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Method for synthesizing polysiloxane having hydroxyethyl group at one end of molecule

A polysiloxane and bishydroxyethyl technology, applied in the field of polysiloxane synthesis, can solve the problems of difficult to obtain unsaturated compounds and harsh reaction conditions for unsaturated compounds, and achieve easy separation and purification and high yield. Effect

Inactive Publication Date: 2009-11-18
山东省农业科学院中心实验室
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Problems solved by technology

[0005] The synthesis methods reported in the above two patents have a common shortcoming, that is, in the process of synthesizing the target compound, the unsaturated compound containing dihydroxyl hydrocarbon group used is not easy to obtain, and the reaction conditions for preparing the unsaturated compound are very harsh

Method used

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  • Method for synthesizing polysiloxane having hydroxyethyl group at one end of molecule

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Hydroxyl protection reaction (molar ratio diethanolamine: hexamethyldisilazane=1:1.5)

[0025] In a 250mL three-necked bottle, add 26.25g of diethanolamine. At room temperature, 60.53 g of hexamethyldisilazane was slowly added dropwise. After the dropwise addition, the temperature of the reaction system was raised to 100° C., and the reaction was continued at this temperature for 8 hours to stop the reaction. The reaction solution was distilled under atmospheric pressure, and the fraction at 218-220°C was collected to obtain 60.38 g of bis(trimethylsiloxy)ethylamine, a colorless liquid, with a yield of 97%.

[0026] Michael addition reaction (molar ratio bis(trimethylsiloxy)ethylamine: allyl acrylate=1:1.3)

[0027] Into a 250 mL three-necked flask, 31.13 g of bis(trimethylsiloxy)ethylamine and 20 mL of methanol were added. At room temperature, slowly add 18.20 g of allyl acrylate dropwise. After the dropwise addition, raise the temperature of the reaction system to 4...

Embodiment 2

[0035] Change the ratio of the amount of diethanolamine and hexamethyldisilazane in the hydroxyl protection reaction of Example 1 to 1:1.2, the reaction temperature is changed to 110°C, the reaction time is changed to 6h, and other reaction conditions are as in Example 1 As described, bis(trimethylsiloxy)ethylamine was obtained with a yield of 93%.

Embodiment 3

[0037] Bis(trimethylsilyloxy)ethylamine: the ratio of the amount of allyl acrylate in the Michael addition reaction of Example 1 becomes 1: 1.1, and other reaction conditions are as described in Example 1, The yield of {3-[bis(trimethylsiloxy)ethyl]}aminopropionic acid allyl alcohol was 93%.

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Abstract

The invention discloses a method for synthesizing polysiloxane having a hydroxyethyl group at one end of a molecule. The preparation method of the invention comprises the following steps that: diethanolamine, hexamethyldisilazane and propenyl propionate, which serve as raw materials, undergo hydroxyl protection and Michael addition reactions to form {3-[bis(trimethylsiloxy)ethyl]}amino propenyl propionate; D3 (hexamethylcyclotrisiloxane ) serving as a raw material undergoes anionic ring opening polymerization to form polysiloxane having a hydrosil group at one end of a molecule; and {3-[bis(trimethylsiloxy)ethyl]}amino propenyl propionate and the polysiloxane having a hydrosil group at one end are used as raw materials to undergo hydrosilylation and alcoholysis reactions to form the polysiloxane having hydroxyethyl group at one end of a molecule, wherein the purity of the product is over 98 percent. The method has the advantages of mild reaction conditions, readily available raw materials, high product yield, high product purity and the like.

Description

technical field [0001] The invention relates to a method for synthesizing polysiloxane containing dihydroxyl hydrocarbon groups at one end. Background technique [0002] Due to the presence of chemically active hydroxyhydrocarbyl functional groups, hydroxyhydrocarbyl polysiloxane can react with isocyanate groups or carboxyl groups to modify certain synthetic resins (such as polyurethane and polyester) to improve resins. surface properties. As a member of the hydroxyhydrocarbyl polysiloxane family, single-ended dihydrocarbyl polysiloxane has become an important intermediate for organosilicon graft-modified polymers. [0003] In 1989, US Pat. No. 4,839,443 disclosed a method for preparing a single-end dihydroxyhydrocarbyl polysiloxane by using 2-allyloxy-1,3-propanediol and a single-end polysiloxane containing a silicon hydrogen group. [0004] In 1991, US Pat. No. 5,059,707 disclosed a method for preparing a single-end dihydroxyhydrocarbyl polysiloxane by using 2-methylene-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388
Inventor 邬元娟张萌陈子雷岳辉郭栋梁汝医
Owner 山东省农业科学院中心实验室
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