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Preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride

A technology of hexafluoroisopropenylene and dicarboxylic acid anhydride, which is applied in the field of 4,4-diorthodicarboxylic acid anhydride synthesis, can solve the problems of unsuitable separation of intermediate products, unsuitable separation of later products, poor economic benefits, etc. Conducive to product separation, improved life and application times, and good economic benefits

Pending Publication Date: 2020-08-28
河北君瑞沣新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] In the original process, the intermediate product should not be separated. For example, the general reducing solvents are methanol, ethanol, ethyl acetate, etc., because these solvents have a high solubility to the product, and the amino compound has heat sensitivity, so it is not suitable for the separation of the later product. Yield Low, more waste, bad economic benefits

Method used

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  • Preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
  • Preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride

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Embodiment

[0021] The preparation process of a kind of 4,4-(hexafluoroisopropenylene) diphthalic anhydride provided by the embodiment of the present invention comprises the following steps:

[0022] 1. Using 2,2-bis(3-nitro-4-hydroxyphenyl)hexafluoropropane as raw material, obtain 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane through reduction reaction, The reduction solvent is a mixed solvent of amyl alcohol and butyl acetate; the mixed solvent of amyl alcohol and butyl acetate is used to reduce the solubility of the product, which is beneficial to product separation and has a higher yield. Pretreatment of the Pd / C catalyst with sulfides can improve the catalyst’s ability to resist sulfur poisoning, improve the life of the catalyst and the number of applications, because the nitro compounds contain a small amount of sulfuric acid and other sulfides, which can easily poison the catalyst.

[0023] Two, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is passed through ammonia gas in ...

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Abstract

The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a preparation process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The preparation process has the advantages of easy separation of intermediate products, high yield, fewer wastes and favorable economic benefit, and adopts a mixed solvent of amyl alcohol and butyl acetate to lower the solubility of the product, thereby being beneficial to product separation and higher yield. Besides, the Pd / C catalyst is pretreated, a proper amount of sulfide is added for pretreatment, the sulfur poisoning resistance of the catalyst is improved, the service life of the catalyst is prolonged, and the application frequency of the catalyst is increased; because nitro compounds contain trace amount of sulfides such as sulfuric acid and like, catalyst is easily poisoned. In the step 2, an alumina-silica gel catalyst is added so that 2, 2-bis (3-amino-4-hydroxyphenyl) molecules can be adsorbed on the surface of the catalyst in a flat shape, hydroxyl is closer to the surface of the catalyst, and the amination reaction of hydroxyl is facilitated; in the step 4, a small amount of urea is added in the cyanolysis reaction to prevent diazonium salt from being oxidized, becoming tar and other side reactions.

Description

technical field [0001] The invention belongs to the technical field of synthesis of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, and in particular relates to a preparation process of 4,4-(hexafluoroisopropenylene) diphthalic anhydride. Background technique [0002] In the original process, the intermediate product should not be separated. For example, the general reducing solvents are methanol, ethanol, ethyl acetate, etc., because these solvents have a high solubility to the product, and the amino compound has heat sensitivity, so it is not suitable for the separation of the later product. Yield Lower, more waste, bad economic benefits. Contents of the invention [0003] The invention provides a preparation process of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, which can solve the problems pointed out in the background technology. [0004] A kind of preparation technology of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, comprises the following ste...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 柴如行刘余峰张朋飞刘金燕
Owner 河北君瑞沣新材料有限公司