A kind of preparation method of alkenyl-terminated unsaturated polyether
An alkenyl-terminated and alkenyl-terminated technology, applied in the field of unsaturated polyether preparation, can solve the problems of double bond destruction, introduction of end-capped polyether impurities, low reaction conversion rate, etc. The effect of wide and high production efficiency
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Embodiment 1
[0042] The concrete reaction process that present embodiment prepares polyether is as follows:
[0043] step 1):
[0044] 1.1) With water, ethylene glycol mixture as initiator (wherein the mass fraction of water is 50wt%), the amount of initiator is 0.2wt% of final polyether product quality, add 0.6wt% (based on polyether product quality) The catalyst is sodium hydroxide, replaced by nitrogen, the temperature is raised to 120°C, and the pressure is reduced to -0.095MPa for dehydration reaction for 2 hours, and the water generated by the reaction is removed;
[0045] 1.2) Add uniformly mixed EO / PO (the mass fraction of EO is 50wt%, and the amount of EO and PO are both 1.6% of the mass of the polyether product) raw material into the system of step 1.1), the reaction temperature is 100°C, and the reaction pressure is 0.05MPa After 1 hour of reaction, neutralize and refine to obtain the bimetallic catalytic polymerization raw material (the neutralization and refining operation is...
Embodiment 2
[0052] The concrete reaction process that present embodiment prepares polyether is as follows:
[0053] step 1):
[0054] 1.1) With the mixture of glycerin and pentaerythritol as initiator (wherein the mass fraction of glycerin is 50%wt), the amount of initiator is 1.07wt% of polyether product quality, add 1wt% (based on polyether product quality) catalyst hydrogen Potassium oxide, replaced by nitrogen, heated to 100°C, depressurized to -0.097MPa for dehydration reaction for 1 hour, and removed the water generated by the reaction;
[0055] 1.2) Add EO raw material (being 63wt% of polyether product quality) to step 1.1) system, reaction temperature 150 ℃, reaction pressure 0.5MPa, after reacting for 10h, obtain bimetallic catalytic polymerization raw material (neutralization and Refined specific operation with reference to embodiment 1, repeats no more). Add a bimetallic catalyst (DMC catalyst, produced by Huai'an Bard Company, the amount used accounts for 0.01wt% of the poly...
Embodiment 3
[0062] The concrete reaction process that present embodiment prepares polyether is as follows:
[0063] step 1):
[0064] 1.1) Using neopentyl glycol as the initiator, the amount of the initiator is 54.2wt% of the mass of the polyether product, additionally adding 0.6wt% (based on the mass of the polyether product) catalyst potassium methoxide, replacing with nitrogen, and raising the temperature to 120°C, Reduce the pressure to -0.095MPa to carry out the desolvation reaction for 2 hours, and remove the methanol generated by the reaction;
[0065] 1.2) Add EO raw material (45.8wt% of the mass of the polyether product) to the system in step 1.1), react at a reaction temperature of 100° C. and a reaction pressure of 0.05 MPa for 3 hours.
[0066] Step 2): Add the calculated isobutylene oxide to the system (the molar ratio of isobutylene oxide to the initiator for capping is 1.2×n:1, n=2, that is, 2.4:1, mature After 3h, add phosphoric acid to neutralize to PH<7, at this time t...
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