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Method for preparing fluorine sulfimide lithium

A technology of lithium fluorosulfonylimide and fluorosulfonimide acid, which is applied in the field of preparing lithium fluorosulfonylimide, can solve the problems of low purity, poor safety, and inconvenient operation of lithium fluorosulfonylimide. Achieve the effects of reducing the content of impurities, preventing excessive temperature rise, and improving operability

Active Publication Date: 2014-03-26
PERIC SPECIAL GASES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] In order to overcome the problems that the fluorosulfonimide lithium prepared by the existing method is not high in purity, the method is inconvenient to operate, and the safety is poor, the object of the present invention is to provide a method for preparing fluorosulfonyl imide lithium, which effectively reduces the The content of impurities in lithium fluorosulfonyl imide improves the operability and safety in the production process, and improves the purity of lithium fluorosulfonyl imide

Method used

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  • Method for preparing fluorine sulfimide lithium
  • Method for preparing fluorine sulfimide lithium
  • Method for preparing fluorine sulfimide lithium

Examples

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Effect test

Embodiment 1

[0054] In a 200L reaction kettle sprayed with polytetrafluoroethylene, put 15kg of lithium carbonate and 60kg of deionized water to form a suspension with a lithium salt mass concentration of 20%. Under stirring, drop deionized water with a mass content of 5 %HN(SO 2 CF 3 ) 2 The reaction solution is obtained from the solution, the reaction temperature is between 50-53°C, the reaction is stopped when the pH value of the reaction solution is 6.0-6.3, and the reaction solution is spray-dried in the spray drying equipment that has been sprayed with polytetrafluoroethylene. The obtained solid powder has a deionized water mass content of 3520ppm, and the solid powder is vacuum-dried at a temperature of 196-200°C and a pressure of 1-6Pa. After 3 hours, 112.6kgLiN(SO 2 CF 3 ) 2 , the yield is 96.8%. Lithium carbonate, high-quality HN(SO 2 CF 3 ) 2 And finally get LiN(SO 2 CF 3 ) 2 The mass content of the components is shown in Table 2.

[0055] Various material components...

Embodiment 2

[0058] In a 200L reaction kettle sprayed with polytetrafluoroethylene, put 15kg of lithium carbonate and 15kg of deionized water to form a suspension with a lithium salt mass concentration of 50%. Under stirring, drop deionized water with a mass content of 20% %HN(SO 2 F) 2 The reaction solution is obtained from the solution, the reaction temperature is between 145-150°C, the reaction is stopped when the pH value of the reaction solution is 7.7-8.0, and the reaction solution is spray-dried in the spray drying equipment that has been sprayed with polytetrafluoroethylene. The mass content of deionized water in the obtained solid powder was 4261ppm. The solid powder was vacuum-dried at a temperature of 100-106°C and a pressure of 493-500Pa. After 15 hours, 73.7kg LiN(SO2F)2 was obtained, with a yield of 97.2%. Lithium carbonate, high-quality HN(SO 2 CF 3 ) 2 And finally get LiN(SO 2 F) 2 The mass content of the components is shown in Table 3.

[0059] Various material comp...

Embodiment 3

[0062] In a 200L reaction kettle sprayed with polytetrafluoroethylene, put 15kg of lithium carbonate and 45kg of deionized water to form a suspension with a lithium salt mass concentration of 25%, and add dropwise deionized water with a mass content of 10% under stirring. %H[N(FSO 2 )(SO 2 C 4 f 9 )] to obtain the reaction solution, the reaction temperature is between 80~84°C, the reaction is stopped when the pH value of the detection reaction solution is 7.7~8.0, and the reaction solution is spray-dried in the spray drying equipment through polytetrafluoroethylene spraying treatment , the obtained solid powder deionized water mass content is 3861ppm, the solid powder is vacuum-dried at a temperature of 120-123 ° C and a pressure of 100-108 Pa, and after 10 hours, 146.9 kg of Li[N(FSO 2 )(SO 2 C 4 f 9 )], the yield is 93.6%. Lithium carbonate, fine H[N(FSO 2 )(SO 2 C 4 f 9 )] and finally Li[N(FSO 2 )(SO 2 C 4 f 9 )] The mass content of the components is shown in...

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Abstract

The invention relates to a method for preparing fluorine sulfimide lithium and belongs to the field of fine chemical industries. The method comprises the steps as follows: lithium salt and deionized water are prepared into a turbid liquid with the mass concentration of the lithium salt in a range of 20-50% in a reaction still, a refined fluorine sulfimide acid solution is added dropwise to obtain a reaction solution under the condition of stirring, the mass content of the deionized water in the fluorine sulfimide acid solution is in a range of 5-20%, the reaction temperature is in a range of 50-150 DEG C, and the reaction is stopped when the pH value of the reaction solution is in a range of 6-8. Non-vacuum drying is performed on the reaction solution firstly, and when the mass content of the deionized water is lower than or equal to 0.5%, vacuum drying is performed. The method is easy to operate, higher in process safety and capable of effectively improving the purity of products and satisfying requirements of lithium battery industries for the high purity.

Description

technical field [0001] The invention relates to a method for preparing lithium fluorosulfonyl imide, which belongs to the field of fine chemical industry. Background technique [0002] Lithium fluorosulfonyl imide is an important fluorine-containing organic ion compound with high withstand voltage and electrical conductivity, and has important industrial application value in many fields. Among them, lithium bis(fluorosulfonyl)imide is a typical representative of lithium fluorosulfonyl imide, which has good thermal stability, high electrochemical stability and electrical conductivity. It is widely used in lithium ion battery organic electrolyte lithium salt, preparation of room temperature ionic liquid, reaction catalyst and antistatic agent, etc. [0003] As a method for producing lithium fluorosulfonyl imide, for example, the following method is known. [0004] U.S. Patent No. 5,874,616 reports that fluoroalkylsulfonyl halides react with fluoroalkylsulfonamides under the ...

Claims

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Application Information

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IPC IPC(8): C07C311/48C07C303/36C01B21/096
Inventor 罗建志蒋玉贵孟祥军吕灵华郭绪涛户帅帅沙婷
Owner PERIC SPECIAL GASES CO LTD
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