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Recyclable eugenol-based 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 and other directions, can solve problems such as difficult recycling and reuse, and achieves narrow molecular weight distribution, mild preparation conditions and high product purity. Effect

Active Publication Date: 2021-07-09
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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  • Recyclable eugenol-based epoxy resin Vitrimer material and preparation method thereof
  • Recyclable eugenol-based epoxy resin Vitrimer material and preparation method thereof
  • Recyclable eugenol-based epoxy resin Vitrimer material and preparation method thereof

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preparation example Construction

[0034] The preparation of step 1, eugenol base epoxy resin:

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

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

[0037]By mass, 40-100 parts of eugenol-based epoxy resin, 20-50 parts of dicarboxylic acid without dynamic disulfide bond, 20-50 parts of 4,4'-dithiodibutyric acid and 0.1- 0.5 parts of the transesterification accelerator are mixed evenly at a temperature of 60-65°C, then poured into a self-made dumbbell-shaped mold and u...

Embodiment 1

[0041] Step 1: Preparation of eugenol-based epoxy resin

[0042] In the reactor, by mass, add 50 parts of allylated eugenol, 150 parts of m-chloroperoxybenzoic acid and 600 parts of acetone, and then stir at a speed of 200 rpm, and carry out cyclone at a temperature of 25 ° C. Oxidation reaction 16h. After the reaction is finished, add saturated sodium bicarbonate solution to wash 2-3 times, and saturated sodium sulfite to wash 1-2 times, then dry through anhydrous magnesium sulfate, filter and rotary evaporate to obtain the target product eugenol-based epoxy resin. The rate is 95.2%.

[0043] Step 2: Preparation of eugenol-based epoxy resin 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-triazepine Cyclo[4.4.0]dec-5-ene was first mixed uniformly at a temperature of 65°C, then poured into a self-made dumbbell-shaped mold and used ...

Embodiment 2

[0046] Step 1: Preparation of eugenol-based epoxy resin

[0047] In the reactor, by mass, add 50 parts of allylated eugenol, 150 parts of m-chloroperoxybenzoic acid and 600 parts of acetone, and then stir at a speed of 200 rpm, and carry out cyclone at a temperature of 25 ° C. Oxidation reaction 16h. After the reaction is finished, add saturated sodium bicarbonate solution to wash 2-3 times, and saturated sodium sulfite to wash 1-2 times, then dry through anhydrous magnesium sulfate, filter and rotary evaporate to obtain the target product eugenol-based epoxy resin. The rate is 95.2%.

[0048] Step 2: Preparation of eugenol-based epoxy resin 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-triazepine Cyclo[4.4.0]dec-5-ene was first mixed uniformly at a temperature of 65°C, then poured into a self-made dumbbell-shaped mold and used ...

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Abstract

The invention relates to a recyclable eugenol-based epoxy resin Vitrimer material and a preparation method of the recyclable eugenol-based epoxy resin Vitrimer material. Biomass-based eugenol is used as a raw material, an eugenol-based epoxy resin matrix similar to DGEBA is prepared through a two-step method including an allyl bromide substitution reaction and a m-chloroperoxybenzoic acid oxidation reaction, then the eugenol-based epoxy resin matrix is mixed with a dicarboxylic acid curing agent system containing and not containing dynamic bonds, curing is conducted in a gradient heating mode, and theeugenol-based epoxy resin Vitrimer material with a dynamic reversible exchange key anddisulfide bond is otained. The epoxy resin Vitrimer material has the advantages of high physical remodeling reprocessability, high chemical recovery efficiency and the like, and overcomes the defects that the traditional epoxy resin takes petrochemical resources as raw materials and is difficult to recycle after being used; and green development and sustainable utilization of the thermosetting polymer material are promoted.

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 vitrimer material with reversible transesterification bonds and disulfide bonds and its preparation. Background technique [0002] Epoxy resin is a common thermosetting polymer material. With its excellent performance, it is widely used in transportation, machinery, petrochemical and construction fields, which brings great convenience to human life. At present, the most widely used epoxy resin on the market is mainly bisphenol A diglycidyl ether type epoxy resin, which is mainly composed of petroleum-based bisphenol A and epichlorohydrin under the action of an alkaline catalyst. Polycondensation, while bisphenol A is mainly synthesized from acetone and phenol. The extensive use of this type of petroleum-based epoxy resin not only intensifies the consumption of non-renewable petroleum resources, but also the ra...

Claims

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Application Information

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Patent Type & Authority Applications(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
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