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Process for preparing amino phenyl silsesquioxane

A technology of silsesquioxane and octaaminobenzene, which is applied in the field of nanomaterials to achieve the effect of improving heat resistance

Inactive Publication Date: 2006-10-11
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its preparation method still uses formic acid as the hydrogen donor and uses the Pd / C catalytic system

Method used

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  • Process for preparing amino phenyl silsesquioxane

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Embodiment 1

[0021] Example 1: Add 1.79 mmol (2.5 g) of octanitrophenyl cage silsesquioxane (hereinafter referred to as ONPS), 50 mL of tetrahydrofuran, and 2 g of Fe / C supported catalyst into a 500 mL three-necked flask, stir and mix, and heat up to 60° C.; add hydrazine hydrate (80%), the weight ratio of hydrazine hydrate to ONPS is 3:1, react for another 4 hours, and stop the reaction. Cool down to room temperature, filter, add ethyl acetate for extraction, precipitate in petroleum ether, separate and dry to obtain a white precipitate, namely octaaminophenyl cage silsesquioxane, with a yield of 82% and a reduction efficiency of 100%.

Embodiment 2

[0022] Embodiment 2: prepare octapolyaminophenyl cage type silsesquioxane with the method of embodiment 1, operation step is identical with example 1, and difference is that the weight ratio of hydrazine hydrate and ONPS is 2: 1, and solvent is 1 , 4-dioxane, and the reaction temperature is 100° C. to finally obtain octaaminophenyl cage silsesquioxane with a yield of 77% and a reduction efficiency of 100%.

Embodiment 3

[0023] Embodiment 3: Prepare octaaminophenyl cage type silsesquioxane with the method of embodiment 1, operation procedure is identical with example 1, difference is octanitrophenyl cage type silsesquioxane, solvent, Fe The weight ratio of the / C catalyst three is 10: 200: 10, the weight ratio of hydrazine hydrate and ONPS is 8: 1, and the temperature of reaction is 50 ℃, finally obtains octaaminophenyl cage silsesquioxane, productive rate 71 %, the reduction efficiency is 99%.

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Abstract

This invention belonging to nano material technology is the synthesis of eight-amino-benzene cage model sesquialter siloxane. The previous method adopts aminic acid as hydrogen donor and Pd / C catalysis system. Our method is as followings:mix the eight-nitrobenzene cage model sesquialter siloxane, solvent and Fe / C catalysis in the weight propotion of 10:50-200:2-10,stiring in the air or nitrogen at 50- 100deg C; add 2-4 weight folds hydrazine hydrate or phenylhydrazine into eight-nitrobenzene cage model sesquialter siloxane, react for 2-12 hours; cool to ambience temperature, filter and add acetic ester for extraction, wait to layers; Get organic facies and precipitate in ligarine,obtain white sediment after separation and dry. This invention is advantageous in cheap, stable and long-term active Fe / C catalysis system, is advantageous in production efficiency.

Description

technical field [0001] The invention relates to a synthesis method of silsesquioxane. More specifically, it relates to a synthesis method of octaaminophenyl cage silsesquioxane, which belongs to the technical field of nanomaterials. Background technique [0002] Silsesquioxane is a class of structural formula (RSiO 1.5 ) n compound of. There are mainly different structural types such as random, trapezoidal, bridge-shaped and cage-shaped. Among them, the cage structure is the most researched class of silsesquioxanes. [0003] Octaaminophenyl cage silsesquioxane is a hexahedron with each face composed of silicon-oxygen eight-membered rings, in which eight aminophenyl cage groups are respectively connected at the vertices of the eight silicon atoms of the polyhedron. The structural symmetry of this macromonomer is very strong, and it has organic functional groups with multiple chemical properties. At the same time, its three-dimensional size is about 1.5nm. Starting from i...

Claims

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Application Information

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IPC IPC(8): C07F7/02
Inventor 余鼎声张骏徐日炜张立群张军营
Owner BEIJING UNIV OF CHEM TECH
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