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CN-121990530-A - Dichloro sulfonyl imide and preparation method and reaction device thereof

CN121990530ACN 121990530 ACN121990530 ACN 121990530ACN-121990530-A

Abstract

The invention provides a dichlor sulfimide, a preparation method and a reaction device thereof, wherein the preparation method comprises the following steps of 1) preparing mixed slurry containing sulfamic acid and chlorosulfonic acid, wherein the particle size of the sulfamic acid is not more than 200 microns, then pumping the mixed slurry into a continuous microchannel reactor by using a metering pump to carry out amination reaction to obtain an intermediate, 2) carrying out chlorination reaction on the mixed system comprising the intermediate and thionyl chloride in a tubular reactor to obtain a reaction product, and 3) separating the reaction product to obtain the dichlor sulfimide. The preparation method provided by the invention can prepare the dichlorosulfimide with high purity, and has simple process and easy operation.

Inventors

  • JIANG XIONG
  • DENG JIANJUN
  • Liu du

Assignees

  • 广州天赐高新材料股份有限公司

Dates

Publication Date
20260508
Application Date
20241106

Claims (10)

  1. 1. The preparation method of the dichloro sulfonyl imide is characterized by comprising the following steps of: 1) Preparing mixed slurry containing sulfamic acid and chlorosulfonic acid, wherein the particle size of the sulfamic acid is not more than 200 micrometers, and then pumping the mixed slurry into a continuous microchannel reactor to carry out amination reaction to obtain an intermediate; Wherein the back pressure at the tail part of the continuous micro-channel reactor is 0-3MPa; 2) The mixed system comprising the intermediate and thionyl chloride is subjected to chlorination reaction in a tubular reactor to obtain a reaction product; wherein the Reynolds number of the mixed system is not lower than 5000, and the back pressure at the tail part of the tubular reactor is 0-2MPa; 3) And separating the reaction product to obtain the dichloro sulfonyl imide.
  2. 2. The method for producing a bischlorosulfonimide according to claim 1, wherein the molar ratio of sulfamic acid to chlorosulfonic acid in said mixed slurry is 1:1.01-2; And/or the molar ratio of the intermediate to the thionyl chloride is 1:2-2.5.
  3. 3. The method for producing a bischlorosulfonimide according to claim 1 or 2, wherein step 1) comprises controlling the reaction temperature of the amination reaction by using a heat transfer medium, wherein the temperature difference between the heat transfer medium after heat exchange and the heat transfer medium before heat exchange is 0 to 2 ℃.
  4. 4. A method for producing a bischlorosulfonimide according to any of claims 1 to 3, wherein said amination reaction is carried out at a reaction temperature of 50 to 90 ℃ for a reaction time of 2 to 4 minutes; And/or the reaction temperature of the chlorination reaction is 80-150 ℃ and the reaction time is 2-4min.
  5. 5. The method for producing a bischlorosulfonimide according to any of claims 1 to 4, wherein said separation treatment comprises the steps of: And (3) distilling the reaction product at the temperature of-0.1-1.5 MPa and the temperature of 30-60 ℃ to obtain the dichloro sulfonyl imide.
  6. 6. A dichloro-sulphonyl-imide is characterized in that, the bischlorosulfonimide is produced by the process for producing a bischlorosulfonimide according to any of claims 1 to 5; Wherein the dichlorsulfoimide comprises, by mass, 85-95% of dichlorsulfoimide compound, 1-5% of sulfur dioxide, 1-5% of hydrogen chloride, 1-5% of water, less than or equal to 4% of bis (sulfamoyl) sulfonamide, 0.1-1% of sulfamic acid and 1-10% of chlorosulfonyl sulfonamide.
  7. 7. The reaction device is characterized by comprising a mixing pump, a stirring kettle, a continuous micro-channel reactor, a tubular reactor and a flash evaporator which are sequentially communicated through pipelines.
  8. 8. The reaction apparatus according to claim 7, further comprising a diaphragm metering pump for delivering a mixed slurry containing sulfamic acid and chlorosulfonic acid to a continuous microchannel reactor, the diaphragm metering pump being disposed between the agitation tank and the continuous microchannel reactor, an inlet of the diaphragm metering pump being in communication with an outlet of the agitation tank, an outlet of the diaphragm metering pump being in communication with an inlet of the continuous microchannel reactor, and a mass flow meter disposed between the diaphragm metering pump outlet and the inlet of the continuous microchannel reactor.
  9. 9. The reaction apparatus of claim 7 or 8, wherein a first housing is sleeved outside the continuous microchannel reactor, wherein a cavity for accommodating a heat transfer medium is formed between the continuous microchannel reactor and the first housing.
  10. 10. The reactor according to any one of claims 7 to 9, wherein a second shell is sleeved outside the tubular reactor, wherein a cavity for accommodating a heat transfer medium is formed between the tubular reactor and the second shell.

Description

Dichloro sulfonyl imide and preparation method and reaction device thereof Technical Field The invention relates to a dichloro sulfonyl imide, belongs to the technical field of chemical material preparation, and particularly relates to a dichloro sulfonyl imide, a preparation method and a reaction device thereof. Background With the rapid development of new energy industries, particularly the lithium battery market, as one of common electrolyte lithium salts, the demand of lithium bis (fluorosulfonyl imide) is increasing. The common preparation method of the lithium bis (fluorosulfonyl) imide at present is that bis (fluorosulfonyl) imide is generated by reacting bis (chlorosulfonyl) imide with a fluorine-containing substance, and then the bis (fluorosulfonyl) imide is reacted with lithium fluoride to prepare the lithium bis (fluorosulfonyl) imide. However, in the industrial production of the bischlorosulfimide, the intermittent reaction route of sulfamic acid, chlorosulfonic acid and thionyl chloride is widely researched and applied, but the bischlorosulfimide prepared by the process has insufficient purity, and the higher content of acidic substances such as sulfur dioxide, hydrogen chloride and the like can cause higher impurity content in the subsequent bisfluorosulfonimide and lithium bisfluorosulfonimide, so that side reactions such as oxidative decomposition electrolyte and the like of the acidic substances occur in the battery application, thereby degrading the electrochemical performance of the battery. Accordingly, a person skilled in the art is required to develop a bischlorosulfonimide having a high purity. Disclosure of Invention The invention provides a preparation method of dichloro sulfonyl imide, which can prepare the dichloro sulfonyl imide with high purity, and has simple process, easy operation and high production efficiency. The invention also provides the dichloro sulfonyl imide which has high purity, and the contents of impurities such as sulfur dioxide, hydrogen chloride and the like are low, so that the dichloro sulfonyl imide is favorable for the wide application of subsequent products. The invention also provides a reaction device which can provide excellent conditions for the preparation of the dichloro-sulfonyl-imide and is favorable for realizing the high-purity dichloro-sulfonyl-imide. In a first aspect, the present invention provides a method for preparing a bischlorosulfonimide, comprising the steps of: 1) Preparing mixed slurry containing sulfamic acid and chlorosulfonic acid, wherein the particle size of the sulfamic acid is not more than 200 micrometers, and then pumping the mixed slurry into a continuous microchannel reactor to carry out amination reaction to obtain an intermediate; Wherein the back pressure at the tail part of the continuous micro-channel reactor is 0-3MPa; 2) The mixed system comprising the intermediate and thionyl chloride is subjected to chlorination reaction in a tubular reactor to obtain a reaction product; wherein the Reynolds number of the mixed system is not lower than 5000, and the back pressure at the tail part of the tubular reactor is 0-2MPa; 3) And separating the reaction product to obtain the dichloro sulfonyl imide. The preparation method of the dichlorsulfoimide comprises the step of mixing the mixed slurry with sulfamic acid and chlorosulfonic acid in a molar ratio of 1:1.01-2. The preparation method of the dichlorsulfimide comprises the step of preparing the dichlorsulfimide, wherein the molar ratio of the intermediate to the thionyl chloride is 1:2-2.5. The preparation method of the dichloro sulfimide, which is described above, wherein the step 1) comprises controlling the reaction temperature of the amination reaction by using a heat conducting medium, wherein the temperature difference between the heat conducting medium after heat exchange and the heat conducting medium before heat exchange is 0-2 ℃. The method for producing a bischlorosulfonimide as described above, wherein said separation treatment comprises the steps of: And (3) distilling the reaction product at the temperature of between 0 and 1.5MPa and the temperature of between 30 and 60 ℃ to obtain the dichloro sulfonyl imide. In a second aspect, the present invention provides a bischlorosulfonimide produced by the process for producing a bischlorosulfonimide of the first aspect; Wherein the dichlorsulfoimide comprises, by mass, 85-95% of dichlorsulfoimide compound, 1-5% of sulfur dioxide, 1-5% of hydrogen chloride, 1-5% of water, less than or equal to 4% of bis (sulfamoyl) sulfonamide, 0.1-1% of sulfamic acid and 1-10% of chlorosulfonyl sulfonamide. In a third aspect, the invention provides a reaction device comprising a mixing pump, a stirred tank, a continuous microchannel reactor, a tubular reactor and a flash evaporator which are sequentially communicated through pipelines. The reaction device, wherein the diaphragm metering pump is used for conveying mixed slurry conta