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Acetyl terminated polyester and preparation method thereof

A technology of acetyl-terminated polyether, which is applied in the field of acetyl-terminated polyether and its preparation, can solve the problems of increased hydroxyl value and lower capping rate, etc.

Active Publication Date: 2017-01-04
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, after adding water, the generated acetyl-terminated polyether is hydrolyzed in the presence of acid, and acetic acid is produced, which increases the hydroxyl value and reduces the end-capping rate.

Method used

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  • Acetyl terminated polyester and preparation method thereof
  • Acetyl terminated polyester and preparation method thereof
  • Acetyl terminated polyester and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A kind of preparation method of acetyl-terminated polyether of the present embodiment, comprises the steps:

[0027] 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°C to 140°C, and reflux for 2.5 hours. Connect to the distillation device, adjust the amount of nitrogen gas, at 120°C ~ 130°C, vacuum degree -0.080MPa ~ -0.085MPa, deacidify by bubbling for 2.5 hours. Cool down to 70°C, transfer to falling film evaporator, deacidify for 1.5 hours under the condition of temperature 100-120°C, vacuum degree ≤100Pa, cool down to 70°C, add 20 parts of heptane, , under the condition of vacuum degree of -0.097MPa, desolventize for 1 hour, and cool down to 60°C to obtain acetyl-terminated allyl alcohol random polyether, with a hydroxyl content of 15ppm, an acetic acid content of 30ppm, an acetic anhydride content of 0ppm, and a moisture content of is...

Embodiment 2

[0031] A kind of preparation method of acetyl-terminated polyether of the present embodiment, comprises the steps:

[0032] 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°C-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 -0.085MPa~-0.090MPa, and deacidify by bubbling for 3.0 hours. Cool down to 70°C, transfer to a falling film evaporator, deacidify at a temperature of 110-130°C, vacuum ≤ 100Pa for 2.0 hours, cool down to 70°C, add 18 parts of octane, at a temperature of 110°C-120°C , under the condition of vacuum degree of -0.098MPa, desolventize for 1.5 hours, and cool down to 60°C to obtain acetyl-terminated allyl alcohol random polyether, with a hydroxyl content of 10ppm, an acetic acid content of 30ppm, an acetic anhydride content of 0ppm, and a moisture conten...

Embodiment 3

[0036] A kind of preparation method of acetyl-terminated polyether of the present embodiment, comprises the steps:

[0037] Add 1600 parts of allyl alcohol polyoxyethylene ether (M=400) and 530 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 3.0 hours. Connect to the distillation device, adjust the amount of nitrogen gas to make the vacuum degree be -0.085MPa~-0.090MPa, and deacidify by bubbling for 3.0 hours. Cool down to 70°C, transfer to falling film evaporator, deacidify for 2.0 hours at a temperature of 110-130°C, vacuum degree ≤100Pa, cool down to 70°C, add 30 parts of octane, , under the condition of vacuum degree of -0.098MPa, desolventize for 1.5 hours, and cool down to 60°C to obtain acetyl-terminated allyl alcohol polyoxyethylene ether, the content of hydroxyl is 32ppm, the content of acetic acid is 55ppm, the content of acetic anhydride is 0ppm, and the moisture content i...

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Abstract

The invention relates to acetyl terminated polyester and a preparation method thereof and belongs to the technical field of organic high-molecular compound synthesizing. The acetyl terminated polyester uses polyether and acetic anhydride as the raw materials. The preparation method is characterized in that after condensation reflux reaction, most of acid is removed by a nitrogen bubbling manner under a vacuumizing condition, the rest acetic acid and acetic anhydride are removed through a falling-film evaporator under high-vacuum condition, and co-boiling solvent, the acetic acid and the acetic anhydride to obtain the acetyl terminated polyester. The preparation method used for synthesizing the acetyl terminated polyester is high in termination rate, clean in alcohol removing, and the like.

Description

technical field [0001] The invention relates to an acetyl-terminated polyether and a preparation method thereof, belonging to the technical field of synthesis of organic polymer compounds. Background technique [0002] Acetyl-terminated polyether refers to a polyether in which the hydrogen on the hydroxyl group at the end of the polyether is replaced by an acetyl group. Acetyl-terminated polyether has the characteristics of low foam, strong lipophilicity, low pour point, low viscosity, enhanced stability in acid and alkali, good oxidation stability, heat resistance and coking resistance, and biodegradability. It is mainly used in the production of silicone polyether modified foam stabilizer in the polyurethane industry. The silicone modified by this product can effectively solve the original crosslinking problem caused by hydroxyl-containing polyether, making the product better in quality and easier to store. Stability is better. [0003] Polyether-modified silicone surfac...

Claims

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Application Information

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IPC IPC(8): C08G65/332
CPCC08G65/3322
Inventor 万庆梅金一丰马定连刘志湘
Owner ZHEJIANG HUANGMA TECH
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