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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 low ion content, stable quality and simple operation

Active Publication Date: 2008-02-06
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
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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

The present invention relates to an acetyl terminated moiety allyl alcohol polyether synthesis method which belongs to the end-terminated polyether synthesis technical field, taking allyl alcohol polyether and acetic anhydride as the raw materials to carry cold reflux reaction, after that, the majority of acid emerges in nitrogen-bubbled pattern under the vacuumized condition, then residual acetic acid and acetic anhydride will emerge with a falling-film evaporator under high vacuumized condition, and then the absorption of water and polyether absorbing agent is added, acetyl terminated moiety allyl alcohol polyether is produced with the addition of filter aid to carry vacuum dehydration. The mol ratio of allyl alcohol polyether to acetic anhydride can be 1:2.0-2.5. The present invention educes the principal part of acetic acid and acetic anhydride with nitrogen bubbling under vacuum condition, then fetches out the remaining acetic acid and acetic anhydride through the falling-film evaporator under high vacuum conditions, and carries the process of absorbing potash ion and sodium ion to produce acetyl terminated moiety allyl alcohol polyether. The technique is reasonable and operation is easy.

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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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
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