CN108899603A - A kind of processing method of waste lithium cell positive electrode and the recovery processing technique of waste lithium cell - Google Patents
A kind of processing method of waste lithium cell positive electrode and the recovery processing technique of waste lithium cell Download PDFInfo
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- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 100
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 95
- 238000000034 method Methods 0.000 title claims abstract description 93
- 239000002699 waste material Substances 0.000 title claims abstract description 85
- 238000011084 recovery Methods 0.000 title claims abstract description 32
- 238000012545 processing Methods 0.000 title claims abstract description 4
- 238000003672 processing method Methods 0.000 title claims description 6
- 239000007774 positive electrode material Substances 0.000 claims abstract description 58
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 42
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 17
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 14
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims abstract description 13
- 239000003513 alkali Substances 0.000 claims abstract description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000706 filtrate Substances 0.000 claims description 72
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 56
- 239000012535 impurity Substances 0.000 claims description 29
- 239000007787 solid Substances 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 15
- 238000002386 leaching Methods 0.000 claims description 15
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims description 14
- 239000010406 cathode material Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 9
- 229960004887 ferric hydroxide Drugs 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 9
- IEECXTSVVFWGSE-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Fe+3] IEECXTSVVFWGSE-UHFFFAOYSA-M 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 9
- 239000007773 negative electrode material Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000000605 extraction Methods 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910000831 Steel Inorganic materials 0.000 claims description 2
- 239000011889 copper foil Substances 0.000 claims description 2
- 239000011888 foil Substances 0.000 claims description 2
- 239000002985 plastic film Substances 0.000 claims description 2
- 229920006255 plastic film Polymers 0.000 claims description 2
- 238000012216 screening Methods 0.000 claims description 2
- 239000010959 steel Substances 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 19
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 14
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 238000001556 precipitation Methods 0.000 abstract description 7
- 239000010926 waste battery Substances 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000002253 acid Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 235000014413 iron hydroxide Nutrition 0.000 description 2
- -1 iron ions Chemical class 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
Classifications
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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
-
- 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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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
一种废旧锂电池正极材料的处理方法及废旧锂电池的回收处理工艺，涉及锂电池领域。该处理方法通过采用碱溶解‑酸浸出‑分离铁‑热法沉淀碳酸锂的工艺流程，有效地回收了废旧锂电池中的铁、铝和锂元素，其中，所采用的硫酸法浸出氢氧化铝工艺中，具备回收成本低、效率高且所得产品纯度高的优点，水热法沉淀碳酸锂具备一次性沉锂率高的优点。因此，上述的废旧锂电池正极材料的处理方法不但简单有效，而且可以使废旧电池中的主要元素Fe、Al和Li得到高效回收，并且不会产生二次污染，故其可以显著提高经济效益；另外，上述废旧锂电池的回收处理工艺包括上述的废旧锂电池正极材料的处理方法，其具备上述处理方法的各项优点。A method for processing positive electrode materials of waste lithium batteries and a recovery and treatment process for waste lithium batteries relate to the field of lithium batteries. This treatment method effectively recovers the iron, aluminum and lithium elements in the waste lithium battery by adopting the technological process of alkali dissolution-acid leaching-separation iron-thermal precipitation of lithium carbonate, wherein the sulfuric acid method is used to leach aluminum hydroxide In the process, it has the advantages of low recovery cost, high efficiency and high purity of the obtained product, and the hydrothermal precipitation of lithium carbonate has the advantage of high lithium precipitation rate at one time. Therefore, the above-mentioned treatment method for the positive electrode material of the waste lithium battery is not only simple and effective, but also can efficiently recover the main elements Fe, Al and Li in the waste battery, and will not produce secondary pollution, so it can significantly improve economic benefits; In addition, the recovery and treatment process of the above-mentioned waste lithium battery includes the above-mentioned treatment method for the positive electrode material of the waste lithium battery, which has various advantages of the above-mentioned treatment method.
Description
技术领域technical field
本发明涉及锂电池领域，具体而言，涉及一种废旧锂电池正极材料的处理方法及废旧锂电池的回收处理工艺。The invention relates to the field of lithium batteries, in particular to a method for processing anode materials of waste lithium batteries and a recycling process for waste lithium batteries.
背景技术Background technique
现有技术中，废旧锂电池的回收处理一直是废物处理领域研究的热点，但是目前存在的主要问题是，工艺复杂，回收率不够高，成本高，并且还容易产生二次污染。In the prior art, the recycling and treatment of waste lithium batteries has always been a research hotspot in the field of waste treatment, but the main problems at present are that the process is complicated, the recovery rate is not high enough, the cost is high, and secondary pollution is easy to occur.
发明内容Contents of the invention
本发明的目的在于提供一种废旧锂电池正极材料的处理方法，其具有方法简单、成本低、回收效率高和不产生二次污染的优点。The object of the present invention is to provide a treatment method for the positive electrode material of the waste lithium battery, which has the advantages of simple method, low cost, high recovery efficiency and no secondary pollution.
本发明的另一目的在于提供一种废旧锂电池的回收处理工艺，其包括上述提供的对废旧锂电池中磷酸铁锂的处理方法，故其具备上述处理方法的各项优点。Another object of the present invention is to provide a recovery and treatment process for waste lithium batteries, which includes the above-mentioned treatment method for lithium iron phosphate in waste lithium batteries, so it has the advantages of the above-mentioned treatment method.
本发明解决其技术问题是采用以下技术方案来实现。The present invention solves its technical problem and adopts the following technical solutions to realize.
本发明提出一种废旧锂电池正极材料的处理方法，其包括：The present invention proposes a kind of treatment method of waste lithium battery cathode material, and it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料；Pretreatment of waste lithium batteries to obtain positive electrode materials with lithium iron phosphate as the main component;
对正极材料进行碱浸取，得到第一滤渣和第一滤液；Alkali leaching is performed on the positive electrode material to obtain the first filter residue and the first filtrate;
向第一滤液中添加硫酸溶液，浸出氢氧化铝固体；Sulfuric acid solution is added to the first filtrate to leach the aluminum hydroxide solid;
向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液；adding a sulfuric acid solution and a hydrogen peroxide solution to the first filter residue, and reacting to obtain a second filter residue and a second filtrate;
向第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液；Add sodium hydroxide solution in the second filtrate, and logical ammonia gas, obtain ferric hydroxide solid and the third filtrate;
利用水热法从第三滤液中沉淀出碳酸锂。Lithium carbonate was precipitated from the third filtrate by hydrothermal method.
本发明实施例还提出一种废旧锂电池的回收处理工艺，其包括上述废旧锂电池正极材料的处理方法。The embodiment of the present invention also proposes a recovery and treatment process for waste lithium batteries, which includes the above-mentioned treatment method for the positive electrode materials of waste lithium batteries.
本发明实施例的废旧锂电池正极材料的处理方法及废旧锂电池的回收处理工艺的有益效果是：本发明实施例提供的废旧锂电池正极材料的处理方法通过采用碱溶解-酸浸出-分离铁-热法沉淀碳酸锂的工艺流程，有效地回收了废旧锂电池中的铁、铝和锂元素，其中，所采用的硫酸法浸出氢氧化铝过程中，具备回收成本低、效率高的优点，并且所得氢氧化铝和氢氧化铁纯度较高，而水热法沉淀碳酸锂过程中一次性沉锂率较高，可达高级产品的要求。因此，本发明实施例提供的废旧锂电池正极材料的处理方法不但简单有效，而且可以使废旧电池中的主要元素Fe、Al和Li得到高效回收，并且不会产生二次污染，故其可以显著提高经济效益；另外，本发明实施例提供的废旧锂电池的回收处理工艺包括上述的废旧锂电池正极材料的处理方法，故其具备上述处理方法的各项优点，因此，其也具备重要的推广应用价值。The beneficial effect of the treatment method of the positive electrode material of the waste lithium battery and the recovery and treatment process of the waste lithium battery of the embodiment of the present invention is: the treatment method of the positive electrode material of the waste lithium battery provided by the embodiment of the present invention adopts alkali dissolution-acid leaching-separation of iron -The technological process of thermal precipitation of lithium carbonate effectively recovers iron, aluminum and lithium elements in waste lithium batteries. Among them, the sulfuric acid method used in the process of leaching aluminum hydroxide has the advantages of low recovery cost and high efficiency. Moreover, the obtained aluminum hydroxide and iron hydroxide have high purity, and the one-time lithium precipitation rate in the process of hydrothermal precipitation of lithium carbonate is high, which can meet the requirements of high-grade products. Therefore, the processing method for the positive electrode material of the waste lithium battery provided by the embodiment of the present invention is not only simple and effective, but also can efficiently recover the main elements Fe, Al and Li in the waste battery without causing secondary pollution, so it can significantly Improve economic benefits; in addition, the waste lithium battery recycling process provided by the embodiment of the present invention includes the above-mentioned treatment method for the waste lithium battery positive electrode material, so it has the advantages of the above-mentioned treatment method, therefore, it also has important promotion Value.
具体实施方式Detailed ways
为使本发明实施例的目的、技术方案和优点更加清楚，下面将对本发明实施例中的技术方案进行清楚、完整地描述。实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。所用试剂或仪器未注明生产厂商者，均为可以通过市售购买获得的常规产品。In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Those who do not indicate the specific conditions in the examples are carried out according to the conventional conditions or the conditions suggested by the manufacturer. The reagents or instruments used were not indicated by the manufacturer, and they were all conventional products that could be purchased from the market.
下面对本发明实施例的废旧锂电池正极材料的处理方法及废旧锂电池的回收处理工艺进行具体说明。The method for treating the positive electrode material of the waste lithium battery and the recovery and treatment process of the waste lithium battery according to the embodiment of the present invention will be described in detail below.
本发明实施例提供的一种废旧锂电池正极材料的处理方法，其主要涉及锂电池领域。具体地，其包括：The embodiment of the present invention provides a method for treating waste lithium battery cathode materials, which mainly relates to the field of lithium batteries. Specifically, it includes:
S1、对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。S1. Pretreating the waste lithium battery to obtain a positive electrode material mainly composed of lithium iron phosphate.
进一步地，本发明实施例在对废旧锂电池进行预处理时，其包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物；对破碎混合物进行过筛，得到正负极材料和粘结剂；以及对正负极材料和粘结剂进行650℃的加热燃烧。Further, in the embodiment of the present invention, when the waste lithium battery is pretreated, it includes crushing and vacuum drying the waste lithium battery to obtain a crushed mixture; sieving the crushed mixture to obtain positive and negative electrode materials and binders; And heat and burn the positive and negative electrode materials and binder at 650°C.
需要说明的是，对废旧锂电池进行破碎和真空干燥以及过筛得到正负极材料是获得废旧锂电池中有用金属的重要基础，其中，破碎可以使整块的废旧锂电池得到尺寸上的减小，从而能使废旧锂电池的各种组分被充分的回收和提取；而真空干燥，一方面是为了去除废旧锂电池中含有的水分，另外一方面也是为了防止干燥过程中对废旧电池的被氧化(抑制氧气和水分共存下的电化学/化学腐蚀)。It should be noted that crushing, vacuum drying and sieving of waste lithium batteries to obtain positive and negative materials is an important basis for obtaining useful metals in waste lithium batteries. Among them, crushing can reduce the size of the whole waste lithium battery. Small, so that the various components of the waste lithium battery can be fully recovered and extracted; and vacuum drying, on the one hand, is to remove the moisture contained in the waste lithium battery, and on the other hand, it is also to prevent the waste battery from being damaged during the drying process. Oxidized (inhibits electrochemical/chemical corrosion in the presence of oxygen and moisture).
进一步地，对正负极材料和粘结剂进行加热燃烧，主要是为了去除负极材料和粘结剂，从而得到正极材料中的磷酸铁锂。需要说明的是，之所以对加热燃烧的温度进行限定，是因为温度过低达不到充分燃烧的条件，温度过高又会对所得正极材料造成损害，影响其材料原始的化学状态。当然了，在本发明的其它实施例当中，并不仅限于本发明实施例中介绍的 650℃，还可以是645℃-655℃的一个范围。Further, heating and burning the positive and negative electrode materials and the binder is mainly to remove the negative electrode materials and the binder, so as to obtain the lithium iron phosphate in the positive electrode material. It should be noted that the reason for limiting the temperature of heating and combustion is because the temperature is too low to achieve sufficient combustion conditions, and the temperature is too high to cause damage to the obtained positive electrode material and affect the original chemical state of the material. Of course, in other embodiments of the present invention, the temperature is not limited to the 650°C described in the embodiment of the present invention, but may also be in a range of 645°C-655°C.
需要强调的是，本发明实施例提供的以磷酸铁锂为主要成分的正极材料是含有Fe、Al和Li金属元素的正极材料，并且本发明实施例主要要提取回收的金属元素即为Fe、Al和Li三种金属元素。It should be emphasized that the positive electrode material with lithium iron phosphate as the main component provided by the embodiment of the present invention is a positive electrode material containing Fe, Al and Li metal elements, and the main metal elements to be extracted and recovered in the embodiment of the present invention are Fe, Al and Li are three metal elements.
进一步地，本发明实施例在对正负极材料和粘结剂进行650℃的加热燃烧时，还产生了气体，并且本发明实施例中还在预处理过程中对产生的气体进行了净化处理，以降低本发明实施例的处理方法有可能所造成的环境污染问题。Further, in the embodiment of the present invention, gas is also generated when the positive and negative electrode materials and the binder are heated and burned at 650°C, and the generated gas is also purified during the pretreatment process in the embodiment of the present invention , to reduce the possible environmental pollution caused by the treatment method of the embodiment of the present invention.
进一步地，本发明实施例提供的回收处理方法中，预处理过程还包括对破碎混合物进行重介质筛分，进而得到重介质，其中重介质包括铝壳、钢壳、铝塑膜、铝箔和铜箔。Further, in the recovery treatment method provided by the embodiment of the present invention, the pretreatment process also includes performing dense medium screening on the broken mixture to obtain dense medium, wherein the dense medium includes aluminum shell, steel shell, aluminum plastic film, aluminum foil and copper foil.
S2、对正极材料进行碱浸取，得到第一滤渣和第一滤液。S2. Alkali leaching is performed on the positive electrode material to obtain a first filter residue and a first filtrate.
需要说明的是，碱浸取过程中，是将正极材料中金属离子化的一个过程中，通过适当浓度的碱液对正极材料进行浸泡，可以溶解得到具有锂离子、铁离子和铝离子的溶液。It should be noted that the alkali leaching process is a process of ionizing the metal in the positive electrode material. The positive electrode material can be dissolved by immersing the positive electrode material in an appropriate concentration of lye to obtain a solution containing lithium ions, iron ions and aluminum ions. .
进一步地，为了达到最佳的碱浸取效果，本发明实施例采用90-110g/L 的氢氧化钠溶液进行碱浸取，并且优选地采用100g/L的氢氧化钠溶液。Furthermore, in order to achieve the best alkali leaching effect, the embodiment of the present invention uses 90-110 g/L sodium hydroxide solution for alkali leaching, and preferably uses 100 g/L sodium hydroxide solution.
S3、向第一滤液中添加硫酸溶液，浸出氢氧化铝固体。S3. Add sulfuric acid solution to the first filtrate to leach solid aluminum hydroxide.
需要说明的是，利用硫酸法浸出氢氧化铝固体，成本低、效率高，从而使得本发明实施例的方案具备高效节能的有益效果。It should be noted that the leaching of aluminum hydroxide solid by sulfuric acid method has low cost and high efficiency, so that the solution of the embodiment of the present invention has the beneficial effect of high efficiency and energy saving.
S4、向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液。S4. Add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, and react to obtain a second filter residue and a second filtrate.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，实质上是对第一滤渣中的金属盐进一步的离子化，从而得到离子化的第二滤液以备下一步提取回收使用。Further, sulfuric acid solution and hydrogen peroxide solution are added to the first filter residue to react to obtain the second filter residue and the second filtrate, which is essentially to further ionize the metal salt in the first filter residue, thereby obtaining ionized second The filtrate is used for extraction and recovery in the next step.
S5、向第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液。S5. Add sodium hydroxide solution to the second filtrate, and pass ammonia gas to obtain iron hydroxide solid and a third filtrate.
进一步地，步骤五是分离出氢氧化铁固体的过程。需要说明的是，通过添加氢氧化钠溶液并通氨气可分离出高纯度的氢氧化铁。Further, step five is the process of separating out the ferric hydroxide solid. It should be noted that high-purity ferric hydroxide can be separated by adding sodium hydroxide solution and flowing ammonia gas.
S6、利用水热法从第三滤液中沉淀出碳酸锂。S6. Precipitate lithium carbonate from the third filtrate by hydrothermal method.
进一步地，利用水热法从第三滤液中沉淀出碳酸锂实质上是溶液中碳酸锂重结晶形成晶体碳酸锂的过程，本发明实施例通过水热法获得的碳酸锂一次沉锂率高，其可达高级产品的要求。Further, using the hydrothermal method to precipitate lithium carbonate from the third filtrate is essentially the process of lithium carbonate recrystallization in the solution to form crystalline lithium carbonate. The lithium carbonate obtained by the hydrothermal method in the embodiment of the present invention has a high primary lithium deposition rate. It can meet the requirements of advanced products.
需要说明的是，本发明实施例在对第一滤液、第二滤液以及第三滤液分别进行相应固体获取之前，均进行了除杂操作。并且具体地，在进行除杂操作时，采用与之对应的萃取剂进行萃取。需要强调的是，通过除杂操作，可以进一步地提高回收所得金属的纯度，这既能够提高回收率，又能提高所回收产品的品质，利于后续的再利用。It should be noted that, in the embodiment of the present invention, before the corresponding solids are obtained from the first filtrate, the second filtrate and the third filtrate, the impurity removal operation is performed. And specifically, during the impurity removal operation, the corresponding extractant is used for extraction. It should be emphasized that the purity of recovered metals can be further improved through the impurity removal operation, which can not only improve the recovery rate, but also improve the quality of the recovered products, which is beneficial to subsequent reuse.
本发明实施例还提供了一种废旧锂电池的回收处理工艺，其包括上述的废旧锂电池正极材料的处理方法。需要说明的是，本发明实施例的废旧锂电池的回收处理工艺具备和废旧锂电池正极材料的处理方法一样的优点，即工艺简单，回收率高，成本高，不产生二次污染，有利于企业经济效益的提高。The embodiment of the present invention also provides a recycling and treatment process for waste lithium batteries, which includes the above-mentioned treatment method for positive electrode materials of waste lithium batteries. It should be noted that the recovery and treatment process of waste lithium batteries in the embodiment of the present invention has the same advantages as the treatment method for the positive electrode material of waste lithium batteries, that is, the process is simple, the recovery rate is high, the cost is high, and no secondary pollution occurs, which is beneficial to Improvement of economic benefits of enterprises.
以下结合实施例对本发明的特征和性能作进一步的详细描述。The characteristics and performance of the present invention will be described in further detail below in conjunction with the examples.
实施例1Example 1
本实施例提供的一种废旧锂电池正极材料的处理方法，其包括：A kind of treatment method of waste lithium battery cathode material provided in this embodiment, it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。具体的预处理过程包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物，然后对破碎混合物进行过筛，得到正负极材料和粘结剂，最后对正负极材料和粘结剂进行650℃的加热燃烧。The waste lithium battery is pretreated to obtain the positive electrode material mainly composed of lithium iron phosphate. The specific pretreatment process includes crushing and vacuum-drying waste lithium batteries to obtain a crushed mixture, and then sieving the crushed mixture to obtain positive and negative materials and binders, and finally 650 to the positive and negative materials and binders ℃ heating combustion.
进一步地，对在预处理过程中产生的气体进行净化处理。Further, the gas generated in the pretreatment process is purified.
进一步地，采用100g/L的氢氧化钠溶液对正极材料进行碱浸取，得到第一滤渣和第一滤液，并对第一滤液进行除杂。Further, 100 g/L sodium hydroxide solution is used to carry out alkali leaching on the positive electrode material to obtain the first filter residue and the first filtrate, and remove impurities from the first filtrate.
进一步地，向经过除杂过的第一滤液中添加硫酸溶液，浸出氢氧化铝固体。Further, sulfuric acid solution is added to the first filtrate that has been cleaned of impurities to leach solid aluminum hydroxide.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，并对第二滤液进行除杂。Further, add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, react to obtain a second filter residue and a second filtrate, and remove impurities from the second filtrate.
进一步地，向经过除杂过的第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液，并对第三滤液进行除杂。Further, sodium hydroxide solution is added to the second filtrate that has been cleaned of impurities, and ammonia gas is passed through to obtain ferric hydroxide solid and a third filtrate, and the third filtrate is cleaned of impurities.
利用水热法从经过除杂过的第三滤液中沉淀出碳酸锂。其中，具体的水热法制备过程为先加热到730℃保持2h，再降低到720℃保持3h，最后缓慢降温至室温。Lithium carbonate is precipitated from the impurity-removed third filtrate by hydrothermal method. Among them, the specific preparation process of the hydrothermal method is to first heat to 730° C. for 2 hours, then lower the temperature to 720° C. for 3 hours, and finally cool down to room temperature slowly.
本实施例还提供了一种废旧锂电池的回收处理工艺，其包括本实施例提供的废旧锂电池正极材料的处理方法。This embodiment also provides a recovery and treatment process for waste lithium batteries, which includes the treatment method for the positive electrode material of waste lithium batteries provided in this embodiment.
实施例2Example 2
本实施例提供的一种废旧锂电池正极材料的处理方法，其包括：A kind of treatment method of waste lithium battery cathode material provided in this embodiment, it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。具体的预处理过程包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物，然后对破碎混合物进行过筛，得到正负极材料和粘结剂，最后对正负极材料和粘结剂进行650℃的加热燃烧。The waste lithium battery is pretreated to obtain the positive electrode material mainly composed of lithium iron phosphate. The specific pretreatment process includes crushing and vacuum-drying waste lithium batteries to obtain a crushed mixture, and then sieving the crushed mixture to obtain positive and negative materials and binders, and finally 650 to the positive and negative materials and binders ℃ heating combustion.
进一步地，对在预处理过程中产生的气体进行净化处理。Further, the gas generated in the pretreatment process is purified.
进一步地，采用90g/L的氢氧化钠溶液对正极材料进行碱浸取，得到第一滤渣和第一滤液，并对第一滤液进行除杂。Further, 90 g/L sodium hydroxide solution was used to perform alkaline leaching on the positive electrode material to obtain the first filter residue and the first filtrate, and the first filtrate was removed from impurities.
进一步地，向经过除杂过的第一滤液中添加硫酸溶液，浸出氢氧化铝固体。Further, sulfuric acid solution is added to the first filtrate that has been cleaned of impurities to leach solid aluminum hydroxide.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，并对第二滤液进行除杂。Further, add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, react to obtain a second filter residue and a second filtrate, and remove impurities from the second filtrate.
进一步地，向经过除杂过的第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液，并对第三滤液进行除杂。Further, sodium hydroxide solution is added to the second filtrate that has been cleaned of impurities, and ammonia gas is passed through to obtain ferric hydroxide solid and a third filtrate, and the third filtrate is cleaned of impurities.
利用水热法从经过除杂过的第三滤液中沉淀出碳酸锂。其中，具体的水热法制备过程为先加热到730℃保持2h，再降低到720℃保持3h，最后缓慢降温至室温。Lithium carbonate is precipitated from the impurity-removed third filtrate by hydrothermal method. Among them, the specific preparation process of the hydrothermal method is to first heat to 730° C. for 2 hours, then lower the temperature to 720° C. for 3 hours, and finally cool down to room temperature slowly.
本实施例还提供了一种废旧锂电池的回收处理工艺，其包括本实施例提供的废旧锂电池正极材料的处理方法。This embodiment also provides a recovery and treatment process for waste lithium batteries, which includes the treatment method for the positive electrode material of waste lithium batteries provided in this embodiment.
实施例3Example 3
本实施例提供的一种废旧锂电池正极材料的处理方法，其包括：A kind of treatment method of waste lithium battery cathode material provided in this embodiment, it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。具体的预处理过程包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物，然后对破碎混合物进行过筛，得到正负极材料和粘结剂，最后对正负极材料和粘结剂进行650℃的加热燃烧。The waste lithium battery is pretreated to obtain the positive electrode material mainly composed of lithium iron phosphate. The specific pretreatment process includes crushing and vacuum-drying waste lithium batteries to obtain a crushed mixture, and then sieving the crushed mixture to obtain positive and negative materials and binders, and finally 650 to the positive and negative materials and binders ℃ heating combustion.
进一步地，对在预处理过程中产生的气体进行净化处理。Further, the gas generated in the pretreatment process is purified.
进一步地，采用110g/L的氢氧化钠溶液对正极材料进行碱浸取，得到第一滤渣和第一滤液，并对第一滤液进行除杂。Further, 110 g/L sodium hydroxide solution was used to perform alkali leaching on the positive electrode material to obtain the first filter residue and the first filtrate, and the first filtrate was removed from impurities.
进一步地，向经过除杂过的第一滤液中添加硫酸溶液，浸出氢氧化铝固体。Further, sulfuric acid solution is added to the first filtrate that has been cleaned of impurities to leach solid aluminum hydroxide.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，并对第二滤液进行除杂。Further, add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, react to obtain a second filter residue and a second filtrate, and remove impurities from the second filtrate.
进一步地，向经过除杂过的第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液，并对第三滤液进行除杂。Further, sodium hydroxide solution is added to the second filtrate that has been cleaned of impurities, and ammonia gas is passed through to obtain ferric hydroxide solid and a third filtrate, and the third filtrate is cleaned of impurities.
利用水热法从经过除杂过的第三滤液中沉淀出碳酸锂。其中，具体的水热法制备过程为先加热到730℃保持2h，再降低到720℃保持3h，最后缓慢降温至室温。Lithium carbonate is precipitated from the impurity-removed third filtrate by hydrothermal method. Among them, the specific preparation process of the hydrothermal method is to first heat to 730° C. for 2 hours, then lower the temperature to 720° C. for 3 hours, and finally cool down to room temperature slowly.
本实施例还提供了一种废旧锂电池的回收处理工艺，其包括本实施例提供的废旧锂电池正极材料的处理方法。This embodiment also provides a recovery and treatment process for waste lithium batteries, which includes the treatment method for the positive electrode material of waste lithium batteries provided in this embodiment.
实施例4Example 4
本实施例提供的一种废旧锂电池正极材料的处理方法，其包括：A kind of treatment method of waste lithium battery cathode material provided in this embodiment, it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。具体的预处理过程包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物，然后对破碎混合物进行过筛，得到正负极材料和粘结剂，最后对正负极材料和粘结剂进行645℃的加热燃烧。The waste lithium battery is pretreated to obtain the positive electrode material mainly composed of lithium iron phosphate. The specific pretreatment process includes crushing and vacuum-drying waste lithium batteries to obtain a crushed mixture, and then sieving the crushed mixture to obtain positive and negative materials and binders, and finally subjecting the positive and negative materials and binders to 645 ℃ heating combustion.
进一步地，对在预处理过程中产生的气体进行净化处理。Further, the gas generated in the pretreatment process is purified.
进一步地，采用100g/L的氢氧化钠溶液对正极材料进行碱浸取，得到第一滤渣和第一滤液，并对第一滤液进行除杂。Further, 100 g/L sodium hydroxide solution is used to carry out alkali leaching on the positive electrode material to obtain the first filter residue and the first filtrate, and remove impurities from the first filtrate.
进一步地，向经过除杂过的第一滤液中添加硫酸溶液，浸出氢氧化铝固体。Further, sulfuric acid solution is added to the first filtrate that has been cleaned of impurities to leach solid aluminum hydroxide.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，并对第二滤液进行除杂。Further, add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, react to obtain a second filter residue and a second filtrate, and remove impurities from the second filtrate.
进一步地，向经过除杂过的第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液，并对第三滤液进行除杂。Further, sodium hydroxide solution is added to the second filtrate that has been cleaned of impurities, and ammonia gas is passed through to obtain ferric hydroxide solid and a third filtrate, and the third filtrate is cleaned of impurities.
利用水热法从经过除杂过的第三滤液中沉淀出碳酸锂。其中，具体的水热法制备过程为先加热到730℃保持2h，再降低到720℃保持3h，最后缓慢降温至室温。Lithium carbonate is precipitated from the impurity-removed third filtrate by hydrothermal method. Among them, the specific preparation process of the hydrothermal method is to first heat to 730° C. for 2 hours, then lower the temperature to 720° C. for 3 hours, and finally cool down to room temperature slowly.
本实施例还提供了一种废旧锂电池的回收处理工艺，其包括本实施例提供的废旧锂电池正极材料的处理方法。This embodiment also provides a recovery and treatment process for waste lithium batteries, which includes the treatment method for the positive electrode material of waste lithium batteries provided in this embodiment.
实施例5Example 5
本实施例提供的一种废旧锂电池正极材料的处理方法，其包括：A kind of treatment method of waste lithium battery cathode material provided in this embodiment, it comprises:
对废旧锂电池进行预处理，得到以磷酸铁锂为主要成分的正极材料。具体的预处理过程包括对废旧锂电池进行破碎和真空干燥，得到破碎混合物，然后对破碎混合物进行过筛，得到正负极材料和粘结剂，最后对正负极材料和粘结剂进行655℃的加热燃烧。The waste lithium battery is pretreated to obtain the positive electrode material mainly composed of lithium iron phosphate. The specific pretreatment process includes crushing and vacuum-drying waste lithium batteries to obtain a crushed mixture, and then sieving the crushed mixture to obtain positive and negative materials and binders, and finally subjecting the positive and negative materials and binders to 655 ℃ heating combustion.
进一步地，对在预处理过程中产生的气体进行净化处理。Further, the gas generated in the pretreatment process is purified.
进一步地，采用100g/L的氢氧化钠溶液对正极材料进行碱浸取，得到第一滤渣和第一滤液，并对第一滤液进行除杂。Further, 100 g/L sodium hydroxide solution is used to carry out alkali leaching on the positive electrode material to obtain the first filter residue and the first filtrate, and remove impurities from the first filtrate.
进一步地，向经过除杂过的第一滤液中添加硫酸溶液，浸出氢氧化铝固体。Further, sulfuric acid solution is added to the first filtrate that has been cleaned of impurities to leach solid aluminum hydroxide.
进一步地，向第一滤渣中添加硫酸溶液和过氧化氢溶液，反应得到第二滤渣和第二滤液，并对第二滤液进行除杂。Further, add sulfuric acid solution and hydrogen peroxide solution to the first filter residue, react to obtain a second filter residue and a second filtrate, and remove impurities from the second filtrate.
进一步地，向经过除杂过的第二滤液中添加氢氧化钠溶液，并通氨气，得到氢氧化铁固体和第三滤液，并对第三滤液进行除杂。Further, sodium hydroxide solution is added to the second filtrate that has been cleaned of impurities, and ammonia gas is passed through to obtain ferric hydroxide solid and a third filtrate, and the third filtrate is cleaned of impurities.
利用水热法从经过除杂过的第三滤液中沉淀出碳酸锂。其中，具体的水热法制备过程为先加热到730℃保持2h，再降低到720℃保持3h，最后缓慢降温至室温。Lithium carbonate is precipitated from the impurity-removed third filtrate by hydrothermal method. Among them, the specific preparation process of the hydrothermal method is to first heat to 730° C. for 2 hours, then lower the temperature to 720° C. for 3 hours, and finally cool down to room temperature slowly.
本实施例还提供了一种废旧锂电池的回收处理工艺，其包括本实施例提供的废旧锂电池正极材料的处理方法。This embodiment also provides a recovery and treatment process for waste lithium batteries, which includes the treatment method for the positive electrode material of waste lithium batteries provided in this embodiment.
试验例Test case
为了证明上述实施例1-5提供的废旧锂电池正极材料的处理方法的有益效果，本试验例选取实施例1-5的方案为实验样本例，并将传统的关于磷酸铁锂系列锂电池正极材料的分离方法作为对比例，其具体的结果如表1 所示：In order to prove the beneficial effect of the treatment method of the waste lithium battery positive electrode material provided by the above-mentioned embodiments 1-5, this test example selects the scheme of embodiment 1-5 as an experimental sample example, and uses the traditional lithium iron phosphate series lithium battery positive electrode The material separation method is used as a comparative example, and its specific results are shown in Table 1:
表1对废旧锂电池正极材料不同处理方法的回收率和成本情况Table 1 The recovery rate and cost of different treatment methods for waste lithium battery cathode materials
从表1中可以看出，本发明实施例的金属回收率要远高于对比例中的金属回收率，并且整体上都具有98％以上的回收率；另外，通过对回收成本的比较可以看出，本发明实施例提供的方案在回收成本上还不到对比例回收成本的一半，表现出了非常强的成本优势。因此，可以看出，本发明实施例提供的废旧电池正极材料的处理方法在回收率和回收成本上均具有非常强的优势，有利于提高企业的经济效益。As can be seen from Table 1, the metal recovery rate of the embodiment of the present invention is much higher than the metal recovery rate in the comparative example, and generally has a recovery rate of more than 98%; in addition, it can be seen by comparing the recovery cost It is shown that the recovery cost of the solution provided by the embodiment of the present invention is less than half of the recovery cost of the comparison example, showing a very strong cost advantage. Therefore, it can be seen that the treatment method for the waste battery positive electrode material provided by the embodiment of the present invention has very strong advantages in recovery rate and recovery cost, which is beneficial to improve the economic benefits of the enterprise.
综上所述，本发明实施例提供的废旧锂电池正极材料的处理方法通过采用碱溶解-酸浸出-分离铁-热法沉淀碳酸锂的工艺流程，有效地回收了废旧锂电池中的铁、铝和锂元素，其中，所采用的硫酸法浸出氢氧化铝工艺中，具备回收成本低、效率高且所得产品纯度高的优点；水热法沉淀碳酸锂具备一次性沉锂率高的优点。因此，本发明实施例提供的废旧锂电池正极材料的处理方法不但简单有效，而且可以使废旧电池中的主要元素Fe、 Al和Li得到高效回收，并且不会产生二次污染，故其可以显著提高经济效益；另外，本发明实施例提供的废旧锂电池的回收处理工艺包括上述的废旧锂电池正极材料的处理方法，故其具备上述处理方法的各项优点。In summary, the treatment method for the positive electrode material of the waste lithium battery provided by the embodiment of the present invention effectively recovers the iron, Aluminum and lithium elements, among them, the sulfuric acid leaching aluminum hydroxide process has the advantages of low recovery cost, high efficiency and high purity of the obtained product; the hydrothermal precipitation of lithium carbonate has the advantages of high lithium deposition rate at one time. Therefore, the processing method for the positive electrode material of the waste lithium battery provided by the embodiment of the present invention is not only simple and effective, but also can efficiently recover the main elements Fe, Al and Li in the waste battery, and will not produce secondary pollution, so it can significantly Improve economic benefits; In addition, the waste lithium battery recycling process provided by the embodiment of the present invention includes the above-mentioned treatment method for the waste lithium battery positive electrode material, so it has the advantages of the above-mentioned treatment method.
以上所描述的实施例是本发明一部分实施例，而不是全部的实施例。本发明的实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The embodiments described above are some, not all, embodiments of the present invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the claimed invention but to represent only selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without creative efforts fall within the protection scope of the present invention.
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