A kind of azido-terminated polycaprolactone adhesive and its synthesis method
A technology of polycaprolactone and synthesis method, which is applied in the direction of adhesives, etc., can solve the problems of low mechanical properties such as tensile strength of elastomers, troublesome post-processing, etc., to increase the content and degree of microphase separation, improve mechanical properties, and synthesize The effect of simple method
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Embodiment 1
[0028] In the there-necked flask equipped with mechanical stirring, reflux condenser, and thermometer, add 30g (0.03mol) polycaprolactone glycol, 0.015g dibutyltin dilaurate and 6.33g 2-chloroethyl isocyanate successively, heat up To 80°C, react for 10h under stirring, then add 100mL dimethylformamide and 4.29g sodium azide to the above reaction system, raise the temperature to 90°C and react for 20h. After the reaction was completed, cool down to room temperature and add water to precipitate, dissolve the precipitate with 60 mL of dichloromethane, wash with water, separate the organic phase, distill off the solvent under reduced pressure to obtain 35.6 g of light yellow solid.
[0029] Characterization data:
[0030] IR, ν max (cm -1 ): 3368 (-NH-), 2945, 2865, 2797 (-CH 2 -), 2101, 1282 (-N 3 ), 1740, 1192, 1097 (ester group).
[0031] 1 H NMR (CDCl 3 , 500MHz): 1.49~1.55, 1.63~1.73, 2.30~2.39, 4.02~4.31, 5.35~5.50.
[0032] The number average molecular weight is 122...
Embodiment 2
[0035] In the there-necked flask equipped with mechanical stirring, reflux condenser, and thermometer, add 60g (0.03mol) polycaprolactone glycol, 0.03g dibutyltin dilaurate and 6.33g 2-chloroethyl isocyanate successively, heat up To 82°C, react for 10h under stirring, then add 150mL dimethylformamide and 4.48g sodium azide to the above reaction system, raise the temperature to 90°C and react for 20h. After the reaction was completed, lower the temperature to room temperature and add water to precipitate, dissolve the precipitate with 120 mL of dichloromethane, wash with water, separate the organic phase, distill off the solvent under reduced pressure and dichloromethane to obtain 66.1 g of a light yellow solid.
[0036] The number average molecular weight is 2215, and the azide group content is 0.89mmol / g.
Embodiment 3
[0038] In the there-necked flask equipped with mechanical stirring, reflux condenser, and thermometer, add 90g (0.03mol) polycaprolactone glycol, 0.03g dibutyltin dilaurate and 6.33g 2-chloroethyl isocyanate successively, heat up To 82°C, react for 10h under stirring, then add 200mL dimethylformamide and 4.48g sodium azide to the above reaction system, raise the temperature to 95°C and react for 24h. After the reaction was completed, lower the temperature to room temperature and add water to precipitate, dissolve the precipitate with 200 mL of dichloromethane, wash with water, separate the organic phase, distill off the solvent under reduced pressure to obtain 95.8 g of light yellow solid.
[0039] The number average molecular weight is 3221, and the azide group content is 0.61 mmol / g.
[0040] The application performance of the azide-terminated polycaprolactone adhesive of the present invention
[0041] Using the AUPCL adhesive of the present invention as a raw material, mix...
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