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Method of producing hollow silicon dioxide microsphere with mercapto on internal and external surfaces

A technology of silica, inner and outer surfaces, applied in the direction of silica, fibrous fillers, etc., can solve the problems of uneven size, complicated method, broken hollow balls, etc., to achieve uniform size, low preparation cost and good sphericity Effect

Inactive Publication Date: 2009-08-26
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the method is more complicated, and the hollow balls prepared are damaged and uneven in size

Method used

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  • Method of producing hollow silicon dioxide microsphere with mercapto on internal and external surfaces
  • Method of producing hollow silicon dioxide microsphere with mercapto on internal and external surfaces

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 250mL four-necked flask equipped with a thermometer, a condenser, a stirrer, and nitrogen, add 100g of PS (polystyrene) emulsion (wherein the PS content is 3wt%) and 40mL of ethanol, stir for 30min under nitrogen protection, and heat up to 50°C. Add 15mL of ammonia water into the flask, stir for 5-10min, then quickly add 1g of 3-mercaptopropyltrimethoxysilane, react for 7-8h, centrifuge the prepared emulsion, wash with ethanol and deionized water for 3-4 times, that is The hollow silica microspheres with mercapto groups on the inner and outer surfaces were obtained. Its infrared spectrum is shown in figure 1 shown.

Embodiment 2

[0025] In a 250mL four-neck flask equipped with a thermometer, a condenser, a stirrer, and nitrogen, add 100g of PS emulsion (PS content is 5wt%) and 55mL of ethanol, stir for 60min under nitrogen protection, and heat up to 60°C. Add 20mL of ammonia water into the flask, stir for 10-15min, then quickly add 2g of 3-mercaptopropyltriethoxysilane, react for 7-8h, centrifuge the prepared emulsion, wash with ethanol and deionized water for 3-4 times, That is, hollow silica microspheres with mercapto groups on the inner and outer surfaces are obtained.

Embodiment 3

[0027] In a 250mL four-neck flask equipped with a thermometer, a condenser, a stirrer, and nitrogen, add 100g of PS emulsion (PS content is 4wt%) and 40mL of ethanol, stir for 45min under nitrogen protection, and heat up to 30°C. Add 30mL of ammonia water into the flask, stir for 5-10min, then quickly add 1.5g of 3-mercaptopropyltrimethoxysilane, react for 7-8h, centrifuge the prepared emulsion, wash with ethanol and deionized water for 3-4 times , that is, hollow silica microspheres with mercapto groups on the inner and outer surfaces.

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Abstract

The invention belongs to the technical field of polymer materials, and in particular relates to a method for preparing hollow silica microspheres with mercapto groups on the inner and outer surfaces. In the present invention, polystyrene microspheres with positive charges on the surface are used as templates, and ammonia water is used as a catalyst and etchant in an ethanol / water system to hydrolyze and polycondense coupling agents containing mercapto groups on the surface of polystyrene microspheres to form The silica shell, while the polystyrene microspheres are removed, finally forms a silica shell with mercapto groups on the inner and outer interfaces. The method of the invention is simple and easy, and avoids high-temperature calcination or reagent etching in the traditional preparation process of inorganic hollow microspheres. Because the inner and outer surfaces of the hollow silica microspheres have mercapto groups, they can be oxidized by oxidants to form hollow microspheres with sulfonic acid groups on the inner and outer surfaces, which can be used as solid acid catalysts and modifiers for hydration proton exchange membranes.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a method for preparing hollow silica microspheres with functional groups on the inner and outer surfaces. Background technique [0002] With the rapid development of nanotechnology, nanoparticles with novel topological structures have attracted great interest in recent years. Among them, composite microspheres with core-shell structure are particularly attractive, mainly because their structure, size and composition are easy to adjust, and they can effectively realize the design and tailoring of optical, electrical, thermal, mechanical and catalytic properties. Especially inorganic oxides (such as SiO 2 、TiO 2 , Ag, Fe 3 o 4 etc.) Hollow microspheres have extremely broad application prospects due to their large specific surface area, low density, and high thermal and mechanical stability. [0003] There are many preparation methods of inorganic hollow m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/113C09C1/28C08G77/28
Inventor 袁俊杰周光斌浦鸿汀
Owner TONGJI UNIV
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