Degradable and thermoplastically processable epoxy thermosetting resin and preparation method thereof

A thermoplastic processing and thermosetting technology, which is applied in the field of epoxy vitrimers and its preparation, can solve the problems of non-reversible properties, epoxy thermosetting resins cannot be thermoplastically processed, and high energy consumption for carbon fiber recycling.

Inactive Publication Date: 2020-04-28
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The cleavable covalent bonds in existing degradable epoxy resins are mainly esters of different substituents (such as: sulfonate, sulfite, carbonate, phosphate) or acetal structure, etc., and the degradation temperature is generally at 140 Above ℃, so the energy consumption of carbon fiber recycling is high
Since the above-mentioned covalent bonds do not have reversible properties, the prepared epoxy thermosetting resins are also not thermoplastically processable

Method used

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  • Degradable and thermoplastically processable epoxy thermosetting resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) Mix 10 parts by weight of vanillin, 10 parts by weight of sodium borohydride or sodium cyanoborohydride and 100 parts by weight of methanol, and react at room temperature for 2 hours. After confirming that the reaction is complete by thin layer chromatography, use 10 After quenching the reaction with 1 mol / L sodium hydrosulfide aqueous solution in parts by weight, the reaction solution was concentrated and then added with ethyl acetate to extract the product, the organic phase was retained by liquid separation, and the organic phase was collected after drying with anhydrous sodium sulfate, and obtained by rotary evaporation Product I.

[0030] (2) Add 10 parts by weight of product I to 100 parts by weight of xylene, then add 10 parts by weight of modified monomer II tert-butyl acetoacetate, heat to 130°C for 5 hours, and remove xylene by vacuum distillation. Separated by column chromatography, the eluent is ethyl acetate / petroleum ether or dichloromethane / ethyl acet...

Embodiment 2

[0037] (1) After mixing 10 parts by weight of p-hydroxybenzaldehyde, 10 parts by weight of sodium borohydride or sodium cyanoborohydride and 100 parts by weight of methanol, react at room temperature for 2 hours, and confirm that the reaction is complete by thin layer chromatography, After quenching the reaction with 10 parts by weight of 1 mol / L sodium hydrogen sulfide aqueous solution, the reaction solution was concentrated and then added to extract the product with ethyl acetate, the organic phase was retained by liquid separation, and the organic phase was collected after drying with anhydrous sodium sulfate. Evaporation affords product I.

[0038] (2) Add 10 parts by weight of product I to 100 parts by weight of xylene, then add 10 parts by weight of modified monomer II tert-butyl acetoacetate, heat to 130°C for 5 hours, and remove xylene by vacuum distillation. Separated by column chromatography, the eluent is ethyl acetate / petroleum ether or dichloromethane / ethyl acetat...

Embodiment 3

[0045] (1) Mix 10 parts by weight of vanillin, 10 parts by weight of sodium borohydride or sodium cyanoborohydride and 100 parts by weight of methanol, and react at room temperature for 2 hours. After confirming that the reaction is complete by thin layer chromatography, use 10 After quenching the reaction with 1 mol / L sodium hydrosulfide aqueous solution in parts by weight, the reaction solution was concentrated and then added with ethyl acetate to extract the product, the organic phase was retained by liquid separation, and the organic phase was collected after drying with anhydrous sodium sulfate, and obtained by rotary evaporation Product I.

[0046] (2) Add 10 parts by weight of product I to 100 parts by weight of xylene, then add 10 parts by weight of modified monomer II ethyl acetoacetate, heat to 130°C for 5 hours, remove xylene by vacuum distillation, and use Separation by column chromatography, the eluent is ethyl acetate / petroleum ether or dichloromethane / ethyl acet...

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Abstract

The invention discloses degradable and thermoplastically processable epoxy vitrimers and a preparation method thereof, and belongs to the technical field of new material synthesis. The preparation method comprises the following steps: mixing an epoxy monomer with a beta-diketone structure with an amine curing agent in proportion, stirring the mixture, pouring the mixture into a mold, and heating the mixture until the curing is complete. The epoxy vitrimers obtained by the invention can be degraded in an acidic solution at the temperature of below 80 DEG C for 24 hours after being cured, and have a thermoplastic processing function; after being damaged, the epoxy resin can be self-repaired through hot pressing (10MPa, 10min) at 130-180 DEG C. The preparation process is simple, and the epoxyresin is expected to be used in the fields of recovery of reinforced fibers in epoxy composite materials, degradable or self-repairing epoxy coatings, degradable epoxy adhesives and the like.

Description

technical field [0001] The invention belongs to the technical field of material synthesis, in particular to a degradable and thermoplastically processable epoxy vitrimers and a preparation method thereof. Background technique [0002] Epoxy resin is widely used in transportation, aerospace, electronic appliances, coating anticorrosion and other fields, and is currently the most widely used thermosetting resin. Since the epoxy resin is cured to form a three-dimensional cross-linked network, the cured epoxy resin is insoluble and difficult to degrade. The increasingly frequent replacement of electronic devices has resulted in the generation of a large amount of electronic waste, and the environmental protection problem has become increasingly severe; the amount of carbon fiber / epoxy composite materials is huge, but the difficulty in recycling high-performance and high-value-added carbon fibers in composite material waste needs to be solved urgently. The research and developme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/20
CPCC08G59/20
Inventor 江献财陈凯胡沤东侯琳熙
Owner FUZHOU UNIV
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