A kind of unsaturated polyether monomer and its preparation method, application and prepared polymer
A polyether monomer and unsaturated technology, applied in the field of application and prepared polymers, unsaturated polyether monomer and preparation method thereof, can solve the problem of low polymerization activity, single structure of polyether monomer, and concrete retention performance. Not good enough, etc., to achieve the effect of improving retention performance
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Embodiment 1
[0061] Under nitrogen protection, put 215 parts of dimethylallyl alcohol in a reaction flask, add 0.45 parts of NaH powder, stir and heat up to 90 ° C, then slowly add 233 parts of butyl glycidyl ether dropwise to the reaction flask at a constant speed, control The reaction temperature is about 90°C, the dropwise addition time is 120 minutes, the temperature is kept for 2 hours after the dropwise addition is completed, and the intermediate (1-1#) is obtained by cooling.
[0062] Add 416 parts of the above-mentioned synthetic intermediate (1-1#) to the reaction kettle, add 7.0 parts of NaH powder, under vacuum conditions, stir and heat up to 120 ° C, slowly feed 970 parts of ethylene oxide into the reaction kettle to carry out In the polymerization reaction, the temperature is maintained at about 120 °C, and the pressure is relatively constant at about 0.4 MPa, until all ethylene oxide is added to the reactor, and the temperature is kept for about 1 hour. material to obtain an ...
Embodiment 2
[0066] Place 300 parts of dimethylallyl alcohol in a three-necked flask with a nitrogen protection device, a thermometer and a stirrer, add 4.5 parts of NaH powder, quickly perform nitrogen replacement, turn on the heating, stir and heat up to 100 ° C, and then add 4.5 parts of NaH powder to the flask. Slowly add 744 parts of butyl glycidyl ether dropwise at a constant speed, control the reaction temperature to 100°C, and dropwise for 180 minutes.
[0067] Add 500 parts of the above-mentioned synthetic intermediate (2-1#) to the autoclave, replace with nitrogen, then under stirring, vacuum the reactor, turn on heating, and slowly feed into the reactor after being warmed up to 120°C 993 parts of ethylene oxide were polymerized, the temperature was maintained at 120°C, and the pressure was relatively constant at about 0.3 MPa, until all the ethylene oxide was added to the reactor, and the temperature was kept for about 1 hour until the pressure of the reactor no longer decreased....
Embodiment 3
[0071]Place 403 parts of dimethylallyl alcohol in a three-necked flask with a nitrogen protection device, a thermometer and a stirrer, add 3.4 parts of NaH powder, quickly carry out nitrogen replacement, turn on the heating, stir and heat up to 100 ° C, then add 3.4 parts of NaH powder to the flask. Slowly add 325 parts of butyl glycidyl ether dropwise at a constant speed, control the reaction temperature to 100°C, dropwise for 180 minutes, keep the temperature for 2 hours after the dropwise addition, and cool to obtain the intermediate (3-1#).
[0072] Then add 360 parts of the above-mentioned synthetic intermediate to the autoclave, add 1.3 parts of sodium hydride, carry out nitrogen replacement, and then under stirring, the reaction kettle is evacuated, the heating is turned on, and the temperature is raised to 120 ℃. Introduce 6375 parts of ethylene oxide to carry out the polymerization reaction, maintain the temperature at 120°C, and keep the pressure relatively constant a...
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