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Production of lithium fluoride

A lithium fluoride and ammonium fluoride technology, which is applied in the direction of alkali metal fluoride, can solve the problems of low yield of high-purity products, low raw material purity requirements, high raw material purity requirements, etc., achieve high reaction conversion rate and improve resource utilization Efficiency and simple operation

Inactive Publication Date: 2007-11-21
BYD CO LTD
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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 overcome the disadvantages of low product purity or low yield of high-purity products and high requirements for raw material purity obtained in the prior art, and provide a fluorinated product with high product purity, high yield and low requirements for raw material purity. Lithium preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] This example is used to illustrate the preparation method of lithium fluoride provided by the present invention.

[0025] 86 grams of 47% by weight of hydrofluoric acid and 174 grams of 25% by weight of ammonia were mixed in a reaction vessel containing a polytetrafluoroethylene liner at 5°C for 80 minutes to prepare an ammonium fluoride solution, and then the solution was transferred to into a 1000 ml round-bottomed three-neck flask, add 96 g of lithium chloride and 300 ml of water, stir and react at 45°C for 90 minutes, then filter the system, wash the resulting solid with deionized water until the pH of the washing solution is 7, and then Dry at 150° C. for 13 hours to obtain 48.8 g of dried lithium fluoride solid with a purity of 99.86%. In addition, the filtered mother liquor is heated and concentrated at 95°C in a device equipped with a tail gas conduit until no hydrogen fluoride gas escapes from the system, wherein the tail gas is absorbed by water, the mother li...

Embodiment 2

[0027]This example is used to illustrate the preparation method of lithium fluoride provided by the present invention.

[0028] 106 grams of 47% by weight of hydrofluoric acid and 174 grams of 25% by weight of ammonia were mixed in a reaction vessel containing a polytetrafluoroethylene liner at 30°C for 30 minutes to prepare an ammonium fluoride solution, and then the solution was transferred to into a 1000 ml round-bottomed three-neck flask, add 76 g of lithium chloride and 200 ml of water, stir and react at 35°C for 110 minutes, then filter the system, wash the resulting solid with deionized water until the pH of the washing solution is 7, and then Dry at 350°C for 6 hours to obtain 37.8 g of dry lithium fluoride solid with a purity of 99.9%. In addition, heat and concentrate the filtered mother liquor at 95°C in a device equipped with a tail gas conduit until no hydrogen fluoride gas escapes from the system, wherein the tail gas is absorbed by water, the mother liquor is sl...

Embodiment 3

[0030] This example is used to illustrate the preparation method of lithium fluoride provided by the present invention.

[0031] 66 grams of lithium chloride, 200 milliliters of water and 174 grams of ammonium fluoride solution with a concentration of 33% by weight were added together in a 1000 milliliter round-bottomed three-necked flask, stirred and reacted at 80° C. for 30 minutes, and then the system was filtered to obtain a solid Wash with deionized water until the pH of the washing solution is 7, and then dry at 250° C. for 9 hours to obtain 37.7 g of dry lithium fluoride solid with a purity of 99.9%. In addition, heat and concentrate the filtered mother liquor at 98°C in a device equipped with a tail gas conduit until no hydrogen fluoride gas escapes from the system, wherein the tail gas is absorbed by water, the mother liquor is slowly cooled to 8°C, and filtered to obtain 77.6 grams of ammonium chloride crystals, the mother liquor is collected for later use.

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Abstract

Production of lithium fluoride is carried out by putting fluorine source and soluble lithium salt into water and contact reacting. It has better purity and resources utilization rate and higher conversion. It can be used to recover lithium salt.

Description

technical field [0001] The invention relates to a preparation method of lithium fluoride. Background technique [0002] Lithium fluoride is a white non-hygroscopic cubic crystal, which is insoluble in water, alcohol and other organic solvents. In the industry, lithium fluoride is widely used as an additive in the production of glaze, glass, and ceramics to reduce the firing temperature and the heat resistance, wear resistance, and acid resistance of the product. High-purity lithium fluoride is also used as a fluorinated glass component; and for the synthesis of electrolytes for secondary lithium batteries (such as lithium hexafluorophosphate). [0003] At present, lithium fluoride is mainly produced from lithium carbonate or lithium hydroxide and fluorine source hydrofluoric acid, because lithium fluoride easily reacts with hydrofluoric acid to form unstable lithium hydrogen fluoride (LiHF 2 ), lithium fluoride easily reacts with lithium hydroxide to generate LiF LiOH doub...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D3/02
Inventor 陆艳玲
Owner BYD CO LTD
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