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A method for extracting lithium hydroxide from lithium phosphate waste residue

A lithium hydroxide, lithium phosphate technology, applied in lithium oxide;/hydroxide, waste collector recycling, lithium carbonate;/acid carbonate, etc., can solve the lack of value-added recycling treatment technology, efficient There are few reports on the recovery of lithium, which achieves the effects of high-efficiency value-added utilization, reduction of anode potential, and short process flow

Active Publication Date: 2019-11-12
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

[0036] Weigh 50g of lithium phosphate waste slag obtained from a lithium carbonate plant, grind and disperse it, mix it with a sulfuric acid solution with a concentration of 2mol / L to form a slurry with a liquid-solid ratio of 3:1, and carry out stirring and leaching treatment at room temperature, and filter after leaching for 30 minutes Obtain the pickling solution, and adjust the pH value of the solution to 6. Put the obtained acid dipping solution into the raw material pool of the three-cell electrolytic cell, put 350 mL of lithium hydroxide with a concentration of 0.05 mol / L in the cathode pool, put 200 mL of 2 mol / L sodium hydroxide in the anode pool, use stainless steel mesh as the cathode, and coat the surface with The titanium mesh covered with ruthenium oxide is the anode, and the model of the cation selective permeable membrane is NAFION 117, and the manufacturer is DuPont Company of the United States. The model of the anion selective permeable membrane is TWDDA2, an...

Embodiment 2

[0039] The operation process is the same as in Example 1, except that the cathode pool is put into 350 mL of lithium hydroxide with a concentration of 0.1 mol / L, the anode pool is put into a ferrous sulfate solution with a pH value of 1 and a concentration of 1 mol / L, and the current density is 100 mA / cm ‐2 Carry out electrolysis, during the electrolysis process, continuously add ferrous sulfate to the anode pool and keep the pH value of the anolyte unchanged, and filter the anolyte intermittently, take out the catholyte after cumulative electrolysis for 18 hours, cool and crystallize after evaporation at 80°C and filtered, and the obtained crystal filter cake was dried at 120° C. to obtain lithium hydroxide monohydrate (purity: 99.4%), and the calculated recovery rate of lithium was 90.8%. Adjust the pH value of the anolyte slurry to 4 and then filter to obtain iron phosphate with a purity of 99.1%.

Embodiment 3

[0041] Operation process is the same as embodiment one, just cathode pool is put into concentration and is the sodium hydroxide 350mL of 0.2mol / L, and anode pool is put into the ferrous chloride solution that pH value is 3 and concentration is 4mol / L, and iron plate is anode, The current density is 30mA / cm ‐2 Carry out electrolysis, maintain the pH value of the anolyte during the electrolysis process, and intermittently filter the anolyte and replace the anode, take out the catholyte after 48 hours of accumulated electrolysis, cool and crystallize after evaporation at 80°C and filter, and filter the obtained The crystal filter cake was dried at 120° C. to obtain lithium hydroxide monohydrate (purity: 97.4%), and the calculated recovery rate of lithium was 89.1%. Adjust the pH value of the anolyte slurry to 8 and then filter to obtain ferrous phosphate with a purity of 97.2%.

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Abstract

Belonging to the technical field of resource recycling, the invention relates to a method for preparation of lithium hydroxide and other phosphates from waste residue containing lithium phosphate. Theinvention aims to provide a method for preparation of lithium hydroxide and other phosphates from waste residue containing lithium phosphate. The key point of the method lies in that: an acidic solution is employed to leach lithium phosphate residue, the leachate is put into a three-tank electrolytic bath for electrolysis, phosphate radicals and lithium ions in the lithium phosphate solution canbe effectively separated and converted into lithium hydroxide and other metal phosphates, thereby reaching the purpose of efficient and value-added utilization of waste residue containing lithium phosphate.

Description

technical field [0001] The invention relates to a method for extracting lithium hydroxide from waste residue containing lithium phosphate; it belongs to the technical field of 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 influence of reactivity, etc., lithium ph...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/02C01D15/08H01M10/54
CPCC01D15/02C01D15/08H01M10/54Y02W30/84
Inventor 陈亚关杰豪曹利涛甘辉陈白珍石西昌
Owner CENT SOUTH UNIV
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