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Cage-type diphenyl sulfone-based oligomeric silsesquioxane and preparation method for same

A technology of polydiphenylsulfone and sesquioxane, applied in the field of nanomaterials, can solve problems such as poor solubility, and achieve mild and stable reaction conditions, good repeatability, and improved dielectric effects.

Active Publication Date: 2013-07-10
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Silsesquioxanes have received more and more attention, among which phenylsilsesquioxane is also favored due to its excellent thermal stability, but its application is limited due to its poor solubility

Method used

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  • Cage-type diphenyl sulfone-based oligomeric silsesquioxane and preparation method for same
  • Cage-type diphenyl sulfone-based oligomeric silsesquioxane and preparation method for same
  • Cage-type diphenyl sulfone-based oligomeric silsesquioxane and preparation method for same

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Experimental program
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Effect test

Embodiment 1

[0031] 1) Add 3.70g of cage-type octaphenylsilsesquioxane and 15ml of chloroform into a 100ml three-neck flask equipped with a reflux condenser, constant pressure dropping funnel, temperature control device, argon protection and magnetic stirring, Stir, the temperature is 60°C, add 3.81g of aluminum trichloride, then dropwise add 5.29g of benzenesulfonyl chloride, and react for 72 hours after the dropwise addition to obtain a reaction solution;

[0032] 2) Filter the reaction solution obtained in step 1), place the filtrate in a conical separatory funnel, wash it 3 times with a mixture of 200ml hydrochloric acid and ice water (the volume ratio of hydrochloric acid and ice water is 1:1), and then The organic layer was added into 500ml of n-hexane to precipitate a precipitate, which was dried in a vacuum oven at 50°C for 24 hours to obtain cage-type diphenylsulfone silsesquioxane with a yield of 3.17g. The obtained cage diphenylsulfone-based silsesquioxane is silsesquioxane cont...

Embodiment 2

[0037]1) Add 5.17g of cage-type octaphenylsilsesquioxane and 20ml of dichloromethane into a 100ml three-neck flask equipped with a reflux condenser, constant pressure dropping funnel, temperature control device, argon protection and magnetic stirring, Stir, the temperature is 25°C, add 5.33g of aluminum trichloride in two times with an interval of 10 minutes, then add 7.08g of benzenesulfonyl chloride dropwise, and react for 48 hours after the dropwise addition to obtain a reaction solution;

[0038] 2) Filter the reaction solution obtained in step 1), place the filtrate in a conical separatory funnel, wash it 3 times with a mixture of 200ml hydrochloric acid and ice water (the volume ratio of hydrochloric acid and ice water is 1:1), and then The organic layer was added to 500ml of ethanol to precipitate a precipitate, which was dried in a vacuum oven at 50°C for 24 hours to obtain cage-type diphenylsulfone silsesquioxane with a yield of 4.42g. The obtained cage diphenylsulfon...

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Abstract

The invention relates to a cage-type diphenyl sulfone-based oligomeric silsesquioxane and a preparation method for the same, and belongs to the technical field of nanometre materials. The cage-type diphenyl sulfone-based oligomeric silsesquioxane disclosed by the invention contains 1, 2, 3, 4, 5, 6, 7 or 8 diphenyl sulfone groups. The cage-type diphenyl sulfone-based oligomeric silsesquioxane disclosed by the invention has the characteristics of being moderate and stable in reaction conditions, good in repeatability, high in productivity, short in cycle and the like, and is suitable for expanded production; and the obtained product is added in a polymer by means of blending or copolymerization and the like, and capable of improving the various performances of dielectricity, mechanical property, flame retardance, high-temperature resistance and the like of the polymer.

Description

technical field [0001] The invention relates to a cage-type oligomeric diphenylsulfone silsesquioxane and a preparation method thereof, belonging to the technical field of nanometer materials. Background technique [0002] The research on organic-inorganic hybrid materials began in the 1980s. This new type of material, which combines the toughness and processability of the organic phase with the rigidity, dimensional stability and thermal stability of the inorganic phase, can play an organic role. The synergistic advantages of phase and inorganic phase. In the past ten years, based on the repeating unit for RSiO 1.5 The silsesquioxane compound has attracted much attention as an organic- Inorganic hybrid materials. The general chemical formula of silsesquioxane is (RSiO 1.5 ) n , where n is usually 6, 8, 10. The core of the compound is a cage-type inorganic skeleton composed of silicon and oxygen. The group R connected to the apex Si can be reactive or non-reactive, suc...

Claims

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Application Information

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IPC IPC(8): C07F7/21
Inventor 杨荣杰李紫千
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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