Synthesis process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride
A technology of hexafluoroisopropenylene and dicarboxylic anhydride, which is applied in the field of synthesis technology of 4,4-diorthodicarboxylic anhydride, can solve the problems of unsuitable separation of products in the later stage, unsuitable separation of intermediate products, poor economic benefits, and the like, To achieve the effect of being conducive to product separation, improving life and applying times, and achieving 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
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[0022] A synthesis process of 4,4-(hexafluoroisopropenylene) diphthalic anhydride provided in the embodiment of the present invention comprises the following steps:
[0023] 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 butanol and butyl acetate; the mixed solvent of butanol 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.
[0024] Two, 2,2-bis(3-amino-4-hydroxyphenyl)hexafluoropropane is passed through ammonia gas in a fixed bed for ammonoly...
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The invention belongs to the technical field of synthesis of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride, in particular to a synthesis process of 4, 4-(hexafluoroisopropenyl) diphthalic anhydride. The synthesis process has the advantages of easy separation of intermediate products, high yield, less waste and good economic benefit, adopts a mixed solvent of long-chain alcohol and ester, reduces the solubility of the product, is beneficial to product separation, and has higher yield. Besides, the Pd / C catalyst is pretreated, a proper amount of sulfide is added for pretreatment, the sulfurpoisoning 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 addedin 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 synthesis 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 synthesis process of 4,4-(hexafluoroisopropenylene) diphthalic anhydride, which can solve the problems pointed out in the background technology. [0004] A kind of synthesis technique of 4,4-(hexafluoroisopropenylidene) diphthalic anhydride, comprising the following steps: ...
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IPC IPC(8): C07D307/89
CPCC07D307/89
Inventor 刘余峰张朋飞柴如行刘金燕
Owner 河北君瑞沣新材料有限公司