Preparation method of organic silicon modified polyether polyol
A polyether polyol and organosilicon technology, which is applied in the field of preparation of organosilicon modified polyether polyol, can solve the problems of low production efficiency, difficult control of the reaction process for synthesizing polyurethane, large difference in reaction rate, etc. The effect of migration, smooth and delicate hand feeling, mild and easy-to-control reaction process
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[0044] A kind of preparation method of organosilicon modified polyether polyol specifically comprises the following steps:
[0045] S101: Preparation of terminal hydrogen-containing silicone oil; in S101, the preparation of the terminal hydrogen-containing silicone oil uses octamethylcyclotetrasiloxane, tetramethyldisiloxane, and catalyst A as raw materials, under nitrogen protection Stir in the reactor of the device to raise the temperature, keep the heat for a certain period of time, and obtain terminal hydrogen-containing silicone oil.
[0046] S102: Preparation of allyl polyether; in S102, the preparation of the allyl polyether uses allyl alcohol, ethylene oxide, propylene oxide, and catalyst B as raw materials, and adds allyl in the reactor Alcohol, catalyst B, close the reactor, replace the air in the reactor with nitrogen, remove trace moisture under reduced pressure at room temperature, raise the temperature, first pass propylene oxide or a mixture of propylene oxide a...
Embodiment 1
[0075] Add 270g of octamethylcyclotetrasiloxane, 40.2g of tetramethyldisiloxane, and 0.03g of trifluoroacetic acid into the reactor, stir and raise the temperature to 35°C, and keep the temperature for 12 hours to obtain terminal hydrogen-containing silicone oil. 1034.
[0076] Add 104.4g of allyl alcohol and 0.31g of potassium hydroxide into the reactor, stir, replace the air in the reactor with nitrogen three times, reduce the pressure to -0.090MPa, raise the temperature to 70°C, and feed 1586g of propylene oxide to adjust the The feed rate of propane keeps the pressure in the reactor ≤0.4MPa and the temperature at 100-150°C. After the reaction, reduce the pressure to ≤0.097MPa and keep for 0.5 hours to remove low boilers, then feed 79g of ethylene oxide, and reduce the pressure after the reaction Keep to ≤0.097MPa for 0.5 hours to remove low boilers. Transfer the above material to the post-treatment reactor, add 0.33g of acetic acid and stir for 15min, then add 35.4g of ac...
Embodiment 2
[0079] Add 315g of octamethylcyclotetrasiloxane, 6.7g of tetramethyldisiloxane, and 0.1g of trifluoromethanesulfonic acid into the reactor, stir and raise the temperature to 60°C, and keep the temperature for 5 hours to obtain terminal hydrogen-containing silicone oil. The relative molecular mass is 6434.
[0080] Add 348g of allyl alcohol and 0.35g of sodium metal into the reactor, stir for 0.5h to completely dissolve the sodium metal, replace the air in the reactor with nitrogen three times, reduce the pressure to -0.085MPa, raise the temperature to 100°C, and feed 1086g of propylene oxide , adjust the feeding rate of propylene oxide to keep the pressure in the reactor ≤0.4MPa, temperature 100-150°C, reduce the pressure to ≤0.097MPa after the reaction and keep for 0.5 hours to remove low boilers, then feed 264g of ethylene oxide, After the reaction, reduce the pressure to ≤0.097MPa and keep for 0.5 hours to remove low boilers. Transfer the above material to the post-treatme...
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