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A kind of tmbp industrial synthesis method

A solution and dimethylphenol technology, applied in the field of TMBP synthesis, can solve the problems that the TMBP synthesis process is not suitable for industrialized large-scale production, and achieve the effects of increasing industrial production capacity, reducing side reactions, and high purity

Active Publication Date: 2022-03-25
甘肃泰升化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention provides a kind of TMBP industrial synthesis method, solves the problem that the TMBP synthesis process reported in the existing literature is not suitable for industrialized large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A TMBP industrial synthesis method, comprising the following steps:

[0032] (1) after dissolving 2,6-dimethylphenol, sodium lauryl sulfate, borax with isopropanol, get pre-solution for subsequent use;

[0033] (2) adding a certain amount of deionized water to the reaction kettle and then adding the pre-solution, heating to a certain temperature and then quickly adding the catalyst, then sealing the reaction kettle, stirring and feeding oxygen, and continuing to react for a certain period of time under a certain pressure;

[0034] (3) After the reaction is completed and the pressure is released to normal pressure, a white needle-like crystal product, namely TMBP, is obtained through cooling, filtration, washing, recrystallization, and drying; wherein, a reducing agent is added in the process of recrystallization.

[0035] Wherein, the catalyst is copper acetate; the reducing agent is sodium hydrosulfite, commonly known as hydrosulfite. Wherein, in molar ratio, the dosa...

Embodiment 2

[0045] A TMBP industrial synthesis method, comprising the following steps:

[0046](1) after dissolving 2,6-dimethylphenol, sodium lauryl sulfate, borax with isopropanol, get pre-solution for subsequent use;

[0047] (2) adding a certain amount of deionized water to the reaction kettle and then adding the pre-solution, heating to a certain temperature and then quickly adding the catalyst, then sealing the reaction kettle, stirring and feeding oxygen, and continuing to react for a certain period of time under a certain pressure;

[0048] (3) After the reaction is completed and the pressure is released to normal pressure, a white needle-like crystal product, namely TMBP, is obtained through cooling, filtration, washing, recrystallization, and drying; wherein, a reducing agent is added in the process of recrystallization.

[0049] Wherein, the catalyst is copper acetate; the reducing agent is sodium hydrosulfite, commonly known as hydrosulfite. Wherein, in molar ratio, the dosag...

Embodiment 3

[0060] A TMBP industrial synthesis method, comprising the following steps:

[0061] (1) after dissolving 2,6-dimethylphenol, sodium lauryl sulfate, borax with isopropanol, get pre-solution for subsequent use;

[0062] (2) adding a certain amount of deionized water to the reaction kettle and then adding the pre-solution, heating to a certain temperature and then quickly adding the catalyst, then sealing the reaction kettle, stirring and feeding oxygen, and continuing to react for a certain period of time under a certain pressure;

[0063] (3) After the reaction is completed and the pressure is released to normal pressure, a white needle-like crystal product, namely TMBP, is obtained through cooling, filtration, washing, recrystallization, and drying; wherein, a reducing agent is added in the process of recrystallization.

[0064] Wherein, the catalyst is copper acetate; the reducing agent is sodium hydrosulfite, commonly known as hydrosulfite. Wherein, in molar ratio, the dosa...

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PUM

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Abstract

The invention relates to an industrial synthesis method of TMBP, which comprises the following steps: (1) dissolving 2,6-dimethylphenol, sodium dodecyl sulfate and borax in isopropanol to obtain a pre-solution for later use; (2) Add a certain amount of deionized water to the reaction kettle and then add the pre-solution, heat to a certain temperature and then add the catalyst quickly, then seal the reaction kettle, stir and introduce oxygen, and continue the reaction for a certain time under a certain pressure; (3) The reaction is completed And after pressure relief to normal pressure, through cooling, filtration, washing, recrystallization, and drying to obtain a white needle-like crystal product, namely TMBP; wherein, a reducing agent is added in the process of recrystallization. The invention innovatively uses pressurized process conditions, and through the selection of raw material types and the adjustment of process conditions, the side reactions under pressurized conditions are greatly reduced under the synergistic effect, and combined with reduction means, the TMBP yield (overall Greater than 85%) and double boost in purity (greater than 99.0%).

Description

technical field [0001] The invention relates to the technical field of TMBP synthesis, in particular to an industrial synthesis method of TMBP. Background technique [0002] 3,3',5,5'-Tetramethylbiphenyldiol (3,5,3',5'-Tetramethyl-biphenyl-4,4'-diol, TMBP), is a typical liquid crystal polymer Intermediate material. At the same time, due to its excellent heat resistance, it is also used as a modified monomer for polyester, polyurethane, polycarbonate, polysulfone, epoxy resin and many other products; and because of its resistance to aging caused by oxygen and heat It can also be used as a rubber, latex antioxidant and plastic antioxidant, as well as a stabilizer for fuel intermediates or petroleum products. For example, it can be used for light-colored vulcanized rubber products, food packaging glue, Medical dairy products and sulfur oxide products. Among them, the application as the raw material of liquid crystal polymer has reached the stage of industrial use. [0003] ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C37/11C07C37/68C07C37/84C07C37/86C07C39/15
CPCC07C37/11C07C37/685C07C37/84C07C37/86C07C39/15
Inventor 彭维恩
Owner 甘肃泰升化工科技有限公司
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