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Method for preparing methylcyclohexene tetracarboxylic dianhydride

A technology of methylcyclohexene tetra-acid dianhydride and methyl tetrahydrophthalic anhydride, which is applied in the field of preparing methylcyclohexene tetra-acid dianhydride, can solve the problems of complexity and low yield of the synthesis method, and achieve simple operation, The effect of high product yield

Inactive Publication Date: 2022-02-25
ZHEJIANG ALPHARM CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

As one of the tetracarboxylic dianhydride compounds, methylcyclohexene tetra-acid dianhydride, the existing synthesis method has low yield and is relatively complicated.

Method used

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Examples

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Embodiment 1

[0020] A method for preparing methylcyclohexene tetrahydrophthalic anhydride, comprising the steps of: putting maleic anhydride and 3-methyltetrahydrophthalic anhydride into a reactor, the molar ratio of maleic anhydride and 3-methyltetrahydrophthalic anhydride being 1 : 1, raised to 170 ° C, after 10 hours of heat preservation reaction, distilled off the unreacted raw materials, added a solvent for recrystallization, and obtained the product of methylcyclohexene tetra-acid dianhydride.

Embodiment 2

[0022] A method for preparing methylcyclohexene tetrahydrodianhydride, comprising the steps of: putting maleic anhydride, 3-methyltetrahydrophthalic anhydride, 2,6-di-tert-butyl-4-methylphenol and xylene solvent into In the reaction kettle, the molar ratio of maleic anhydride and 3-methyltetrahydrophthalic anhydride is 4:1, and the amount of xylene is 5 times the total weight of maleic anhydride and 3-methyltetrahydrophthalic anhydride. Under nitrogen protection, it rises to 160 ℃, heat preservation reaction for 2 hours, evaporate unreacted raw materials, add acetone solvent for recrystallization, and obtain methylcyclohexene tetra-acid dianhydride product.

Embodiment 3

[0024] A method for preparing methylcyclohexene tetra-acid dianhydride, comprising the steps of: putting maleic anhydride, 3-methyltetrahydrophthalic anhydride, p-tert-butyl catechol and xylene solvent into the reactor, maleic anhydride and 3 - The molar ratio of methyltetrahydrophthalic anhydride is 3:1, p-tert-butyl catechol is 2.5% of the total weight of maleic anhydride and 3-methyltetrahydrophthalic anhydride, and the amount of xylene is maleic anhydride and 3-methyltetrahydrophthalic anhydride 3 times the total weight of phthalic anhydride, under the protection of nitrogen, rise to 220 ° C, keep warm for 7 hours, evaporate unreacted raw materials, add 4-methyl-2-pentanone solvent to recrystallize, and obtain methylcyclohexene Tetraacid dianhydride products.

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Abstract

The invention relates to the technical field of anhydride synthesis, in particular to a method for preparing methylcyclohexene tetracarboxylic dianhydride. The invention provides the method for preparing methylcyclohexene tetracarboxylic dianhydride, the method comprises the following steps: adding maleic anhydride and 3-methyltetrahydrophthalic anhydride into a reaction kettle, heating to a reaction temperature, carrying out heat preservation reaction, evaporating to remove unreacted raw materials, adding a solvent, and recrystallizing to obtain the methylcyclohexene tetracid dianhydride product. The method for preparing methylcyclohexene tetracarboxylic dianhydride is easy to operate, high in final product yield, less in generated waste residue, recyclable in raw material, reusable in solvent, economical and environment-friendly, and the reaction yield can reach more than 50%.

Description

[0001] This application is a divisional application with an application date of December 27, 2018, an application number of 201811608962.X, and an invention title of "A Method for Preparing Methylcyclohexene Tetradianhydride". technical field [0002] The invention relates to the technical field of acid anhydride synthesis, in particular to a method for preparing methylcyclohexene tetra-acid dianhydride. Background technique [0003] Tetracarboxylic dianhydride series products can be used as raw materials for the manufacture of thermosetting polyimide resins, vinyl chloride polymer plasticizers and water-soluble polyesters, and its applications are very extensive and diverse. Wherein methylcyclohexene tetracarboxylic dianhydride (MCTC) is aliphatic tetracarboxylic dianhydride, has good solubility in various solvents, and its fusing point is lower than common aromatic tetracarboxylic dianhydride, and Epoxy resin has good heat resistance and electrical properties after curing....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D493/04
CPCC07D493/04
Inventor 沈纪达张骏
Owner ZHEJIANG ALPHARM CHEM TECH
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