Multifunctional benzoxazine composite material and preparation method thereof

A benzoxazine and composite material technology, which is applied in the field of new functional polymer materials, can solve the problems of high flammability and toughness of benzoxazine resin, and high temperature of ring-opening reaction, so as to improve the flame retardant performance and toughness, the process is simple, the The effect of reducing the rate of heat release and

Active Publication Date: 2017-12-15
SHAANXI TIANCE NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Another purpose of the present invention is to solve technical defects such as high benzoxazine monomer ring-opening reaction temperature, benzoxazine resin flammability and poor toughness in the prior art, and provide a benzoxazine monomer ring-opening curing Multifunctional benzoxazine composites with reduced temperature, excellent flame retardancy and toughness

Method used

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  • Multifunctional benzoxazine composite material and preparation method thereof
  • Multifunctional benzoxazine composite material and preparation method thereof
  • Multifunctional benzoxazine composite material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0056] Preparation of cross-linked polyphosphazene solid microspheres: Weigh 60 parts of hexachlorotripolyphosphazene and 58 parts of hydroquinone, add them to 3000 parts of acetonitrile solvent, and ultrasonically disperse and mix evenly under the conditions of power 200W and frequency 40 Hz Finally, add 220 parts of acid-binding agent triethylamine; raise the temperature of the mixed reaction solution to 40°C, power 200W, and ultrasonically react at a frequency of 40 Hz for 4 hours; after the reaction solution is cooled to room temperature, centrifuge at a speed of 10,000rpm to obtain a yellow crude product; Using centrifugal cleaning method, the crude product was washed 4 times with acetone, deionized water and ethanol in sequence, and the purified product was placed in a vacuum oven and dried at 80°C for 8 hours to obtain a light yellow cross-linked polyphosphorus with an average particle size of 3um. Nitrile solid microspheres.

[0057] Preparation of sulfonated cross-lin...

Embodiment 2

[0060] Preparation of cross-linked polyphosphazene solid microspheres: Weigh 100 parts of hexachlorotripolyphosphazene and 217 parts of silicon-containing diamine (1,3-bis(3-aminopropyl)-1,1,3,3- Tetramethyldisiloxane), added to 1000 parts of acetone-acetonitrile mixed solvent with a volume ratio of 1:99, ultrasonically mixed at a power of 100W and a frequency of 20 Hz; then added 120 parts of N,N-dipropylene Base-1-propylamine, heat up to 60°C, ultrasonically react for 0.5h under the condition of power 100W, frequency 80 Hz, then stir the reaction at 400rpm at a constant temperature of 60°C for 8h, stop the reaction; after the reaction solution is cooled to room temperature, centrifuge at 3000rpm The white crude product was isolated; the crude product was washed three times with acetone, deionized water and ethanol successively by centrifugal cleaning method, and the purified product was placed in a vacuum oven and dried at 60°C for 4 hours to obtain a white product with an av...

Embodiment 3

[0064] Preparation of cross-linked polyphosphazene solid microspheres: Weigh 120 parts of hexachlorotripolyphosphazene and 93 parts of p-2-nitro-1,4-phenylenediamine, add them to 2500 parts of pyridine solvent, under the power of 300W, 100 Ultrasonic mixing under Hz conditions; then add 300 parts of N,N-dimethylaniline, heat up to 60°C, power 300W, and ultrasonically react at 100 Hz for 8 hours; after the reaction solution is cooled to room temperature, centrifuge at 15000rpm to obtain white Crude product; using centrifugal cleaning method, the crude product was washed 5 times with acetone, deionized water and ethanol in sequence, and the purified product was placed in a vacuum oven and dried at 90°C for 8 hours to obtain a white cross-linked structure with an average particle size of 0.2um Polyphosphazene solid microspheres.

[0065] Preparation of sulfonated cross-linked polyphosphazene solid microspheres: Weigh 5 parts of prepared cross-linked polyphosphazene solid microsph...

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Abstract

The invention discloses a multifunctional benzoxazine composite material. The multifunctional benzoxazine composite material is prepared from benzoxazine monomers through an open-loop curing reaction under the catalytic action of sulfonated crosslinking structured polyphosphazene microspheres. A preparation method comprises steps as follows: S1, the sulfonated crosslinking structured polyphosphazene microspheres are prepared; S2, the benzoxazine monomers are dissolved in solvents, the sulfonated crosslinking structured polyphosphazene microspheres are added, and a mixture is subjected to ultrasonic dispersion; S3, acetone and alcohol as the solvents are removed through evaporation, and air in the mixture is removed; S4, the mixture of the benzoxazine monomers and the sulfonated crosslinking structured polyphosphazene microspheres is poured into a glass mold while being still hot; S5, the glass mold is cured for 2-3 h at the temperature of 150-180 DEG C, cured for 1-3 h at the temperature of 190-200 DEG C and cooled, and the multifunctional benzoxazine composite material is obtained. The open-loop curing temperature of the benzoxazine monomers in the preparation process of the composite material is reduced, and the composite material integrates remarkable flame retardance and good fracture toughness property, thereby being widely applied to the field with higher requirements for overall performance of the materials.

Description

technical field [0001] The invention relates to a multifunctional benzoxazine composite material and a preparation method thereof, belonging to the field of new functional polymer materials. Background technique [0002] Benzoxazine resin is a new type of thermosetting resin developed on the basis of phenolic resin. It has all the advantages of traditional phenolic resins, such as excellent mechanical properties, good chemical stability, sample dimensional stability, high chemical resistivity, thermal stability, and the corresponding monomer thermal curing process has nearly zero shrinkage rate. The sample has low water absorption. In addition, the raw materials for the synthesis of benzoxazine monomers have a wide range of sources, and the molecular structure design and synthesis operations of the monomers are simple, and can be used to prepare functional benzoxazine resins that meet different performance requirements. Therefore, it can replace traditional phenolic resins ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G14/06C08L61/34C08L85/02
Inventor 赵春霞赵玲李云涛谢雪东苟浩澜
Owner SHAANXI TIANCE NEW MATERIAL TECH
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