Synthesis method of high-purity chlorosulfonyl isocyanate

A technology of chlorosulfonyl isocyanate and synthesis method, which is applied in the preparation of sulfonic acid amide, organic chemistry, etc., can solve the problems of unsuitability for industrial production, inability to run for a long time, and harsh reaction conditions, so as to reduce energy consumption and labor costs, and improve production efficiency. The process is safe and reliable, and the effect of avoiding the use of solvents

Active Publication Date: 2019-03-01
四平市精细化学品有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in patents JP77855 and EP294613, the reaction conditions are harsh and not suitable for industrial production; CN101891657 uses an inert solvent, and direct distillation does not deal with impurities generated by side reactions, which may easily cause low product purity and cannot be operated for a long time

Method used

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  • Synthesis method of high-purity chlorosulfonyl isocyanate
  • Synthesis method of high-purity chlorosulfonyl isocyanate
  • Synthesis method of high-purity chlorosulfonyl isocyanate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The present embodiment provides a continuous distillation system comprising:

[0047]The light removal upper tower, the light removal middle tower and the light removal lower tower connected successively from top to bottom, the middle part of the light removal upper tower is provided with a feed liquid inlet;

[0048] A weight-removing tower in which the liquid inlet is connected to the liquid outlet of the lower tower. The upper part of the weight-removing tower is provided with an outlet for fractions before distillation. The middle part of the weight-removing tower is provided with a finished product outlet. Heavy components are exported.

[0049] The upper light removal tower, the middle light removal tower, the lower light removal tower and the heavy weight removal tower are packed towers, and the filler is selected from 700Y wire mesh corrugated packing.

[0050] Wherein, the packing in the light removal upper tower is arranged in sections, the packing in the lig...

Embodiment 2

[0063] Add 20mL of chlorosulfonic acid isocyanate into the reaction device as a reaction solvent, and then feed in a certain amount of sulfur trioxide 80.06g and cyanogen chloride 61.47g at the same time, and keep the temperature at 30°C for reaction. Raise the temperature of the reaction solution to 120°C for thermal decomposition, recover sulfur trioxide, and pass it into the next sulfonation reaction. The thermally decomposed reaction liquid is rectified, and the reaction liquid is carried out by means of continuous distillation. While feeding the material, heat the bottom of the light removal lower tower, and then open the light middle tower and the light removal upper tower to heat. When the pressure in the kettle reaches 1.7Mpa and the temperature at the top of the tower reaches 95°C, reflux for 2 hours to ensure thermal decomposition After it is fully completed, the feed is continuously re-fed, and the front fraction and the finished product are continuously extracted a...

Embodiment 3

[0065] Add 20mL of the fraction before the batch to the reaction device as a reaction solvent, and then feed 80.06g of sulfur trioxide, 61.47g of cyanogen chloride and recovered gas at the same time according to a certain amount, and keep the temperature at 34°C for reaction. The temperature of the reaction solution is raised to 100°C for thermal decomposition, and sulfur trioxide is recovered. The thermally decomposed reaction liquid is rectified, and the reaction liquid is carried out by means of continuous distillation. While feeding the material, heat the bottom of the light removal lower tower, and then open the light middle tower and the light removal upper tower to heat. When the pressure in the kettle reaches 1.5Mpa and the temperature at the top of the tower reaches 93°C, reflux for 2 hours to ensure thermal decomposition After it is fully completed, the feed is continuously re-fed, and the forward distillation and the finished product are continuously extracted at th...

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Abstract

The invention provides a synthesis method of high-purity chlorosulfonyl isocyanate. The synthesis method includes the steps that (A) under the condition of a diluent, sulfur trioxide and cyanogen chloride are subjected to sulfonation reaction to obtain a reaction solution; (B) the reaction solution is subjected to thermal decomposition reaction to obtain a reaction solution after thermal decomposition; (C) the reaction solution after thermal decomposition is subjected to positive pressure continuous distillation to obtain the high-purity chlorosulfonyl isocyanate and a distillate before distillation; and the diluent is selected from the chlorosulfonyl isocyanate or the distillate before distillation. According to the synthesis method of the high-purity chlorosulfonyl isocyanate, the totalyield of the process is increased; the distillate before distillation is used as a reaction solvent, use of a high boiling point solvent is avoided, in the pyrolysis process, the cyanogen chloride andthe sulfur trioxide are partially recovered, thus the utilization rate of raw materials is increased, and the production cost is lowered; and meanwhile, the rectification process is conducted throughthe mode of positive pressure distillation and continuous feeding, the yield of products is greatly increased, the distillation time is shortened, energy consumption and labor costs are lowered, andthe synthesis method of the high-purity chlorosulfonyl isocyanate is suitable for industrial mass production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing high-purity chlorosulfonyl isocyanate. Background technique [0002] Chlorosulfonyl isocyanate is a very reactive intermediate. The substance reacts with hydroxyl, amino, and carboxyl groups to generate N-chlorosulfonyl carbamate, urea, and amide. It can be added with water, active hydrogen, alcohol, phenol, amine, amide, carboxylic acid, olefin, aldehyde, ketone, ester to obtain various new compounds, which can be used as dehydrating agent and oxidizing agent. Chlorosulfonyl isocyanate is mainly used in the production of cefuroxime, cefoxitin, carumonam and other drugs. [0003] The manufacturing process of chlorosulfonyl isocyanate in industrial production is not complicated. Generally, the reaction between cyanogen chloride and sulfur trioxide is used, and then the crude chlorosulfonyl isocyanate obtained from the reaction is ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C303/36C07C311/65
CPCC07C303/36C07D291/06C07C311/65
Inventor 薛李冰刘长宝李士龙刘春喜王春艳赵立成罗冬琦
Owner 四平市精细化学品有限公司
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