Production process of bis (chlorosulfonyl) imide

A bischlorosulfonimide and production technology technology, applied in the field of bischlorosulfonimide production technology, can solve the problem of lowering the profit margin of the bischlorosulfonimide market, difficulty in large-scale use, and large production of three wastes, etc. problem, to achieve the effect of optimizing the reaction process parameters, improving the utilization rate and shortening the reaction cycle

Active Publication Date: 2021-12-17
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It uses chlorosulfonic acid and chlorosulfonyl isocyanate as raw materials. Under the action of a catalyst, it reacts at a high temperature of 120-140°C and distills to obtain dichlorosulfonimide. The reaction equation is as follows. The advantage of this process is that there is no side effect of sulfur dioxide and hydrogen chloride. Gas production, high atomic utilization rate, but its problem is also prominent, chlorosulfonyl isocyanate raw material is prepared from cyanogen chloride and sulfur trioxide, cyanogen chloride is not only extremely toxic, but also very expensive, resulting in the production of chlorosul

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  • Production process of bis (chlorosulfonyl) imide
  • Production process of bis (chlorosulfonyl) imide

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 97.1g (1mol) of sulfamic acid and 273.7g (2.3mol) of thionyl chloride to the reaction kettle, start stirring, turn on the condenser reflux device, control the temperature at 55°C, set the back pressure valve pressure to 0.4MPa, and wait for the solid After all dissolved, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 3 hours. After adding sulfur trioxide, raise the temperature to 110°C to continue the reaction for 7.5 hours, return to normal pressure, open the condensate outlet valve of the condenser, Continue the reaction for 2 hours until no condensate flows out of the condenser, start vacuum distillation, collect fractions at 90-105°C, and obtain 212.4 g of the product of the present invention, dichlorosulfonimide liquid, with a reaction yield of 99.1% and a product purity of 99.9 %.

Embodiment 2

[0029] Add 97.1g (1mol) of sulfamic acid and 238g (2.0mol) of thionyl chloride into the reactor, start stirring, turn on the reflux device of the condenser, control the temperature at 40°C, set the pressure of the back pressure valve to 0.1MPa, and wait until the solids are completely After dissolving, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 1 hour. After adding sulfur trioxide, raise the temperature to 90°C and continue the reaction for 5 hours, return to normal pressure, open the condensate outlet valve of the condenser, and continue the reaction After 1 hour, until no condensate flowed out from the condenser, vacuum distillation was started, and fractions at 90-105°C were collected to obtain 205.5 g of the liquid dichlorosulfonimide product of the present invention, with a reaction yield of 96.0% and a product purity of 99.8%.

Embodiment 3

[0031] Add 97.1g (1mol) of sulfamic acid and 297.5g (2.5mol) of thionyl chloride into the reaction kettle, start stirring, turn on the reflux device of the condenser, control the temperature at 70°C, set the pressure of the back pressure valve to 0.7MPa, and wait for the solid After all dissolved, add 80g (1mol) sulfur trioxide into the reaction kettle at a constant speed within 6 hours. After adding sulfur trioxide, raise the temperature to 120°C to continue the reaction for 10 hours, return to normal pressure, open the condensate outlet valve of the condenser, and continue React for 3 hours, until no condensate flows out from the condenser, start vacuum rectification, collect fractions at 90-105°C, and obtain 211.0 g of dichlorosulfonimide liquid of the present invention, with a reaction yield of 98.5% and a product purity of 99.9% .

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Abstract

The invention relates to the technical field of production of bis (chlorosulfonyl) imide, in particular to a production process of bis (chlorosulfonyl) imide. The production process of the bis (chlorosulfonyl) imide comprises the steps of adding sulfamic acid and thionyl chloride into a reaction kettle until solids are completely dissolved, then adding sulfur trioxide into the reaction kettle at a constant speed, after the sulfur trioxide is completely added, heating to the temperature of 90-120 DEG C, continuing to react for 5-10 hours, restoring to normal pressure, opening a condensate outlet valve of a condenser, continuing to react for 1-3 hours, carrying out reduced pressure rectification until no condensate flows out of the condenser, and obtaining the target product bis (chlorosulfonyl) imide. Compared with an original chlorosulfonic acid method process, the production process has the advantages that the hydrogen chloride waste gas amount is reduced by 1/3, the sulfur dioxide tail gas can be recycled and reused in a thionyl chloride production device, the yield of three wastes is further reduced, and the production process belongs to an innovative process meeting the development requirements of the green chemical industry.

Description

technical field [0001] The invention relates to the technical field of bischlorosulfonimide production, in particular to a production process of bischlorosulfonimide. Background technique [0002] As the market demand for bisfluorosulfonimide, a new type of electrolyte for lithium batteries, continues to increase in recent years, the production process of its raw material bischlorosulfonimide is becoming more and more important. Further production of bisfluorosulfonimide is currently the most valuable production method. [0003] The mainstream production process of dichlorosulfonimide includes two types: one is to synthesize dichlorosulfonimide with sulfamic acid, thionyl chloride and chlorosulfonic acid as raw materials, and the reaction process is as follows: [0004] [0005] For example, patent CN101747242B discloses a preparation method of bisfluorosulfonimide, including the synthesis process of bischlorosulfonimide, which uses sulfamic acid, thionyl chloride, and c...

Claims

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Application Information

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IPC IPC(8): C01B21/096C01B21/086
CPCC01B21/096C01B21/086Y02E60/10
Inventor 张泰铭李光辉孙庆民王军孙丰春孙健杨建玲薛居强王永
Owner SHANDONG KAISHENG NEW MATERIALS
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