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Amino phenyl cage type sesqui siloxane and its preparing method

A technology of silsesquioxane and aminophenyl, which is applied in the direction of silicon organic compounds, can solve the problems of low yield, complicated route, and low reactivity of aliphatic amines, so as to improve mechanical properties and dielectric properties, Delayed glass transition and increased heat resistance temperature

Inactive Publication Date: 2007-08-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The cage silsesquioxanes that have been synthesized so far are hydrolyzed products of chlorosilanes and alkoxysilanes, and there are many groups such as cyclopentyl, cyclohexyl, isobutyl or trimethoxysilyl on the top angle. If you want to synthesize functionalized cage silsesquioxane by never fully condensing heptatrisilanol and trichlorosilane by the "top angle-capping" method, you must first functionalize trichlorosilane, because trichlorosilane Hydrogen silicon is flammable and explosive and complicates the route, the operating conditions are harsh, and the yield is not high (F.J.Feher, K.J.Weller, J.J.Schwab, Organometallics 1995, 14 (4), 2009); Functionalized cage silsesquioxanes, the above route is not feasible
American hybrid plastics company synthesized fatty amine silsesquioxane (1-(3-aminopropyl)- 3,5,7,9,11,13,15-heptacyclohexylpentacycol-[9.5.1.13.9.15,15.17.13]octasiloxane)( www.hybridplastics.com ), this route is only suitable for the synthesis of aliphatic amine silsesquioxanes, and the yield is low and the purification process is complicated
At the same time, in the reaction with epoxy resin, aliphatic amines have low reactivity and slow reaction speed, and their modification effect is not as good as that of aromatic amines.
And there is no report about aminophenyl cage type silsesquioxane and preparation method thereof

Method used

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  • Amino phenyl cage type sesqui siloxane and its preparing method
  • Amino phenyl cage type sesqui siloxane and its preparing method
  • Amino phenyl cage type sesqui siloxane and its preparing method

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Aminophenyl heptacyclopentyl octacage silsesquioxane (1-(2(4)-aminophenyl)-3,5,7,9,11,13,15-heptacyclopentylpentacycol-[9.5.1.1 3.9. 15, 15.17.13] synthesis of octasiloxane).

[0026] (1) Add 8.22g (9.41mmol) of dry heptacyclopentylheptasilatriol, 200mL of tetrahydrofuran, and 5mL of pyridine to a 500mL round-bottomed flask, stir well at 0°C, and inject 2.0g (9.41mmol) of phenyl Trichlorosilane ((C 6 h 5 ) SiCl 3 ). Thereafter, the temperature was raised to 10° C., and the reaction was carried out for 4 hours. The insoluble matter was filtered off, and the filtrate was evaporated with a rotary evaporator to 10 mL of the solvent remaining, and a white solid was precipitated, filtered with suction, and the filter cake was washed with acetone and water respectively, and dried to obtain 8.45 g (8.66 mmol) of a white crystalline powder, which was benzene Cage silsesquioxane (C 6 h 5 )(C 5 h 9 ) 7 Si 8 o 12 . Yield: 92%. Through nuclear magnetic resonance spectr...

Embodiment 2

[0030] Aminophenyl heptacyclohexyl cage octapolysilsesquioxane (1-(2(4)-aminophenyl)-3,5,7,9,11,13,15-heptacyclohexylpentacycol-[9.5.1.13.9.15, 15.17.13] Synthesis of octasiloxane).

[0031] (1) Add 6.52g (6.71mmol) dry incompletely condensed heptacyclohexylheptasilatriol, 150mL tetrahydrofuran, and 5mL pyridine to a 500mL round-bottomed flask, stir well at 5°C, and inject 1.56g (7.38mmol) of benzene trichlorosilane, stirred. Thereafter, the temperature was raised to 30° C., and the reaction was carried out for 8 hours. Then the reaction solution was vacuum-filtered, and the filtrate was evaporated to 15 mL of solvent with a rotary evaporator, and a white solid was precipitated. After suction filtration, the filter cake was washed with acetone and water respectively, and dried to obtain 7.45 g (6.94 mmol) of a white crystalline powder. , is cage silsesquioxane ((C 6 h 5 )(C 6 h 11 ) 7 Si 8 o 12 ). Calculated yield: 94%. Characterization data: 29 Si NMR (119MHz, CDC...

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Abstract

The present invention relates to a kind of cage type amino phenyl sesqui siloxane and its preparation process. Industrial phenyl trichloro silane as primary material is first synthesized into cage type sesqui siloxane with phenyl group, and through further nitration of the phenyl group and amino group functionalization, cage type amino phenyl sesqui siloxane is prepared. Without the step of trichloro silane with trichlorohydro silicide, the present invention has simplified preparation process, low cost and raised epoxy resin modifying performance.

Description

Technical field: [0001] The invention relates to an aminophenyl cage silsesquioxane and a preparation method thereof. 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 certain high-temperature electronic composite materials. The use of materials requires that only the modification method can make epoxy resin a cost-effective and ideal electronic composite 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 mater...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/02
Inventor 李齐方张立培
Owner BEIJING UNIV OF CHEM TECH