Isocyanate biuret containing polyunsaturated group and its preparation and application
A polyisocyanate and isocyanate technology, applied in the field of isocyanate biuret containing polyunsaturated groups and its preparation and application, can solve problems such as gelation and agglomeration, difficult reaction stages, etc.
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Embodiment 1
[0063] Synthesis of TMI-TMSDI biuret:
[0064] Weigh an appropriate amount of water and place it in a test tube connected to the peristaltic pump, weigh 500g of TMI monomer and 30mg of MEHQ and place it in a four-necked flask, stir vigorously to raise the temperature to 98°C and keep it constant, set the speed of the peristaltic pump, and within 6 hours 22.4 Add 2 g of water dropwise to the four-necked flask. After the addition of water is completed, react for 1 h; add 24.4 g of TMSDI, then gradually raise the temperature to 130 ° C, and react at a constant temperature. During the reaction, samples are taken every half an hour, and the mass content of -NCO groups is measured by chemical titration until -NCO mass fraction ≤8%, stop heating, remove unreacted monomers through a thin film evaporator at 120 ° C, cool and discharge, and obtain 68.5 g of yellow viscous liquid (H NMR (CDCl3): 1.0 (s, 6H, -CH3),1.76(s,6H,-CH3),2.3(s,6H,-CH3),3.1(s,2H,-CH3),3.3(s,2H,-CH3),5.0(s,2H, =CH...
Embodiment 2
[0070] AOI-HDI biuret synthesis:
[0071] Weigh an appropriate amount of water and place it in a test tube connected to the peristaltic pump, weigh 500g AOI monomer and 30mg MEHQ and place it in a four-necked flask, stir vigorously to raise the temperature to 98°C and keep it constant, set the speed of the peristaltic pump, and within 6 hours 31.9 Add 2 g of water dropwise to the four-necked flask. After the dropwise addition of water, react for 1 h; add 29.8 g of HDI, then gradually raise the temperature to 130 ° C, and react at a constant temperature. During the reaction, samples are taken every half an hour, and the mass content of -NCO groups is measured by chemical titration until -NCO mass fraction ≤ 10%, stop heating, remove unreacted monomers through a thin film evaporator at 120 ° C, cool and discharge, and obtain 75.4 g of yellow viscous liquid (H NMR (CDCl3): 1.2 ~ 1.5 (m, 8H, -CH2-), 3.1~3.4(s, 8H, N-CH2-), 4.5(t, 4H, O-CH2-), 5.5(t, 2H, =CH2), 6.0(t, 2H, = CH-), ...
Embodiment 3
[0075] Polymer Dispersion 1 Preparation:
[0076] The 500ml four-necked bottle is equipped with a stirrer, a heating device, a temperature control device and a feeder as a reactor. Add 55.4g of basic polyether (Wanhua 3156), 5.6g of Stabilizer 1, after nitrogen replacement, the temperature was slowly raised to 110°C with stirring, and topping materials (10.47g of isopropanol, 85.71g of basic polyether 3156, a mixture of 46.55g of acrylonitrile, 69.83g of styrene, and 1.21g of azobisisobutyronitrile), and the temperature is controlled at 115°C to 120°C. The dropwise addition was completed within 100 minutes, the feeding was completed, the aging reaction was carried out for 1 hour, and the vacuum sheet removal was continued for 2 hours to obtain the product, and the product index was measured. The hydroxyl value is 29.2mgKOH / g, the solid content is 44.6%, and the viscosity is 5059cp@25℃.
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