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T16 cage structure epoxy phenyl silsesquioxane and preparation method thereof

A technology of epoxy phenyl and silsesquioxane, which is applied in the field of organic-inorganic hybrid material science, can solve problems such as unsuitable for expanding production and application, and achieve easy control, good thermal stability, and mild reaction conditions Effect

Active Publication Date: 2021-05-04
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The products of silsesquioxane with regular cage structure obtained through hydrolysis and condensation are mostly mixtures of T8, T10 and T12 cage structures, which are not suitable for expanded production applications

Method used

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  • T16 cage structure epoxy phenyl silsesquioxane and preparation method thereof
  • T16 cage structure epoxy phenyl silsesquioxane and preparation method thereof
  • T16 cage structure epoxy phenyl silsesquioxane and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0022] 1) In a 2L three-neck flask equipped with a magnetic stirrer, a condensing reflux device, a constant pressure dropping funnel and a constant temperature device, add 600ml of dichloromethane, 54.1g of phenyltriethoxysilane and 108.1g of 2-(3,4 -Epoxycyclohexane) ethyltriethoxysilane, stirred and heated up to 25°C, added 48ml of 0.015g / ml NaOH lye, maintained the reaction temperature at 40°C, stirred and refluxed for 12 hours to obtain a condensation reaction solution .

[0023] 2) Add an appropriate amount of 0.1mol / L hydrochloric acid solution dropwise to make the reaction solution neutral, wash with deionized water, add anhydrous sodium sulfate to remove residual moisture in the organic phase, filter, take the filtrate and spin evaporate at 40°C to remove the solvent dichloromethane, and dry the product at 80° C. for 12 hours to obtain a colorless and transparent viscous liquid T16 cage structure epoxy phenyl silsesquioxane.

[0024] figure 1 It is the FT-IR spectrum...

Embodiment 2

[0030] 1) In a 2L three-necked flask equipped with a magnetic stirrer, a condensing reflux device, a constant pressure dropping funnel and a constant temperature device, add 1200ml of methylene chloride, 108.2g of phenyltriethoxysilane and 216.3g of 2-(3,4 -Epoxycyclohexane) ethyltriethoxysilane, stirred and heated up to 25°C, added 96ml of 0.015g / ml NaOH lye, maintained the reaction temperature at 40°C, stirred and refluxed for 18 hours to obtain a condensation reaction solution .

[0031] 2) Add an appropriate amount of 0.1mol / L hydrochloric acid solution dropwise to make the reaction solution neutral, wash with deionized water, add anhydrous sodium sulfate to remove residual moisture in the organic phase, filter, take the filtrate and spin evaporate at 40°C to remove the solvent dichloromethane, and dry the product at 90° C. for 12 hours to obtain a colorless and transparent viscous liquid T16 cage structure epoxy phenyl silsesquioxane.

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Abstract

The invention relates to T16 cage structure epoxy phenyl silsesquioxane and a preparation method thereof, and belongs to the technical field of organic-inorganic hybrid materials. The preparation method comprises the following steps: adding silane containing phenyl and epoxy groups and a solvent into a reactor, stirring, controlling the temperature of the reactor to be 25 DEG C, dropwise adding a catalyst namely a NaOH solution, controlling the temperature of the reactor to be 40 DEG C, and reacting for 1-2 hours to obtain a reaction solution; and adjusting the reaction solution to be neutral by using diluted hydrochloric acid, washing by using deionized water, drying, filtering, carrying out rotary evaporation on the filtrate, and drying to obtain the T16 cage structure epoxy phenyl silsesquioxane. The single T16 cage structure epoxy phenyl silsesquioxane containing 7 phenyl groups and 9 epoxy groups obtained in the invention has good thermal stability and reaction activity; and the preparation method is mild in condition, easy to control and suitable for expanded production.

Description

technical field [0001] The invention relates to a T16 cage structure epoxy phenyl silsesquioxane and a preparation method thereof, belonging to the scientific field of organic-inorganic hybrid materials. Background technique [0002] Polyhedral Oligomeric Silsesquioxane (Polyhedral Oligomeric Silsesquioxane, POSS) is a nanoscale organic-inorganic hybrid material at the molecular level. The shell composition of the organic substituents with different properties introduced by the atoms connected. The general structural formula of POSS is (RSiO 1.5 ) n , the value of n is generally 6, 8, 10 or 12, etc. R is a variety of organic substituent groups connected to silicon atoms, which can be inactive or active groups, and the connected R groups can be changed through organic chemical reactions to obtain Functionalized POSS for specific properties. POSS has the characteristics of low molecular density, low dielectric constant, small physical size, good organic compatibility and h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/04C08G77/08
CPCC08G77/045C08G77/08
Inventor 杨荣杰周海莲张文超
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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