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Fire-retarding hexagonal boron nitride/thermosetting resin composite material and preparation method thereof

A technology of resin composite material and hexagonal boron nitride, which is applied in the field of flame retardant hexagonal boron nitride/thermosetting resin composite material and its preparation, can solve the problems of flame retardancy, low thermal expansion coefficient and the like, and achieves simple operation, abundant sources and good quality. The effect of interfacial forces

Inactive Publication Date: 2013-04-24
SUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there is no report on the preparation of new thermosetting resin composite materials based on hexagonal boron nitride and phosphazene, which have high flame retardancy, low thermal expansion coefficient and good interfacial force with resin.

Method used

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  • Fire-retarding hexagonal boron nitride/thermosetting resin composite material and preparation method thereof
  • Fire-retarding hexagonal boron nitride/thermosetting resin composite material and preparation method thereof
  • Fire-retarding hexagonal boron nitride/thermosetting resin composite material and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0026] 1. Preparation of hexagonal boron nitride with phosphazene structure

[0027] in N 2 Under protection, 150 g of toluene and 3 g of hexagonal boron nitride were mixed in 1# reactor to obtain a uniform suspension. Add 0.15g of γ-aminopropyltriethoxysilane into the reactor, and then reflux at 100°C for 8h. After the reaction, filter with suction, wash with toluene and absolute ethanol for 5 times, and dry to obtain hexagonal boron nitride treated by coupling.

[0028] In the 2# reactor, 3 g of coupling-treated hexagonal boron nitride and 150 g of tetrahydrofuran were mixed to obtain a uniform suspension. 24g triethylamine is added into 2# reactor, under N 2 Under atmosphere and cooling with ice water, the reactant was stirred for 1.5 h. Dissolve 9g of chlorophosphazene in 50g of tetrahydrofuran, slowly add to 2# reactor within 1h, heat the 2# reactor, and make the material in the reactor react at 75°C for 8h. After the reaction, wash with tetrahydrofuran and absolute ...

Embodiment 2

[0042] Weigh 45.7g N,N'-4,4'-diphenylmethane bismaleimide and 34.3g O,O'-diallyl bisphenol A in a beaker, mechanically stir at 135°C for prepolymerization After 15 minutes, a brownish-yellow transparent clear liquid was obtained; 8.89g of hexagonal boron nitride (accounting for 10wt% of the total mass of the resin system) prepared in Example 1 containing a phosphazene structure was added to the liquid, and mechanically stirred for prepolymerization for 15min to obtain a prepolymer . Pour the prepolymer into the preheated mold, vacuumize at 135°C for 1h, and then follow the processes of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 230°C / 4h respectively After curing and post-treatment, the hexagonal boron nitride / bismaleimide resin composite material is obtained. For its thermal expansion coefficient and limiting oxygen index in the glassy state (50-250°C), see Figures 5 and 6, respectively.

Embodiment 3

[0044] Weigh 45.7g N,N'-4,4'-diphenylmethane bismaleimide and 34.3g O,O'-diallyl bisphenol A in a beaker, mechanically stir at 135°C for prepolymerization After 15 minutes, a brownish-yellow transparent clear liquid was obtained; 20 g of hexagonal boron nitride containing a phosphazene structure (accounting for 20 wt% of the total mass of the resin system) prepared in Example 1 was added to the liquid, and mechanically stirred for 15 minutes to prepolymerize to obtain a prepolymer. Pour the prepolymer into the preheated mold, vacuumize at 135°C for 1h, and then follow the processes of 150°C / 2h+180°C / 2h+200°C / 2h+220°C / 2h and 230°C / 4h respectively After curing and post-treatment, the hexagonal boron nitride / bismaleimide resin composite material is obtained. For its thermal expansion coefficient and limiting oxygen index in the glassy state (50-250°C), see Figures 5 and 6, respectively.

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Abstract

The invention discloses a fire-retarding hexagonal boron nitride / thermosetting resin composite material and a preparation method thereof. The preparation method comprises the following steps of: uniformly mixing hexagonal boron nitride with methylbenzene; adding silane coupling agent to obtain coupled hexagonal boron nitride; mixing the hexagonal boron nitride with a solvent, and adding a catalyst to obtain a mixer; dissolving chloride phosphonitrile in the solvent, and slowly adding the phosphonitrile chloride into the mixture to obtain chloride phosphonitrile hexagonal boron nitride; mixing the solvent and a reagent with the chloride phosphonitrile hexagonal boron nitride, and then adding a catalyst to obtain hexagonal boron nitride with a phosphonitrile structure; uniformly mixing the hexagonal boron nitride with molten thermocuring resin, and then obtaining a fire-retarding hexagonal boron nitride / thermosetting resin composite material after curing. The hexagonal boron nitride with the phosphonitrile structure is a function body with both organic resin high fire resistance and low thermal expansion coefficient, contains lots of active groups, ensures good dispersion of the hexagonal boron nitride in resin basal body and obtains a good interfacial force, and the prepared composite material has both high fire resistance and low thermal expansion coefficient.

Description

technical field [0001] The invention relates to a composite material and a preparation method thereof, in particular to a flame-retardant hexagonal boron nitride / thermosetting resin composite material and a preparation method thereof. Background technique [0002] In recent years, the rapid development of electronic information, electrical insulation and other industries has put forward more and higher requirements for the performance of high-performance polymer materials, among which low thermal expansion coefficient and high flame retardancy have become important performance indicators. [0003] We know that polymers themselves often do not have good low thermal expansion coefficients and high flame retardancy. In order to obtain high flame retardancy or low thermal expansion coefficient, a lot of research and development work has been carried out. However, the publicly reported work is carried out for a single performance (low thermal expansion coefficient or high fl...

Claims

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Application Information

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IPC IPC(8): C08L79/08C08L79/04C08L63/00C08K9/10C08K9/06C08K9/04C08K9/02C08K3/38
Inventor 梁国正金文琴顾嫒娟袁莉
Owner SUZHOU UNIV
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