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Preparation method of p-hydroxyl biphenol

A technology of hydroxybiphenol and di-tert-butylphenol is applied in the field of preparation of p-hydroxybiphenol, and can solve the problems of low purity of 4,4'-biphenol, many steps, low yield and the like , to achieve the effect of reducing the use of other reagents, good reaction selectivity, and high product purity

Active Publication Date: 2020-12-29
威海金泓高分子有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Yet the 4 of above-mentioned method preparation, 4 ' diphenol purity is not high, and yield is low, has restricted 4, the output of 4 ' diphenol
In view of the current 2,6'di-tert-butylphenol oxidative coupling reductive dealkylation method is a relatively mainstream preparation method, but this method has many steps, many types of reagents are added, and the yield is relatively low; Improvements are made on the base material of the method to increase catalytic efficiency and product yield and purity

Method used

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  • Preparation method of p-hydroxyl biphenol
  • Preparation method of p-hydroxyl biphenol
  • Preparation method of p-hydroxyl biphenol

Examples

Experimental program
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Effect test

Embodiment 1

[0042](1) 206.33g of 2,6-di-tert-butylphenol, 106.17g of xylene, and 0.52g of aluminum chloride are respectively added in a 1000ml three-necked flask with a reflux condenser and a packed tower, and clean air is introduced, and the reaction temperature is 50 °C, reacted for 7.5 hours, and the content of oxidation products was 37%. At this time, stop feeding air, switch to nitrogen protection, add 95.86g sodium bisulfite, and carry out reduction reaction at 150° C. for 8 hours, and the content of the reduction product is 73.8%. Cool down to 80°C, filter and transfer to a 1000ml three-neck flask equipped with a reflux condenser and a packed tower for recrystallization and filtration to obtain a white solid.

[0043] (2) Add 0.52g aluminum chloride to the three-necked flask of step (1) under the protection of nitrogen, and add dropwise 106.17g xylene. The dropwise addition is completed within 40 minutes, and the temperature is raised to 150° C. for de-tert-butyl reaction at the sa...

Embodiment 2

[0045] (1) 206.33g of 2,6-di-tert-butylphenol, 212.34g of xylene, and 0.40g of aluminum chloride are respectively added in a 1000ml three-necked flask with a reflux condenser and a packed tower, and clean air is introduced, and the reaction temperature is 50 °C, reacted for 10 hours, and the oxidation product content was 46.5%. At this time, stop feeding air, switch to nitrogen protection, add 93.65g of sodium bisulfite, and carry out reduction reaction at 150°C for 7.5 hours, and the content of the reduction product is 91.5%. Cool down to 80°C, filter and transfer to a 1000ml three-neck flask equipped with a reflux condenser and a packed tower for recrystallization and filtration to obtain a white solid.

[0046] (2) Add 0.40 g of aluminum chloride to the three-necked flask of step (1) under nitrogen protection, and add 212.34 g of xylene dropwise. The addition is completed within 45 minutes, and the temperature is raised to 135° C. for tert-butyl reaction for 6 hours. After...

Embodiment 3

[0048] Add 206.33g of 2,6-di-tert-butylphenol, 318.51g of xylene, and 0.27g of aluminum chloride into a 1000ml three-neck flask equipped with a reflux condenser and a packed tower respectively, pass in clean air, and react at a temperature of 50°C. After 8.5 hours, the oxidation product content was 46%. At this point, stop feeding the air, switch to nitrogen protection, add 104.06g of sodium bisulfite, and carry out reduction reaction at 150° C. for 7 hours, and the content of the reduction product is 91.5%. Cool down to 80°C, filter and transfer to a 1000ml three-neck flask equipped with a reflux condenser and a packed tower for recrystallization and filtration to obtain a white solid.

[0049] (2) Add 0.27g of aluminum chloride to the three-necked flask of step (1) under the protection of nitrogen, and dropwise add 212.34g of dimethylbenzene, dropwise within 50min, and simultaneously raise the temperature to 120°C for tert-butyl reaction for 7 hours, The content of the inte...

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Abstract

The invention discloses a preparation method of p-hydroxyl biphenol, which adopts a two-step method to prepare a target product, and comprises the following steps: carrying out oxidative coupling reaction and reduction reaction on 2,6-di-tert-butyl phenol, recrystallizing to obtain white powder, adding a catalyst, dropwise adding xylene, and carrying out tert-butyl removal reaction to obtain the target product. By selecting the catalyst and dropwise adding xylene to capture tert-butyl, free tert-butyl in the reaction liquid is reduced, complete reaction is promoted, isomers or byproducts whichare difficult to remove are not generated, and the obtained product is easy to purify. Few types of reagents are added in the preparation process, xylene and isobutene obtained by reaction can be recycled, and the yield and purity of the finally obtained product are very high.

Description

technical field [0001] The invention relates to the technical field of p-hydroxybiquinone, in particular to a preparation method of p-hydroxybiquinone. Background technique [0002] According to the "Electronic Information Industry Adjustment and Revitalization Plan" issued by the state, the focus of breaking through the bottleneck of the development of the new display industry and improving the new display system is panel materials, and the focus of industrial policy support is to open up the liquid crystal industry chain to achieve high-purity 4,4' The industrial production of biphenol is an important link, and it is also one of the core problems that urgently need to be broken through. The mainland is the world's largest production and supply base for liquid crystal monomers and intermediates. In recent years, with the rapid development of China's home appliance industry, my country has a large demand for glass fiber reinforced aromatic polyester, accounting for more than...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/11C07C37/50C07C39/15
CPCC07C37/11C07C37/50C07C39/15
Inventor 宋吉巍向琼周耀国刘祥臣徐平
Owner 威海金泓高分子有限公司
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