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A kind of production method of battery grade lithium fluoride

A production method, lithium fluoride technology, applied in the direction of lithium halide, etc., can solve the problems of long production process, high equipment cost, high production cost, etc., achieve good economic value and social value, short production process, and raw material utilization rate high effect

Active Publication Date: 2012-02-08
DO FLUORIDE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of the direct method is that the quality of the raw material lithium carbonate is too high, and the production cost is also high
Ion exchange method and extraction method have a long production process and frequent process changes, so it is easy to introduce impurities in the production process, and there is a problem of high equipment cost
Moreover, the current production method also produces waste acid and waste gas by-products, pollutes the environment, and has poor environmental protection benefits.

Method used

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  • A kind of production method of battery grade lithium fluoride
  • A kind of production method of battery grade lithium fluoride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Take industrial grade lithium carbonate as raw material, specifically comprising the following steps:

[0016] (1) 50g technical grade lithium carbonate is dissolved in 450g water, is mixed with the lithium carbonate slurry that contains lithium carbonate weight percent concentration and is 10%, passes into CO in the slurry 2 Gas, the inflow rate is 15m 3 / h, the control temperature is 30°C, the carbonization reaction is 4 hours, and then filtered. The filter cake is uncarbonated lithium carbonate and trace impurities, which are used to produce industrial-grade lithium fluoride. The filtrate is lithium bicarbonate solution, and the weight percentage concentration is 2%, reserve;

[0017] (2) The filtrate obtained in step (1) is mixed with 100% hydrofluoric acid in a volume ratio of 35:1 for reaction, and the controlled temperature is 70° C. for 4 hours to generate lithium fluoride slurry, which is filtered. The filtrate is returned to step (1) for the preparation of l...

Embodiment 2

[0019] Take industrial grade lithium carbonate as raw material, specifically comprising the following steps:

[0020] (1) 50g industrial grade lithium carbonate is dissolved in 200g water, is mixed with the lithium carbonate slurry that contains lithium carbonate weight percentage concentration and is 20%, passes into CO in the slurry 2 Gas, the inflow rate is 10m 3 / h, the control temperature is 40°C, the carbonization reaction is carried out for 5 hours, and then filtered. The filter cake is uncarbonated lithium carbonate and trace impurities, which are used to produce industrial-grade lithium fluoride. The filtrate is lithium bicarbonate solution, and the weight percentage concentration is 5%, reserve;

[0021] (2) The filtrate obtained in step (1) is mixed with hydrofluoric acid with a weight percent concentration of 55% in a volume ratio of 22: 1, reacted, and the controlled temperature is 80° C., and reacted for 3 hours to generate lithium fluoride slurry, filter, The ...

Embodiment 3

[0023] Take industrial grade lithium carbonate as raw material, specifically comprising the following steps:

[0024] (1) 50g technical grade lithium carbonate is dissolved in 120g water, is mixed with the lithium carbonate slurry that contains lithium carbonate weight percentage concentration and is 30%, passes into CO in the slurry 2 Gas, the inflow rate is 5m 3 / h, the control temperature is 40°C, the carbonization reaction is 4 hours, and then filtered. The filter cake is uncarbonated lithium carbonate and trace impurities, which are used to produce industrial-grade lithium fluoride. The filtrate is lithium bicarbonate solution, and the weight percentage concentration is 6%, reserve;

[0025] (2) The filtrate obtained in step (1) is mixed with 20% hydrofluoric acid in a volume ratio of 10:1 for reaction, and the controlled temperature is 80° C. for 3 hours to generate lithium fluoride slurry, filter, The filtrate is returned to step (1) for the preparation of lithium car...

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Abstract

The invention discloses a production method of battery-grade lithium fluoride. The specific steps are as follows: (1) dissolving industrial-grade lithium carbonate in water to prepare lithium carbonate slurry containing lithium carbonate with a concentration of 10% to 30% by weight , put CO2 gas into the slurry, control the temperature at 30°C-40°C, carbonize for 4-5 hours, and then filter, the filter cake is uncarbonated lithium carbonate and trace impurities, used to produce industrial-grade lithium fluoride , the filtrate is for subsequent use; (2) the filtrate obtained in step (1) is mixed with hydrofluoric acid in a volume ratio of 10 to 35: 1, reacted for 3 to 4 hours, and the controlled temperature is 70°C to 80°C to generate lithium fluoride slurry, Filtration, the filtrate is returned to step (1) for preparing lithium carbonate slurry, the filter cake is lithium fluoride ointment, and dried to obtain the product lithium fluoride. The invention has easy-to-obtain raw materials, short production process, simple equipment and easy operation; the whole process is a circulation system, the utilization rate of raw materials is high, and the environmental pollution is small.

Description

technical field [0001] The invention belongs to the field of inorganic fine chemicals, and in particular relates to a production method of battery-grade lithium fluoride. Background technique [0002] Battery-grade lithium fluoride is one of the necessary raw materials for the production of lithium hexafluorophosphate, a commonly used electrolyte for lithium-ion batteries. At present, the production methods of battery-grade lithium fluoride mainly include direct method, ion exchange method, and extraction method. The direct method is a common method for the early production of high-purity or battery-grade lithium fluoride. This method reacts high-purity lithium carbonate with hydrofluoric acid solution to produce high-purity or battery-grade lithium fluoride. The ion exchange method and the extraction method are methods to purify the raw material lithium compound first, and then use it to produce high-purity or battery-grade lithium fluoride. The disadvantage of the direct ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D15/04
Inventor 李云峰罗成果刘海霞李凌云李洁薛峰峰孙永明张梅
Owner DO FLUORIDE CHEM CO LTD