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Octa-aminopropyl cage type sesquialter siloxane and preparation thereof

A technology of silsesquioxane and octaaminopropyl cages, which is applied in the direction of silicon organic compounds, can solve the problems of complex formation process, insufficient understanding of formation mechanism, and numerous influencing factors, so as to improve yield and avoid random compounds The formation and the effect of simplifying the preparation process

Active Publication Date: 2009-08-12
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

However, due to the extremely complex formation process of cage silsesquioxanes, many influencing factors, and insufficient understanding of its formation mechanism, only a handful of cage silsesquioxanes with active functional groups can be prepared in one step. , reported in the literature are octavinyl clathrate silsesquioxane, octaammonium salt clathrate silsesquioxane, etc.

Method used

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  • Octa-aminopropyl cage type sesquialter siloxane and preparation thereof
  • Octa-aminopropyl cage type sesquialter siloxane and preparation thereof
  • Octa-aminopropyl cage type sesquialter siloxane and preparation thereof

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example 1

[0024] Add 500ml of ethanol, 50ml of deionized water, and 1.3ml of tetramethylammonium hydroxide into a 1000ml flask in sequence, and stir at room temperature to make the mixture even. Then, 66.39 g of γ-aminopropyltriethoxysilane was added dropwise to the above mixed solution, followed by stirring. After the dropwise addition, the reaction was continued at this temperature for 3h. Then the temperature was raised to 80° C., and the reaction was continued for 10 h under reflux, and the reaction ended. The reaction solution obtained in step (1) was distilled under reduced pressure, concentrated to 80ml, and then the concentrated solution was added dropwise to 1600ml of petroleum ether. After the dropwise addition, it was left to stand for 3 hours, and a large amount of white solids were precipitated. After vacuum filtration, washing the crude product with acetone, and vacuum drying, 29.73 g of octaaminopropyl clathrate silsesquioxane was finally obtained, with a yield of 90%. ...

example 2

[0029] Add 360ml of methanol, 30ml of deionized water, and 1.4ml of tetraethylammonium hydroxide into a 500ml flask, and stir at room temperature to make the mixture even. Then, 35.85 g (0.2 mol) of γ-aminopropyltrimethoxysilane was added dropwise to the above mixed solution, followed by stirring. After the dropwise addition, the reaction was continued at this temperature for 5h. Then the temperature was raised to 70° C., and the reaction was continued for 12 h under reflux, and the reaction was completed. The above reaction solution was distilled under reduced pressure, concentrated to 50ml, and then the concentrated solution was added dropwise to 1000ml of petroleum ether, and left to stand after the dropwise addition until a large amount of white solids were precipitated. After vacuum filtration, washing the crude product with acetone, and vacuum drying, 20.27 g of octaaminopropyl clathrate silsesquioxane was finally obtained, with a yield of 92%. The structural character...

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Abstract

The invention relates to octa-aminopropyl cage-like silsesquioxane and a preparation method thereof. The cage-like silsesquioxane has the advantages of organic and inorganic compounds, thus arousing wide concern among the people as a novel functional material. At present, the cage-like silsesquioxane which can be synthesized is generally not functionalized, and has a plurality of synthesis steps and lower yield. The preparation method directly prepares the cage-like silsesquioxane with eight active functional groups by taking industrialized aminopropyltrimethoxysilane (aminopropyltriethoxysilane) as a primary raw material and alcohols and deionized water as solvents under the catalysis of tetramethyl ammonia hydroxide (tetraethyl ammonia hydroxide) through hydrolytic condensation. The preparation method has the advantages of cheap and easily obtained raw materials, green environment-protective used solvents, short preparation period, high yield, and the like, is suitable for industrialized production in large scale, is easy for epoxy resin compounding and can significantly improve the comprehensive performance of epoxy resin, thus having good industrial application prospect.

Description

Technical field: [0001] The present invention relates to the preparation method of octaaminopropyl clathrate silsesquioxane Background technique: [0002] With the development of social informatization, high-speed information processing and information dissemination, it is urgent to provide an electronic composite material with high heat resistance. Epoxy resin has become a widely used electronic composite material due to its good processing performance, low price, sufficient supply, and excellent comprehensive performance. However, the existing pure epoxy resin has poor heat resistance and cannot meet the requirements of some high-temperature electronic composite materials. Only by modifying it can epoxy resin become a cost-effective electronic packaging material. [0003] Generally speaking, plastics can have good mechanical properties and dimensional stability only below the glass transition temperature. To improve the heat resistance of materials, their glass transition...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 李齐方宋江选
Owner BEIJING UNIV OF CHEM TECH
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