Dihydroxyl-terminated polydimethylsiloxane and preparation thereof

A technology of dihydroxyalkyl polydimethylsiloxane and epoxyalkyl polydimethylsiloxane, which is applied in the field of synthesizing single-end dihydroxylalkyl polydimethylsiloxane and can solve the problem of single-end dihydroxylalkyl polydimethylsiloxane The industrialization cost of polydimethylsiloxane is increased, unsaturated compounds are not easy to obtain, and the total reaction time is longer, etc., to achieve the effect of easy separation and purification, shorter reaction time, and fewer synthesis steps

Inactive Publication Date: 2008-10-01
QILU UNIV OF TECH
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Problems solved by technology

[0004] In the synthetic methods reported in the above two patents, there are the following disadvantages: (1) the unsaturated compound containing dihydroxyl used in the synthesis of the target compound is not easy to obtain, and the price is expensive
(2) The synthetic method adopts hexamethyldisilazane or trimethylchlorosilane as protecting group, and the cost is higher
(3) The protection and deprotection reaction of the hydroxyl group increases the reaction steps and makes the total reaction time of the synthetic target compound longer
The above three disadvantages increase the industrialization cost of single-ended dihydroxyalkyl polydimethylsiloxane, and the market price is high, which is not conducive to expanding the application field

Method used

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  • Dihydroxyl-terminated polydimethylsiloxane and preparation thereof

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Embodiment 1

[0020] Anionic ring-opening polymerization reaction: Add D 3 (19.52g) of benzene solution and 0.014mol n-butyllithium, stirred at room temperature for 0.5h, then added 60ml of tetrahydrofuran, stirred at 25°C, reacted for 8h, added end-capping agent dimethylchlorosilane, after the end, filtered off The generated lithium chloride was distilled under reduced pressure to remove low boilers, and cooled to obtain 20.68 g of a colorless and transparent liquid single-ended hydrogen polydimethylsiloxane, with a yield of 98%.

[0021] Hydrosilylation reaction: In a 100ml four-neck flask, add a toluene solution of allyl glycidyl ether (2.78g) and an appropriate amount of catalyst (isopropanol solution of chloroplatinic acid), and after passing nitrogen gas for 0.5h, continue Ventilate and heat the reaction system to raise the temperature. After it is stabilized to 100°C, stir, add single-ended hydrogen polydimethylsiloxane (7.33g) dropwise, react for 8h, cool, remove low boilers by dist...

Embodiment 2

[0024] The ethanol in the epoxy ring-opening reaction of Example 1 was changed to methanol, and the reaction temperature was changed to 65° C., and other reaction conditions were as described in Example 1 to obtain the target compound single-ended dihydroxyalkyl polydimethylsiloxane, Yield 95%.

Embodiment 3

[0026] The ethanol in the epoxy ring-opening reaction in Example 1 was changed to n-propanol, the reaction temperature was changed to 90°C, and other reaction conditions were as described in Example 1 to obtain the target compound single-ended dihydroxyalkyl polydimethylsiloxane Alkanes, yield 92%.

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Abstract

The invention provides a new method for preparing single-ended double-hydroxyl alkyl polydimethylsiloxane and the preparation method of the invention is different from prior synthetic methods. The preparation method takes D3 (Hexamethylcyclotrisiloxane), allyl glycidyl ether and methylaminoethanol as starting raw materials which go through three-step reactions of anion ring-opening polymerization, hydrosilylation and epoxy ring-opening to synthesize the target product of the single-ended double-hydroxyl alkyl polydimethylsiloxane of which the product purity is over 98 percent. The invention has the advantages of simple and convenient reaction steps, easily accessible raw materials, low production cost, high product yield, high purity, etc.

Description

Technical field: [0001] The invention relates to a new method for synthesizing single-end dihydroxyl hydrocarbon-based polydimethylsiloxane. The method is based on D 3 , allyl glycidyl ether and methylaminoethanol were used as starting materials, and the target compound single-ended dihydroxyalkyl polydimethylsiloxane was synthesized through three-step reactions of anionic ring-opening polymerization, hydrosilylation and epoxy ring-opening. Background technique: [0002] Single-ended dihydroxyalkyl polydimethylsiloxane is an important intermediate of organosilicon graft-modified polymers. Since the dihydroxyl groups of this type of organosilicon compound are relatively active, its reactivity can be used to Some synthetic resins (such as polyurethane, polyester, etc.) are grafted and modified to improve the surface properties of the resin. [0003] European Patent EP 0 356 963 (1989) discloses a method for the synthesis of single-ended dihydroxyalkyl polydimethylsiloxanes. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/388C08G77/38C08G77/12
Inventor 张庆思孙海峰张萌于一涛
Owner QILU UNIV OF TECH
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