Preparation method of terminal alkenyl end-capped unsaturated polyether
A technology of alkenyl end capping and alkenyl end capping, which is applied in the field of unsaturated polyether preparation, can solve the problems of low reaction conversion rate, strong reversibility, double bond destruction, etc., and achieve high production efficiency and wide application range
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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 and ethylene glycol mixture as initiator (wherein the mass fraction of water is 50wt%), the amount of initiator is 0.2wt% of the 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 reacting for 1 hour, neutralize and refine to obtain the raw material for bimetallic catalytic polymerization (the neutralization and refining ...
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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Abstract
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