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Ditert-butyl and diether linkage structure-containing aromatic dibasic acid and preparation method thereof and application thereof

An aromatic type, dibasic acid technology, applied in the direction of nitrile preparation, organic chemistry, etc., can solve the problems that affect the application range, difficult to dissolve, difficult to process and shape, and achieve the effect of wide application prospects

Inactive Publication Date: 2010-01-13
杨金田
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The key problem is that the aromatic PBI polymer made from general aromatic dibasic acid is difficult to melt and dissolve, difficult to process and shape, which seriously affects the further expansion of its application range

Method used

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  • Ditert-butyl and diether linkage structure-containing aromatic dibasic acid and preparation method thereof and application thereof
  • Ditert-butyl and diether linkage structure-containing aromatic dibasic acid and preparation method thereof and application thereof
  • Ditert-butyl and diether linkage structure-containing aromatic dibasic acid and preparation method thereof and application thereof

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Embodiment 1

[0025] The preparation steps of an aromatic dibasic acid containing 2 tert-butyl groups and 2 ether bond structures are as follows:

[0026] Step 1: Synthesis of intermediate 2,5-di-tert-butyl-1,4-bis(p-benzonitrileoxy)benzene. Add 12.62g of 4-fluorobenzonitrile, 11.12g of 2,5-di-tert-butylhydroquinone, 100mL of DMF, 40mL of xylene, and 13.85g of anhydrous potassium carbonate into a 250mL three- In the neck bottle, stir with magnetic force, heat the oil bath to 160°C for reaction, the formed water and xylene azeotrope, enter the water separator to separate. As the reaction proceeds, the color of the material gradually deepens, and finally turns dark brown. Then the temperature was raised to 175° C., the xylene was distilled off, and the reaction was carried out at constant temperature for 4 hours. Let it cool, pour the material into cold water under vigorous stirring, and precipitate a brown precipitate. Filtration and repeated washing with deionized water gave a yellow cru...

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Abstract

The invention discloses ditert-butyl and diether linkage structure-containing aromatic dibasic acid and a preparation method thereof and application thereof. The preparation method comprises the following steps of: (1) under the temperature of 167-170 DEG C, taking dimethyl fomamide (DMF) and dimethylbenzene as solvent, taking anhydrous potassium carbonate as alkalescence agent, subjecting 4-fluorobenzonitrile to a nucleophilic substitution reaction with 2, 5-ditert-butylhydroquinone for about 4 hours; depositing, filtering, crystallizing and drying to obtain white crystalloid 2, 5-ditert-1, 4-di (p-oxybenzonitrile) benzene; (2) under the temperature of 150 DEG C, taking diethylene glycol ether as solvent, hydrolytically reacting the 2, 5-ditert-1, 4-di (p-oxybenzonitrile) benzene prepared by (1) in hyperbasophilic KOH solution for about 15 hours to generate the 2, 5-ditert-1, 4-di (p-oxybenzonitrile) benzene; and acidifying, depositing, vacuum filtrating, crystallizing and drying to obtain a product. The composite compound 2, 5-ditert-1, 4-di (p-oxybenzonitrile) benzene can be used as raw material for synthesizing soluble polybenzimidazole resin and has wide application prospect.

Description

technical field [0001] The invention relates to an aromatic dibasic acid containing two tert-butyl groups and two ether bond structures, a preparation method and application thereof. Background technique [0002] Aromatic dibasic acids are essential raw materials for the preparation of polybenzimidazole (PBI) polymers, and polybenzimidazole is one of the most high-grade engineering thermoplastics today, and is considered to be a new generation of high-strength, high-modulus, durable A typical representative of high-temperature polymer materials, widely used in radome, fairing and empennage of supersonic aircraft, spacecraft radiation-resistant materials, ablation-resistant coatings, printed circuit boards, electrical insulation materials, incandescent or fluorescent lamp high temperature High-tech fields such as contacts, FPC substrates for electronic and microelectronic instruments, gas separation membranes, reverse osmosis membranes, proton exchange membranes, and fuel cel...

Claims

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Application Information

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IPC IPC(8): C07C65/24C07C51/08C08G73/18
Inventor 杨金田程海星黄卫
Owner 杨金田
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