Narrow distribution gemini surfactant and preparation method thereof
A technology of gemini surface and active agent, applied in the field of narrow distribution gemini surfactant and its preparation, can solve the problems of poor product performance synthesis method, unable to guarantee the stability of alkynyl group, wide product molecular weight distribution, etc., and achieve the alkynyl group retention rate Low, improve the narrow distribution characteristics, the effect of strong alkalinity
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[0028] Example 1
[0029] Add 1 mol of alkynediol and 5g 1,8-diazabicycloundec-7-ene (DBU) into a 1 L autoclave with stirring, and check the airtightness of the reactor, and wait for the reactor for 1 hour After there is no pressure drop, perform nitrogen replacement and vacuum operation at 50℃ to ensure that the vacuum time is greater than 30min. The number of high-purity nitrogen replacement operations is 5 times, and the pressure is discharged to 0-30KPa, and then the reaction kettle Feed ethylene oxide, control the reaction temperature to 120℃±3℃ and the reaction pressure to 0.3MPa~0.5MPa, stop feeding ethylene oxide until the total amount of ethylene oxide is 10mol, and carry out Post-treatment aging maintains the temperature of the reactor at 120°C±3°C until the pressure in the reactor no longer drops, indicating that the maturation reaction is completed. The temperature is lowered to 60°C, neutralized with glacial acetic acid and the low boiling temperature is removed to ...
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[0031] Example 2
[0032] Add 1 mol of alkynediol and 5 g of 1,8-diazabicycloundec-7-ene (DBU) into a 1 L autoclave with stirring, and check the air tightness of the reactor. After there is no pressure drop within 1 hour, perform nitrogen replacement and vacuum operation at 50℃ to ensure that the vacuum time is greater than 30min. The number of high-purity nitrogen replacement operations is 5 times, and the pressure is discharged to 0~30KPa, and then the reaction Feed ethylene oxide into the kettle, control the reaction temperature to 90°C±3°C and the reaction pressure to 0.3MPa~0.5MPa, and stop feeding ethylene oxide until the total amount of ethylene oxide is 10mol. The product undergoes post-treatment and aging to maintain the temperature of the reactor at 90°C±3°C until the pressure in the reactor no longer drops, indicating that the maturation reaction is completed. The temperature is lowered to 60°C, neutralized with glacial acetic acid and the low boiling temperature is r...
Example Embodiment
[0033] Example 3
[0034] Add 1 mol of alkynediol and 2.5g of 1,4-diazabicyclo[2.2.2]octane (ABCO) and 2.5g of 1,4-diazobicyclo[ 2.2.2] Octane (DABCO) is used as a catalyst to check the air tightness of the reactor. After the reactor does not lose pressure within 1 hour, perform nitrogen replacement and vacuum operation at 50℃ to ensure that Vacuum time is greater than 30min, high-purity nitrogen replacement is performed 5 times, the pressure is discharged to 0~30KPa, and then ethylene oxide is introduced into the reactor, and the reaction temperature is controlled to 00℃±3℃ and the reaction pressure is 0.3MPa~0.5 MPa, stop feeding ethylene oxide until the total amount of ethylene oxide fed is 10mol, and post-process the product to maintain the temperature of the reactor at 90℃±3℃ until the reactor pressure no longer drops, indicating completion Maturation reaction. Reduce to 60°C, neutralize with glacial acetic acid and remove low boiling.
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