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
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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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