Method for preparing hollow silicon dioxide microspheres

A technology of silicon dioxide and microspheres, which is applied to the preparation of silicon dioxide, microspheres, silicon oxide, etc., can solve the problems of complicated steps, high price, increased cost, etc., and achieves simple preparation process, simplified synthesis procedure, and easy control. and the effect achieved

Inactive Publication Date: 2012-01-11
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The prior art uses expensive surfactants (such as cetyltrimethylammonium bromide, etc.) or other functional groups to modify negatively charged PS microspheres, the steps are complicated, and the cost is increased

Method used

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  • Method for preparing hollow silicon dioxide microspheres
  • Method for preparing hollow silicon dioxide microspheres
  • Method for preparing hollow silicon dioxide microspheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, add 65ml ethanol and 5ml water into the beaker, magnetically stir for 10min, add 5ml 25% ammonia water and continue stirring for 5min, then add 7.5ml ethyl orthosilicate, react for 1min and quickly add 7g polystyrene microspheres at room temperature Continue to stir the reaction for 2h and then end the synthesis reaction. The reaction mixture was filtered with suction and washed until the clear liquid after the filtering was free of foam; dried at room temperature for 3 days; the dried powder was heated to 550°C at a heating rate of 1°C / min, and kept for 6 hours. The furnace was cooled to room temperature, and samples were collected.

Embodiment 2

[0020] First add 65ml of ethanol and 5ml of water into the beaker, magnetically stir for 10min, add 5ml of 25% ammonia water and continue stirring for 30min, then add 10ml of ethyl orthosilicate, react for 1min and quickly add 2g of polystyrene microspheres, at room temperature Continue to stir the reaction for 2 hours and then end the synthesis reaction. The reaction mixture was filtered with suction and washed until the clear liquid after the filtering was free of foam; dried at room temperature for 3 days; the dried powder was heated to 550°C at a heating rate of 1°C / min, and kept for 6 hours. The furnace was cooled to room temperature, and samples were collected.

Embodiment 3

[0022] First add 65ml ethanol and 5ml water into the beaker, magnetically stir for 10min, add 10ml 25% ammonia water and continue to stir for 5min, then add 10ml ethyl orthosilicate, after reacting for 1min, quickly add 3.5g polystyrene microspheres at room temperature Continue to stir the reaction for 3 hours and then end the synthesis reaction. The reaction mixture was filtered with suction and washed until the clear liquid after the filtering was free of foam; dried at room temperature for 3 days; the dried powder was heated to 550°C at a heating rate of 1°C / min, and kept for 6 hours. The furnace was cooled to room temperature, and samples were collected.

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Abstract

The invention discloses a method for preparing hollow silicon dioxide microspheres, which comprises the following steps of: adding absolute ethyl alcohol and water into a beaker; uniformly stirring the absolute ethyl alcohol and water, then adding ammonia water into the mixture and keeping on stirring the mixture for 5 to 30 min; then adding tetraethoxysilane into the mixture and then quickly adding polystyrene microspheres within 1 to 5min; then stirring the mixture for reaction for 1 to 3h at normal temperature; filtering and washing the mixture after the reaction; drying the filter cake first at normal temperature and then at the temperature of between 500 and 600 DEG C; preserving the heat for 5 to 8h; and finally cooling the reaction product. The hollow SiO2 microspheres can be directly prepared by reacting unmodified PS microspheres at normal temperature so as to simplify the synthesis process and ensure simple preparation process and easy control and implementation; the nanoparticles of the formed hollow microspheres have micropores of less than 2nm; and mesopores and macropores of dozens of nanometers are formed among the nanoparticles; therefore, the multilayer nanoporousstructure contributes to the adsorption and transport of materials.

Description

Technical field [0001] The invention relates to the preparation of silicon dioxide microsphere materials, in particular to a method for preparing hollow silicon dioxide microspheres. Background technique [0002] Hollow microsphere materials are functional materials, and they are widely used in many fields such as catalyst carriers, drug storage and slow release, bioactive molecule coating, cosmetics, and lightweight fillers. Template method is a common method for preparing hollow microspheres. Polystyrene (PS) microspheres are often used as templates. Newly generated SiO2 silica nanoparticles are coated on them to form spherical shells, and the PS templates are then calcined to remove the PS template. The hollow SiO2 microspheres were obtained. [0003] Wu Xiaofeng, Tan Bing, Zhang Shigang, Yang Mu, etc. (Rare Metal Materials and Engineering, 2007, 36, p217-291; Langumir, 2005, 21, 8180-8187; Materials Chemistry and Physcis, 2008, 11, p5-8.) Using cetyltrimethylammonium bromide ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12B01J13/02
Inventor 刘世权邱芹
Owner UNIV OF JINAN
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