A kind of polyene-terminated copolyether adhesive and its synthesis method
An alkenyl copolyether and adhesive technology, used in polyether adhesives, adhesive types, adhesives, etc., can solve the problems of high curing temperature, water sensitivity, harsh curing conditions, etc., and achieve high mechanical properties , high flexibility, the effect of improving regularity
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Embodiment 1
[0028] (1) Synthesis of MHPET
[0029] In a 250ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 50g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 1.68g Boron trifluoride·tetrahydrofuran complex, stirred for 0.5h, cooled to 2°C, began to slowly add 4.08g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 4h, and the dropwise addition was completed After that, continue the insulation reaction for 24h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed 3 times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 52.7 g of light yellow viscous transparent liquid with a yield of 97.4%.
[0030] Structural identification: IR, ν max (cm -1 ): 3440(-OH), 2846, 2965(-CH 3 、-CH 2 ), 1101 (C-O-C).
[0031] 1 H NMR (CDCl 3 , 500MHz): 1...
Embodiment 2
[0040] (1) Synthesis of MHPET
[0041] In a 250ml four-neck flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 50g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 2.24g Boron trifluoride·tetrahydrofuran complex, stirred for 0.5h, cooled to 3°C, began to slowly add 6.12g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 5h, and the dropwise addition was completed After that, continue the insulation reaction for 28h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed 3 times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 54.5 g of light yellow viscous transparent liquid with a yield of 97.1%.
[0042] The number average molecular weight is 2810, and the hydroxyl value is 96.8 mgKOH / g.
[0043] (2) Synthesis of MAPET
[0044] In a 250ml four-n...
Embodiment 3
[0047] (1) Synthesis of MHPET
[0048] In a 250ml four-necked flask equipped with mechanical stirring, reflux condenser, thermometer and dropping funnel, 60g (0.02mol) of hydroxyl-terminated oxirane-tetrahydrofuran copolyether (PET), 100ml of dichloromethane and 2.24g Boron trifluoride tetrahydrofuran complex, stirred for 0.5h, cooled to 4°C, began to slowly add 6.12g of 3-hydroxymethyl-3-methyloxetane dropwise, the dropping time was 5h, and the dropwise addition was completed After that, continue the insulation reaction for 28h, and use Na 2 CO 3 The aqueous solution was neutralized, then washed three times with distilled water, poured into a separatory funnel, the organic phase was separated, and the solvent was evaporated under reduced pressure to obtain 64.5 g of light yellow viscous transparent liquid with a yield of 97.5%.
[0049] The number average molecular weight was 3320, and the hydroxyl value was 83.1 mgKOH / g.
[0050] (2) Synthesis of MAPET
[0051] In a 250m...
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