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Reaction catalyst system for synthesizing bridged polysilsesquioxane microspheres and application thereof

A polysilsesquioxane, catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, microsphere preparation, etc., can solve the problem of high size uniformity, low yield, Large size dispersion and other problems, to achieve the effects of high size uniformity, simple and easy process, and less side reactions

Inactive Publication Date: 2014-07-30
CHANGAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has few side reactions in the reaction system, simple process and easy preparation, and the yield of the obtained bridged polysilsesquioxane microspheres reaches more than 96%. The microspheres are monodisperse and have high size uniformity, which effectively solves the existing problem The bridged polysilsesquioxane prepared by the process has the disadvantages of low yield and large size dispersion, and the synthesized bridged polysilsesquioxane microspheres have good storage stability, and there is no obvious change for more than one year in airtight storage

Method used

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  • Reaction catalyst system for synthesizing bridged polysilsesquioxane microspheres and application thereof
  • Reaction catalyst system for synthesizing bridged polysilsesquioxane microspheres and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1. Under nitrogen protection, under constant temperature conditions of 60°C, mix 60mL of ethanol with a volume concentration of 95% or more, 3mL of tetramethylammonium hydroxide and 100mL of ammonia water with a concentration of 5mol / L, and then stir evenly to obtain a mixed solution;

[0027] Step 2. Under the protection of nitrogen, under the condition of constant temperature stirring at 60 ° C, 50 mL of bridging bistrimethoxysilane (1,2-bis(trimethoxysilyl) ethane with ethyl as the bridging group) ) was added dropwise to the mixed solution described in step 1, and after the dropwise addition was completed, reflux and stirred for 12h, and then the reaction solution was filtered to obtain a white solid crude product; the 1,2-bis(trimethoxysilyl)ethane Molecular formula is

[0028] Step 3. Wash the crude white solid product described in step 2 with deionized water and acetone three times in sequence, and then vacuum-dry the crude white solid product after washing...

Embodiment 2

[0031] Step 1. Under nitrogen protection, under constant temperature conditions of 50°C, mix 80mL of ethanol with a volume concentration of 95% or more, 4mL of tetramethylammonium hydroxide and 80mL of ammonia water with a concentration of 10mol / L, and then stir evenly to obtain a mixed solution;

[0032] Step 2, under the protection of nitrogen, under the condition of constant temperature stirring at 50 ° C, 60 mL of bridged bistrichlorosilane (1,8-bis(trichlorosilyl) n-octane) with n-octyl as the bridging group ) was added dropwise to the mixed solution described in step 1, and after the dropwise addition was completed, reflux and stirred for 15 hours, and then the reaction solution was filtered to obtain a white solid crude product; the 1,8 - The molecular formula of bis(trichlorosilyl)-n-octane is

[0033] Step 3. Wash the crude white solid product described in step 2 with deionized water and acetone four times in sequence, and then vacuum-dry the crude white solid produ...

Embodiment 3

[0036] Step 1. Under nitrogen protection, under constant temperature conditions of 70°C, mix 90mL of acetone with a volume concentration of 95% or more, 5mL of tetraethylammonium hydroxide and 100mL of ammonia water with a concentration of 3mol / L, and then stir evenly to obtain a mixed solution;

[0037] Step 2. Under the protection of nitrogen, under the condition of constant temperature stirring at 70 ° C, 100 mL of bridged bistrimethoxysilane (1,4-bis(trimethoxysilyl) benzene) with phenyl as the bridging group Add it dropwise to the mixed solution described in step 1, reflux and stir for 5 hours after the dropwise addition is completed, then filter the reaction solution to obtain a white solid crude product; the molecular formula of the 1,4-bis(trimethoxysilyl)benzene is

[0038] Step 3. The white solid crude product described in step 2 is washed twice with deionized water and acetone in turn, and then the washed white solid crude product is vacuum-dried to obtain a white po...

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Abstract

The invention discloses a synthesis method of monodisperse bridged polysilsesquioxane microspheres, which comprises the following steps: 1. in a nitrogen protective atmosphere, mixing and uniformly stirring a cosolvent, a cocatalyst and ammonia water at constant temperature of 0-90 DEG C to obtain a mixed solution; 2. while stirring at constant temperature of 0-90 DEG C in a nitrogen protective atmosphere, dropwisely adding bridged bis-trifunctional silane into the mixed solution, stirring under reflux for 5-15 hours, and filtering the reaction solution to obtain a white solid crude product; and 3. sequentially washing the white solid crude product with deionized water and acetone 1-4 times, and carrying out vacuum drying to obtain the white powdery monodisperse bridged polysilsesquioxane microspheres. The reaction system has fewer side reactions, the technique is simple and controllable, and the yield of the obtained bridged polysilsesquioxane microspheres is up to more than 96%; and the microspheres have the advantages of monodispersity, high dimensional homogeneity and favorable storage stability.

Description

[0001] This application is a divisional application. The filing date of the original application is February 14, 2012, the application number is 201210032100.3, and the title of the invention is "a method for synthesizing monodisperse bridged polysilsesquioxane microspheres". technical field [0002] The invention belongs to the technical field of microsphere materials, and in particular relates to a reaction catalyst system and application for synthesizing bridged polysilsesquioxane microspheres. Background technique [0003] Silsesquioxanes are widely used in the fields of liquid crystal materials, ablation-resistant materials, dielectric materials, polymer material modification, biomedicine, organic-inorganic hybrid polymer materials, and as microsphere materials, especially It has good applications in the fields of biomedicine and high-performance liquid chromatography analysis. Silsesquioxane can be introduced into the matrix of polymer materials by blending, copolymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07F7/21B01J13/02
Inventor 张增平
Owner CHANGAN UNIV
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