorganic materials 0.000 claims description 3
- 159000000002 lithium salts Chemical class 0.000 claims description 3
- 229910052754 neon Inorganic materials 0.000 claims description 3
- GKAOGPIIYCISHV-UHFFFAOYSA-N neon atom Chemical compound [Ne] GKAOGPIIYCISHV-UHFFFAOYSA-N 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 230000000996 additive effect Effects 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- 230000001172 regenerating effect Effects 0.000 claims 1
- 239000010439 graphite Substances 0.000 abstract description 11
- 229910002804 graphite Inorganic materials 0.000 abstract description 11
- 238000000926 separation method Methods 0.000 abstract description 8
- 230000009471 action Effects 0.000 abstract description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract description 2
- 238000010335 hydrothermal treatment Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 description 8
- 238000004064 recycling Methods 0.000 description 8
- 150000002431 hydrogen Chemical class 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 4
- 238000005188 flotation Methods 0.000 description 4
- 229910052744 lithium Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 description 1
- 229910052808 lithium carbonate Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000011812 mixed powder Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000009469 supplementation Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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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Abstract
Description
技术领域：Technical field:
本发明涉及废旧锂电池回收再利用技术领域，具体涉及一种利用热处理分离正负极粉回收磷酸铁锂的方法。The invention relates to the technical field of recycling and reuse of waste lithium batteries, in particular to a method for recovering lithium iron phosphate by separating positive and negative electrode powders by heat treatment.
背景技术：Background technique:
锂离子电池因其能量密度高、循环性能好、自放电低等优势在各个领域得到了广泛的应用。废弃的动力锂电池主要是早期应用量巨大的磷酸铁锂电池，从保护环境和节约资源的角度来看，开展退役磷酸铁锂电池回收再生工艺研究是必要的。目前电池回收的主流工艺是电池经过放电、破碎后再进行处理得到正负极粉和铜、铝等金属产物。正负极粉石墨粉和磷酸铁锂粉的混合物，正负极粉的有效分离是确保石墨和磷酸铁锂回收再利用的前提。Lithium-ion batteries have been widely used in various fields due to their high energy density, good cycle performance, and low self-discharge. Abandoned power lithium batteries are mainly lithium iron phosphate batteries with huge early applications. From the perspective of protecting the environment and saving resources, it is necessary to carry out research on the recycling and regeneration of retired lithium iron phosphate batteries. At present, the mainstream process of battery recycling is that the battery is discharged and crushed and then processed to obtain positive and negative electrode powder and metal products such as copper and aluminum. The mixture of positive and negative electrode powder graphite powder and lithium iron phosphate powder, the effective separation of positive and negative electrode powder is the premise to ensure the recycling of graphite and lithium iron phosphate.
传统的分离正负极粉的方法是浮选，申请号为CN201811416385.4的中国发明专利介绍了一种电极粉浮选除碳工艺，工艺经过物相分析、确定浮选药剂、三步浮选法后得到正极材料；另一种常用的正负极粉处理方法是直接进行化学方法回收有价金属，例如专利号为CN113443640A的发明专利提供一种利用磷酸铁锂电池正负极废粉制备电池级碳酸锂和电池级磷酸铁的方法，该方法可以实现磷酸铁锂电池正负极废粉中锂、铁、磷的综合回收；专利号CN109179358A、CN106684485A、CN108899601A公开的方法大同小异，都是运用化学方法直接回收有价金属，并未对混合粉中的石墨碳实施有效的利用。现有的正负极粉分离方法中均未考虑石墨碳的回收利用问题，只关注了正极材料的回收利用。The traditional method for separating positive and negative powders is flotation. The Chinese invention patent with the application number CN201811416385.4 introduces an electrode powder flotation carbon removal process. The process undergoes phase analysis, determination of flotation reagents, and three-step flotation. The positive electrode material is obtained after the method; another commonly used method for processing positive and negative electrode powder is to directly recover valuable metals by chemical method, for example, the invention patent with the patent number of CN113443640A provides a method for preparing batteries by using waste powder of positive and negative electrodes of lithium iron phosphate batteries The method of lithium carbonate and battery grade iron phosphate, this method can realize the comprehensive recovery of lithium, iron and phosphorus in the positive and negative electrode waste powder of lithium iron phosphate battery; the methods disclosed by patent numbers CN109179358A, CN106684485A and CN108899601A are similar, all of which use chemical The method directly recovers valuable metals, but does not effectively utilize the graphitic carbon in the mixed powder. None of the existing methods for separating positive and negative electrode powders considers the recycling of graphitic carbon, and only focuses on the recycling of positive electrode materials.
发明内容：Invention content:
本发明的目的是提供一种利用热处理分离正负极粉回收磷酸铁锂的方法，通过添加水热处理实现了正负极粉中石墨碳和磷酸铁锂的有效分离，石墨碳在高温和水蒸气的作用下转化为氢气、一氧化碳、二氧化碳等合成气体，实现了负极石墨粉的资源化利用，磷酸铁锂在惰性气体和还原性气体的氛围中不会发生改变，热处理得到的固体即为不含碳杂质的磷酸铁锂粉末，不引入新的无机杂质元素，不需要分离、过滤等操作程序，工艺方法操作简单，工艺流程短，提升后续再生修复的正极粉磷酸铁锂的品质，提高负极石墨碳的利用价值，解决了现有技术均未考虑石墨碳的回收利用的技术问题。The purpose of this invention is to provide a kind of method that utilizes heat treatment to separate positive and negative electrode powder to recover lithium iron phosphate, realizes effective separation of graphitic carbon and lithium iron phosphate in positive and negative electrode powder by adding hydrothermal treatment, graphitic carbon is at high temperature and water vapor It is converted into hydrogen, carbon monoxide, carbon dioxide and other synthetic gases under the action of the action, realizing the resource utilization of the negative electrode graphite powder. The lithium iron phosphate will not change in the atmosphere of inert gas and reducing gas, and the solid obtained by heat treatment is free of Carbon impurity lithium iron phosphate powder does not introduce new inorganic impurity elements, does not require separation, filtration and other operating procedures, the process method is simple to operate, and the process flow is short, improving the quality of the cathode powder lithium iron phosphate for subsequent regeneration and repair, and improving the anode graphite The utilization value of carbon solves the technical problem that the recycling and utilization of graphitic carbon are not considered in the prior art.
本发明是通过以下技术方案予以实现的：The present invention is achieved through the following technical solutions:
一种利用热处理分离正负极粉回收磷酸铁锂的方法，该方法包括以下步骤：A method for recycling lithium iron phosphate using heat treatment to separate positive and negative electrode powder, the method comprising the following steps:
(1)废旧磷酸铁锂电池经破碎、热解后得到铜、铝箔片和正负极黑粉；(1) After the waste lithium iron phosphate battery is crushed and pyrolyzed, copper, aluminum foil and black powder of positive and negative electrodes are obtained;
(2)将步骤(1)得到的黑粉进行化学多元素和物相分析，以确定黑粉中磷酸铁锂和石墨碳的含量；(2) the black powder obtained in step (1) is carried out to chemical multi-element and phase analysis to determine the content of lithium iron phosphate and graphitic carbon in the black powder;
(3)将步骤(1)得到的黑粉在惰性气体的气氛下、加入水作为添加剂进行热处理，热处理温度为600-800℃，时间为1-2小时，水的添加量为5-20ml/h，然后通过气固分离得到产物气体和固体；(3) the black powder obtained in step (1) is heat-treated by adding water as an additive in an atmosphere of inert gas, the heat-treatment temperature is 600-800 ° C, the time is 1-2 hours, and the addition amount of water is 5-20ml/ h, and then obtain product gas and solid through gas-solid separation;
(4)将步骤(3)得到的产物气体经过冷凝、干燥、除尘实现清洁合成气的收集利用；(4) the product gas obtained in step (3) is condensed, dried and dedusted to realize the collection and utilization of clean synthesis gas;
(5)将步骤(3)得到的固体进行收集，得到不含碳杂质的磷酸铁锂粉末，进行修复再生。(5) collecting the solid obtained in step (3) to obtain lithium iron phosphate powder without carbon impurities, and performing repair and regeneration.
步骤(2)磷酸铁锂含量范围为30wt％-70wt％。In step (2), the content of lithium iron phosphate ranges from 30wt% to 70wt%.
步骤(2)所述惰性气体包括氮气、氩气及氖气。The inert gas in step (2) includes nitrogen, argon and neon.
步骤(4)所述的清洁气体主要包含氢气、一氧化碳、二氧化碳、甲烷等小分子气体。The cleaning gas in step (4) mainly includes small molecular gases such as hydrogen, carbon monoxide, carbon dioxide, and methane.
步骤(5)所述修复再生包括磷酸铁锂补锂再生、锂元素回收再利用及锂盐和磷酸铁回收再制备磷酸铁锂等。The repairing and regeneration in step (5) includes lithium iron phosphate supplementation and regeneration, lithium element recovery and reuse, and lithium salt and iron phosphate recovery and preparation of lithium iron phosphate.
本发明正负极黑粉中的石墨碳与磷酸铁锂得到有效的分离，石墨碳在高温和水蒸气的作用下转化为氢气、一氧化碳、二氧化碳等合成气体，实现了负极石墨粉的资源化利用，磷酸铁锂在惰性气体和还原性气体的氛围中不会发生改变，热处理得到的固体即为不含碳杂质的磷酸铁锂粉末，运用适当的方法即可实现其修复再生。The graphite carbon and the lithium iron phosphate in the positive and negative black powder of the present invention are effectively separated, and the graphite carbon is converted into hydrogen, carbon monoxide, carbon dioxide and other synthetic gases under the action of high temperature and water vapor, thereby realizing the resource utilization of the negative electrode graphite powder. , lithium iron phosphate will not change in the atmosphere of inert gas and reducing gas, and the solid obtained by heat treatment is lithium iron phosphate powder without carbon impurities, which can be repaired and regenerated by using appropriate methods.
本发明的有益效果如下：The beneficial effects of the present invention are as follows:
1)本发明利用简单的热处理技术实现正负极黑粉中石墨碳与磷酸铁锂粉末分离的目的，不仅可以提高负极石墨碳的利用价值，还能够提升后续再生修复的正极粉磷酸铁锂的品质，工艺流程简单易行。1) The present invention utilizes a simple heat treatment technology to achieve the purpose of separating graphite carbon from the lithium iron phosphate powder in the positive and negative black powder, which can not only improve the utilization value of the negative electrode graphite carbon, but also improve the subsequent regeneration and repair of the positive electrode powder lithium iron phosphate. Quality, process flow is simple and easy.
2)本发明中水的加入能够有效的将石墨碳转化为氢气、一氧化碳等清洁的合成气体，实现石墨碳的资源化利用，整个处理过程无有机溶剂、酸碱溶剂的加入，不会产生大量的废水，工艺流程对环境友好。2) The addition of water in the present invention can effectively convert the graphitic carbon into clean synthetic gases such as hydrogen and carbon monoxide, and realize the resource utilization of the graphitic carbon. waste water, and the process flow is environmentally friendly.
附图说明：Description of drawings:
图1是本发明的工艺流程示意图。Fig. 1 is the process flow schematic diagram of the present invention.
具体实施方式：Detailed ways:
以下是对本发明的进一步说明，而不是对本发明的限制。The following is a further description of the present invention, rather than a limitation of the present invention.
实施例1：Example 1:
(1)废旧磷酸铁锂电池经破碎、500℃热解后得到铜、铝箔片和正负极黑粉。(1) The waste lithium iron phosphate battery is crushed and pyrolyzed at 500°C to obtain copper, aluminum foil and black powder of positive and negative electrodes.
(2)得到的黑粉进行化学多元素和物相分析，黑粉中磷酸铁锂的含量为30wt％，石墨碳含量为70wt％。(2) The obtained black powder is subjected to chemical multi-element and phase analysis, and the content of lithium iron phosphate in the black powder is 30 wt %, and the content of graphite carbon is 70 wt %.
(3)将黑粉置于固定床反应炉中，热处理气氛为氩气气体，设置热处理温度为600℃，通入水的流速为20ml/h，反应时间为1.5小时，通过气固分离得到产物气体和固体。(3) The black powder is placed in a fixed-bed reaction furnace, the heat treatment atmosphere is argon gas, the heat treatment temperature is set to 600 ° C, the flow rate of the water is 20ml/h, the reaction time is 1.5 hours, and the product gas is obtained by gas-solid separation and solid.
(4)气体经过冷凝、干燥、除尘实现清洁合成气的收集利用，收集得到的产物气体以氢气、一氧化碳、甲烷、二氧化碳为主。(4) The gas is condensed, dried and dedusted to realize the collection and utilization of clean syngas. The collected product gas is mainly hydrogen, carbon monoxide, methane and carbon dioxide.
(5)收集得到的固体为不含碳杂质的磷酸铁锂粉末，进行锂盐和磷酸铁回收再制备磷酸铁锂。(5) The collected solid is lithium iron phosphate powder without carbon impurities, and lithium salt and iron phosphate are recovered to prepare lithium iron phosphate.
实施例2Example 2
(1)废旧磷酸铁锂电池经破碎、500℃热解后得到铜、铝箔片和正负极黑粉。(1) The waste lithium iron phosphate battery is crushed and pyrolyzed at 500°C to obtain copper, aluminum foil and black powder of positive and negative electrodes.
(2)得到的黑粉进行化学多元素和物相分析，黑粉中磷酸铁锂的含量为50wt％，石墨碳含量为50wt％。(2) The obtained black powder is subjected to chemical multi-element and phase analysis, and the content of lithium iron phosphate in the black powder is 50 wt %, and the content of graphite carbon is 50 wt %.
(3)将黑粉置于固定床反应炉中，热处理气氛为氖气气体，设置热处理温度为800℃，通入水的流速为10ml/h，反应时间为2小时，通过气固分离得到产物气体和固体。(3) The black powder is placed in a fixed-bed reaction furnace, the heat treatment atmosphere is neon gas, the heat treatment temperature is set to 800 ° C, the flow rate of the introduced water is 10ml/h, the reaction time is 2 hours, and the product gas is obtained by gas-solid separation and solid.
(4)气体经过冷凝、干燥、除尘实现清洁合成气的收集利用，收集得到的产物气体以氢气、一氧化碳、甲烷为主。(4) The gas is condensed, dried and dedusted to realize the collection and utilization of clean syngas. The collected product gas is mainly hydrogen, carbon monoxide and methane.
(5)收集得到的固体为不含碳杂质的磷酸铁锂粉末，进行锂元素回收再利用。(5) The collected solid is lithium iron phosphate powder without carbon impurities, and lithium element is recovered and reused.
实施例3Example 3
(1)废旧磷酸铁锂电池经破碎、400℃热解后得到铜、铝箔片和正负极黑粉。(1) The waste lithium iron phosphate battery is crushed and pyrolyzed at 400°C to obtain copper, aluminum foil and black powder of positive and negative electrodes.
(2)得到的黑粉进行化学多元素和物相分析，黑粉中磷酸铁锂的含量为70wt％，石墨碳含量为30wt％。(2) The obtained black powder is subjected to chemical multi-element and physical phase analysis, and the content of lithium iron phosphate in the black powder is 70 wt %, and the content of graphite carbon is 30 wt %.
(3)将黑粉置于固定床反应炉中，热处理气氛为氮气气体，设置热处理温度为700℃，通入水的流速为5ml/h，反应时间为1小时，通过气固分离得到产物气体和固体。(3) The black powder is placed in a fixed-bed reaction furnace, the heat treatment atmosphere is nitrogen gas, the heat treatment temperature is set to 700 ° C, the flow rate of the introduced water is 5 ml/h, the reaction time is 1 hour, and the product gas and solid.
(4)气体经过冷凝、干燥、除尘实现清洁合成气的收集利用，收集得到的产物气体以氢气、一氧化碳、甲烷为主。(4) The gas is condensed, dried and dedusted to realize the collection and utilization of clean syngas. The collected product gas is mainly hydrogen, carbon monoxide and methane.
(5)收集得到的固体为不含碳杂质的磷酸铁锂粉末，进行磷酸铁锂补锂再生。(5) The collected solid is lithium iron phosphate powder without carbon impurities, and lithium iron phosphate is supplemented for lithium regeneration.
以上仅是本发明的优选实施方式，应当指出的是，上述优选实施方式不应视为对本发明的限制，本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说，在不脱离本发明的精神和范围内，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above are only the preferred embodiments of the present invention. It should be noted that the above preferred embodiments should not be regarded as limitations of the present invention, and the protection scope of the present invention should be based on the scope defined by the claims. For those skilled in the art, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, and these improvements and modifications should also be regarded as the protection scope of the present invention.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114865133A (en) * | 2022-05-26 | 2022-08-05 | 双登集团股份有限公司 | A kind of resource recycling and repairing method of lithium iron phosphate battery |
| CN115149139A (en) * | 2022-08-19 | 2022-10-04 | 中南大学 | Method for coupling, regenerating and repairing positive and negative active substances of waste lithium iron phosphate batteries |
| CN115472945A (en) * | 2022-09-16 | 2022-12-13 | 湖南宏杉新能源科技有限公司 | Method for repairing and regenerating waste lithium iron phosphate positive electrode material |
| CN118983560A (en) * | 2024-10-15 | 2024-11-19 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | A method and system for removing impurities and comprehensively utilizing positive electrode materials of lithium-ion batteries |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101383441A (en) * | 2007-09-06 | 2009-03-11 | 深圳市比克电池有限公司 | Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell |
| CN101394015A (en) * | 2007-09-20 | 2009-03-25 | 深圳市比克电池有限公司 | Regeneration method for waste lithium ion phosphate positive pole material |
| CN110112481A (en) * | 2019-04-23 | 2019-08-09 | 北京科技大学 | Waste lithium iron phosphate battery recycles the method for preparing lithium iron phosphate positive material |
| CN111495925A (en) * | 2020-04-20 | 2020-08-07 | 北京矿冶科技集团有限公司 | Method for pyrolyzing and defluorinating chlorine of waste lithium battery |
| CN111790728A (en) * | 2020-07-15 | 2020-10-20 | 重庆大学 | A kind of disposal method for efficient reduction and recovery of waste lithium batteries using water vapor |
| CN112047335A (en) * | 2020-08-31 | 2020-12-08 | 湖南宸宇富基新能源科技有限公司 | Combined treatment method for black powder of waste lithium ion battery |
| CN112157107A (en) * | 2020-08-28 | 2021-01-01 | 威立雅新能源科技(江门)有限公司 | Method for separating positive and negative electrode materials from waste lithium batteries |
| CN112207119A (en) * | 2020-10-10 | 2021-01-12 | 荆门市格林美新材料有限公司 | Method for treating battery black powder |
-
2021
- 2021-12-17 CN CN202111552163.7A patent/CN114400393A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101383441A (en) * | 2007-09-06 | 2009-03-11 | 深圳市比克电池有限公司 | Synthetic recovering method for positive pole waste tablet from ferric phosphate lithium cell |
| CN101394015A (en) * | 2007-09-20 | 2009-03-25 | 深圳市比克电池有限公司 | Regeneration method for waste lithium ion phosphate positive pole material |
| CN110112481A (en) * | 2019-04-23 | 2019-08-09 | 北京科技大学 | Waste lithium iron phosphate battery recycles the method for preparing lithium iron phosphate positive material |
| CN111495925A (en) * | 2020-04-20 | 2020-08-07 | 北京矿冶科技集团有限公司 | Method for pyrolyzing and defluorinating chlorine of waste lithium battery |
| CN111790728A (en) * | 2020-07-15 | 2020-10-20 | 重庆大学 | A kind of disposal method for efficient reduction and recovery of waste lithium batteries using water vapor |
| CN112157107A (en) * | 2020-08-28 | 2021-01-01 | 威立雅新能源科技(江门)有限公司 | Method for separating positive and negative electrode materials from waste lithium batteries |
| CN112047335A (en) * | 2020-08-31 | 2020-12-08 | 湖南宸宇富基新能源科技有限公司 | Combined treatment method for black powder of waste lithium ion battery |
| CN112207119A (en) * | 2020-10-10 | 2021-01-12 | 荆门市格林美新材料有限公司 | Method for treating battery black powder |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114865133A (en) * | 2022-05-26 | 2022-08-05 | 双登集团股份有限公司 | A kind of resource recycling and repairing method of lithium iron phosphate battery |
| CN115149139A (en) * | 2022-08-19 | 2022-10-04 | 中南大学 | Method for coupling, regenerating and repairing positive and negative active substances of waste lithium iron phosphate batteries |
| CN115472945A (en) * | 2022-09-16 | 2022-12-13 | 湖南宏杉新能源科技有限公司 | Method for repairing and regenerating waste lithium iron phosphate positive electrode material |
| CN118983560A (en) * | 2024-10-15 | 2024-11-19 | 合肥综合性国家科学中心能源研究院(安徽省能源实验室) | A method and system for removing impurities and comprehensively utilizing positive electrode materials of lithium-ion batteries |
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