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Octa-epoxy cage type sesquialter siloxane and preparation thereof

A technology of silsesquioxane and tetraethoxysilane, which is applied in the field of octaepoxy cage silsesquioxane and its preparation, can solve the problems affecting the dispersion and preparation of epoxy cage silsesquioxane The method has not been reported, and the problems such as affecting the use performance have achieved the effect of simple post-treatment method, improved compatibility, and improved reactivity.

Inactive Publication Date: 2009-08-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the epoxy group that this kind of method obtains is directly connected on the skeleton Si of cage silsesquioxane, because the steric hindrance is bigger, reactivity reduces greatly, has influenced epoxy group cage silsesquioxane in other resins. Dispersion in the medium, which in turn affects its performance
[0007] And there is no report about the eight epoxy group cage type silsesquioxane with certain length flexible chain and preparation method thereof

Method used

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

Examples

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example 1

[0023] (1) Synthesis of hydrated octapolyclathosilicate (Tetramethylammonium silicate "Octanion').

[0024] At room temperature, 104.0 g of tetraethoxysilane was added dropwise to 590 g of 10 wt % tetramethylammonium hydroxide aqueous solution, stirred evenly, and then heated to 50° C., and reacted at this temperature for 15 hours to obtain a reaction liquid. Concentrate the reaction solution 10 times with a rotary evaporator, freeze in a refrigerator to crystallize, wash the crystals with acetone, and dry in vacuo to obtain 106.1 g of white hydrated octameric clathrosilicate, with a yield of 95%. Its nuclear magnetic resonance and infrared absorption analysis characterization data are: 29 Si-NMR (119MHz, CD 3 OD, 300K, ppm)-99.1; 13 C-NMR (159MHz, CD 3 OD, 300K, ppm) 15.10; 1 H-NMR (600MHz, CD 3 OD, 300K, ppm) 3.19; FTIR (cm -1 , KBr) 3393, 1643 (v N-O ), 1489 (v as C-N ), 1116 (v Si-O-Si ).

[0025] (2) Add 20ml of dimethylchlorosilane to a mixed solvent containing...

example 2

[0029] (1) Synthesis of hydrated octapolyclathosilicate (Tetramethylammonium silicate "Octanion').

[0030] At room temperature, 104.0 g of tetraethoxysilane was added dropwise to 936 g of 10 wt % tetramethylammonium hydroxide aqueous solution, stirred evenly, then heated to 60° C., and continued to react for 10 h to obtain a reaction liquid. Concentrate the reaction solution to 8 times with a rotary evaporator, freeze in a refrigerator to crystallize, wash the crystals with acetone, and dry them in vacuum to obtain 108.3 g of white hydrated octameric clathrosilicate, with a yield of 97%. Its nuclear magnetic resonance and infrared absorption analysis characterization data are: 29 Si-NMR (119MHz, CD 3 OD, 300K, ppm)-99.1; 13 C-NMR (159MHz, CD 3 OD, 300K, ppm) 15.10; 1 H-NMR (600MHz, CD 3 OD, 300K, ppm) 3.19; FTIR (cm -1 , KBr) 3393, 1643 (v N-O ), 1489 (v asC-N ), 1116 (v Si-O-Si ).

[0031] (2) Add 30ml of dimethylchlorosilane to a mixed solvent containing 90ml of n...

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Abstract

The invention relates to octa-epoxy group cage-like silsesquioxane and a preparation method thereof. At present, the preparation of the cage-like silsesquioxane is generally not functionalized, and has a plurality of synthesis steps, low yield and too high cost. The cage-like silsesquioxane with epoxy groups is most noticeable with unique performance, but the existing cage-like silsesquioxane prepared by taking vinyl trichlorosilane as a raw material through hydrolytic condensation and oxidation is not completely epoxidized, and most of final products are mixtures. The preparation method takes industrialized tetramethyl orthosilicate or tetraethyl orthosilicate as a primary raw material, firstly synthesizes hydrated octa cage-like silicate through hydrolytic condensation, and then prepares the octa-epoxy group cage-like silsesquioxane with flexible chains through hydrosilation reaction and hydrosilylation reaction. The invention is simple and feasible, has high yield and single product structure, and is suitable for industrialized production; and the octa-epoxy group cage-like silsesquioxane has high reactivity, and is easily modified by being compounded with resins such as epoxy resin, phenolic resin, nylon, and the like so as to prepare composite materials with high performance.

Description

Technical field: [0001] The invention relates to an octaepoxy cage-type silsesquioxane and a preparation method thereof. Background technique: [0002] Silsesquioxane (silsesquioxane) is a class of substances containing RSiO1.5 (O:Si=1.5:1 in the molecule) structure, R substituents are hydrogen, alkyl, alkenyl, aryl, arylene, ring Oxygen and their derivatives. Silsesquioxane can be used as the precursor of organic-inorganic hybrid materials, functional polymers, liquid crystal materials and electroluminescent materials, etc., and has extremely broad application prospects. According to different structures, silsesquioxane can be divided into random structure, ladder structure, semi-cage structure and cage structure. Among them, the performance of clathrate silsesquioxane is outstanding, which has aroused great interest and attention in recent years. [0003] Polyhedral Oligomeric Silsesquioxane (Polyhedral Oligomeric Silsesquioxane, POSS) is called cage silsesquioxane beca...

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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