Method of producing hollow silicon dioxide microsphere with mercapto on internal and external surfaces
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A technology of silica, inner and outer surfaces, applied in the directions of silica, fibrous fillers, etc., can solve the problems of complex method, uneven size, broken hollow balls, etc., and achieves low preparation cost, uniform size and good sphericity. Effect
Inactive Publication Date: 2008-05-07
TONGJI UNIV
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But the method is more complicated, and the hollow balls prepared are damaged and uneven in size
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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.
Embodiment 2
[0025] In a 250mL four-necked 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 ammonia water into the flask, stir for 10-15min, then quickly add 293-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 the polymeric material, in particular relates to a preparation method of hollow silicon dioxide spherical particles with mercapto on the internal and the external surfaces. The invention uses polystyrene spherical particles with positive charges on the surface as a module, under the system of ethanol or water and with ammonia as a catalyst and an etching agent, causing the hydrolytic condensation of a coupling agent with the mercapto on the surface of the polystyrene spherical particles, thus a silicon dioxide shell is formed and the polystyrene spherical particles are eliminated, finally the silicon dioxide shell with the mercapto is formed on the internal and the external surfaces. The invention has simple operation, avoids high-temperature calcinations and reagent etching in the traditional preparation process of inorganic and hollow spherical particles. Because the hollow silicon dioxide spherical particles have the mercaptos on the internal and the external surfaces, the hollow spherical particles with sulfonic groups on the internal and the external surfaces can be formed through oxidization with oxidizer, and can be not only a solid acid catalyst, but also be a modifier for a hydrated proton exchange membrane.
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...
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