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Preparation method of acetyl-terminated 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 can solve the problems of high molecular weight, low peroxide value and low peroxidation Value and other issues

Active Publication Date: 2021-08-10
NANJING WELL BIOCHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The Chinese patent publication with the publication number "CN102911352A" introduces a method for preparing a low molecular weight, low peroxide value acetyl-terminated allyl alcohol polyether, but this method can only be used for allyl alcohol with a molecular weight of less than 1000 Polyether, its method procedure is loaded down with trivial details, does not mention the specific data of peroxide value in the embodiment; Publication No. is " CN101497560A " in the Chinese patent publication that introduced another kind of allyl alcohol ether of low peroxide value The preparation method is formed by esterifying and capping allyl alcohol polyether and acetic anhydride, but the peroxide value of the prepared allyl alcohol esterified capped polyether can only be less than 50 ppm, and the molecular weight of allyl alcohol polyether Between 200 and 1000, it cannot meet the downstream requirements for products with high molecular weight and low peroxide value

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  • Preparation method of acetyl-terminated allyl alcohol polyether

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Embodiment 1

[0024] A preparation method of acetyl-terminated allyl alcohol polyether, comprising the steps of:

[0025] (1) Add 1000g of allyl alcohol polyether with a molecular weight of 1000 and 122.5g of acetic anhydride to a 2L reactor at room temperature. After nitrogen replacement, turn on the stirring function of the reactor and raise the temperature to 125°C. Stir at temperature for 4 hours. The allyl alcohol polyether in this step uses allyl alcohol as an initiator, is formed by ring-opening polymerization with epoxide under the catalysis of potassium methylate, and is a finished polyether refined through a post-treatment process. Wherein the epoxide is butylene oxide.

[0026] (2) Raise the temperature of the mixture in the reactor to 135°C, and then carry out vacuum nitrogen degassing treatment in the reactor. The treatment time is 4 hours, and the vacuum degree in the reactor is less than -0.09 MPa.

[0027] (3) Stop nitrogen filling and degassing, lower the temperature of t...

Embodiment 2

[0032] A preparation method of acetyl-terminated allyl alcohol polyether, comprising the steps of:

[0033] (1) Add 1000g of allyl alcohol polyether with a molecular weight of 2000 and 66.5g of acetic anhydride to a 2L reactor at room temperature. After nitrogen replacement, turn on the stirring function of the reactor and raise the temperature to 130°C. Stir at temperature for 3.5 hours. The allyl alcohol polyether in this step uses allyl alcohol as an initiator, and is formed by ring-opening polymerization with epoxide under the catalysis of potassium hydroxide, and is a finished polyether refined through a post-treatment process. Wherein the epoxide is a random copolymer of ethylene oxide and propylene oxide, wherein ethylene oxide accounts for 20% of the total molecular weight of the copolymer.

[0034] (2) Raise the temperature of the mixture in the reactor to 140°C, and then carry out vacuum nitrogen degassing treatment in the reactor. The treatment time is 4 hours, and...

Embodiment 3

[0040] A preparation method of acetyl-terminated allyl alcohol polyether, comprising the steps of:

[0041] (1) Add 1000g of allyl alcohol polyether with a molecular weight of 5000 and 26g of acetic anhydride to a 2L reactor at room temperature. After nitrogen replacement, turn on the stirring function of the reactor and raise the temperature to 125°C. Stirring was continued for 4 hours. The allyl alcohol polyether in this step uses allyl alcohol as the starting agent, under the catalysis of potassium methylate and potassium hydroxide, it is formed by ring-opening polymerization with epoxide and refined through the post-treatment process. . Wherein the epoxide is propylene oxide.

[0042] (2) Raise the temperature of the mixture in the reactor to 145°C, and then carry out vacuum nitrogen degassing treatment in the reactor. The treatment time is 5 hours, and the vacuum degree in the reactor is less than -0.09 MPa.

[0043] (3) Stop nitrogen filling and degassing, lower the t...

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Abstract

The invention provides a preparation method of acetyl-terminated allyl alcohol polyether, which comprises the following steps: (1) adding reactants allyl alcohol polyether and acetic anhydride into a reaction kettle at room temperature, conducting replacing with inert gas, conducting heating to 125-135 DEG C, and conducting reacting for 3-5 hours; (2) heating the mixture in the reaction kettle to 135-145 DEG C, and then carrying out vacuum nitrogen charging and degassing for 3-5 hours; (3) stopping nitrogen charging and degassing, cooling the mixture in the reaction kettle to 70-80 DEG C, adding an aldehyde adsorbent, and conducting stirring; (4) vacuumizing the reaction kettle for one hour, and cooling the mixture to 40-50 DEG C; and (5) discharging the mixture in the reaction kettle, and conducting packaging and bagging under the protection of inert gas. The method has the beneficial effects that the peroxide value of acetyl-terminated allyl alcohol polyether can be effectively reduced, and meanwhile, the taste and the aldehyde content of polyether polyol can be remarkably reduced.

Description

technical field [0001] The invention belongs to the technical field of chemical product preparation, and in particular relates to a preparation method of acetyl-terminated allyl alcohol polyether. Background technique [0002] Acetyl-terminated allyl alcohol polyether is a special polyether in which the hydrogen on the terminal hydroxyl group of allyl alcohol polyether is replaced by an acetyl group. It is a colorless to pale yellow transparent liquid. Acetyl-terminated allyl alcohol polyether has low foam, strong lipophilicity, low pour point, low viscosity, enhanced stability in acid and alkali, good oxidation stability, heat resistance and coking resistance, and biodegradable 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 cross-linking problem caused by hydroxyl-containing polyether, making the product quality better , better storage stability...

Claims

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Application Information

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IPC IPC(8): C08G65/331
CPCC08G65/331
Inventor 陈丹钱昌强朱兵王保成袁鹏周大伟
Owner NANJING WELL BIOCHEM
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