Preparation of acetyl end capping allyl alcohol polyether
A technology of allyl alcohol polyether and terminal allyl alcohol, which is applied in the field of preparation of acetyl-terminated allyl alcohol polyether, and achieves the effects of high end capping rate, simple operation and reasonable process.
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Embodiment 1
[0016] Example 1: Add 1600 parts of allyl alcohol atactic polyether (M=5000) and 82 parts of acetic anhydride into the reactor, connect it to a condensing reflux device, raise the temperature to 130-140° C., and reflux for 2.5 hours. Connect to the distillation device, adjust the amount of nitrogen gas to make the vacuum degree be -0.080~-0.085MPa, and deacidify by bubbling for 2.5 hours. Cool down to 70°C, add 50 parts of water, stir for 40 minutes, vacuumize for 0.8 hours at a temperature of 90°C, and a vacuum degree of -0.070 to -0.090 MPa, then transfer to a falling film evaporator, at a temperature of 100 to 120 Deacidification for 1.5 hours under the condition of ℃ and vacuum degree ≤100Pa, and then purified and adsorbed by polyether to obtain acetyl-capped allyl alcohol random polyether, the capping rate is 96%, the content of acetic acid is 45ppm, and the content of acetic anhydride is 0ppm .
Embodiment 2
[0017] Example 2: Add 1600 parts of allyl alcohol atactic polyether (M=7000) and 68 parts of acetic anhydride to the reactor, connect it to a condensing reflux device, raise the temperature to 130-140° C., and reflux for 2.5 hours. Connect to the distillation device, adjust the amount of nitrogen gas to make the vacuum degree be -0.085~-0.090MPa, and deacidify by bubbling for 3.0 hours. Cool down to 70°C, add 65 parts of water, stir for 40 minutes, vacuumize for 1.0 hour at a temperature of 90°C, and a vacuum degree of -0.070 to -0.090 MPa, then transfer to a falling film evaporator, and at a temperature of 110 to 130 Deacidification for 2.0 hours under the condition of ℃ and vacuum degree ≤100Pa, and then refined and adsorbed by polyether to obtain acetyl-capped allyl alcohol random polyether, the capping rate is 95%, the content of acetic acid is 72ppm, and the content of acetic anhydride is 0ppm .
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