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Production method of high-purity lithium sulfide

A technology of lithium sulfide and lithium hydrogen sulfide, applied in the direction of alkali metal sulfide/polysulfide, etc., can solve the problems of low sulfur utilization rate and high risk

Inactive Publication Date: 2014-02-05
四川宝利丰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since hydrogen sulfide gas is used as a sulfur source in this method, the operation is dangerous and the utilization rate of sulfur is not high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of typical general operation process of production method of the present invention:

[0020] 1': Fully stir and dissolve 42.4~44.5 parts of lithium chloride in 300~500 parts of N-methylpyrrolidone (NMP), then add 56 parts of sodium hydrosulfide (or 72 parts of potassium hydrosulfide) and fully stir to suspend (The molar ratio of sodium hydrosulfide to lithium chloride is 0.95-1:1, and the molar ratio of NMP to sodium hydrosulfide is 3~5:1), in N 2 Heating to 70~110°C under the condition of atmosphere protection, reacting for 2~4 hours, filtering and removing sodium chloride, and preparing N-methylpyrrolidone solution of lithium hydrosulfide.

[0021] 2': The sodium chloride filtered out in the above 1' is washed with 30~50 parts of N-methylpyrrolidone at 30~45°C for 2~3 times, and the washing liquid is merged into the lithium sulfide filtrate in the above 1', and the filter cake is Then wash with 20-30 parts of ethanol for 1-2 times, filter and dry to obtain whi...

Embodiment 2

[0026] 445g of lithium chloride was fully stirred and dissolved in 5000g of N-methylpyrrolidone, then 560g of sodium hydrosulfide was added to fully stir and suspend. 2 Under atmospheric conditions, slowly heat to 95° C., react for 2 hours, and filter to obtain a solution of lithium hydrosulfide in N-methylpyrrolidone. The filter cake sodium chloride was washed twice with 300g of 45°C N-methylpyrrolidone, the two washes were incorporated into the N-methylpyrrolidone solution of lithium hydrogen sulfide, the filter cake was washed three times with 200g of ethanol, filtered and dried. 575 g of high-purity white sodium chloride crystals were obtained. Filtrate reclaims ethanol, obtains 546g, and ethanol recovery rate is 91%. in N 2 Under atmospheric conditions, heat the N-methylpyrrolidone solution of lithium hydrosulfide obtained above to 190° C., react until no hydrogen sulfide gas escapes in the system, and obtain a N-methylpyrrolidone suspension of lithium sulfide. The hyd...

Embodiment 3

[0028] 430g of lithium chloride was fully stirred and dissolved in 4000g of N-methylpyrrolidone, then 560g of sodium hydrosulfide was added to fully stir and suspend. 2 Under atmospheric conditions, slowly heat to 90° C., react for 3 hours, and filter to obtain a solution of lithium hydrosulfide in N-methylpyrrolidone. The filter cake sodium chloride was washed 3 times with 400g of 40°C hot N-methylpyrrolidone, and the three washes were incorporated into the N-methylpyrrolidone solution of lithium sulfide, and the filter cake was washed 2 times with 300g ethanol, filtered, and dried. 572 g of high-purity white sodium chloride crystals were obtained. Filtrate reclaims ethanol, obtains 540g, and ethanol recovery rate is 90%. in N 2 Under atmospheric conditions, heat the N-methylpyrrolidone solution of lithium hydrosulfide obtained above to 170° C., react until no hydrogen sulfide gas escapes in the system, and obtain a suspension of lithium sulfide in N-methylpyrrolidone. The...

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PUM

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Abstract

A production method of high-purity lithium sulfide is disclosed. The production method comprises the following steps: using hydrogen sulfide and lithium chloride used as raw materials to carry out a hydrosulfide reaction in N-methyl 2 pyrrolidone and under inert gas protection so as to obtain lithium hydrogen sulfide; filtering a precipitate, heating a N-methyl 2 pyrrolidone solution of lithium hydrogen sulfide under inert gas protection for decomposition and conversion so as to obtain a lithium sulfide precipitate, and separating, wherein mol ratio of the raw material hydrogen sulfide to the raw material lithium chloride is 0.95-1:1. According to the method, a high-risk hydrogen sulfide gas is not used such that the production process is safer and more convenient; lithium sulfide obtained is a white crystal; and the yield is greater than 98%, and the content of lithium sulfide is greater than 99%, wherein the content of lithium sulfite is less than 0.1% and the content of lithium sulfate is less than 0.5%.

Description

technical field [0001] The invention relates to a production method of high-purity lithium sulfide. Background technique [0002] High-purity lithium sulfide is a commonly used potential electrolyte material in lithium-ion batteries. In recent years, high-purity lithium sulfide has also been used in the preparation of new polymer functional materials such as polyarylene sulfide. The application of high-purity lithium sulfide can not only increase the molecular weight of such polymer functional materials, but also reduce the molecular weight distribution. At the same time, it can also reduce the ash content of the polymer, so that the application of the polymer can be improved to a higher level. [0003] Due to the relatively active chemical properties of lithium sulfide, it is very easy to decompose or oxidize, so it is not easy to produce high-purity lithium sulfide, which makes it expensive. At present, there are mainly methods for producing high-purity lithium sulfide: ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/22
Inventor 李晶晶杨琴罗芩李朝祥
Owner 四川宝利丰科技有限公司
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