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Method for synthesizing n-butyl isocyanate by adopting micro-channel reactor

A technology of microchannel reactor and n-butyl isocyanate, applied in chemical instruments and methods, preparation of isocyanic acid derivatives, chemical/physical/physicochemical reactors, etc., can solve unstable yield and product quality , FNC heating instability, long reaction time and other problems, to achieve excellent mass and heat transfer effects, improve phosgene utilization, and low labor intensity

Pending Publication Date: 2021-12-24
NINGXIA RUITAI TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction yield is high, but this method still adopts batch reaction, which has the disadvantages of long reaction time and FNC being unstable when heated for a long time.
At the same time, the batch reaction has the disadvantages of high labor intensity, low production capacity, unstable yield and product quality, etc.

Method used

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  • Method for synthesizing n-butyl isocyanate by adopting micro-channel reactor
  • Method for synthesizing n-butyl isocyanate by adopting micro-channel reactor
  • Method for synthesizing n-butyl isocyanate by adopting micro-channel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Such as figure 1 As shown, prepare 10% n-butylamine-o-dichlorobenzene liquid, and pass the n-butylamine-o-dichlorobenzene liquid and hydrogen chloride into the microchannel reactor simultaneously according to the hydrogen chloride and n-butylamine molar ratio of 1.2:1 to form a salt, The salt-forming temperature is 20°C, and the residence time is 50s; (2) n-butylamine hydrochloride-o-dichlorobenzene liquid and phosgene are continuously passed into the phosgenation plate for phosgenation reaction, phosgene: n-butylamine hydrochloride The salt molar ratio is 1.3:1. By adjusting the back pressure valve at the outlet of the reactor, the pressure of the reaction system was kept at 0.5 MPa, the reaction temperature was controlled at 95° C. by the heat exchanger, and the residence time was 100 s. The synthetic solution obtained by the reaction was sent to the sample for analysis. The normalized content of FNC in the synthetic solution was 99.2%, and the yield of FNC was 98.1%...

Embodiment 2

[0038] Such as figure 1 As shown, prepare 5% n-butylamine-chlorobenzene liquid, according to hydrogen chloride and n-butylamine molar ratio is 1.1:1, pass n-butylamine-chlorobenzene liquid and hydrogen chloride in the microchannel reactor simultaneously and carry out salt formation, and salt formation temperature 10°C, residence time 200s. (2) The n-butylamine hydrochloride-chlorobenzene solution and phosgene are continuously passed into the phosgenation plate for phosgenation reaction, and the molar ratio of phosgene: n-butylamine hydrochloride is 1.2:1. By adjusting the back pressure valve at the outlet of the reactor, the pressure of the reaction system was kept at 0.30MPa, the reaction temperature was controlled at 120°C by the heat exchanger, and the residence time was 300s. The synthetic liquid was obtained after the reaction, and the sample was sent for analysis after being drained. The normalized content of FNC in the synthetic liquid is 98.5%, and the yield of FNC is...

Embodiment 3

[0040] Such as figure 1 As shown, prepare 15% n-butylamine-toluene solution, and pass the n-butylamine-toluene solution and hydrogen chloride into the microchannel reactor at the same time according to the molar ratio of hydrogen chloride and n-butylamine as 1.5:1 to form a salt, and the salt-forming temperature is 30°C , dwell time 100s. (2) The n-butylamine hydrochloride-toluene liquid and phosgene are continuously passed into the phosgenation plate for phosgenation reaction, and the molar ratio of phosgene: n-butylamine hydrochloride is 1.5:1. By adjusting the back pressure valve at the outlet of the reactor, the pressure of the reaction system was kept at 0.20MPa, the reaction temperature was controlled at 110°C by the heat exchanger, and the residence time was 200s. The synthetic liquid was obtained after the reaction, and the sample was sent for analysis after being drained. The normalized content of FNC in the synthetic liquid is 99.5%, and the yield of FNC is 98.7%. ...

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Abstract

The invention discloses a method for synthesizing n-butyl isocyanate by adopting a micro-channel reactor, the method comprises the following steps: preparing n-butylamine and a solvent into an n-butylamine solution, and simultaneously introducing the n-butylamine solution and hydrogen chloride into a salifying plate of the micro-channel reactor at a reaction temperature for salifying reaction to generate a salifying solution; and introducing the salifying liquid generated in the steps and phosgene into a phosgenation plate of the micro-channel reactor at reaction temperature and pressure to carry out phosgenation reaction, and sampling and analyzing the content of the synthetic liquid after the synthetic liquid is subjected to phosgenation. According to the invention, the continuous salification and phosgenation reaction is realized through the micro-channel reactor, and the n-butyl isocyanate can be continuously prepared. The method has the advantages of high phosgene utilization rate, few side reactions, high product yield, small liquid holding volume of the microchannel reactor, and greatly improved reaction safety compared with the traditional kettle reaction.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for synthesizing n-butyl isocyanate by using a microchannel reactor. Background technique [0002] N-butyl isocyanate (hereinafter referred to as FNC) is mainly used to synthesize insecticides such as benomyl, and is also used as a catalyst for the synthesis of sulfonylurea herbicides. As an important intermediate, it can be used to synthesize medicines, pesticides and other products. At present, the preparation methods of FNC are mainly the two-step method of phosgene at low temperature and high temperature, and the two methods of first forming salt and then passing light. The reaction formulas of the two synthetic methods are as follows: [0003] (1) The reaction formula of the low temperature and high temperature two-step method is as follows: [0004] Low temperature section: [0005] [0006] High temperature section: [0007] [0008] (2) The light-passi...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C265/04B01J19/00
CPCC07C263/10B01J19/0093B01J19/0013B01J19/0006B01J19/0053B01J2219/00162B01J2219/00051C07C265/04
Inventor 石苏洋严绘孟海娟廖强王明晨马荣慧
Owner NINGXIA RUITAI TECH
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