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Industrial synthesis method of TMBP

A catalyst and solution technology, which is 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 improving industrial production capacity, high product purity, and reducing side reactions

Active Publication Date: 2019-08-09
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

[0032] A kind of TMBP industrial synthesis method, comprises the following steps:

[0033] (1) Dissolving 2,6-dimethylphenol, sodium lauryl sulfate, and borax with isopropanol to obtain a pre-solution for subsequent use;

[0034] (2) Add a certain amount of deionized water in the reaction kettle and then add the pre-solution, heat to a certain temperature and quickly add the catalyst, then close the reaction kettle, stir and feed oxygen, and continue to react for a certain period of time under a certain pressure;

[0035] (3) After the reaction is completed and the pressure is released to normal pressure, the white needle-like crystal product, namely TMBP, is obtained through cooling, filtering, washing, recrystallization, and drying; wherein, a reducing agent is added during the recrystallization process.

[0036] Wherein, the catalyst is copper acetate; the reducing agent is sodium dithionite, commonly known as hydrosulfite.

[0037] Wherein, according to molar mass ratio, ...

Embodiment 2

[0048] A kind of TMBP industrial synthesis method, comprises the following steps:

[0049] (1) Dissolving 2,6-dimethylphenol, sodium lauryl sulfate, and borax with isopropanol to obtain a pre-solution for subsequent use;

[0050] (2) Add a certain amount of deionized water in the reaction kettle and then add the pre-solution, heat to a certain temperature and quickly add the catalyst, then close the reaction kettle, stir and feed oxygen, and continue to react for a certain period of time under a certain pressure;

[0051] (3) After the reaction is completed and the pressure is released to normal pressure, the white needle-like crystal product, namely TMBP, is obtained through cooling, filtering, washing, recrystallization, and drying; wherein, a reducing agent is added during the recrystallization process.

[0052] Wherein, the catalyst is copper acetate; the reducing agent is sodium dithionite, commonly known as hydrosulfite.

[0053] Wherein, according to molar mass ratio, ...

Embodiment 3

[0064] A kind of TMBP industrial synthesis method, comprises the following steps:

[0065] (1) Dissolving 2,6-dimethylphenol, sodium lauryl sulfate, and borax with isopropanol to obtain a pre-solution for subsequent use;

[0066] (2) Add a certain amount of deionized water in the reaction kettle and then add the pre-solution, heat to a certain temperature and quickly add the catalyst, then close the reaction kettle, stir and feed oxygen, and continue to react for a certain period of time under a certain pressure;

[0067] (3) After the reaction is completed and the pressure is released to normal pressure, the white needle-like crystal product, namely TMBP, is obtained through cooling, filtering, washing, recrystallization, and drying; wherein, a reducing agent is added during the recrystallization process.

[0068] Wherein, the catalyst is copper acetate; the reducing agent is sodium dithionite, commonly known as hydrosulfite.

[0069] Wherein, according to molar mass ratio, ...

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Abstract

The invention relates to an industrial synthesis method of TMBP. The method comprises the following steps of 1, dissolving 2,6-xylenol, sodium dodecyl sulfate and borax with isopropanol to obtain a preliminary solution for use; 2, adding a certain amount of deionized water in a reaction kettle, then adding the preliminary solution, after heating the mixture to a certain temperature, quickly addinga catalyst, then keeping the reaction kettle hermetic, conducting stirring, introducing oxygen, and continuously carrying out a reaction under certain pressure for a period of time; 3, after the reaction is finished, relieving pressure to normal pressure, and then conducting cooling, filtering, washing, re-crystallization and drying to obtain a white needle crystal product, namely the TMBP, wherein a reducing agent is added in the re-crystallization process. According to the industrial synthesis method, the process condition of pressurizing is innovatively adopted, the side reactions under the pressurizing condition are greatly reduced under the synergistic effect of the process condition of pressurizing and selection of types of raw materials and adjustment of the process condition, andthrough the further utilization of a reduction means, double increase of the yield (larger than 85% as a whole) and purity (larger than 99.0%) of the TMBP is achieved.

Description

technical field [0001] The invention relates to the technical field of TMBP synthesis, in particular to a TMBP industrial synthesis method. Background technique [0002] 3,3',5,5'-Tetramethylbiphenyl-diol (3,5,3',5'-Tetramethyl-biphenyl-4,4'-diol, TMBP), is a typical liquid crystal polymer intermediate material. At the same time, because of its excellent heat resistance, it is also used as a modified monomer for many products such as polyester, polyurethane, polycarbonate, polysulfone, and epoxy resin; and because it is resistant to aging caused by oxygen and heat. It can also be used as rubber, latex anti-aging agent 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 a raw material of liquid crystal polymers has reached the stage of industrial use. [00...

Claims

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Application Information

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Patent Type & Authority Applications(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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