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Method for synthesizing biphenyldianhydride in continuous flow microchannel reactor

A technology of microchannel reactor and channel reactor, which is applied in organic chemistry, chemical recycling, etc., can solve the problems of low product consistency, high equipment cost, and low consistency, and achieve energy utilization rate improvement, easy maintenance, and consistent sex enhancing effect

Active Publication Date: 2022-03-15
SHANDONG GUANSEN POLYMER MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] 2. There are many problems in the existing technology, such as many by-products, low product consistency, serious pollution, etc.
[0010] For the tank-type liquid-phase oxidation process, it needs to react under high temperature and high pressure for a long time, and the product may continue to participate in the oxidation reaction during the process, resulting in many by-products and low consistency; due to the particularity of strong exothermic oxidation reaction , very strict requirements on process and equipment, high equipment cost, difficult to scale up, and a very big challenge in terms of safety

Method used

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  • Method for synthesizing biphenyldianhydride in continuous flow microchannel reactor
  • Method for synthesizing biphenyldianhydride in continuous flow microchannel reactor
  • Method for synthesizing biphenyldianhydride in continuous flow microchannel reactor

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Experimental program
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Effect test

Embodiment 1

[0031] Add 100kg of 2,2', 3,3'-tetramethylbiphenyl and 400kg of glacial acetic acid into the mixing kettle, and add 600g of cobalt acetate, 400g of manganese acetate and 500g of tetrabromoethane into the kettle, stir and mix evenly and preheat Tetramethylbiphenyl dissolves. The mixed liquid is pumped into the microchannel reactor through the feed pump, and oxygen is introduced at the same time, and the oxygen amount: tetramethylbiphenyl molar ratio is 8:1. The reaction pressure is controlled at 1.5MPa, the temperature is 200°C, and the reaction time of the reactants in the microchannel reactor is 45s. After cooling, the oxidized product is transferred to the receiving tank for separation. After cooling, the tetraacid is precipitated, filtered and washed. 3,3'-biphenyldianhydride was prepared by melting and heating dehydration, with a comprehensive yield of 92%. Acetic acid can be reused through refining, and the residue can be refined to recover the catalyst.

Embodiment 2

[0033]Add 42kg of 2,3', 3,4'-tetramethylbis, 130kg of glacial acetic acid into the mixing kettle, and add 35g of cobalt acetate, 70g of manganese acetate and 110g of tetrabromoethane into the kettle, stir and mix evenly and preheat to Tetramethylbiphenyl dissolves. The mixed liquid is pumped into the microchannel reactor through the feed pump, and oxygen is introduced at the same time, and the amount of oxygen: the amount of chlorinated o-xylene is 10:1. The reaction pressure is controlled at 2.5MPa, the temperature is 180°C, and the reaction time of the reactants in the microchannel reactor is 80s. After cooling, the oxidized product is transferred to the receiving tank for separation. After cooling, the tetraacid is precipitated, filtered and washed. 3,3'-biphenyldianhydride was prepared by melting and heating dehydration with a comprehensive yield of 92.6%. Acetic acid can be reused through refining, and the residue can be refined to recover the catalyst.

Embodiment 3

[0035] 21kg of 2,2', 3,3'-tetramethylbiphenyl, 2,3', 3,4'-tetramethylbiphenyl, 3,3', 4,4'-tetramethylbiphenyl The mixture, 84kg of glacial acetic acid was added to the mixing kettle, and 200g of cobalt acetate, 200g of manganese acetate, and 100g of tetrabromoethane were added to the kettle, and stirred and mixed evenly. And the mixed solution is pumped into the microchannel reactor through the feed pump, and oxygen is introduced at the same time, and the ratio of the molar amount of oxygen to the amount of chlorinated o-xylene is 6.5:1. The reaction pressure is controlled at 1.25MPa, the temperature is 300°C, and the reaction time of the reactants in the microchannel reactor is 50s. After cooling, the oxidized product is transferred to a receiving tank for gas-liquid separation, and the acetic acid is removed by flash evaporation, and the remaining product is subjected to vacuum distillation to obtain mixed biphenyldianhydride. The comprehensive yield of this embodiment is 8...

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Abstract

The invention discloses a method for synthesizing biphenyl dianhydride in a continuous-flow microchannel reactor: step 1 configures a reaction solution, mixes tetramethylbiphenyl, glacial acetic acid, a catalyst and an accelerator uniformly; step 2 preheats the reaction solution, Then enter the reaction module, and at the same time pass pure oxygen into the reaction module, and the reactants are mixed and reacted in the reaction module; after a certain period of time in step 3, the reaction product enters the receiving tank; in step 4, the acetic acid solvent is recovered, dehydrated, refined and recycled , the remaining product is washed and extracted to obtain biphenyl tetraic acid, and biphenyl dianhydride is obtained through melting and dehydration; step 5 biphenyl dianhydride is further purified to obtain 3,3'-BPDA, 3,4'-BPDA and 4, 4'‑BPDA.

Description

technical field [0001] The invention relates to a method for preparing biphenyl dianhydride by using tetramethylbiphenyl liquid-phase oxygen oxidation in a continuous flow microchannel reactor, which can obtain biphenyl dianhydride in a high-yield, safe and environment-friendly manner. [0002] The invention belongs to the technical field of organic synthesis application. In a continuous flow microchannel reactor, tetramethylbiphenyl is used as a raw material, cobalt and manganese are used as catalysts, and the methyl group on the benzene ring is oxidized to a carboxyl group within a reaction time of several seconds to several minutes under high temperature and pressure. , and then a new process for preparing biphenyl dianhydride through dehydration. The method has the advantages of being safe, reliable, and easy to operate, and can continuously produce biphenyl dianhydride with high yield. The adoption of this process can greatly reduce the discharge of three wastes, the pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/89
CPCC07D307/89Y02P20/584
Inventor 李晓斐巴广芝
Owner SHANDONG GUANSEN POLYMER MATERIAL TECH CO LTD
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