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Self-setting epoxy resin containing acid anhydride radicals and preparation method thereof

An epoxy resin, self-curing technology, applied in the direction of organic chemistry, can solve the problem of inability to form thermosetting cross-linked polymers, achieve high modulus and strength, and easy to use

Inactive Publication Date: 2014-05-28
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since these compounds contain only one epoxy group and one other active reactive group, they can only form linear polymers after thermal curing, and cannot form thermosetting cross-linked polymers.

Method used

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  • Self-setting epoxy resin containing acid anhydride radicals and preparation method thereof
  • Self-setting epoxy resin containing acid anhydride radicals and preparation method thereof
  • Self-setting epoxy resin containing acid anhydride radicals and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1 mole of α-caryoic acid and 6 moles of epichlorohydrin into a three-necked flask equipped with a thermometer and a reflux condenser, and raise the temperature to 117° C. for 2 hours. Cool to 20°C, add 1 mole of solid sodium hydroxide and 0.001 mole of benzyltriethylammonium chloride, and stir for 12 hours. Filtrate and recover excess epichlorohydrin to obtain α-glycidyl chertate. 1 mole of α-glycidyl cartonate was reacted with 1 mole of maleic anhydride at 90°C for 2 hours to obtain a self-curing epoxy resin containing anhydride groups.

[0022] 100 grams of self-curing epoxy resin containing anhydride groups obtained in Example 1 and 0.1 grams of 2-ethyl-4-methylimidazole catalyst are mixed, injected into the V type mold designed according to ASTM D638, at 120 ° C Curing was performed for 2 hours, followed by post-curing at 160° C. for 4 hours. After demoulding, 5 parallel specimens were obtained, and tensile tests were performed on the specimens according to AS...

Embodiment 2

[0026] Add 1 mole of α-carnitic acid and 6 moles of epichlorohydrin into a three-neck flask equipped with a thermometer and a reflux condenser, and raise the temperature to 100° C. for 6 hours. Cool to 60°C, add 1 mole of solid sodium hydroxide and 0.001 mole of benzyltriethylammonium chloride, and stir for 6 hours. Filtrate and recover excess epichlorohydrin to obtain α-glycidyl chertate. 1 mole of α-glycidyl chertate was reacted with 1 mole of maleic anhydride at 110° C. for 0.5 hour to obtain a self-curing epoxy resin containing anhydride groups.

Embodiment 3

[0028] Add 1 mole of dehydrated ricinoleic acid and 6 moles of epichlorohydrin into a three-necked flask equipped with a thermometer and a reflux condenser, and raise the temperature to 117° C. for 2 hours. Cool to 20°C, add 1 mole of solid sodium hydroxide and 0.001 mole of benzyltriethylammonium chloride, and stir for 12 hours. Filtrate, recover excess epichlorohydrin to obtain dehydrated castor oil glycidyl ester. 1 mole of dehydrated castor oil glycidyl ester was reacted with 1 mole of maleic anhydride at 90°C for 2 hours to obtain a self-curing epoxy resin containing acid anhydride groups.

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Abstract

The invention relates to self-setting epoxy resin containing acid anhydride radicals and a preparation method thereof. The preparation method comprises the following steps: reacting 1 mol of unitary fatty acid containing conjugated double bonds with 6-10 mol of epoxy chloropropane in a proportion at a temperature of 100-120 DEG C for 2-6 h, cooling to a temperature of 20-60 DEG C, then adding 1 mol of solid sodium hydroxide and 0.001 mol of a phase transfer catalyst for a ring-closure reaction for 6-12 h, filtering and recycling excess epoxy chloropropane so as to obtain conjugated fatty acid glycidyl ester; enable 1 mol of the conjugated fatty acid glycidyl ester and 1 mol of maleic anhydride to perform a Diels-Alder diene addition reaction for 0.5-2 h at 90-110 DEG C so as to obtain the self-setting epoxy resin containing the acid anhydride radicals. Compared with a linear polymer formed in the prior art, the self-setting epoxy resin provided by the invention has mechanical properties of a thermosetting cross-linked polymer, and has higher modulus and strength after setting.

Description

technical field [0001] The invention relates to a preparation method of epoxy resin, in particular to a self-curing epoxy resin containing both epoxy groups and acid anhydride groups and a preparation method thereof. Background technique [0002] Epoxy resin is one of the most important thermosetting resins. The application of epoxy resin generally requires two components: epoxy resin and curing agent. After the epoxy resin and the curing agent are mixed, they can cross-link each other through different chemical reactions to form a high-strength thermosetting cured product. The types of curing agents mainly include amines, acid anhydrides and latent curing agents. During the mixing process of epoxy resin and curing agent, due to uneven mixing or air bubbles, there will be some defects in the formed cured product, and these defects are the weak points of the material, which directly lead to the failure of the material. Premature failure under stress. In addition, some epo...

Claims

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Application Information

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IPC IPC(8): C07D407/12C08G59/24
CPCC07D407/12C08G59/20C08G59/4238
Inventor 黄坤夏建陵李守海李梅张燕杨小华陈瑶
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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