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5-methyol resorcinol diglycidyl ether and preparation method thereof

A technology of hydroxymethyl resorcinol and diglycidyl ether, which is applied in the field of glyceryl ether and its preparation, can solve problems such as poor bonding strength, and achieve the effects of mild reaction conditions, high yield and purity

Active Publication Date: 2019-03-22
INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention aims to solve the problem that the existing glycidyl ether epoxy resin has poor bonding strength at high temperature, and provides 5-hydroxymethyl resorcinol diglycidyl ether and its preparation method

Method used

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  • 5-methyol resorcinol diglycidyl ether and preparation method thereof
  • 5-methyol resorcinol diglycidyl ether and preparation method thereof
  • 5-methyol resorcinol diglycidyl ether and preparation method thereof

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specific Embodiment approach 1

[0030] Specific embodiment one: the molecular structural formula of the present embodiment 5-hydroxymethyl resorcinol diglycidyl ether is:

[0031]

specific Embodiment approach 2

[0032] Specific embodiment two: the preparation method of 5-hydroxymethyl resorcinol diglycidyl ether comprises the following steps:

[0033] 1. Add 5-formyl resorcinol diglycidyl ether and organic solvent in a mass ratio of 1: (10~20) into a fully dry reaction kettle, and stir at a low temperature of -15°C~0°C for 0.5h~ 2h, and nitrogen protection;

[0034] 2. Add catalyst solid powder in batches, add once every 30min, and add in 4 times in total; after adding, continue to react at -15℃~0℃ for 2h~8h, then raise the temperature to 25℃~50℃ for 0.5h~ 4h; wherein the number of moles of catalyst solid powder is 1.1 to 1.5 times the number of moles of 5-formyl resorcinol diglycidyl ether;

[0035] 3. After the reaction, add water and stir for 30-40 minutes, add toluene to extract and separate the organic phase, and distill under reduced pressure to remove the organic solvent, then recycle and reuse to obtain 5-hydroxymethyl resorcinol diglycidyl ether.

specific Embodiment approach 3

[0036] Specific embodiment three: the difference between this embodiment and specific embodiment two is: the preparation method of 5-formyl resorcinol diglycidyl ether in step one, specifically:

[0037] 1. Put 3,5-dihydroxybenzaldehyde, epibromohydrin and catalyst into the reaction kettle, raise the temperature to 80℃~100℃, stir for 2h~8h, then raise the temperature to the reflux temperature to remove the excess epoxybromopropane Evaporate under reduced pressure, recover and recycle to obtain a concentrated solution; wherein the molar ratio of 3,5-dihydroxybenzaldehyde and epibromohydrin is 1: (6-20), the ratio of 3,5-dihydroxybenzaldehyde and catalyst The mass ratio is 100: (0.1~5);

[0038] 2. After the temperature of the concentrated solution is cooled to 40°C to 60°C, add organic solvent and metal alkali solid particles, and continue to stir for 2h to 6h; wherein the mass ratio of 3,5-dihydroxybenzaldehyde to organic solvent is 1:(10 ~25), the molar ratio of 3,5-dihydrox...

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Abstract

The invention discloses 5-methyol resorcinol diglycidyl ether and a preparation method thereof, relates to glycidyl ether and a preparation method thereof and aims at solving the problem of poorer bonding strength of the conventional glycidyl ether epoxy resin at high temperature. The preparation method of the 5-methyol resorcinol diglycidyl ether comprises the following steps: firstly, adding 5-aldehyde resorcinol diglycidyl ether and an organic solvent into an intensive drying reactor, stirring and introducing nitrogen for protection; secondly, adding catalyst solid powder by stages for reaction; thirdly, after the reaction ends, adding water for stirring, adding methylbenzene for extracting to separate an organic phase, removing the organic solvent by reduced pressure distillation, andrecycling, thus obtaining the 5-methyol resorcinol diglycidyl ether. The 5-methyol resorcinol diglycidyl ether is used for preparing a high temperature resisting epoxy resin adhesive. The epoxy resinadhesive prepared from the 5-methyol resorcinol diglycidyl ether disclosed by the invention has the characteristic of high temperature resistance. The 5-methyol resorcinol diglycidyl ether and the preparation method thereof disclosed by the invention are used for the field of the epoxy resin adhesives.

Description

technical field [0001] The invention relates to a glycerol ether and a preparation method thereof. Background technique [0002] Epoxy resin refers to a compound containing two or more epoxy groups in its molecular structure. It not only has excellent bonding properties, mechanical properties and corrosion resistance, but also has low curing shrinkage and dielectric loss, and can be widely used in various fields such as coatings, adhesives and composite materials. Although my country's epoxy resin production capacity has grown rapidly, most of them are low-end products, and special products with high added value are very scarce. [0003] Traditional glycidyl ether epoxy resin has excellent mechanical properties and processing properties, and is widely used in aerospace and other fields. However, this type of resin generally requires a higher curing temperature and post-treatment temperature. Such high-temperature treatment conditions will generate greater internal stress, ...

Claims

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Application Information

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IPC IPC(8): C07D303/30C07D301/02C09J163/00C08G59/24
CPCC09J163/00C07D301/02C07D303/30C08G59/245Y02P20/584
Inventor 张斌刘彩召孙明明李栓张绪刚李坚辉王磊薛刚赵明宋彩雨史利利李奇力梅格
Owner INST OF PETROCHEM HEILONGJIANG ACADEMY OF SCI
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