Method for preparing 3-nitro-4-chlorobenzotrifluoride through continuous adiabatic nitration and micro-reaction equipment

A chlorobenzotrifluorotoluene and adiabatic nitration technology, which is applied in the preparation of nitro compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problem of the reduction of nitration reaction rate, the restriction of industrial production of micro-reaction systems, and the reduction of reaction conversion rate, etc. problems, to achieve the effects of comprehensive cost reduction, safe production process, and short response time

Pending Publication Date: 2021-10-29
SHANDONG DOCRIS CHEM +1
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Problems solved by technology

At the same time, for some heterogeneous reactions, after the droplets are dispersed through the microreactor, they may gradually coalesce along the reaction delay tube, and the droplets of the organic phase and the acid phase gradually become larger, eventually leading to the separation of the two phases, thereby reducing the nitrification reaction rate. Significant decline or ter

Method used

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  • Method for preparing 3-nitro-4-chlorobenzotrifluoride through continuous adiabatic nitration and micro-reaction equipment
  • Method for preparing 3-nitro-4-chlorobenzotrifluoride through continuous adiabatic nitration and micro-reaction equipment
  • Method for preparing 3-nitro-4-chlorobenzotrifluoride through continuous adiabatic nitration and micro-reaction equipment

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Effect test

Embodiment 1

[0042] (1) under stirring state, add concentrated sulfuric acid (mass fraction is 98%) in concentrated nitric acid and cool reaction solution, obtain mixed acid material, the mass ratio of concentrated sulfuric acid and concentrated nitric acid is 8:1;

[0043] (2) In a constant temperature oil bath, the mixed acid material and p-chlorobenzotrifluoride are preheated to 70°C respectively (the flow rates of the mixed acid and chlorobenzene plunger pumps are respectively 160ml / min and 30ml / min), and they are continuously transported to In the micro-reaction system, according to the reaction molar ratio of nitric acid and chlorobenzene is 1.08:1; first enter the micro-sieve reactor for adiabatic nitration reaction, the outlet temperature of the micro-sieve reactor is 130 ° C, and then continuously flow through the static mixing A device and a reaction delay tube are used to carry out a continuous nitration reaction, and the residence time of the reaction solution in the micro-react...

Embodiment 2

[0046] (1) under stirring state, add concentrated sulfuric acid (mass fraction is 98%) in concentrated nitric acid and cool reaction solution, obtain mixed acid material, the mass ratio of concentrated sulfuric acid and concentrated nitric acid is 10:1;

[0047](2) In a constant temperature oil bath, the mixed acid material and p-chlorobenzotrifluoride are preheated to 80°C respectively (the flow rates of the mixed acid and chlorobenzene plunger pumps are respectively 160ml / min and 30ml / min), and they are continuously transported to In the micro-reaction system, according to the reaction molar ratio of nitric acid and chlorobenzene is 1.05:1; first enter the micro-sieve reactor for adiabatic nitration reaction, the outlet temperature of the micro-sieve reactor is 140 ° C, and then continuously flow through static mixing A device and a reaction delay tube are used to carry out a continuous nitration reaction, and the residence time of the reaction solution in the micro-reaction ...

Embodiment 3

[0050] (1) under stirring state, add concentrated sulfuric acid (mass fraction is 98%) in concentrated nitric acid and cool reaction solution, obtain mixed acid material, the mass ratio of concentrated sulfuric acid and concentrated nitric acid is 12:1;

[0051] (2) In a constant temperature oil bath, the mixed acid material and p-chlorobenzotrifluoride are preheated to 75°C respectively (the flow rates of the mixed acid and chlorobenzene plunger pumps are respectively 160ml / min and 30ml / min), and they are continuously transported to In the micro-reaction system, according to the reaction molar ratio of nitric acid and chlorobenzene is 1.15:1; first enter the micro-sieve reactor for adiabatic nitration reaction, the outlet temperature of the micro-sieve reactor is 135 ° C, and then continuously flow through static mixing A device and a reaction delay tube are used to carry out a continuous nitration reaction, and the residence time of the reaction solution in the micro-reaction...

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Abstract

The invention discloses a method for preparing 3-nitro-4-chlorobenzotrifluoride through continuous adiabatic nitrification and micro-reaction equipment. The method comprises the following steps: (1) under a stirring state, adding concentrated sulfuric acid into concentrated nitric acid, and cooling the reaction liquid to obtain a mixed acid material; (2) respectively preheating the mixed acid material and p-chlorobenzotrifluoride to a reaction temperature, simultaneously and continuously conveying into a micro-reaction system, continuously flowing through a micro-sieve pore reactor, a static mixer and a reaction delay tube, and carrying out a continuous nitration reaction; and (3) carrying out phase separation, extraction and washing to obtain the product 3-nitro-4-chlorobenzotrifluoride. The micro-reaction equipment comprises a micro-sieve pore reactor, and one end of an outlet of the micro-sieve pore reactor is sequentially communicated with a static mixer and a reaction delay tube; and the static mixer is filled with small stainless steel balls. The reaction rate is not reduced at the later stage of the reaction, so that the reaction conversion rate is effectively improved. And the production process is safe, controllable, short in time and high in product content.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of 3-nitro-4-chlorobenzotrifluoride. Background technique [0002] 3-nitro-4-chlorobenzotrifluoride is mainly used in organic synthesis in industry, it is an intermediate for the synthesis of 3,5-dinitro-4-chlorobenzotrifluoride, and industrially prepares 3-nitro-4- Chlorotrifluorotoluene adopts a batch still production process, as shown in chemical reaction formula 1. The traditional batch kettle production process takes a long time, the temperature is not easy to control, the yield is low, the by-products are more, and the safety risk is high, which is not in line with the development of society. Therefore, the intrinsically safe continuous adiabatic nitrification process came into being under this background. [0003] [0004] The nitrification reaction is an exothermic reaction. The higher the temperature, the faster the nitrification react...

Claims

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Application Information

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IPC IPC(8): C07C205/12C07C201/08C07C201/16B01J19/00
CPCC07C201/08C07C201/16B01J19/0093B01J2219/00013B01J2219/00889C07C205/12
Inventor 邓建骆广生卢凤阳类成存彭雪莹马南宁于文智
Owner SHANDONG DOCRIS CHEM
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