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Synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride

A technology of hexafluoroisopropenylene and diformic anhydride, which is applied in the field of synthesis of 4,4-diphthalic anhydride, can solve problems such as unfavorable separation of later products, unsuitable separation of intermediate products, and poor economic benefits. It is beneficial to the separation of products, improves the service life and application times, and has 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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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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  • Synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
  • Synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride

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Embodiment

[0021] A kind of synthetic method 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, Reduction solvent is the mixed solvent of isobutanol and butyl acetate; Adopt the mixed solvent of isobutanol and butyl acetate, reduce the solubility of product, be conducive to product separation, yield is higher, in addition, add Pd / C catalyst, Pretreatment of Pd / C catalyst with appropriate sulfide can improve the catalyst’s ability to resist sulfur poisoning, improve catalyst life and application times, because the nitro compound contains a small amount of sulfuric acid and other sulfide, which can easily poison the catalyst.

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

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Abstract

The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a synthesis method of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The synthesis method has the advantages of easy separation of intermediate products, high yield, less waste and good economic benefit, and a mixed solvent of isobutanol and butyl acetate is adoptedto reduce the solubility of the product, facilitate the separation of the product and increase the 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 canbe 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 synthesizing 4,4-(hexafluoroisopropenylene) diphthalic anhydride, in particular to a synthesis method 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 synthesis method of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, which can solve the problems pointed out in the background technology. [0004] A kind of synthetic method of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, comprising the following steps: [0005] 1. Using ...

Claims

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Application Information

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