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Method for synthesizing acetyl blocked allyl alcohol polyether

A technology of terminal allyl alcohol polyether and allyl alcohol polyether, which is applied in the field of synthesis of acetyl-terminated allyl alcohol polyether, and achieves the effects of simple operation, stable quality and low ion content

Active Publication Date: 2009-10-14
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are few reports on the synthesis process of acetyl-terminated allyl alcohol polyether

Method used

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  • Method for synthesizing acetyl blocked allyl alcohol polyether
  • Method for synthesizing acetyl blocked allyl alcohol polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 1800 parts of allyl alcohol atactic polyether (M=1500) and 245 parts of acetic anhydride into the reactor, connect it to a condensing reflux device, raise the temperature to 130°C to 140°C, and reflux for 2.5 hours. Connect to the distillation device, adjust the amount of nitrogen gas flow, so that the vacuum degree is -0.080MPa~-0.085MPa, and deacidify by bubbling for 2.5 hours. Cool down to 70°C, transfer to falling film evaporator, deacidify under the condition of vacuum degree ≤ 100Pa for 1.5 hours, cool down to 70°C, add 37.5 parts of water, 30 parts of polyether refined adsorbent, at a temperature of 60°C to 70°C Stir at ℃ for 30 minutes, then add 14 parts of diatomite filter aid, dehydrate for 1 hour under the condition of vacuum degree of -0.095MPa~-0.097MPa, temperature of 90℃~100℃, cool to 60℃ and filter to obtain Acetyl-terminated allyl alcohol random polyether, the capping rate is 98%.

Embodiment 2

[0023] Add 1600 parts of allyl alcohol atactic polyether (M=4000) and 102 parts of acetic anhydride into the reactor, connect it to a condensing reflux device, raise the temperature to 130°C to 140°C, and reflux for 2.5 hours. Connect to the distillation device, adjust the amount of nitrogen gas flow, so that the vacuum degree is -0.085MPa~-0.090MPa, and deacidify by bubbling for 3.0 hours. Cool down to 70°C, transfer to falling film evaporator, deacidify under the condition of vacuum degree ≤ 100Pa for 2.0 hours, then cool down to 70°C, add 48 parts of water and 48 parts of polyether refined adsorbent, at a temperature of 60°C~ Stir at 70°C for 50 minutes, then add 16 parts of diatomite filter aid, dehydrate for 1.5 hours at a vacuum of -0.095MPa to -0.097MPa and a temperature of 90°C to 100°C, and then cool down to 60°C Acetyl-terminated allyl alcohol random polyether was obtained by filtration, and the end-capping rate was 95%.

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Abstract

A method for synthesizing acetyl-terminated allyl alcohol polyether, which belongs to the technical field of synthesis of end-capped polyethers. It uses allyl alcohol polyether and acetic anhydride as raw materials to perform a condensation reflux reaction. After the condensation reflux reaction, first vacuum Most of the acid is removed by nitrogen bubbling under the conditions, and then the remaining acetic acid and acetic anhydride are removed through a falling film evaporator under high vacuum conditions, and then water and polyether adsorbent are added for adsorption, and filter aids are added for vacuum dehydration and filtration to obtain acetyl. End-capped allyl alcohol polyether; the molar ratio of the allyl alcohol polyether to acetic anhydride can be 1:2.0~2.5. The present invention removes most of the acetic acid and acetic anhydride by bubbling nitrogen under vacuum conditions, then removes the remaining acetic acid and acetic anhydride through a falling film evaporator under high vacuum conditions, and adsorbs potassium and sodium ions to prepare acetyl end-capping processes. Allyl alcohol polyether has reasonable technology and simple operation.

Description

technical field [0001] The invention relates to a method for synthesizing acetyl-terminated allyl alcohol polyether, which belongs to the technical field of synthesizing the 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 synthetic method of acetyl-terminated allyl alcohol polyether with reasona...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/332C08G65/48
Inventor 王伟松王新荣孟照平王胜利朱红军
Owner ZHEJIANG HUANGMA TECH