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Method for preparing battery-stage anhydrous lithium chloride

A battery-grade lithium chloride technology, applied in the direction of alkali metal chloride, can solve the problems of wasting energy, high content of barium chloride, and increased evaporation in the process, so as to shorten the process route, reduce the loss of lithium, and operate The effect of step simplification

Active Publication Date: 2009-03-18
TIANQI LITHIUM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] However, there are some deficiencies in this method: (1) This method does not propose a reliable method for removing Na + , Mg 2+ , Fe 3+ , CO 3 2- , acid insolubles and other impurities, resulting in LiCl product quality can not be guaranteed; (2) the method removes Ca with lithium carbonate solution 2+ 、Ba 2+ , because the solubility of lithium carbonate is low, a large amount of water will be brought in, resulting in increased evaporation in the subsequent process and a waste of energy; (3) under the Li concentration described in it, CO 3 2- Ba 2+ Completely removed, resulting in high content of barium chloride in lithium chloride products, affecting product quality
[0013] In addition, the methods of producing LiCl such as liquid membrane method, ion exchange adsorption method, salting out method, flotation method and extraction method are still in the laboratory research stage, and the industrial implementation is not yet mature.

Method used

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  • Method for preparing battery-stage anhydrous lithium chloride

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Embodiment 1

[0063] see figure 1 , the preparation method of battery grade anhydrous lithium chloride of the embodiment of the present invention 1 comprises the following steps:

[0064] (1) Will Li 2 Li with an O concentration of 25 g / l 2 SO 4 Solution—Add 6000ml of lithium concentrate acid clinker leaching solution into a stainless steel reaction vessel, and add 659g of CaCl under stirring 2 80% CaCl 2 2H 2 Add NaOH to adjust the pH value to 11.5, and react at 90°C for 50 minutes. After keeping the temperature for 80 minutes, vacuum filter and wash the filter cake with deionized water. The washing water is used for the next preparation of CaCl 2 Solution, filter cake as by-product CaSO 4 2H 2 0, the filtrate is LiCl solution (conversion solution);

[0065] (2) Adding 102g of BaCO with a main content of 99% in the conversion liquid obtained in step (1) 3 , after stirring and reacting for 120min, vacuum filtration, the filter cake was washed with deionized water, and the filter ca...

Embodiment 2

[0072] see figure 1 , the preparation method of the embodiment of the present invention 2 battery-grade lithium chloride anhydrous comprises the following steps:

[0073] (1) Will Li 2 Li with an O concentration of 25 g / l 2 SO 4 Solution—Add 6000ml of lithium concentrate acid clinker leaching solution into a stainless steel reaction vessel, and add 555g of CaCl under stirring 2 80% CaCl 2 2H 2 Add NaOH to adjust the pH value to 9, and react at 65°C for 30 minutes. After keeping the temperature for 60 minutes, vacuum filter, wash the filter cake with deionized water, and use the washing water for the next preparation of CaCl 2 Solution, filter cake as by-product CaSO 4 2H 2 0, the filtrate is LiCl solution (conversion solution);

[0074] (2) Adding 118g of BaCO with a main content of 99% in the conversion liquid obtained in step (1) 3 , after stirring and reacting for 80min, vacuum filtration, the filter cake was washed with deionized water, and the filter cake was the...

Embodiment 3

[0080] see figure 1 , the preparation method of the embodiment of the present invention 3 battery-grade lithium chloride anhydrous comprises the following steps:

[0081] (1) Will Li 2 Li with an O concentration of 25 g / l 2 SO 4 Solution 1: Add 6000ml of lithium concentrate acid clinker leaching solution into a stainless steel reaction vessel, and add 590g of CaCl under stirring 2 80% CaCl 2 2H 2 Add NaOH to adjust the pH value to 10, and react at 80°C for 50 minutes. After keeping the temperature for 70 minutes, vacuum filter and wash the filter cake with deionized water. The washing water is used for the next preparation of CaCl 2 Solution, filter cake as by-product CaSO 4 2H 2 0, the filtrate is LiCl solution (conversion solution);

[0082] (2) Adding 109g of BaCO with a main content of 99% in the conversion liquid obtained in step (1) 3 , after stirring and reacting for 100min, vacuum filtration, the filter cake was washed with deionized water, and the filter cake...

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Abstract

The invention provides a preparation method of a battery grade lithium chloride, comprising: (1) calcium chloride is added into the acid clinker extracting solution of lithium concentrate - lithium sulfate solution, the PH value of the solution is regulated by NaOH to eliminate Fe and Mg, and the precipitation of CaSO4.2H2O, Fe(OH)3 and Mg(OH)2 and lithium chloride solution are obtained after the reaction; (2) the products of step (1) are filtered and cleaned to eliminate the precipitation of CaSO4.2H2O, Fe(OH)3 and Mg(OH)2, and the LiCl solution, i.e. a conversion solution is prepared; (3) the conversion solution is added with BaCO3, and filtered and cleaned after the reaction, to eliminate SO42- and Ca2+, and the LiCl concentrate liquid 1 is prepared; (4) the LiCl concentrate liquid is added with HCL and boiled to eliminate CO32-, and added with NaOH solution to back blend PH, then be evaporated, condensed, cooled, crystallized and separated, and the LiCl concentrate liquid 2 is obtained; (5) the LiCl concentrate liquid is added with refining agent, and filtered and cleaned after the reaction to eliminate Na, and the LiCl finish liquid is prepared, the LiCl finish liquid is condensed and dried, and finally the battery grade LiCl product is prepared. The invention has simple production process and can be easily operated.

Description

Technical field: [0001] The invention relates to a preparation method of battery-grade anhydrous lithium chloride. Background technique: [0002] Lithium chloride is an important lithium salt product, in addition to being used in air-conditioning dehumidifiers, bleaches, insecticides, synthetic fibers, pharmaceutical industry, lithium batteries, solar cells, metal alloy welding agents or fluxes, polymer material synthesis As a catalyst, another very important use is to produce metal lithium by molten salt electrolysis. At present, metal lithium has not only become one of the most important strategic substances in national defense, but also an important metal element closely related to human daily life. Lithium metal and its alloys and compounds are widely used in atomic energy industry, metallurgical industry, battery, glass, ceramics, chemical industry, aerospace industry manufacturing and other fields. In recent years, lithium chloride has also begun to be widely used in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D3/04
Inventor 姚开林金鹏霍立明涂明江黄春莲
Owner TIANQI LITHIUM CORP
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