High-efficiency purification process for acid leaching solutions of active substances in waste lithium batteries

A waste lithium battery and acid leaching solution technology, which is applied in the direction of improving process efficiency, can solve the problems of high cost, large loss of cobalt in hydrolysis precipitation, and difficult regeneration of extraction agent, etc., and achieve the effect of large flexible operation and simple operation

Inactive Publication Date: 2009-12-09
CENT SOUTH UNIV
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Problems solved by technology

The method of the purification process report of the waste lithium-ion battery cathode material acid leaching solution in the solution is as follows, Wu Fang (Journal of Nonferrous Metals, 2004, 14 (4), p697) introduces the use of P204 to extract and purify the acid leaching solution, and this method is suitable for impurity content Constant feed liquid, and the impurity content cannot be too low. For waste lithium batteries recovered from industrialization, the content of various metals fluctuates greatly, and the operating conditions of the method of using P204 to extract and separate iron, aluminum, copper, and manganese also fluctuate greatly , is unfavorable for industrialized operation, and simultaneously P204 is difficult to regenerate extractant after extracting and separating iron, needs 6mol / L hydrochloric acid to be stripping agent and just can iron stripping completely, and cost is high, and environmental pollution is big; Hu Chuanyue (Battery, 2006, 36 (6 ), p481) introduces the use of NaOH solution to adjust the pH of the pickling solution to remove impurity ions in the pickling solution. This method uses NaOH solution to hydrolyze the impurity, and the obtained hydroxide precipitate is generally an amorphous colloidal precipitate. Cobalt ions The amount of adsorption by hydrolysis precipitation is very large, the recovery rate of cobalt is low, and this method does not involve the recovery of impurity manganese; Impurity removal, the cost of this method is high, the loss of cobalt by hydrolysis precipitation is large, and this method does not involve the recovery of impurity manganese

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  • High-efficiency purification process for acid leaching solutions of active substances in waste lithium batteries

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Embodiment 1

[0019] Measure 500ml of the acidic leaching solution of the positive electrode active material of the waste lithium battery, which contains metal ions such as cobalt, copper, aluminum, manganese, iron, nickel, etc., and the initial pH value is 0.4. After the temperature rises to 90°C, add 500g / L to the solution NaOH solution to adjust the pH value to 1.0, then slowly add NaOH solution with a mass percentage concentration of 10% to adjust the pH value to 1.5, stir for 2 hours, then control the end point pH value to 2.0, filter, and slowly add a theoretical amount of 110% mass to the filtrate The percentage concentration is 10% sodium hypochlorite solution, react at 50°C for 2 hours, use the NaOH solution with a mass percentage concentration of 5% to control the pH to about 2.5 during the reaction, filter, and slowly add a mass percentage concentration of 10% ammonium bicarbonate solution to the filtrate , adjust the pH value to 3.5 at 90°C, react for half an hour and filter, slo...

Embodiment 2

[0021] Measure 500ml of the acidic leaching solution of the positive electrode active material of the waste lithium battery, which contains metal ions such as cobalt, copper, aluminum, manganese, iron, nickel, etc., and the initial pH value is 0.5. After the temperature rises to 90°C, add 500g / L to the solution NaOH solution to adjust the pH value to 1.2, then slowly add NaOH solution with a mass percentage concentration of 10% to adjust the pH value to 1.7, stir for 2 hours, then control the end point pH value to 2.3, filter, and slowly add a theoretical amount of 110% by mass to the filtrate Fraction is 10% sodium hypochlorite solution, reacts at 70 DEG C for 2 hours, and the reaction process is controlled pH 2.5 with the NaOH solution of 5% mass percent concentration, filters, and slowly adding mass percent concentration in the filtrate is 10% mass percent concentration Ammonium bicarbonate solution, Adjust the pH value to 3.7 at 90°C, react for half an hour and filter, slow...

Embodiment 3

[0023]Measure 500ml of the acidic leaching solution of the positive electrode active material of the waste lithium battery, which contains metal ions such as cobalt, copper, aluminum, manganese, iron, nickel, etc., and the initial pH value is 0.6. After the temperature rises to 90°C, add 500g / L to the solution NaOH solution to adjust the pH value to 1.4, then slowly add NaOH solution with a mass percentage concentration of 10% to adjust the pH value to 1.7, stir for 3 hours, then adjust the final pH value to 2.3, filter, and slowly add a theoretical amount of 120% by mass to the filtrate Fraction is 10% sodium hypochlorite solution, reacts at 70 DEG C for 2 hours, and the reaction process is controlled pH 2.5 with the NaOH solution of 5% mass percent concentration, filters, and slowly adding mass percent concentration in the filtrate is 10% mass percent concentration Ammonium bicarbonate solution, Adjust the pH value to 4.0 at 90°C and react for half an hour to filter, slowly a...

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Abstract

The invention discloses a high-efficiency purification process for acid leaching solutions of active substances in waste lithium batteries. The process comprises working procedures of the purification of the acid leaching solutions of the active materials of positive poles in the waste lithium batteries. The process is mainly characterized by adopting an improved hydrolysis precipitation method and an improved oxidation precipitation method to remove impurity ions in the acid leaching solutions. The process comprises four steps of removing iron by a sodium jarosite method; removing manganese by the oxidation precipitation method; removing aluminum by ammonium bicarbonate; and removing copper by sodium carbonate. A method used by the invention has the advantages of low cost, large operation flexibility, and high cobalt recovery rate, can comprehensively recover valuable metals such as the aluminum, the copper, the manganese and the like, and is suitable for lithium cobalt oxide battery materials which are widely used at present and heavily doped battery materials which may be used in the future. The use of the method can ensure that the total recovery rate of cobalt in waste lithium ion batteries is about 98 percent, and the content of impurities is lower than 2 percent.

Description

technical field [0001] The invention relates to the comprehensive recovery of valuable components in waste lithium batteries, in particular to a method for purifying and removing impurities from the acidic leaching solution of positive electrode active materials of waste lithium batteries. Background technique [0002] Since the commercialization of lithium-ion batteries in 1990, they have been widely used in portable electronic devices such as mobile phones, notebook computers and cameras due to their advantages such as high energy density, light weight, long life and no memory. According to statistics, in 2000, the global production of lithium-ion batteries exceeded 580 million, and the domestic production was about 100 million; in 2003, the global production reached 1.255 billion; in 2005, the output was close to 1.5 billion; The life of lithium-ion batteries is usually between 500-1000 times. After using hundreds of times (usually 2-3 years), the electrodes will expand, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/46C22B23/00
CPCY02P10/20
Inventor 唐新村满瑞林张阳陈亮曾智文李连兴肖源化王志敏瞿毅
Owner CENT SOUTH UNIV
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