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Preparation method for co-producing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide

A technology for lithium bisfluorosulfonimide and bischlorosulfonimide acid is applied in the field of co-production of bischlorosulfonimide acid and lithium bisfluorosulfonimide, and can solve the problem of high product cost, fluorine Sulfonate isocyanates have problems such as high price and difficult industrial production, which can achieve the effects of easy operation, reduced consumption of raw and auxiliary materials, and fewer by-products.

Inactive Publication Date: 2020-05-05
合肥利夫生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the high price of raw material fluorosulfonic acid isocyanate, which leads to high product cost and is difficult to industrialized production

Method used

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  • Preparation method for co-producing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide
  • Preparation method for co-producing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide
  • Preparation method for co-producing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide

Examples

Experimental program
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Embodiment 1

[0050] A preparation method for co-producing bischlorosulfonylimide acid and lithium bisfluorosulfonylimide, comprising the steps of:

[0051] S1. Add 0.25L of anhydrous acetonitrile into the PTFE-lined stainless steel reaction kettle, then add 135g of sulfuryl chloride, and slowly add 73.2g of octamethylcyclotetrasilazane with a pneumatic diaphragm pump while stirring. Stir the reaction at ℃ for 2 hours, and recover the remaining sulfuryl chloride and the by-product octamethylchlorosilane respectively by distillation under pressure. After recovery, acetonitrile is recovered by distillation under reduced pressure to obtain 53 g of dichlorosulfonylimide acid;

[0052] S2. Add 53.5g of bischlorosulfimidic acid and 0.042g of antimony pentachloride into the PTFE-lined stainless steel reaction kettle, raise the temperature to 90°C, slowly introduce 10g of anhydrous hydrofluoric acid gas under stirring, and cool down after 20 hours of reaction to room temperature, blowing nitrogen f...

Embodiment 2

[0055] A preparation method for co-producing bischlorosulfonylimide acid and lithium bisfluorosulfonylimide, comprising the steps of:

[0056] S1. Add 0.2L of N,N-dimethylformamide to the PFA-lined stainless steel reaction kettle, then add 135g of sulfuryl chloride, slowly add 146.4g of octamethylcyclotetrasilazane with a pneumatic diaphragm pump while stirring, drop After the addition was completed, the reaction was stirred at 30°C for 12 hours, and the remaining sulfuryl chloride and the by-product octamethylchlorosilane were respectively recovered by pressure distillation. After recovery, acetonitrile was recovered by vacuum distillation to obtain 104.6 g of dichlorosulfonylimide acid ;

[0057] S2. Add 107g of bischlorosulfimidic acid and 0.084g of antimony pentachloride to the PTFE-lined stainless steel reaction kettle, heat up to 110°C, slowly introduce 20g of anhydrous hydrofluoric acid gas under stirring, and cool down to At room temperature, blow nitrogen for 15 hour...

Embodiment 3

[0060] A preparation method for co-producing bischlorosulfonylimide acid and lithium bisfluorosulfonylimide, comprising the steps of:

[0061] S1. In the PTFE-lined stainless steel reaction kettle, add 0.1L ethyl acetate, then add 135g of sulfuryl chloride, and slowly add 117.1g of octamethylcyclotetrasilazane dropwise with a pneumatic diaphragm pump while stirring. Stir and react at ℃ for 8 hours, and recover the remaining sulfuryl chloride and the by-product octamethylchlorosilane respectively by distillation under pressure. After recovery, acetonitrile is recovered by distillation under reduced pressure to obtain 84.7 g of dichlorosulfonylimide acid;

[0062] S2. Add 85.6g of bischlorosulfimidic acid and 0.067g of antimony pentachloride into the PTFE-lined stainless steel reaction kettle, raise the temperature to 95°C, slowly introduce 16.8g of anhydrous hydrofluoric acid gas under stirring, and react for 18 hours Cool down to room temperature, blow nitrogen for 15 hours to...

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Abstract

The invention discloses a preparation method for coproducing bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide, which comprises the following steps: S1, adding sulfuryl chloride into a first solvent, dropwisely adding octamethylcyclotetrasilazane for reaction, and carrying out purification to obtain bis(chlorosulfonyl)imide; S2, taking bis(chlorosulfonyl)imide and anhydrous hydrofluoric acid to react under the action of a catalyst to obtain bis(fluorosulfonyl)amide; and S3, taking the bis(fluorosulfonyl)amide and lithium fluoride to react in a second solvent, and carrying out purification to obtain the lithium bis(fluorosulfonyl)imide. According to the invention, proper raw materials are selected and matched with a solvent method to co-produce bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide. The method has the advantages of simple preparation process, few and recyclable byproducts, high yield, no water participation in the production process, high purity of the obtained bis(chlorosulfonyl)imide and lithium bis(fluorosulfonyl)imide, no wastewater generation and green and environment-friendly process route, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the technical field of new energy materials, in particular to a preparation method for co-producing bischlorosulfonylimide acid and lithium bisfluorosulfonylimide. Background technique [0002] As a portable high specific energy chemical power source, lithium ion battery has been widely used in portable instruments, notebook computers, military fields, mobile communications, cameras and other fields. It is currently the preferred supporting power source for power vehicles and can also be widely used in energy storage batteries. It has been extensively researched and applied all over the world. Lithium-ion batteries are mainly composed of positive electrodes, negative electrodes, diaphragms, electrolytes, battery systems, etc., and electrolytes are mainly composed of electrolytes and organic solvents, which are the active components that connect the positive and negative electrodes and are important factors related to battery pe...

Claims

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Application Information

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IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/086C01B21/096C01P2006/80C01P2006/82
Inventor 刘涛曹文兵徐海
Owner 合肥利夫生物科技有限公司
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