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Preparation method of battery-grade Ni-Co-Mn mixed solution and battery-grade Mn solution

A ni-co-mn, battery-level technology, applied in the field of lithium-ion batteries, can solve the problems of low recovery rate and unsatisfactory impurity removal effect, and achieve the effect of improving recovery rate, reducing impurity content, and improving large-scale application of the process

Active Publication Date: 2020-05-19
JINGMEN GEM NEW MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing battery-grade Ni-Co-Mn mixed solution and battery-grade Mn solution, which is used to solve the problem of low recovery rate when reclaiming Co, Ni and Mn elements in waste lithium ion batteries in the prior art. Low, and the impurity removal effect is not ideal

Method used

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  • Preparation method of battery-grade Ni-Co-Mn mixed solution and battery-grade Mn solution
  • Preparation method of battery-grade Ni-Co-Mn mixed solution and battery-grade Mn solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 100g of mixed positive and negative electrode powder of lithium ion battery, add 100ml of sulfuric acid, 60g of 30% hydrogen peroxide for acid leaching, filter to remove insoluble residue to obtain leaching solution, and the leaching rates of cobalt, nickel and manganese are: 91.64%, 91.65%, and 90.67%, respectively. The leaching solution was adjusted to pH 5.0 with 10% liquid caustic soda while being fed with air, and filtered to remove iron and aluminum after reacting for 2 hours to obtain an alkalized mixed solution. Add 1.5 times the theoretical amount of sodium fluoride to the alkalized mixed solution, stir and react at 60°C for 2 hours, then filter to remove lithium, calcium and magnesium, and obtain a synchronous precipitation filtrate; age the obtained synchronous precipitation filtrate at room temperature for 4 hours to remove calcium, magnesium, lithium, Filter to obtain the aged filtrate containing 55g / L of cobalt, nickel and manganese, wherein Fe: 0.000...

Embodiment 2

[0030] Weigh 100g of the positive and negative electrode mixed powder of the lithium-ion battery, add 123ml of sulfuric acid, 135g of 30% hydrogen peroxide for acid leaching, and filter to remove the insoluble residue to obtain the leaching solution. The leaching rates of cobalt, nickel and manganese are: 99.64%, 99.65%, and 98.67%, respectively. Filter to remove insoluble residue, add 1.05 times the theoretical molar amount of hydrogen peroxide to the leaching solution, and add 10% liquid caustic soda to adjust the pH to 4.5, react for 2 hours and filter to remove iron and aluminum to obtain an alkalized mixed solution. Add 1.2 times the theoretical amount of sodium fluoride to the alkalized mixture, stir and react at 60°C for 2 hours, then filter to remove lithium, calcium and magnesium to obtain a synchronous precipitation filtrate; age the obtained synchronous precipitation filtrate at room temperature for 4 hours to remove calcium and magnesium Lithium, filtered to obtain ...

Embodiment 3

[0032] Using the aging filtrate prepared in Example 1, the aging filtrate and the P204 organic solvent with a saponification rate of 45% were subjected to 7-stage countercurrent extraction at a ratio of 1:3, and all the nickel, cobalt, and manganese in the solution were extracted, and the obtained The organic phase loaded with nickel, cobalt and manganese was washed with 0.8mol / L dilute acid at a ratio of 3:1 for 8 stages of countercurrent washing. After washing, the organic phase and 4mol / L sulfuric acid are subjected to 8-stage countercurrent back-extraction at a ratio of 8:1, and the back-extraction solution can obtain a battery-grade nickel-cobalt-manganese solution, wherein the total content of nickel-cobalt-manganese is >100g / L. A manganese-containing solution outlet is set up in the middle of the stripping section, and the manganese-containing solution is refined and removed with P204 extractant to obtain a battery-grade manganese sulfate solution.

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Abstract

The invention discloses a preparation method of a battery-grade Ni-Co-Mn mixed solution and a battery-grade Mn solution. The preparation method comprises the following steps: acid dissolution, alkalization and impurity removal, calcium-magnesium-lithium synchronous precipitation, deep aging and impurity removal, collaborative extraction and refined extraction. The deep aging impurity removal and synergistic extraction step comprises the following steps: carrying out deep aging on filtrate obtained after the calcium-magnesium-lithium synchronous precipitation step, and performing filtering to remove impurities, so as to obtain aged filtrate; and extracting the aged filtrate by using P204 to obtain a loaded organic phase, and carrying out graded reverse extraction on the loaded organic phaseto obtain a battery-grade Ni-Co-Mn mixed solution and a Mn-containing solution. Through cooperation of multiple process steps of calcium-magnesium-lithium synchronous precipitation, deep aging impurity removal and synergistic extraction, the impurity content of the obtained battery-grade Ni-Co-Mn mixed solution is remarkably reduced, and the battery-grade Ni-Co-Mn mixed solution can be directly applied to preparation of a lithium battery ternary precursor material; and meanwhile, a battery-grade Mn solution can be obtained, large-scale application of the process is facilitated, and economic benefits are improved.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, in particular to a method for preparing a battery-grade Ni-Co-Mn mixed solution and a battery-grade Mn solution. Background technique [0002] my country's automotive power lithium-ion battery market has experienced explosive growth, and the application market has increasingly strict requirements on the performance of lithium-ion batteries. At present, the most widely used power lithium-ion battery systems at home and abroad are mainly lithium iron phosphate and ternary systems, such as nickel A battery system composed of three metal elements, manganese-cobalt or nickel-cobalt-aluminum, and the manufacturing cost of high-performance lithium-ion batteries for vehicles is relatively high; due to the increasing use of lithium batteries used in new energy vehicles, a large amount of waste will be generated Therefore, how to effectively recycle waste lithium-ion batteries has become an urgent proble...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/54H01M10/0525
CPCH01M10/54H01M10/0525Y02W30/84Y02E60/10H01M4/525H01M4/505H01M4/1391H01M10/052C22B7/007C22B23/0453C22B23/0407C22B47/00Y02P10/20C01D15/04C01F5/28C01F11/22C01G45/003C01G51/003C01G53/003
Inventor 许开华蒋振康李琴香张坤王文杰王峻温世红
Owner JINGMEN GEM NEW MATERIAL
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