Method for preparing imidodisulfuryl fluoride through micro-channel reactor

Abstract

The invention discloses a method for preparing imidodisulfuryl fluoride through micro-channel reactor. The method comprises the following operation steps: S1, preparation of materials: preparing a certain amount of ammonia gas, an organic solvent, ammonium salt, an organic alkali acid-binding agent, sulfuryl fluoride gas, alkali and acid, and preparing a plunger pump, a gas flowmeter, a micro-mixer, a silicon carbide micro-channel reactor, a rectification device and the like; S2, preparation of a reaction solution: introducing the ammonia gas into the organic solvent or dissolving ammonium salt in the organic solvent, and adding the organic alkali acid-binding agent to prepare a solution; and S3, gas-liquid mixing: adding the solution obtained in the step S2 and sulfuryl fluoride gas into a micro-mixer through the plunger pump and the gas flowmeter respectively. The method for preparing imidodisulfuryl fluoride through the micro-channel reactor is realized through the mature silicon carbide micro-channel reactor, is safe, short in reaction time, stable and reliable in process and simple to operate, does not have the problem of equipment corrosion, and brings better application prospects.

Description

technical field [0001] The invention relates to the field of fine chemical products, in particular to a method for preparing bisfluorosulfonimide in a microchannel reactor. Background technique [0002] Bisfluorosulfonimide (HFSI), chemical formula (FSO2) 2NH, melting point 17°C, boiling point 170°C, is the raw material for preparing lithium bisfluorosulfonimide (LIFSI) electrolyte for lithium secondary batteries. LIFSI is due to its huge anion The structure, as well as the strong electronegativity of sulfonyl and fluoride ions, make its interaction with lithium ions weak, so that lithium ions are highly dissociated in a molten state or dissolved in an organic solvent, and have excellent conductivity. performance, can be used in lithium secondary battery electrolytes, supercapacitors, ionic liquid catalysts, etc., have very important industrial and commercial application prospects and value, with the country's increasingly higher requirements and regulatory measures on chemi...

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Problems solved by technology

[0003] There are certain disadvantages in the existing method for preparing bisfluorosulfonimide in use, as reported in patents CN102046523, CN 106044728, CN 111483986, CN 110217763, CN 112320772 and CN 110155967, it is based on sulfamic acid (chlorosulfonic acid isocyanate), chlorosulfonic acid and chlorinated reagents as starting materials, first synthesize dichlorosulfonimide under the action of catalyst, and then perform fluorine and chlorine exchange under the action of catalyst to obtain bisfluorosulfonimide. Although the raw materials used in the method are very cheap and easy to obtain, there are still many problems such as long process route, low yield, large discharge of three wastes, high production safety risk, and serious equipment corrosion. It is not suitable as a green and safe production route. Patents CN104495767 and CN 111099566 use sulfuryl chloride and ammonia gas or inorganic ammonium salt as starting materials to synthesize dichlorosulfonimide first, and then perform fluorine and chlorine exchange under the action of a catalyst to obtain bisfluorosulfonimide. The existing problems are similar to those above. In addition, sulfuryl chloride has high activity, and the reaction is difficult to control without oligomerization, which is not conducive to people's use. In addition, in the prior art route for preparing bisfluorosulfonimide, it is mainly divided into Taking traditional sulfamic acid (chlorosulfonic acid isocyanate), chlorosulfonic acid as the technical route of starting raw material, sulfuryl chloride and ammonia gas or inorganic ammonium salt as the technical route of starting raw material, raw material is cheap, but yield is low, The three wastes are high, the equipment is corroded seriously, and the risk factor of safety production is high, which has brought certain adverse effects on people's use process. Therefore, we propose a method for preparing bisfluorosulfonimide in a microchannel reactor.

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