Synthesis of polysiloxane containing bishydroxymethyl at single end

A polysiloxane and bismethylol technology, which is applied in the field of polysiloxane synthesis, can solve the problems such as difficult to obtain unsaturated compounds and harsh reaction conditions for unsaturated compounds, and achieve easy separation and purification, mild conditions, and high yield. high rate effect

Inactive Publication Date: 2009-08-19
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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  • Synthesis of polysiloxane containing bishydroxymethyl at single end

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Esterification reaction (molar ratio 2,2-dimethylolpropionic acid: allyl bromide: potassium carbonate = 1: 1.2: 0.5)

[0025] In a 250mL three-necked flask, add 13.37g of 2,2-dimethylolpropionic acid, 7.00g of potassium carbonate and 100mL of N,N-dimethylformamide. The temperature of the reaction system was raised to 60° C., and 14.42 g of allyl bromide was slowly added dropwise with stirring. After the dropwise addition, the reaction was continued for 6 hours, and the reaction was stopped. Low boilers and solvents were distilled off under reduced pressure, and the fraction at 148-150°C (1.33Kpa) was collected to obtain 15.22g of colorless transparent liquid 2,2-dimethylol propionate allyl alcohol, with a yield of 87.7%

[0026] Hydroxyl protection reaction (molar ratio 2,2-dimethylol propionate: hexamethyldisilazane=1:1.5)

[0027] Into a 100 mL three-necked flask, 10.03 g of allyl 2,2-dimethylol propionate was added. At room temperature, 14.25 g of hexamethyldisilaz...

Embodiment 2

[0035] In the esterification reaction of Example 1, the ratio of the amount of 2,2-dimethylolpropionic acid and allyl bromide is changed to 1:1.5, potassium carbonate is changed to sodium carbonate, the reaction temperature is changed to 80°C, and the reaction The time was changed to 10 h, and other reaction conditions were as described in Example 1 to obtain allyl 2,2-dimethylol propionate with a yield of 84%.

Embodiment 3

[0037] The ratio of the amount of 2,2-dimethylolpropionic acid and allyl bromide in the esterification reaction of Example 1 is changed to 1:1, and other reaction conditions are as described in Example 1 to obtain 2,2 - allyl dimethylol propionate, the yield is 80%.

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Abstract

The invention discloses a method for synthesizing polysiloxane which contains bis-hydroxyl alkyl at one end. In the preparation method, allyl bromide, 2, 2-dimethylol propionic acid, hexamethyldisilazane and D3 (hexamethylcyclotrisiloxane) are used as initial raw materials on which esterification reaction, hydroxyl group protection, anionic ring opening polymerization, hydrosilylation and alcoholysis reaction are carried out to obtain a target compound of the polysiloxane which contains bis-hydroxyl alkyl at one end, and the purity of the product is higher than 98 percent. The invention has the advantages of mild reaction condition, available raw materials, high yield and purity of the product, etc.

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): C08G77/38C08G77/06
Inventor 邬元娟张萌陈子雷张红王文博汝医
Owner 山东省农业科学院中心实验室
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