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Boron-nitrogen structured multi-aromatic-ring flame-retardant epoxy monomer as well as preparation method and application thereof

A technology of epoxy monomer and aromatic ring, which is applied in the field of flame-retardant epoxy resin with boron-nitrogen structure polyaromatic ring and its preparation, can solve the problems of poor flame retardancy, achieve improved flame retardancy, simple reaction process, and improved cross-fertilization The effect of link density

Inactive Publication Date: 2019-11-22
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The object of the present invention is to provide a kind of boron-nitrogen structure multi-aromatic ring flame-retardant epoxy monomer and its preparation method in order to solve the problems of poor flame retardancy of traditional epoxy resins. Simple and easy to implement, B and N flame retardant elements can significantly improve the flame retardant performance of epoxy resin, promote the charring of the material during combustion, and the aromatic structure on the epoxy monomer also helps to improve the thermal stability of the material

Method used

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  • Boron-nitrogen structured multi-aromatic-ring flame-retardant epoxy monomer as well as preparation method and application thereof
  • Boron-nitrogen structured multi-aromatic-ring flame-retardant epoxy monomer as well as preparation method and application thereof
  • Boron-nitrogen structured multi-aromatic-ring flame-retardant epoxy monomer as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) In a three-necked flask equipped with a nitrogen protection device, add 0.06mol 4-carboxyphenylboronic acid and 0.06mol thionyl chloride, stir at room temperature for 10min, raise the temperature to 60°C, and react for 10h. During the reaction, the reaction system is kept at in a nitrogen atmosphere. Thionyl chloride and the water produced by the reaction were distilled off under reduced pressure to obtain a white solid, which was dried in vacuum at 50°C for 3 hours to obtain a white powdery solid 4,4′,4″-(boroxine-2,4,6) - Tribenzoyl chloride.

[0038] (2) Add 0.016mol 4,4′,4″-(boroxine-2,4,6)-tribenzoyl chloride and 50ml acetone to a four-necked flask equipped with a nitrogen protection device, and stir at room temperature for 10min ; Weigh 0.048mol of methanol and place it in a constant pressure dropping funnel, add it dropwise to the flask under stirring conditions, and the dropping time is controlled at 20min. After the methanol is added dropwise, stir at room...

Embodiment 2

[0046] (1) In a three-necked flask equipped with a nitrogen protection device, add 0.06mol 4-carboxyphenylboronic acid and 0.06mol thionyl chloride, stir at room temperature for 60min, raise the temperature to 90°C, and react for 20h. During the reaction, the reaction system is kept at in a nitrogen atmosphere. Thionyl chloride and the water produced by the reaction were distilled off under reduced pressure to obtain a white solid, which was dried in vacuum at 80°C for 6 hours to obtain a white powdery solid 4,4′,4″-(boroxine-2,4,6) - Tribenzoyl chloride.

[0047] (2) In a four-necked flask equipped with a nitrogen protection device, add 0.016mol 4,4′,4″-(boroxine-2,4,6)-tribenzoyl chloride and 120ml tetrahydrofuran, and stir at room temperature for 60min Weigh 0.048mol of methanol and place it in a constant pressure dropping funnel, add it dropwise to the flask under stirring, and the dropping time is controlled at 90min. After the dropwise addition of methanol is completed,...

Embodiment 3

[0055] (1) In a three-necked flask equipped with a nitrogen protection device, add 0.06mol 4-carboxyphenylboronic acid and 0.06mol thionyl chloride, stir at room temperature for 40min, raise the temperature to 70°C, and react for 13h. During the reaction, the reaction system is kept at in a nitrogen atmosphere. Thionyl chloride and the water produced by the reaction were distilled off under reduced pressure to obtain a white solid, which was dried in vacuum at 70°C for 5 hours to obtain a white powdery solid 4,4′,4″-(boroxine-2,4,6) - Tribenzoyl chloride.

[0056] (2) In a four-necked flask equipped with a nitrogen protection device, add 0.016mol 4,4′,4″-(boroxine-2,4,6)-tribenzoyl chloride and 70ml of dichloromethane, at room temperature Stir for 30 minutes; weigh 0.048 mol of methanol and place it in a constant pressure dropping funnel, add it dropwise to the flask under stirring conditions, and the dropping time is controlled at 70 minutes. After the dropwise addition of m...

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Abstract

The invention discloses a boron-nitrogen structured multi-aromatic-ring flame-retardant epoxy monomer, which has the following structure: B and N flame-retardant elements are introduced into the epoxystructure so that the prepared epoxy resin has excellent flame retardancy, and boroxine and multi-benzene-ring structures endows the epoxy resin with excellent thermal stability and mechanical properties. Through detection, the limit oxygen index of the epoxy resin can reach 28.3% at most, and the vertical combustion grade reaches V-1 grade. The invention discloses a preparation method of the epoxy monomer.

Description

technical field [0001] The invention relates to a boron-nitrogen structure polyaromatic flame-retardant epoxy resin and a preparation method thereof. B and N flame-retardant elements are introduced into epoxy monomers, so that the cured epoxy resin has good flame-retardant performance. Background technique [0002] Epoxy resin is one of the three commonly used thermosetting resins, and is widely used due to its good toughness, moisture resistance, solvent and chemical corrosion resistance, low cure shrinkage, excellent adhesion, electrical properties and mechanical properties Composite materials, laminated materials, surface coatings, adhesives, paints, filling materials, insulating materials for electrical devices and sealing materials for semiconductors, etc. Although the unique advantages of epoxy resin make it have broad development prospects, its flammability greatly limits its application fields. The fire caused by such polymer materials not only affects the surroundi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/05C08G59/36C08G59/32C08G59/30
CPCC07F5/05C08G59/30C08G59/3254C08G59/36
Inventor 丁寅
Owner NANJING UNIV
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