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Preparation method of bio-based self-repairing flame-retardant material with high dielectric property

A flame-retardant material and bio-based technology, applied in the field of polymer synthesis and functional application, can solve the problems of difficult secondary processing, poor dielectric properties, etc., and achieve the effects of stable quality, reduced pollution, and high product purity

Pending Publication Date: 2022-01-21
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

Aiming at the disadvantages of traditional epoxy resins such as easy microcracks, difficult secondary processing, poor dielectric properties and flammability, an additive-free bio-based self-healing system was synthesized by introducing disulfide bonds during the polymerization process. flame retardant material

Method used

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  • Preparation method of bio-based self-repairing flame-retardant material with high dielectric property
  • Preparation method of bio-based self-repairing flame-retardant material with high dielectric property
  • Preparation method of bio-based self-repairing flame-retardant material with high dielectric property

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preparation example Construction

[0032] A preparation method of a bio-based self-healing flame-retardant material with high dielectric properties and its products are mainly divided into three steps: first, the bio-based compound eugenol is used as the main raw material, and the bio-based polyester is synthesized by "click chemistry" Monomer: Add 2-4mol eugenol and 1mol polymercapto ester into a quartz glass cup with a sealed cover and magnetic stirring, use ultraviolet light as the reaction light source, heat up to 30-60°C, add catalyst, the amount of catalyst is 1% of the total mass 2-5%, after reacting for 6-12 hours, the bio-based polyester monomer is obtained after natural cooling.

[0033] The polyhydric mercapto ester is any one of bis(3-mercaptopropionate) ethylene glycol, trimethylolpropane tris(3-mercaptopropionate) and tetrakis(3-mercaptopropionate) pentaerythritol ester. All were purchased from Shanghai Macklin Biochemical Technology Co., Ltd.

[0034] The catalyst is photoinitiator-184 or photoi...

Embodiment 1

[0045] Add 2 mol eugenol and 1 mol bis(3-mercaptopropionate) ethylene glycol ester into a quartz glass cup with a sealed cover and magnetic stirring, use ultraviolet light as the reaction light source, heat up to 30°C, add photoinitiator-184, The amount of the catalyst used was 2% of the total mass. After reacting for 12 hours, the eugenol-based polyester monomer (EU-EGMP) was obtained after natural cooling. Under a nitrogen gas atmosphere, add 1mol EU-EGMP and 6mol epichlorohydrin to a three-necked flask equipped with a reflux condenser, magnetic stirring and a thermometer, raise the temperature to 120°C, add 0.01mol benzyltriethylammonium chloride, and condense Reflux reaction for 30 minutes, after cooling down to 40°C, add 2mol sodium hydroxide and 2mol calcium oxide, keep at 40°C and continue to react for 2 hours, after the reaction is completed, the reaction product is filtered, the filtrate is distilled under reduced pressure to recover excess epichlorohydrin, and the sol...

Embodiment 2

[0047] Add 3mol eugenol and 1mol trimethylolpropane tris(3-mercaptopropionate) into a quartz glass cup with a sealed cover and magnetic stirring, use ultraviolet light as the reaction light source, heat up to 40°C, add photoinitiator- 184, the amount of catalyst used was 3% of the total mass, and after reacting for 10 hours, eugenol-based polyester monomer (EU-TTMP) was prepared after natural cooling. Under a nitrogen gas atmosphere, add 1 mol of eugenyl polyester and 8 mol of epichlorohydrin to a three-necked flask equipped with a reflux condenser, magnetic stirring and a thermometer, raise the temperature to 110°C, and add 0.05 mol of tetradecyl trimethyl Ammonium chloride, condensed and refluxed for 3 hours, cooled to 50°C, added 3mol sodium hydroxide and 3mol anhydrous sodium sulfate, kept at 50°C and continued to react for 3 hours, after the reaction was completed, the reaction product was filtered, and the filtrate was recovered by vacuum distillation Epoxidized eugenol-...

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Abstract

The invention discloses a preparation method of a bio-based self-repairing flame-retardant material with high dielectric property and a product thereof. The bio-based self-repairing flame-retardant material with high dielectric property is synthesized by taking eugenol, multi-sulfydryl ester and disulfide bond-containing amine as main raw materials and sequentially adopting click chemistry, epoxidation and melt polymerization methods. The main raw materials are wide in source, renewable and independent of petroleum; the preparation process is simple and reasonable and low in energy consumption; the product has good thermal stability, can be recycled, and is easy to degrade and recover. Test results show that the self-repairing self-flame-retardant epoxy resin prepared by the invention has a 100% repairing effect (160DEG C) and excellent dielectric properties and flame retardancy.

Description

technical field [0001] The invention relates to a development and preparation technology of a bio-based self-repairing material, specifically relates to a preparation method of a bio-based self-repairing flame-retardant material with high dielectric properties, and belongs to the technical field of polymer synthesis and functional application. Background technique [0002] The use of renewable resources instead of traditional non-renewable petrochemical resources as raw materials to prepare polymer materials has gradually become a research hotspot. Thermosetting epoxy resin is an important polymer material that is widely used in adhesives, coatings, molded plastics, composite materials, etc. due to its excellent bonding properties, heat / chemical resistance, insulation, mechanical strength, etc. field. However, due to its unique three-dimensional network structure during molding and use, epoxy resin can hardly undergo secondary processing, cannot be recycled after the end of...

Claims

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Application Information

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IPC IPC(8): C08G59/06C08G59/66
CPCC08G59/063C08G59/66
Inventor 聂小安李文斌陈洁王义刚
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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