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Method for nitration synthesis of acifluorfen in microreactor

A technology of acifluorfen and microreactors, which is applied in the preparation of nitro compounds, chemical instruments and methods, chemical/physical/physical chemical reactors, etc., can solve the harsh and safe synthesis conditions of acifluorfen Low problems, to achieve the effect of fast mass transfer rate and reaction rate, increased heat transfer efficiency, and easy to scale up

Pending Publication Date: 2021-02-12
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the existing problems of harsh synthetic conditions of acifluorfen and low safety, and to provide a kind of acifluorfen that can obtain higher conversion rate and yield under mild conditions and ensure safe operation. method, and the microreactor used in it

Method used

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  • Method for nitration synthesis of acifluorfen in microreactor

Examples

Experimental program
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Effect test

Embodiment 1

[0028] The mixed acid was prepared by using 98 wt% fuming nitric acid and 20 wt% fuming sulfuric acid according to the nitric acid:sulfuric acid molar ratio of 0.55:1, and the temperature of the mixed acid preparation process was controlled at 15-20 °C. The mass fractions of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid, acetic anhydride, and dichloroethane in the organic phase were 15.8%, 5.3%, and 78.9%, respectively.

[0029] At 15 °C, the mixed acid and organic phase were pumped into the micro-mixer by a high-pressure syringe pump through the pipeline. The micro-mixer adopted a T-shaped mixing method and passed into a microchannel reactor with a diameter of 500 μm; nitric acid and 3-(2 The molar ratio of -chloro-4-trifluoromethylphenoxy)benzoic acid is 1.4:1, the reaction residence time is 540 s, the reaction product flows out of the reactor, and the product is obtained by phase separation, drying and washing, and the reaction conversion rate reaches 99.19 %, selectivi...

Embodiment 2

[0043]The process is the same as in Example 1, the molar ratio of mixed acid nitric acid: sulfuric acid remains unchanged, and the mass fraction of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid in the organic phase is 8%. At 10 °C, the molar ratio of nitric acid to 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid was 0.96:1, the reaction residence time was 30 s, the reaction conversion was 53.13%, and the selectivity was 80.32 %.

Embodiment 3

[0045] The process is the same as in Example 1, the molar ratio of mixed acid nitric acid: sulfuric acid remains unchanged, and the mass fraction of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid in the organic phase is 30%. At 35 °C, the molar ratio of nitric acid to 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid was 1.8:1, the reaction residence time was 780 s, the reaction conversion rate was 99.98%, and the selectivity was 69.21 %.

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Abstract

The invention relates to a method for nitration synthesis of acifluorfen in a microreactor. The method for nitration synthesis of acifluorfen in the microreactor comprises the following steps: proportionally pumping a nitrating agent composed of a solution containing raw materials 3 (2chlorine 4trifluoromethyl phenoxy) benzoic acid, fuming sulfuric acid and fuming nitric acid into the micro-channel reactor in parallel through a metering pump; and reacting to synthesize the 5 (2chlorine 4trifluoromethyl phenoxy) 2nitrobenzoic acid (acifluorfen). The acifluorfen is synthesized by nitration of the micro-channel reactor, the phase contact area is increased, and the mass transfer rate and the reaction rate are high; The heat transfer efficiency is increased, reaction heat is transferred quickly, and safety is improved; The continuous operation is achieved, product quality is stable, operation is flexible, and amplification is easy; under optimized conditions, the reaction conversion rate can reach 99.19%, and the reaction selectivity is 81.08%.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and relates to a method for synthesizing acifluorfen by nitration of 3-(2-chloro-4-trifluoromethylphenoxy) benzoic acid mixed with nitric acid and a microreactor, that is, in the microreactor Into the raw material ether compound and nitric acid mixed acid in proportion to synthesize acifluorfen. Background technique [0002] Acifluorfen is an important pesticide intermediate, mainly used in the synthesis of fomesafen and other low-toxic pesticides containing fluorine-containing diphenyl ethers. The nitrating agent used for nitration of 3-(2-chloro-4-trifluoromethylphenoxy)benzoic acid to synthesize acifluorfen in industry is a higher concentration of nitric acid and sulfuric acid mixed acid, and the nitration reaction kettle used is mostly Batch kettle with mechanical stirring, and this kind of batch kettle has uneven mixing, low heat transfer efficiency, and prone to local temperature rise of m...

Claims

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Application Information

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IPC IPC(8): C07C201/08C07C205/59B01J19/00
CPCC07C201/08B01J19/0093C07C205/59Y02P20/10
Inventor 赵玉潮李申芳孙文星金楠王清强翟哲杨浩吕宏缨
Owner YANTAI UNIV
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