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Method for synthesizing asymmetric cyclotetrasiloxane

The technology of a cyclotetrasiloxane and a synthesis method, which is applied in the direction of silicon organic compounds and the like, can solve the problems of difficult separation and difficult to obtain high-purity asymmetric cyclotetrasiloxane, and achieves efficient synthesis, easy separation and purification, and reaction. mild conditions

Active Publication Date: 2014-06-18
HANGZHOU NORMAL UNIVERSITY
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the problem that it is difficult to separate and obtain high-purity asymmetric cyclotetrasiloxane due to the complex composition of the product and the similar properties of the components of the mixture when preparing asymmetric cyclotetrasiloxane, the present invention proposes a A kind of synthesis method of asymmetric cyclotetrasiloxane, the synthesis method of the present invention has the advantages of mild reaction conditions, simple product composition, easy separation and purification, high synthesis efficiency, etc.

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  • Method for synthesizing asymmetric cyclotetrasiloxane
  • Method for synthesizing asymmetric cyclotetrasiloxane
  • Method for synthesizing asymmetric cyclotetrasiloxane

Examples

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Embodiment 1

[0027] Example 1: Preparation of 1, 1, 3, 3-tetramethyl-5, 7-diphenyl-5, 7-divinylcyclotetrasiloxane

[0028] 0°C, a solution of 0.1 g of 1, 1, 3, 3-tetramethyldisiloxane-1, 3-diol sodium salt in 10 ml of tetrahydrofuran was added dropwise to a solution containing 1.0 g of 1, 3-diiodo -1, 3-diphenyl-1, 3-divinyldisiloxane and 10 ml tetrahydrofuran in a 50 ml three-neck flask, stirred for 8 hours, then added 10 ml deionized water and 10 ml n-hexane for extraction , washed the organic layer with water until neutral, and dried over anhydrous sodium sulfate. Distilled under reduced pressure to obtain a colorless liquid, i.e. 1, 1, 3, 3-tetramethyl-5, 7-diphenyl-5, 7-divinylcyclotetrasiloxane, yield 65%, product purity 96%.

Embodiment 2

[0029] Example 2: Preparation of 1, 1, 3, 3-tetravinyl-5, 7-diphenylcyclotetrasiloxane

[0030] -20°C, add 200 g of 1, 1, 3, 3-tetravinyldisiloxane-1, 3-diol in 200 ml of ether solution dropwise to 280 g of 1, 3-dichloro- 1, 3-diphenyldisiloxane, 130 grams of diethylamine and 200 milliliters of diethyl ether in a 1000 milliliter three-neck flask, after stirring for 2 hours, add 400 milliliters of deionized water for extraction, wash the organic layer with water until neutral , dried over anhydrous sodium sulfate. Distillation under reduced pressure gave a colorless liquid, namely 1, 1, 3, 3-tetraethenyl-5, 7-diphenylcyclotetrasiloxane, with a yield of 90% and a product purity of 98%.

Embodiment 3

[0031] Example 3: Preparation of 1, 3, 5, 5, 7, 7-hexamethylcyclotetrasiloxane

[0032] 10°C, 50 g of 1, 1, 3, 3-tetramethyl-1, 3-disilanol in 200 ml of 1, 4-dioxane solution was added dropwise to 55 g of 1, 3- Dichloro-1,3-dimethyldisiloxane, 50 g of pyridine and 200 ml of 1,4-dioxane in a 1000 ml three-necked flask, stirred for 15 hours, then added 200 ml of deionized water for extraction , washed the organic layer with water until neutral, and dried over anhydrous sodium sulfate. Distillation under reduced pressure gave a colorless liquid, namely 1, 3, 5, 5, 7, 7-hexamethylcyclotetrasiloxane, with a yield of 70% and a product purity of 97%.

[0033] The infrared spectrum of 1, 3, 5, 5, 7, 7-hexamethylcyclotetrasiloxane is shown in figure 1 Shown, the gas chromatography-mass spectrum of 1, 3, 5, 5, 7, 7-hexamethylcyclotetrasiloxane is as figure 2 Shown, the 1, 3, 5, 5, 7, 7-Hexamethylcyclotetrasiloxane proton nuclear magnetic resonance spectrogram is as image 3 Shown, ...

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Abstract

The invention relates to the synthesis technology field of cyclotetrasiloxane; the invention provides a method for synthesizing the asymmetric cyclotetrasiloxane in order to solve the problems that when asymmetric cyclotetrasiloxane is prepared at present, because components of a product are complicate, and partial properties of all components of a mixture are similar, the components are difficultly separated, and high-purity asymmetric cyclotetrasiloxane is difficultly obtained. The method comprises the following steps: by taking a compound represented by a general formula (I) and 1,3-dihaldisiloxane as materials, performing a synthesis reaction in an organic solvent, and separating and purifying after the reaction to obtain the asymmetric cyclotetrasiloxane. The synthesis method has the advantages of mild reaction condition, simple product components, easy separation purification and high synthesis efficiency.

Description

technical field [0001] The invention relates to the technical field of cyclosiloxane synthesis, in particular to an efficient synthesis method of asymmetric cyclotetrasiloxane. Background technique [0002] Asymmetric cyclotetrasiloxane has important uses, such as the synthesis of polysiloxanes with special structures such as hyperbranched, "beaded" polysiloxanes, and ladder polysiloxanes and the development of new silane coupling agents. The existing synthetic techniques for synthesizing asymmetric cyclotetrasiloxane all adopt the method of cohydrolysis / condensation of different difunctional silanes, which cannot control the ratio and position of functional groups, and the ring size of cyclosiloxane and avoid the formation of linear molecules , so when asymmetric cyclotetrasiloxane is prepared by cohydrolysis / condensation of difunctional silanes, a complex mixture is usually obtained, and the properties of each component are similar, it is difficult to separate, and it is d...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 李泽刘利锋吴春勇来国桥
Owner HANGZHOU NORMAL UNIVERSITY
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