Method for preparing 3,5-dichlorophenyl isocyanate by microchannel reactor

A technology of dichlorophenyl isocyanate and microchannel reactor, which is applied in chemical instruments and methods, preparation of isocyanate derivatives, preparation of organic compounds, etc., can solve the problems of long reaction time, high environmental protection pressure and high production cost , to achieve the effect of improved reaction yield, less equipment corrosion and low production cost

Inactive Publication Date: 2019-01-11
JIANGXI HEYI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the domestic production process of 3,5-dichlorophenyl isocyanate is mainly the solid-light method and the gas-light method. 3,5-Dichloroaniline is first photochemically treated at low temperature, then photochemically at high temperature, and then the product is obtained by precipit

Method used

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  • Method for preparing 3,5-dichlorophenyl isocyanate by microchannel reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] (1) Preparation link: Press figure 1 Assemble the Corning microchannel continuous flow reactor, and mix 3,5-dichloroaniline and toluene uniformly in a mass ratio of 1:1 to obtain a 3,5-dichloroaniline solution.

[0054] (2) Complete in sequence in Corning microchannel continuous flow reactor: set the flow control of each raw material metering pump so that the molar ratio of 3,5-dichloroaniline and phosgene is 1:1.1, and control the 3,5-dichloroaniline solution The mass flow rate of phosgene is 27g / min, the mass flow rate of phosgene is controlled to be 10g / min, the 3,5-dichloroaniline solution and phosgene are respectively injected into the preheating module 1 of Corning microchannel reactor, and the temperature is controlled to 80℃ and the pressure is 0.5MPa, then enter the first microchannel reactor 2 for mixed reaction, the reaction residence time is 15s, and then pass into the subsequent two serial microchannel reactors 3, the reaction residence time in each microchann...

Embodiment 2

[0057] (1) Preparation link: Press figure 1 Assemble the Corning microchannel continuous flow reactor, mix 3,5-dichloroaniline and toluene uniformly at a mass ratio of 1:1 to obtain a 3,5-dichloroaniline solution.

[0058] (2) Complete in sequence in Corning microchannel continuous flow reactor: set the flow control of each raw material metering pump so that the molar ratio of 3,5-dichloroaniline and phosgene is 1:1.1, and control the 3,5-dichloroaniline solution The mass flow rate of phosgene is 20g / min, the mass flow rate of phosgene is controlled to be 7.4g / min, and the 3,5-dichloroaniline solution and phosgene are respectively injected into the preheating module 1 of Corning microchannel reactor, and the temperature is controlled at 80℃, and the pressure It enters the first microchannel reactor 2 for mixed reaction, and the reaction residence time is 15s, and then passes into the subsequent two series-connected microchannel reactors 3, and the reaction in each microchannel re...

Embodiment 3

[0061] (1) Preparation link: Press figure 1 Assemble the Corning microchannel continuous flow reactor, mix 3,5-dichloroaniline and toluene uniformly at a mass ratio of 1:1 to obtain a 3,5-dichloroaniline solution.

[0062] (2) Complete in sequence in Corning microchannel continuous flow reactor: set the flow control of each raw material metering pump so that the molar ratio of 3,5-dichloroaniline and phosgene is 1:1.1, and control the 3,5-dichloroaniline solution The mass flow rate of phosgene is 15g / min, and the mass flow rate of phosgene is controlled at 5.6g / min. The 3,5-dichloroaniline solution and phosgene are respectively injected into the preheating module 1 of the Corning microchannel reactor, and the temperature is controlled at 80℃ and the pressure It enters the first microchannel reactor 2 for mixed reaction, and the reaction residence time is 15s, and then enters the subsequent two series-connected microchannel reactors 3, and the reaction in each microchannel reactor...

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Abstract

The invention discloses a method for preparing 3,5-dichlorophenyl isocyanate by a microchannel continuous flow reactor. With 3,5-dichloroaniline (3,5-DCA) and gaseous phosgene as raw materials, the 3,5-DCA and a solvent are firstly mixed to form a homogeneous solution in a Corning microchannel reactor; the homogeneous solution and phosgene are preheated respectively, introduced into a first microchannel reactor, mixed and subjected to a reaction; the obtained mixture is introduced into two microchannel reactors in series subsequently to obtain a 3,5-dichlorophenyl isocyanate solution; and thenexcess phosgene is removed by nitrogen gas, and 3,5-dichlorophenyl isocyanate is obtained by reduced pressure rectification. The preparation method shortens the reaction time from a few hours of a traditional method to a few minutes, allows the reaction time generally not to exceed 30 min, the reaction efficiency is significantly improved, the selectivity of the product is significantly improved,a by-product urea is obviously reduced, the three wastes are reduced, the reaction yield is increased, the yield reaches 95-98%, the purity of the product is more than 99%, and the production cost islow.

Description

Technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a method for preparing 3,5-dichlorophenyl isocyanate by adopting a microchannel reactor. Background technique [0002] 3,5-Dichlorophenyl isocyanate is an important organic synthesis intermediate, which is widely used in the synthesis of many fine products in the fields of pesticides, medicine, dyes, pigments, etc., such as dimethyl sclerotium, sclerotium , Diclofenac, Chlorfluzamide and Meclozamide, etc., especially as a key intermediate for the synthesis of iprodione, and can also be used to make pesticides and pest repellents, azo dyes and pigments in the dye industry, etc. . [0003] At present, the domestic production process of 3,5-dichlorophenyl isocyanate is mainly solid-light method and gas-light method. 3,5-dichloroaniline is firstly photochemically at low temperature, then photochemically at high temperature, and then blasted off, desolventized and rectified to obt...

Claims

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Application Information

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IPC IPC(8): C07C263/10C07C265/12
CPCC07C263/10C07C265/12
Inventor 吴勇柴明根高金平廖永候云飞
Owner JIANGXI HEYI CHEM
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