Preparation method of short range ordered cage type aminopropyl silsesquioxane spherical particles

A technology of silsesquioxane and aminopropyltrimethoxysilane, which is applied in the field of preparation of spherical aminopropylsilsesquioxane particles, can solve the problems of irregular morphology and structure of the product, and achieve a simple reaction system Ease of operation, high yield, and ease of large-scale production

Inactive Publication Date: 2015-04-22
YUNCHENG UNIVERISTY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the traditional synthesis method, the reaction system is a homogeneous react

Method used

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  • Preparation method of short range ordered cage type aminopropyl silsesquioxane spherical particles
  • Preparation method of short range ordered cage type aminopropyl silsesquioxane spherical particles
  • Preparation method of short range ordered cage type aminopropyl silsesquioxane spherical particles

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0023] Example 1

[0024] 1. Dehydration treatment of tribenzoic acid

[0025] Put s-tribenzoic acid in an oven, heat and dehydrate at 80°C for 2h.

[0026] 2. Preparation of ethanol solution of γ-aminopropyltrimethoxysilane

[0027] Add 20mL of absolute ethanol into a 50mL three-necked flask, then measure 1mL of γ-aminopropyltrimethoxysilane into the flask, seal it, and stir with a stirrer at 180 rpm for 30-50min to obtain γ-aminopropyltrimethoxysilane ethanol solution of silane.

[0028] 3. Hydrolysis and condensation reaction

[0029] Weigh the m-tribenzoic acid prepared in step 1 and add it to the ethanol solution of gamma-aminopropyltrimethoxysilane prepared in step 2. The molar ratio of m-tribenzoic acid to gamma-aminopropyltrimethoxysilane is 1: 3. Stir for 30 minutes until the solids are completely dissolved. Then, 0.3 mL of ammonia solution with a pH of 10 was added, the stirring was continued for 10 min, and then the stirring was stopped. The reaction was left t...

Example Embodiment

[0032] Example 2

[0033] 1. Dehydration treatment of tribenzoic acid

[0034] Put s-tribenzoic acid in an oven, heat and dehydrate at 80°C for 2h.

[0035] 2. Preparation of ethanol solution of γ-aminopropyltrimethoxysilane

[0036] Add 20mL of absolute ethanol into a 50mL three-necked flask, then measure 1mL of γ-aminopropyltrimethoxysilane into the flask, seal it, and stir with a stirrer at 180 rpm for 30-50min to obtain γ-aminopropyltrimethoxysilane ethanol solution of silane.

[0037] 3. Hydrolysis and condensation reaction

[0038] Weigh the m-tribenzoic acid prepared in step 1 and add it to the ethanol solution of gamma-aminopropyltrimethoxysilane prepared in step 2. The molar ratio of m-tribenzoic acid to gamma-aminopropyltrimethoxysilane is 1: 1. Stir for 30 minutes until the solid is completely dissolved; then, add 0.3 mL of ammonia solution with a pH of 10, continue stirring for 10 minutes, stop stirring, let stand for 24 hours, and separate by centrifugation to...

Example Embodiment

[0041] Example 3

[0042] 1. Dehydration treatment of tribenzoic acid

[0043] Put s-tribenzoic acid in an oven, heat and dehydrate at 80°C for 2h.

[0044] 2. Preparation of ethanol solution of γ-aminopropyltrimethoxysilane

[0045] Add 20mL of absolute ethanol into a 50mL three-necked flask, then measure 1mL of γ-aminopropyltrimethoxysilane into the flask, seal it, and stir with a stirrer at 180 rpm for 30-50min to obtain γ-aminopropyltrimethoxysilane ethanol solution of silane.

[0046] 3. Hydrolysis and condensation reaction

[0047] Weigh the m-tribenzoic acid prepared in step 1 and add it to the ethanol solution of gamma-aminopropyltrimethoxysilane prepared in step 2. The molar ratio of m-tribenzoic acid to gamma-aminopropyltrimethoxysilane is 1: 2. Stir for 30 minutes until the solid is completely dissolved; then, add 0.3 mL of ammonia solution with a pH of 10, continue stirring for 10 minutes, stop stirring, let stand for 24 hours, and separate by centrifugation to...

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Abstract

The invention relates to a preparation method of short range ordered cage type aminopropyl silsesquioxane spherical particles, belongs to the technical field of materials and particularly relates to a preparation method of cage type aminopropyl silsesquioxane spherical particles of short range ordered structures. The aminopropyl silsesquioxane spherical particles prepared by the method can be used for removing metal ions in a solution and adsorbing carbon dioxide gas. The invention provides the preparation method of the short range ordered cage type aminopropyl silsesquioxane spherical particles, wherein the preparation method is simple and convenient to operate, short in reaction time and mild in reaction condition. The preparation method comprises the following steps: dehydrating trimethylbenzoic acid; preparing an ethanol solution of gamma-aminopropyl trimethoxy silane; carrying out hydrolysis-condensation reaction; and washing by alkali. The short range ordered cage type aminopropyl silsesquioxane spherical particles provided by the invention are mainly applied to the field of adsorption and separation, drug delivery, modification of high polymers and the like.

Description

technical field [0001] The preparation method of short-range ordered cage-type aminopropyl silsesquioxane spherical particles of the present invention belongs to the field of material technology, and specifically relates to a preparation method of spherical aminopropyl silsesquioxane particles with a short-range ordered structure , the aminopropyl silsesquioxane particles prepared by the method can be used for the removal of metal ions in the solution and the adsorption of carbon dioxide gas. Background technique [0002] The general formula of cage polysilsesquioxane is (RSiO 1.5 )n, wherein R is an organic group connected by eight vertex Si atoms, and common R groups are reactive or inert groups such as vinyl, epoxy, amino, and phenyl groups. The cage frame structure of cage polysilsesquioxane makes it have good dielectric and optical properties, and is widely used in high temperature resistant materials, flame retardant materials, electrical insulation materials, electro...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 宋少飞周福林李平弓巧娟薛娜娜吕宝华
Owner YUNCHENG UNIVERISTY
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