Method for preparing high-purity lithium fluoride

A fluorinated, high-purity technology, applied in lithium halide and other directions, can solve the problems of production restrictions and high quality requirements, and achieve the effects of low raw material cost, high product conversion rate and uniform particle size.

Inactive Publication Date: 2019-08-30
GUIZHOU INST OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has high requirements on the quality of raw materials, and the production is greatly limited by raw materials.

Method used

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  • Method for preparing high-purity lithium fluoride

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1) Weigh 28g of lithium carbonate powder and add it to a 200ml polytetrafluoroethylene beaker, slowly add 90ml of 36% hydrochloric acid under stirring, and stir until lithium carbonate is completely dissolved;

[0031] 2) Heat the solution obtained by the above reaction to 80° C., slowly add 50 ml of hydrofluoric acid with a mass percent concentration of 40% under stirring, and continue to stir and react for 1.5 hours to obtain a mixed solution containing lithium fluoride precipitate;

[0032] 3) The above-mentioned mixed solution was left to stand for 1 hour, and then separated by a centrifuge to obtain a fluoride physical precipitate and a mother liquor of hydrochloric acid, and the mother liquor of hydrochloric acid can be recovered as a raw material for the reaction with lithium carbonate in step 1).

[0033] 4) Wash the fluoride precipitate obtained in step 3) with 75°C deionized water for 5 times, separate it with a centrifuge, put it in a vacuum drying oven, and d...

Embodiment 2

[0035] 1) Weigh 28g of lithium carbonate powder and add it to a 200ml polytetrafluoroethylene beaker, slowly add 90ml of 36% hydrochloric acid under stirring, and stir until lithium carbonate is completely dissolved;

[0036] 2) Heat the solution obtained by the above reaction to 90° C., slowly add 150 ml of hydrofluoric acid with a mass percent concentration of 10% under stirring, and continue to stir and react for 2 hours to obtain a mixed solution containing lithium fluoride precipitate;

[0037] 3) The above-mentioned mixed solution was left to stand for 1 hour, and then separated by a centrifuge to obtain a fluoride physical precipitate and a mother liquor of hydrochloric acid, and the mother liquor of hydrochloric acid can be recovered as a raw material for the reaction with lithium carbonate in step 1).

[0038] 4) Wash the fluoride precipitate obtained in step 3) with 75°C deionized water for 5 times, separate it with a centrifuge, put it in a vacuum drying oven, and dr...

Embodiment 3

[0040]1) Weigh 28g of lithium carbonate powder and add it to a 200ml polytetrafluoroethylene beaker, slowly add 90ml of 36% hydrochloric acid under stirring, and stir until lithium carbonate is completely dissolved;

[0041] 2) Heat the solution obtained by the above reaction to 70° C., slowly add 20 ml of hydrofluoric acid with a mass percentage concentration of 99.9% under stirring, and continue stirring for 0.5 hours to obtain a mixed solution containing lithium fluoride precipitate;

[0042] 3) The above-mentioned mixed solution was left to stand for 1 hour, and then separated by a centrifuge to obtain a fluoride physical precipitate and a mother liquor of hydrochloric acid, and the mother liquor of hydrochloric acid can be recovered as a raw material for the reaction with lithium carbonate in step 1).

[0043] 4) Wash the fluoride precipitate obtained in step 3) with 75°C deionized water for 5 times, separate it with a centrifuge, put it in a vacuum drying oven, and dry it...

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Abstract

The invention discloses a method for preparing high-purity lithium fluoride, comprising the following steps of 1) sufficiently mixing lithium carbonate powder and hydrochloric acid for reaction to obtain a lithium chloride solution with the pH value of 6 to 7; 2) adding excessive hydrofluoric acid solutin into the lithium chloride solution obtained in the step 1) for sufficient mixing, and reacting to obtain a mixed solution containing lithium fluoride precipitate; 3) standing the mixed solution obtained in the step 2) and filtering to obtain a lithium fluoride wet solid and hydrochloric acidmother liquor; 4) washing and performing vacuum drying on the lithium fluoride wet solid obtained in the step 3) to obtain the high-purity lithium fluoride solid. According to the method provided by the invention, cheap and available hydrochloric acid is taken as an intermediate raw material for preparing lithium fluoride, lithium chloride with good water solubility is firstly prepared using hydrochloric acid and lithium carbonate, then lithium chloride is reacted with hydrogen fluoride to obtain lithium fluoride and the hydrochloric acid mother liquor, and the hydrochloric acid solution withlithium fluoride separated out is recycled to be reacted with lithium carbonate; the method has the advantages that the raw material cost is low, the process is simple, and the product conversion rateis high.

Description

technical field [0001] The invention relates to the field of inorganic fine chemicals, in particular to a method for preparing high-purity fluorine chemicals. Background technique [0002] Lithium fluoride is an important inorganic fluoride, which is widely used in enamel, glass, ceramics, communication optical fiber, lithium battery and other fields. Lithium battery stands out from the battery industry due to its high energy density, long service life, and no memory effect, and has become a leader in the battery industry. With the rapid development of the lithium battery industry, the demand for lithium hexafluorophosphate, a commonly used electrolyte for lithium batteries, has increased significantly, and the demand for lithium fluoride as an important raw material for the preparation of lithium hexafluorophosphate has also increased. The synthesis technology of lithium hexafluorophosphate has very strict requirements on the purity of lithium fluoride, so the preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D15/04
CPCC01D15/04C01P2006/80
Inventor 张建刚肖超陈学航王晓雄苏向东
Owner GUIZHOU INST OF TECH
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