A kind of synthetic method of the alkynyl-terminated polybutadiene containing carbamate unit
A technology of alkyne-terminated polybutadiene and hydroxyl-terminated polybutadiene, which is applied in the field of polymer materials, can solve the problems of poor mechanical properties and affect the mechanical properties of polytriazole elastomers, and achieve the effect of excellent mechanical properties
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0016] (1) Preparation of propargyl (3-isocyanato-4-methyl) phenyl carbamate
[0017] Under nitrogen protection, 5.6 g (0.1 mol) of propynyl alcohol was added dropwise to a mixture of 52.2 g (0.3 mol) of toluene-2,4-diisocyanate and 100 mL of toluene, and the temperature was kept at 40° C. during the dropwise addition. After the dropwise addition, react at 60° C. for 6 hours to end the reaction. After cooling down, a solid was precipitated, filtered and dried to obtain 14 g of a white solid with a yield of 60.9%.
[0018] Characterization data:
[0019] 1 H NMR (DMSO-d 6 ,500MHz): δ=9.90(s,1H),7.31(s,1H),7.19(m,2H),4.76(d,2H,J=2.0Hz),3.56(t,1H,J=2.0Hz) ,2.23(s,3H); 13 C NMR (DMSO-d 6 ,125MHz): δ=153.0,138.2,132.3,131.3,127.2,124.6,116.4,114.9,79.3,78.0,52.5,17.6.
[0020] IR(KBr,cm -1 ):ν=3331, 3294, 2281, 2124, 1714, 1623, 1553, 1516, 1388, 1314, 1283, 1227, 1075, 916;
[0021] Elemental Analysis: C 12 h 10 N 2 o 3 , theoretical value C 62.6, H 4.38, N 12.17; cal...
Embodiment 2
[0030] (1) Preparation of propargyl (3-isocyanato-4-methyl) phenyl carbamate
[0031] Under nitrogen protection, 5.6 g (0.1 mol) propynyl alcohol was added dropwise to a mixture of 69.6 g (0.4 mol) toluene-2,4-diisocyanate and 100 mL toluene, and the temperature was kept at 50° C. during the dropwise addition. After the dropwise addition, react at 60° C. for 6 hours to end the reaction. After cooling down, a solid was precipitated, filtered and dried to obtain 14.2 g of a white solid, with a yield of 62.0%.
[0032] (2) Synthesis of alkynyl-terminated polybutadiene containing carbamate units
[0033] Under nitrogen protection, 9.4g (40.9mmol) propargyl (3-isocyanato-4-methyl) phenylcarbamate, 60g hydroxyl-terminated polybutadiene (40.9mmol OH) and 250mL dry toluene were added to the reaction bottle. After stirring at 70°C for 24 hours, the reaction was terminated, and the toluene was removed by concentration to obtain 68.0 g of a light yellow solid, with a yield of 98.0%. ...
Embodiment 3
[0035] (1) Preparation of propargyl (3-isocyanato-4-methyl) phenyl carbamate
[0036] Under nitrogen protection, 5.6 g of propynyl alcohol (0.1 mol) was added dropwise to a mixture of 87 g (0.5 mol) of toluene-2,4-diisocyanate and 100 mL of toluene, and the temperature was kept at 50° C. during the dropwise addition. After the dropwise addition, react at 70° C. for 5 hours to end the reaction. After cooling down, a solid was precipitated, filtered and dried to obtain 15.6 g of a white solid with a yield of 68.1%.
[0037] (2) Synthesis of alkynyl-terminated polybutadiene containing carbamate units
[0038] Under nitrogen protection, 9.4g (40.9mmol) propargyl (3-isocyanato-4-methyl) phenylcarbamate, 60g hydroxyl-terminated polybutadiene (40.9mmol OH) and 250mL dry toluene were added to the reaction bottle. After stirring at 60°C for 24 hours, the reaction was terminated, and the toluene was removed by concentration to obtain 67.0 g of a light yellow solid, with a yield of 96...
PUM
| Property | Measurement | Unit |
|---|---|---|
| tensile strength | aaaaa | aaaaa |
| tensile strength | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More