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A kind of method adopting loop reactor to synthesize 4,4'-dihydroxybiphenyl

A dihydroxybiphenyl and loop reactor technology, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve environmental pollution, low reaction efficiency, and 4,4'-dihydroxybiphenyl yield Low-level problems, to achieve the effect of reducing energy consumption, improving efficiency, and reducing production costs

Active Publication Date: 2022-03-22
四川圣效科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention solves the problems of low yield, inefficient reaction and environmental pollution of the existing method for synthesizing 4,4'-dihydroxybiphenyl, and provides a high-efficiency, high-yield, low-tar by-product synthesis of 4,4' -Dihydroxybiphenyl method

Method used

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  • A kind of method adopting loop reactor to synthesize 4,4'-dihydroxybiphenyl
  • A kind of method adopting loop reactor to synthesize 4,4'-dihydroxybiphenyl
  • A kind of method adopting loop reactor to synthesize 4,4'-dihydroxybiphenyl

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specific Embodiment approach 1

[0028] Specific embodiment one: In this embodiment, a method for synthesizing 4,4'-dihydroxybiphenyl using a loop reactor, the method includes the following steps:

[0029] 1. Add phenol to the reactor equipped with a loop reaction system;

[0030] 2. Introduce nitrogen for evacuation, add a Lewis acid catalyst, then introduce isobutylene, use a reactor equipped with a loop reaction system to react, control the temperature at 90-120°C, and react for 4-8 hours to obtain di-tert-butylphenol;

[0031] 3. Dissolve di-tert-butylphenol in an organic solvent, add an alkali catalyst and an oxidant in sequence, and use a reactor equipped with a loop reaction system for the reaction, control the temperature at 50-100°C, react for 2-4 hours, and then heat up to 180-100°C 200°C, react for 3 to 5 hours, then cool down and filter to obtain tetra-tert-butylbiphenol;

[0032] 4. Dissolve tetra-tert-butylbiphenyldiphenol in a mixed solvent, add a strong acid catalyst, control the temperature ...

specific Embodiment approach 2

[0036] Specific embodiment two: the difference between this embodiment and specific embodiment one is: the reaction kettle of the configuration loop reaction system described in step one includes reactor 1 and loop reaction system, and loop reaction system includes Venturi ejector 3, loop circulation pump 4 and heat exchanger 2; Venturi ejector 3 is arranged on the top of reactor 1, the inlet of Venturi ejector 3 communicates with the outlet of heat exchanger 2, the outlet at the bottom of reactor 1 communicates with the inlet at the bottom of heat exchanger 2, And a loop circulation pump 4 is arranged on the pipeline in which the outlet at the bottom of the reactor 1 communicates with the inlet at the bottom of the heat exchanger 2 . Others are the same as in the first embodiment.

specific Embodiment approach 3

[0037] Specific embodiment three: the difference between this embodiment and specific embodiment one or two is: the Lewis acid catalyst described in step two is one of ferric chloride, aluminum chloride, zinc chloride, isopropyl aluminum and phenyl aluminum One or more kinds are mixed, and the dosage of the Lewis acid catalyst is 0.1% to 10% of the mass of phenol. Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a method for synthesizing 4,4'-dihydroxybiphenyl by using a loop reactor, and the invention relates to the field of synthesis methods of 4,4'-dihydroxybiphenyl. The present invention aims to solve the problems of low yield, inefficient reaction and environmental pollution in the synthesis of 4,4'-dihydroxybiphenyl by the existing method. Method: Use cheap and easy-to-obtain phenol as raw material, add di-tert-butylene to isobutene under Lewis acid catalyzed conditions to generate di-tert-butylphenol, and then dissolve di-tert-butylphenol in an organic solvent under alkaline conditions, and oxidize the di-tert-butylphenol Combined into tetra-tert-butylbiphenyldiphenol, and finally add strong acid to the mixed solvent to catalyze the removal and recover isobutene, and obtain high-purity 4,4'-dihydroxybiphenyl through recrystallization or sublimation method. The invention has a total yield of more than 90%, and has the advantages of simple operation, high conversion rate, low cost, less waste, high product purity and the like. The invention is used for preparing 4,4'-dihydroxybiphenyl.

Description

technical field [0001] The present invention relates to the field of synthetic methods of 4,4'-dihydroxybiphenyl. Background technique [0002] 4,4'-Dihydroxybiphenyl is widely used in the chemical industry to prepare engineering composite materials, polyester, polyurethane, poly Phenylsulfone, epoxy resin, dye intermediates, photosensitive materials, etc. Among them, high-purity 4,4'-dihydroxybiphenyl is mainly used in thermotropic liquid crystal polymer engineering plastics. my country, as the production center of electronic products in the world, accounts for half of the global annual demand for thermotropic liquid crystal polymer engineering plastics, but basically Can only rely on imports. 4,4'-Dihydroxybiphenyl is the basic raw material of thermotropic liquid crystal polymer engineering plastics, and the domestic market is huge. With the upgrading of the domestic communication electronics industry, the market scale will maintain a relatively high growth rate. [0003...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/50C07C39/15
CPCC07C37/50C07C37/11C07C37/14C07C39/15C07C39/11
Inventor 夏吾炯苟宝权孙光辉郭小忠冯永胜洪国良许峰熊勇钱红林袁鹏
Owner 四川圣效科技有限公司
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