A kind of azido-terminated oxirane-tetrahydrofuran block copolyether containing carbamate structural unit and its synthesis method
A technology of tetrahydrofuran block and hydroxyl-terminated oxirane, which is applied in the direction of polyether adhesives, adhesive types, adhesives, etc., can solve the problem of propellant combustion performance, mechanical properties, processing costs and safety performance, and limit propulsion Solve the problems of low-temperature mechanical properties, simple post-processing, and stable yield by eliminating the problems of poor energy level and mechanical strength.
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Embodiment 1
[0027] The first step: Synthesis of chlorine-terminated oxirane-tetrahydrofuran block copolyether (ClTUTPE)
[0028] In a 250mL three-necked round-bottomed flask equipped with mechanical stirring, reflux condenser, and thermometer, sequentially add hydroxyl-terminated oxirane-tetrahydrofuran block copolyether (22.200g, 7.818mmol) and dibutyltin dilaurate (0.0138g , 0.022mmol), stir evenly. Then 2-chloroethyl isocyanate (1.741 g, 16.5 mmol) was added, and after stirring evenly, the temperature was slowly raised to 80° C., and the reaction was continued for 19 h. After the reaction, the unreacted 2-chloroethyl isocyanate was removed to obtain 23.8189 g of a colorless viscous liquid, which was chloro-terminated oxirane-tetrahydrofuran block copolyether, with a yield of 99.87%.
[0029] Structure Identification:
[0030] IR, ν max (cm -1 ): 3510, 3330(-NH-), 2940, 2860(-CH 2 -), 1724 (C=O), 1114 (-C-O-C-), 778 (C-Cl).
[0031] 1 H NMR (CDCl 3 , 500MHz): 5.47, 4.23, 3.63, 3...
Embodiment 2
[0041] The first step: Synthesis of chlorine-terminated oxirane-tetrahydrofuran block copolyether (ClTUTPE)
[0042] In a 250mL three-neck round-bottomed flask equipped with mechanical stirring, reflux condenser, and thermometer, sequentially add hydroxyl-terminated oxirane-tetrahydrofuran block copolyether (22.200g, 7.818mmol) and dibutyltin dilaurate (0.0095g , 0.015mmol), stir evenly. Then 2-chloroethyl isocyanate (2.146g, 20.338mmol) was added, after stirring evenly, the temperature was slowly raised to 70°C, and the reaction was continued for 22h. After the reaction, the unreacted 2-chloroethyl isocyanate was distilled off under reduced pressure to obtain 23.843 g of a colorless viscous liquid, chloro-terminated oxirane-tetrahydrofuran block copolyether, with a yield of 99.97%.
[0043] The second step: Synthesis of azido-terminated oxirane-tetrahydrofuran block copolyether (ATUTPE) In a 250mL three-necked round-bottomed flask equipped with mechanical stirring, reflux co...
Embodiment 3
[0045] The first step: Synthesis of chlorine-terminated oxirane-tetrahydrofuran block copolyether (ClTUTPE)
[0046] In a 250mL three-necked round-bottomed flask equipped with mechanical stirring, reflux condenser, and thermometer, sequentially add hydroxyl-terminated oxirane-tetrahydrofuran block copolyether (22.200g, 7.818mmol) and dibutyltin dilaurate (0.016g , 0.025mmol), stir evenly. Then 2-chloroethyl isocyanate (3.282g, 31.099mmol) was added, after stirring evenly, the temperature was slowly raised to 90°C, and the reaction was continued for 7h. After the reaction, the unreacted 2-chloroethyl isocyanate was distilled off under reduced pressure to obtain 23.810 g of a colorless viscous liquid, chloro-terminated oxirane-tetrahydrofuran block copolyether, with a yield of 99.83%.
[0047] The second step: Synthesis of azido-terminated oxirane-tetrahydrofuran block copolyether (ATUTPE)
[0048] In a 250mL three-necked round-bottomed flask equipped with mechanical stirring,...
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