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.

Active Publication Date: 2009-08-05
ZHEJIANG HUANGMA TECH
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  • Claims
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Problems solved by technology

At present, there are few reports on the synthesis

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  • Preparation of acetyl end capping allyl alcohol polyether
  • Preparation of acetyl end capping allyl alcohol polyether

Examples

Experimental program
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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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Abstract

The invention relates to a preparation method of acetyl terminated allyl alcohol polyether, which belongs to the field of synthesis technology of terminated polyether. Allyl alcohol polyether and acetic anhydride are taken as raw materials and are deacidified with most of acid in a nitrogen bubbling deacidifying way under the vacuumized condition, water is added in to enable the rest acetic anhydride to be hydrolyzed to acetic acid, acetic acid and trace quantity acetic anhydride are deacidified by creation of vacuum and a falling film evaporator under the vacuumized condition, and last the acetyl terminated allyl alcohol polyether is obtained during the refining adsorption process of the polyether. The invention adopts the mol ratio of 1:1.2 to 3.0 of the allyl alcohol polyether and the acetic anhydride , the temperature of 120-130 DEG C in the nitrogen bubbling deacidifying process under the vacuumized condition, the vacuum negative pressure of -0.080 to -0.090 MPa and the time of 2.0-3.0 hours. The invention has reasonable technology, simple operation and better use performance.

Description

technical field [0001] The invention relates to a preparation method of an acetyl-terminated allyl alcohol polyether, which belongs to the technical field of synthesis of a capped polyether. Background technique [0002] Acetyl-terminated allyl alcohol polyether refers to a polyether in which the hydrogen on the terminal hydroxyl group of the allyl alcohol polyether is replaced by an acetyl group. In addition to the properties of allyl alcohol polyether, acetyl-terminated allyl alcohol polyether has many special properties, such as low foam, strong lipophilicity, low pouring point, and low viscosity after the end-capped polyether. , suitable for the synthesis of polyether modified silicone and other fields. At present, there are few reports on the synthesis process of acetyl-terminated allyl alcohol polyether. Contents of the invention [0003] The purpose of the present invention is to provide a method for preparing acetyl-terminated allyl alcohol polyether with reasona...

Claims

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Application Information

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IPC IPC(8): C08G65/00
Inventor 王伟松王新荣孟照平王胜利朱红军
Owner ZHEJIANG HUANGMA TECH
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