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A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene

A trifluoromethylphenoxy, production process technology, applied in the field of pesticides, can solve the problems of affecting the yield and purity of products, severe heat release, etc., to suppress side reactions, improve reaction efficiency, and improve heat and mass transfer. effect of ability

Active Publication Date: 2021-05-18
浙江禾本科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The obvious disadvantage of the improved process is that the process of dropping the mixed acid will exotherm violently, which will cause the local temperature of the dropping site to be too high, and easily generate dinitrogen compounds and sulfonated compounds, which will affect the yield and purity of the final product.

Method used

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  • A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene
  • A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene

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Effect test

Embodiment 1

[0030] A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene, comprising the following steps:

[0031] Step S1, add 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene dichloroethane solution in No. 1 storage tank, add concentrated sulfuric acid and A mixed acid solution composed of fuming nitric acid; among them, the dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)benzene is used as a reactant; the mixture composed of concentrated sulfuric acid and fuming nitric acid Mixed acid solution as a nitrating reagent; 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoro Methylphenoxy) benzene is solute, and ethylene dichloride is solvent; The quality of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene is 467kg; The mass is 1401kg; the mass of the mixed acid solution composed of concentrated sulfuric acid and fuming nitric acid is 467kg; in the mixed acid solution compos...

Embodiment 2

[0038] A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene, comprising the following steps:

[0039] Step S1, add 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene dichloroethane solution in No. 1 storage tank, add concentrated sulfuric acid and A mixed acid solution composed of fuming nitric acid; among them, the dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)benzene is used as a reactant; the mixture composed of concentrated sulfuric acid and fuming nitric acid Mixed acid solution as a nitrating reagent; 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoro Methylphenoxy) benzene is solute, and ethylene dichloride is solvent; The quality of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene is 467kg; The mass is 4670kg; the mass of the mixed acid solution composed of concentrated sulfuric acid and fuming nitric acid is 389.17kg; in the mixed acid solution com...

Embodiment 3

[0046] A production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene, comprising the following steps:

[0047] Step S1, add 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene dichloroethane solution in No. 1 storage tank, add concentrated sulfuric acid and A mixed acid solution composed of fuming nitric acid; among them, the dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)benzene is used as a reactant; the mixture composed of concentrated sulfuric acid and fuming nitric acid Mixed acid solution as a nitrating reagent; 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)dichloroethane solution of 1,3-bis-(2-chloro-4-trifluoro Methylphenoxy) benzene is solute, and ethylene dichloride is solvent; The quality of 1,3-bis-(2-chloro-4-trifluoromethylphenoxy) benzene is 467kg; The mass is 1500kg; the mass of the mixed acid solution composed of concentrated sulfuric acid and fuming nitric acid is 424.55kg; in the mixed acid solution com...

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Abstract

The invention discloses a production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene: the microreactor heating device is turned on, and two conveying Pump, the dichloroethane solution and the mixed acid solution of 1,3-two-(2-chloro-4-trifluoromethylphenoxy)benzene in the two storage tanks are sent into the microreactor respectively to carry out nitration reaction; Collect the reaction solution from the outlet; let the reaction solution stand still, and separate the organic layer; add water to the organic layer, and reflux to recover dichloroethane; after the recovery of dichloroethane, cool the reaction system to room temperature, filter, wash with water, and dry Pesticide intermediates can be obtained by drying. The production process disclosed by the invention effectively suppresses the generation of side reactions, improves the reaction efficiency, and utilizes the characteristics of high-efficiency mass and heat transfer of the microchannel reactor, and the process has better operability and safety.

Description

technical field [0001] The invention relates to the technical field of pesticides, in particular to a production process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene. Background technique [0002] 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene is an important intermediate in the synthesis of oxyfluorfen, which is synthesized from resorcinol and 3,4-bis Chlorobenzotrifluorotoluene is produced by forming ether compounds at high temperature, and then nitrated with nitric acid mixed acid (the reaction equation is shown below). The current process for synthesizing 1,3-bis-(2-chloro-4-trifluoromethylphenoxy)-4-nitrobenzene is to dissolve the ether compound in an appropriate amount of organic solvent, and add nitric acid mixed acid dropwise at low temperature. The obvious disadvantage of the improved process is that the process of dropping the mixed acid will exotherm violently, which will cause the local temperature of the dropping site ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C205/38C07C201/08B01J19/00
CPCB01J19/0093C07C201/08C07C205/38Y02P20/10
Inventor 徐齐恩王进潘光飞陈华戴光炳陈云南彭彩群李成斌
Owner 浙江禾本科技股份有限公司
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