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A kind of recyclable eugenol base epoxy resin vitrimer material and preparation method thereof

A technology of eugenol-based epoxy resin and dithiodibutyric acid, which is applied in recycling technology, plastic recycling, etc., can solve problems such as difficult recycling, achieve narrow molecular weight distribution, mild preparation conditions, and high product purity Effect

Active Publication Date: 2022-06-03
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In order to solve the problem that the existing epoxy resin is mainly derived from non-renewable petrochemical resources, and it is difficult to recycle and reuse after cross-linking and curing, the present invention provides a recyclable eugenol-based epoxy resin with biomass resource eugenol as raw material The preparation method of epoxy resin Vitrimer material

Method used

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  • A kind of recyclable eugenol base epoxy resin vitrimer material and preparation method thereof
  • A kind of recyclable eugenol base epoxy resin vitrimer material and preparation method thereof
  • A kind of recyclable eugenol base epoxy resin vitrimer material and preparation method thereof

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preparation example Construction

[0034] Step 1, the preparation of eugenol-based epoxy resin:

[0035] In the reaction kettle, by mass, add 50 parts of allyl eugenol, 150-200 parts of m-chloroperoxybenzoic acid and 600-1000 parts of solvent, then stir at a rotating speed of 200-300 rpm while stirring at 20 The epoxidation reaction was carried out at a temperature of -25 °C for 16-40 h. After the reaction is completed, add saturated sodium bicarbonate solution to wash 2-3 times, saturated sodium sulfite for 1-2 times, then dry with anhydrous magnesium sulfate, filter and rotary steam to obtain the target product eugenol-based epoxy resin.

[0036] Step 2, the preparation of eugenol-based epoxy resin Vitrimer material:

[0037]By mass, 40-100 parts of eugenol-based epoxy resin, 20-50 parts of dicarboxylic acid without dynamic disulfide bonds, 20-50 parts of 4,4'-dithiodibutyric acid and 0.1- 0.5 part of transesterification accelerator is firstly mixed uniformly at a temperature of 60-65 ℃, then poured into a ...

Embodiment 1

[0041] Step 1: Preparation of Eugenol-Based Epoxy Resin

[0042] In the reaction kettle, by mass, add 50 parts of allyl eugenol, 150 parts of m-chloroperoxybenzoic acid and 600 parts of acetone, and then stir at a rotating speed of 200 rpm while carrying out cyclization at a temperature of 25 ° C. Oxidation reaction 16h. After the reaction is completed, add saturated sodium bicarbonate solution for washing 2-3 times, saturated sodium sulfite for washing 1-2 times, and then dry, filter and rotate through anhydrous magnesium sulfate to obtain the target product eugenol-based epoxy resin. The rate is 95.2%.

[0043] Step 2: Preparation of Eugenol-based Epoxy Vitrimer Material

[0044] By mass, 50 parts of eugenol-based epoxy resin, 10 parts of azelaic acid, 40 parts of 4,4'-dithiodibutyric acid and 0.3 parts of transesterification accelerator 1,5,7-triazadi Cyclo[4.4.0]dec-5-ene was first mixed uniformly at 65 °C, then poured into a self-made dumbbell-shaped mold and used a va...

Embodiment 2

[0046] Step 1: Preparation of Eugenol-Based Epoxy Resin

[0047] In the reaction kettle, by mass, add 50 parts of allyl eugenol, 150 parts of m-chloroperoxybenzoic acid and 600 parts of acetone, and then stir at a rotating speed of 200 rpm while carrying out cyclization at a temperature of 25 ° C. Oxidation reaction 16h. After the reaction is completed, add saturated sodium bicarbonate solution for washing 2-3 times, saturated sodium sulfite for washing 1-2 times, and then dry, filter and rotate through anhydrous magnesium sulfate to obtain the target product eugenol-based epoxy resin. The rate is 95.2%.

[0048] Step 2: Preparation of Eugenol-based Epoxy Vitrimer Material

[0049] By mass, 50 parts of eugenol-based epoxy resin, 20 parts of azelaic acid, 30 parts of 4,4'-dithiodibutyric acid and 0.3 parts of transesterification accelerator 1,5,7-triazadi Cyclo[4.4.0]dec-5-ene was first mixed uniformly at 65 °C, then poured into a self-made dumbbell-shaped mold and used a va...

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Abstract

The invention relates to a recyclable eugenol-based epoxy resin Vitrimer material and a preparation method thereof. Using biomass-based eugenol as raw material, a eugenol-based epoxy resin matrix similar to DGEBA was prepared through the two-step method of "allyl bromide substitution reaction" and "m-chloroperoxybenzoic acid oxidation reaction". Then it is mixed with the dicarboxylic acid curing agent system containing dynamic bonds and non-dynamic bonds, and then cured by gradient heating method to obtain recyclable eugenol groups with dynamic reversible transesterification bonds and disulfide bonds Epoxy resin Vitrimer material has the advantages of good physical remodeling and reprocessing and high chemical recycling efficiency. It solves the defect that traditional epoxy resins use petrochemical resources as raw materials and is difficult to recycle after use, and helps the green development and development of thermosetting polymer materials. sustainable use.

Description

technical field [0001] The invention belongs to the technical field of biomass-based epoxy resin Vitrimer materials, in particular to a recyclable eugenol-based epoxy resin Vitrimer material with reversible transesterification bonds and disulfide bonds and preparation thereof. Background technique [0002] Epoxy resin is a common thermosetting polymer material. It is widely used in transportation, machinery, petrochemical and construction fields due to its excellent properties, bringing great convenience to human life. At present, the most widely used epoxy resin in the market is mainly bisphenol A diglycidyl ether type epoxy resin, which is mainly composed of bisphenol A and epichlorohydrin derived from petroleum base under the action of alkaline catalyst. Polycondensation, while bisphenol A is mainly synthesized from acetone and phenol. The extensive use of such petroleum-based epoxy resins not only aggravates the consumption of non-renewable petroleum resources, but also...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G59/14
CPCC08G59/1438C08G59/1483Y02W30/62
Inventor 张跃宏纪拓吕斌翟梦姣马菲
Owner SHAANXI UNIV OF SCI & TECH