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Siliceous alkynes fragrant polytriazoles resin and method for making same

A polytriazole resin and polytriazole technology, which is applied in the field of silicon-containing aromatic polytriazole resin and its preparation, can solve the problems of high brittleness of silicon-containing aryne resin and unsatisfactory adhesion between resin and fiber, etc. Achieve excellent physical and mechanical properties and thermal properties, high glass transition temperature, and wide application prospects

Inactive Publication Date: 2008-02-06
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the brittleness of the cured silicon-containing aryne resin is still too high, and the adhesion between the resin and the fiber is still not ideal.

Method used

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  • Siliceous alkynes fragrant polytriazoles resin and method for making same
  • Siliceous alkynes fragrant polytriazoles resin and method for making same
  • Siliceous alkynes fragrant polytriazoles resin and method for making same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1 Preparation of dimethyl-type silyne-containing aromatic polytriazole resin (A1-1)

[0051] 1. Synthesis of 4,4'-diazidemethylbiphenyl

[0052] Add 12.55 g (0.05 mol) of p-dichloromethylbiphenyl, NaN 3 9.75g (0.15mol), benzene (20ml) and DMF (20ml), heated to 70~75°C under stirring, and reacted at constant temperature for 3h. After the reaction, cooled the reaction product to room temperature, poured it into 200ml deionized water, and let it stand Overnight, a white solid was precipitated, filtered, the filter cake was washed with deionized water, and dried to obtain a white powdery solid with a yield of 89.0% and a melting point of 67-71°C.

[0053] 2. Synthesis of dimethyl-type silicon-containing aryne resin

[0054] Add treated 6.00g (0.247mol) magnesium powder and 50ml THF into a 250ml four-neck flask equipped with a stirring, constant pressure funnel and spherical condenser, and then slowly add 21.6g (0.198mol) of magnesium powder dropwise through the c...

Embodiment 2

[0060]Example 2 Preparation of dimethyl-type silyne-containing aromatic polytriazole resin (A1-2)

[0061] The preparation of 4,4'-diazidemethylbiphenyl and dimethyl type silicon-containing aryne resin is the same as in Example 1.

[0062] Add 3.96g of 4,4'-diazidemethylbiphenyl (0.015mol of azide group, 0.030mol), 5.48g of dimethyl type silicon-containing aryne resin (0.0073mol, 0.065mol of alkynyl group) and 30ml of THF In the reactor, the reaction was stirred under reflux for 2 h, and finally the solvent was removed to obtain a reddish-brown solid resin. In the range of 70-110°C, the viscosity of the resin is 0.7Pa.s; when the temperature is higher than 120°C, the viscosity rises rapidly and begins to gel. Infrared spectrum: 3300cm -1 There is a ≡C-H vibration peak at 2098cm -1 and 2156cm -1 -N=N=N and C≡C vibrational absorption peaks appear at about 3140cm -1 The C-H vibrational absorption peak on the triazole ring appears.

[0063] The resin was cured at 80°C / 12h, 1...

Embodiment 3

[0064] Example 3 Preparation of dimethyl-type silyne-containing aromatic polytriazole resin (A1-3)

[0065] The preparation of 4,4'-diazidemethylbiphenyl and dimethyl type silicon-containing aryne resin is the same as in Example 1.

[0066] Add 3.96g (0.015mol, azide group 0.030mol) of 4,4'-diazidemethylbiphenyl and 5.48g (0.0073mol, alkynyl group 0.065mol) of dimethyl type silicon-containing aryne resin into the reactor , the reaction was stirred at 80° C. for 0.5 h to obtain a reddish-brown solid resin. In the range of 70-110°C, the viscosity of the resin is 0.9 Pa.s; when the temperature is higher than 120°C, the viscosity rises rapidly and begins to gel. Infrared spectrum: 3300cm -1 There is a ≡C-H vibration peak at 2098cm -1 and 2156cm -1 -N=N=N and C≡C vibrational absorption peaks appear at about 3150cm -1 The C-H vibrational absorption peak on the triazole ring appears.

[0067] The resin was cured at 80°C / 12h, 120°C / 2h, 150°C / 2h, 170°C / 2h, 210°C / 2h, and post-trea...

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Abstract

The invention relates to an aromatic poly-triazole containing silicon and alkyne and the preparation method, a novel aromatic poly-triazole containing silicon and alkyne which can be solidified with low temperature is prepared by the addition polymerization of the aryne resin containing silicon and the azide. The resin is of low viscosity (less than 1Pa.s) and good wetting quality for fiber, and can be solidified at low temperature such as 70 to 80 DEG C; the glass-transition temperature of the solidified resin is more than 300 DEG C, the solidified resin has good resistance to effect of heat; the common temperature bending strength of the composite material of the aromatic poly-triazole containing silicon and alkyne of unilateral carbon fiber reinforcement is 1800 MPa, the bending modulus is about 120 GPa, the retention rate of the bending strength achieves about 70 percent at 250 DEG C, the bending modulus is almost not changed, the aromatic poly-triazole containing silicon and alkyne has excellent mechanical property and resistance to effect of high temperature. As resin basal body of the composite material of high temperature resistance, the aromatic poly-triazole containing silicon and alkyne has extensive application prospect in the high technology field such as aeronautics, spaceflight, electron apparatus, and chemical industry, etc.

Description

technical field [0001] The invention relates to a silicon-containing aryne aromatic polytriazole resin and a preparation method thereof, in particular to a novel polytriazole-containing polytriazole resin prepared by 1,3-dipolar cycloaddition polymerization using a silicon-containing aryne resin and an azide compound. Silyne aromatic polytriazole resin, which has good processability, excellent heat resistance and mechanical properties, etc., can be used as a resin matrix for advanced composite materials. Background technique [0002] Resin-based composite materials have the advantages of high specific strength and specific modulus, strong designability, good fatigue resistance, and good corrosion resistance. Through the design and combination of materials, composite materials with special functions can also be obtained. Therefore, composite materials are used in aviation It has been widely used in aerospace and other industrial fields, and has become the most rapidly develop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F138/00C08F8/30C08L49/00
Inventor 杜磊黄发荣黄健翔万里强张健田建军扈艳红周燕齐会民沈学宁
Owner EAST CHINA UNIV OF SCI & TECH
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