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Continuous preparation method of bis(fluorosulfonyl)imide

A technology of bisfluorosulfonimide and chlorosulfonic acid, which is applied in the direction of sulfamic acid, nitrogen and non-metallic compounds, etc., can solve the problems of unsuitable industrial production, difficulty in obtaining raw materials, difficulty in obtaining raw materials, etc., and achieve equipment loss Small size, high product yield, avoiding the effect of non-corrosion resistance

Active Publication Date: 2021-06-18
ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Patent CN106829891A discloses a method for preparing bisfluorosulfonimide by direct reaction of fluorosulfonyl isocyanate and fluorosulfonic acid, but this method is difficult to obtain raw materials and is not suitable for industrial production
[0009] In summary, the preparation methods of bisfluorosulfonimide disclosed in the prior art are all traditional step-by-step and batch-type preparation methods, which have long reaction time, low product yield, difficulty in obtaining raw materials, and introduction of catalysts. Impurities and equipment corrosion are serious, not suitable for industrial production and other issues

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  • Continuous preparation method of bis(fluorosulfonyl)imide
  • Continuous preparation method of bis(fluorosulfonyl)imide

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Experimental program
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Effect test

Embodiment 1

[0034] In this embodiment, the attached figure 2 Corning Microchannel Reaction Modules (Corning Straight Channel Module and Corning Cardioid Channel Module) as shown, and follow the attached figure 1 Determine the connection mode of the microchannel reactor, the number of reaction modules is determined according to the flow rate and reaction residence time, and the heat transfer medium is heat transfer oil.

[0035] Set the temperature of the heat exchanger to 100°C (ie, the reaction temperature), and the reaction pressure to 0.3MPa. Set the mass flow rate F chlorosulfonic acid=38.7g / min of each metering pump, F chlorosulfonic acid isocyanate=47.0g / min, the reaction raw material chlorosulfonic acid and chlorosulfonic acid isocyanate pass through the microchannel respectively After the module is preheated, it enters the heart-shaped microchannel reaction module. Hydrogen fluoride passes through the gas mass flow meter F hydrogen fluoride = 14.6g / min, and directly enters the h...

Embodiment 2

[0037] This embodiment adopts the same Corning microchannel reactor as Embodiment 1, and according to the same connection mode and control method.

[0038] Set the heat exchanger temperature to 150°C (ie the reaction temperature), and the reaction pressure to 0.4MPa. Set the mass flow rate F chlorosulfonic acid=65.8g / min of each metering pump, F chlorosulfonic acid isocyanate=80.0g / min, the reaction raw material chlorosulfonic acid and chlorosulfonic acid isocyanate pass through the microchannel respectively After the module is preheated, it enters the heart-shaped microchannel reaction module. Hydrogen fluoride passes through the gas mass flow meter F hydrogen fluoride = 22.6g / min, and directly enters the heart-shaped microchannel reaction module for fluorination reaction. Hydrogen fluoride, chlorosulfonic acid, and chlorosulfonic acid isonitrile The molar ratio of the acid ester is 2.0:1:1, and the reaction residence time is 13s. The reaction product was separated by a gas-...

Embodiment 3

[0040] This embodiment adopts the same Corning microchannel reactor as Embodiment 1, and according to the same connection mode and control method.

[0041] Set the heat exchanger temperature to 30°C (ie the reaction temperature), and the reaction pressure to 0.1MPa. Set the mass flow rate F chlorosulfonic acid=8.2g / min of each metering pump, F chlorosulfonic acid isocyanate=10.0g / min, the reaction raw material chlorosulfonic acid and chlorosulfonic acid isocyanate pass through the microchannel respectively After the module is preheated, it enters the heart-shaped microchannel reaction module. Hydrogen fluoride passes through the gas mass flow meter F hydrogen fluoride = 3.5g / min, and directly enters the heart-shaped microchannel reaction module for fluorination reaction. Hydrogen fluoride, chlorosulfonic acid, and chlorosulfonic acid isonitrile The molar ratio of the acid ester is 2.5:1:1, and the reaction residence time is 100s. The reaction product was separated by a gas-li...

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Abstract

The invention discloses a continuous preparation method of bis(fluorosulfonyl)imide. The continuous preparation of bis(fluorosulfonyl)imide is carried out in a microchannel reactor, and comprises the following steps: A1, preheating a first raw material chlorosulfonic acid and a second raw material chlorosulfonyl isocyanate in a preheating module at the preheating temperature of 30-150 DEG C; A2, feeding a third raw material hydrogen fluoride, the preheated first raw material chlorosulfonic acid and the preheated second raw material chlorosulfonyl isocyanate into a reaction module for mixed reaction, wherein the molar ratio of the hydrogen fluoride to the chlorosulfonic acid to the chlorosulfonyl isocyanate is (2-2.5):1:1, the flow rate of the chlorosulfonic acid is 1-100g / min, the flow rate of the chlorosulfonyl isocyanate is 1-100g / min, the reaction temperature is 30-150 DEG C, the reaction pressure is 0-0.5 MPa, and the retention time is 1-100s; and A3, carrying out gas-liquid separation on the product at the outlet of the reaction module to obtain bis(fluorosulfonyl)imide. The method has the advantages of simple process, low equipment loss, high yield and the like.

Description

technical field [0001] The invention relates to the preparation of bisfluorosulfonimide, in particular to a method for preparing bisfluorosulfonimide in continuous flow in a microchannel reactor. Background technique [0002] Bisfluorosulfonimide is the main raw material for preparing lithium bisfluorosulfonimide, with a boiling point of 170°C and a melting point of 17°C. Lithium bisfluorosulfonyl imide is a new type of lithium salt, which has many advantages such as high electrical conductivity, high thermal stability, hydrolysis resistance, and inhibition of battery inflation. It can specifically solve the common problems of current lithium-ion batteries in terms of performance. Common technical problems in the industry such as short cycle life (especially at high temperature) and potential safety hazards have good application prospects and market demand. [0003] Patent CN106430129A discloses a method for preparing dichlorosulfonimide by using sulfamic acid, thionyl chlo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/096
CPCC01B21/096
Inventor 项文勤陈明炎张勇耀赵卫娟张国立万宝峰
Owner ZHEJIANG LANTIAN ENVIRONMENTAL PROTECTION HI TECH
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