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A kind of method for extracting lithium hydroxide from waste residue containing lithium phosphate

A lithium hydroxide and lithium phosphate technology, applied in electrochemical generators, waste collector recycling, recycling technology, etc., can solve the problems of lack of value-added recycling processing technology, few reports on efficient lithium recovery, and reduce the purification process. The effect of burden, efficient value-added utilization, and short process flow

Active Publication Date: 2020-06-02
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In addition, in order to achieve the purpose of resource recycling, domestic and foreign countries have also paid more attention to the process technology of recovering valuable metals from waste lithium-ion batteries, but a large number of research and production technology work mainly revolves around the recovery of Co, Ni and other metals. However, there are few reports on technical research on efficient lithium recovery
Especially when dismantling and cleaning waste batteries, a large amount of waste electrolyte enters the cleaning water and undergoes hydrolysis, resulting in waste residue containing a large amount of transition metal phosphate, lithium phosphate, conductive agent, etc., and there is still a lack of effective value-added recovery treatment technology

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 50g of lithium phosphate waste residue and grind it to -80 mesh, mix it with barium oxide powder with a stoichiometric ratio of 100%, add water at a solid-to-liquid ratio of 1:5 to make a slurry, and put it in a ball mill reaction kettle for grinding at 60°C For leaching, the volume ratio of grinding balls to slurry is 1:3, the grinding speed is 200 rpm, and the leaching time is 0.5 hours. After the leaching is completed, filter the slurry, and add water to wash the filter cake of the leach residue according to the solid-to-liquid ratio of 1:2, mix the collected washing liquid with the filtrate, add 5 ml of 300 g / L sodium carbonate solution and stir for 0.5 Hours, the purified solution was obtained after filtration. The obtained purified solution was evaporated at 80°C, cooled and crystallized, and filtered, and the filtered crystal filter cake was dried at 120°C to obtain lithium hydroxide monohydrate. The lithium leaching rate was calculated to be 84.6% after a...

Embodiment 2

[0035] The operation process is the same as that in Example 1, except that calcium oxide is replaced by barium oxide, the dosage is 120% of the stoichiometric ratio, the solid-to-liquid ratio of the leaching slurry is 1:50, the leaching temperature is 150°C, the grinding speed is 800 rpm, and the leaching time is 5 Hours, the solid-to-liquid ratio of the leaching residue filter cake washing is 1:5, the number of washings is 5 times, and the purification reaction time is 2 hours. The obtained purified solution was evaporated at 80°C, cooled and crystallized, and filtered, and the filtered crystal filter cake was dried at 120°C to obtain lithium hydroxide monohydrate. The lithium leaching rate was calculated to be 87.1% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.01%.

Embodiment 3

[0037] The operation process is the same as in Example 1, except that barium hydroxide is replaced by barium oxide, and the dosage is 110% of the stoichiometric ratio, the solid-to-liquid ratio of the leaching slurry is 1:7, the leaching temperature is 90°C, the grinding speed is 300 rpm, and the leaching time is 1.5 hours, the solid-to-liquid ratio of leaching residue filter cake washing is 1:3, the number of washings is 3 times, and the purification reaction time is 1 hour. The obtained purified solution was evaporated at 80°C, cooled and crystallized, and filtered, and the filtered crystal filter cake was dried at 120°C to obtain lithium hydroxide monohydrate. The lithium leaching rate was calculated to be 92.1% after atomic absorption analysis of the washed leaching residue. The purity of the obtained lithium hydroxide monohydrate was 99.22%.

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Abstract

The invention relates to a method for extracting lithium hydroxide from lithium phosphate-containing waste, and belongs to the technical field of lithium ion battery materials and resource recycling.A purpose of the present invention is to provide a method for extracting lithium hydroxide from lithium phosphate-containing waste. According to the present invention, the method is characterized in that lithium phosphate-containing waste and more than one alkaline earth metal oxides or hydroxides are mixed, the mixture is heated, the heated mixture is subjected to strong grinding leaching, the leaching solution is purified to remove the residual alkaline earth metal ions, and evaporating crystallizing is performed to prepare lithium hydroxide monohydrate so as to achieve the efficient value-added utilization of lithium phosphate-containing waste; and the method has advantages of reasonable process design, high resource utilization rate, high product purity and convenient large-scale industrial application.

Description

technical field [0001] The invention relates to a method for extracting lithium hydroxide from waste residue containing lithium phosphate, belonging to the technical field of lithium ion battery materials and resource recycling. [0002] technical background [0003] Lithium-ion batteries are widely used in the mobile electronic communication market due to their advantages such as high specific energy, long cycle life, and no memory effect, and have also become one of the preferred power batteries for pure electric vehicles. With the rapid development of the lithium-ion battery industry, the demand for related battery materials continues to grow. When preparing electrode materials for lithium-ion batteries, whether it is the early LiCoO 2 Or the LiMn that was gradually developed in the later stage 2 o 4 、LiFePO 4 Or ternary materials, without exception, must use high-purity lithium salts as raw materials, mainly lithium carbonate or lithium hydroxide. Due to the influenc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): H01M10/54H01M10/0525
CPCH01M10/0525H01M10/54Y02E60/10Y02W30/84
Inventor 陈亚甘辉曹利涛关杰豪陈白珍石西昌
Owner CENT SOUTH UNIV
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