Preparation method of cage type n-propyl oligomeric silsesquioxane

A technology of polysilsesquioxane and propyltrimethoxysilane, applied in the direction of organic silicon compounds, etc., can solve the problems of difficult reaction control, complicated treatment process, a large amount of waste acid, etc., and achieves short preparation period and high yield. High and pollution-reducing effect

Active Publication Date: 2012-07-11
SHANDONG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation method adopted in the prior art has the disadvantages that the reaction is not easy to control, a large amount of waste acid will be produced in the process of hydrolysis and condensation, the treatment process is relatively complicated and the yield is low.

Method used

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  • Preparation method of cage type n-propyl oligomeric silsesquioxane
  • Preparation method of cage type n-propyl oligomeric silsesquioxane
  • Preparation method of cage type n-propyl oligomeric silsesquioxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 1L grinding bottle, add 0.6L of ethanol, 56.0mL of concentrated hydrochloric acid (38wt%), and 50.0mL of n-propyltriethoxysilane in sequence, mix well, and seal the bottle. Control the temperature of the reaction solution at 0-5°C, let the system hydrolyze and condense for 96 hours under stirring conditions, remove the reaction solution by filtration to obtain a white powder solid, wash with methanol three times, and dry in a vacuum oven for 5.0 hours to obtain 15.1997 g products. The yield was 73.9%. Structure Characterization: 29 Si-NMR, -66.93ppm (CDCl 3 ); 1 H-NMR, 0.63ppm (t, Si-CH 2 -, 2H), 0.98ppm (t, -CH 3 , 3H) and 1.47ppm (m, -CH 2 -,2H)(CDCl 3 ); 13 C-NMR, 14.40ppm, 16.33ppm and 17.33ppm (CDCl 3 ); FTIR, 1114cm -1 (νSi-O-Si), 1220cm -1 (νSi-C), 2958cm -1 , 2930cm -1 and 2872cm -1 (ν C-H), 1464cm -1 and 1378cm -1 (δC-H); MS, [M] + =762.5925; single crystal diffraction, C 24 h 56 Si 8 o 12 , M=761.88, triclinic, space group P -1 , ...

Embodiment 2

[0032] In a 3L round bottom flask, add 1.6L of methanol, 200.0mL of concentrated hydrochloric acid (37%), and 150.0mL of n-propyltriethoxysilane in sequence, mix well, and seal the bottle. Control the temperature of the reaction solution at 0-5°C, let the system hydrolyze and condense for 120 hours under stirring conditions, and use the filtered reaction solution for later use to obtain a white powder solid, wash it with methanol three times, and dry it in a vacuum oven for 5 hours to obtain 43.9950g product. The yield was 71.3%, and the structural characterization of the product was as in Example 1.

Embodiment 3

[0034] In a 500mL ground-mouth Erlenmeyer flask, add 200mL of ethanol and 80.0mL of the filtered mother liquor in Example 1, 20.0mL of concentrated hydrochloric acid (36.5wt%), and 21.0mL of n-propyltrimethoxysilane, mix well, and seal bottle mouth. Control the temperature of the reaction solution at 0-5°C, let the system hydrolyze and condense for 80 hours under stirring conditions, remove the reaction solution by filtration to obtain a white powder solid, wash with methanol three times, and dry in a vacuum oven for 5 hours to obtain 9.4327g product. The yield was 83.2%, and the structural characterization of the product was as in Example 1.

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Abstract

The invention relates to a preparation method of cage type n-propyl oligomeric silsesquioxane. N-propyl triethoxy silane or n-propyl trimethoxy silane is utilized as a raw material and alcohol serves as a solvent. The method includes performing hydrolytic condensation reaction under catalysis of concentrated hydrochloric acid of 36-38 wt% to prepare the cage type n-propyl oligomeric silsesquioxane with 8 n-propyls. The preparation method is convenient to operate, the raw material is easy to obtain, the polymerization reaction is mild in reaction condition and easy to control, and the product is high in yield, low in cost and small in pollution.

Description

technical field [0001] The invention relates to a preparation method of cage-type n-propyl oligomeric silsesquioxane. Background technique [0002] As a new type of inorganic / organic hybrid material, cage silsesquioxane can achieve hybridization on the nanoscale, combining the toughness and excellent processing performance of organic polymer materials with the oxidation resistance and high temperature resistance of inorganic materials. Combined with excellent mechanical properties, it has potential application value in fillers, liquid crystals, catalysts and biocompatible materials, and has attracted widespread attention. [0003] Polyhedral oligomeric silsesquioxane refers to the molecular formula (RSiO 1.5 ) n (n = 6, 8, 10, 12, 14, ...; R = H, alkyl, aryl or other organic functional groups) silicon-containing compounds, wherein the typical n = 8 cage octahedral low Polysilsesquioxane has a structure shown in Formula 1 below. In the cage octahedral oligomeric silsesqui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 朱庆增刘慧
Owner SHANDONG UNIV
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