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Methods for preparing imidodisulfuryl fluoride and alkali metal salt thereof

A technology of alkali metal salt and fluorosulfonyl, which is applied in the field of preparation of bisimine and its alkali metal salt, can solve the problems of low purity, complicated purification process, and low product yield, and achieve high product purity, simple operation, Good effect of fluoridation

Active Publication Date: 2016-12-14
武汉松石科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] There are also direct use (ClSO 2 ) 2 The reaction of NH with KF, NaF or LiF gives the corresponding (FSO 2 ) 2 NM, such as WO2002053494, CN201280050861, US20040097757, but (ClSO 2 ) 2 NH is easy to decompose, producing a large amount of impurities, the product yield is low, the purity is low, and the purification process is very complicated

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 214g (ClSO 2 ) 2 NH was mixed with 79g ether-4HF, stirred and reacted for 8 small tests at 35°C, and after the reaction was completed, 171g (FSO 2 ) 2 NH. The content is 99%.

[0039] The ratio of 171g to (FSO 2 ) 2 NH and 55gKF were mixed, reacted in a planetary ball mill with a stainless steel liner at 20°C for 3 hours, carried out pressure filtration at 5°C in a glove box, and dried the filter cake under reduced pressure to obtain 184g of pure (FSO 2 ) 2 NK.

[0040] Add 15.5 g of diethyl ether to the filtrate while stirring at 5° C. to obtain a diethyl ether-4HF complex, and analyze the content for later use.

Embodiment 2

[0042] 214g (ClSO 2 ) 2 NH was mixed with 610g isopropyl ether-HF, stirred and reacted for 3 small tests at 70°C, after the reaction was completed, 179g (FSO 2 ) 2 NH. The content is 99%.

[0043] 179g (FSO 2 ) 2 NH and 25.7gLiF were mixed and reacted in a planetary ball mill at 0°C for 8 hours. After the reaction, pressure filtration was carried out at 5°C in a glove box, and the filter cake was dried under reduced pressure to obtain 185g of pure (FSO 2 ) 2 N Li.

[0044]Add 101 g of isopropyl ether to the filtrate while stirring at 5° C. to obtain the isopropyl ether-HF complex, and analyze the content for later use.

Embodiment 3

[0046] 214g (ClSO 2 ) 2 NH was mixed with 300g ethyl butyl ether-3HF, stirred and reacted for 3 small tests at 70°C, after the reaction was completed, 178g (FSO 2 ) 2 NH. The content is 99%.

[0047] 178g (FSO 2 ) 2 NH and 41.3gNaF were mixed and reacted in a planetary ball mill at 0°C for 8 hours. After the reaction, pressure filtration was carried out at 5°C in a glove box, and the filter cake was dried under reduced pressure to obtain 199.5g of pure (FSO 2 ) 2 NNa.

[0048] Add 33 g of isopropyl ether to the filtrate while stirring at 5° C. to obtain ethyl butyl ether-3HF complex, and analyze the content for later use.

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Abstract

The invention belongs to the technical field of fluorochemical industry, and particularly relates to methods for preparing imidodisulfuryl fluoride and alkali metal salt thereof. The method for preparing imidodisulfuryl fluoride comprises the steps of mixing imidodisulfuryl chloride with ether-nHF complex, conducting stirring reaction for 1-20 h at 0-100 DEG C, and conducting reduced pressure distillation after reaction to obtain imidodisulfuryl fluoride. The method for preparing alkali metal salt of imidodisulfuryl fluoride comprises the step of mixing imidodisulfuryl fluoride with MF for reaction under ball milling to obtain a crude product of alkali metal salt of imidodisulfuryl fluoride, wherein reaction temperature is 10-30 DEG C, reaction time is 2-20 h, and M is Li, Ma or K. The technical scheme is safe, efficient and suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of fluorine chemical industry, and in particular relates to a preparation method of bis(fluorosulfonyl)imide and alkali metal salt thereof. Background technique [0002] Bis(fluorosulfonyl)imide [(FSO 2 ) 2 NH] and its alkali metal salts [(FSO 2 ) 2 NM, M=Li, Na, K] are important fluorine-containing compounds, especially lithium bis(fluorosulfonyl)imide [(FSO 2 ) 2 NLi] is a new lithium battery additive, which is different from the traditional lithium battery additive LiPF 6 It has better conductivity and stability compared to LiPF 6 Alternatives have been extensively studied. [0003] Synthesized in the literature ((FSO 2 ) 2 The method of NH is usually to fluorinate bis(chlorosulfonyl)imides with a fluorinating reagent: for example, CN200810197928 uses antimony trifluoride as a fluorinating agent, but antimony trifluoride is highly toxic and has a large impact on the environment; CN200910063820 us...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/086
CPCC01B21/086
Inventor 陈立霞杨磊周烈平张银霞
Owner 武汉松石科技股份有限公司
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