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Preparation method of mono-disperse silicon dioxide micro-spheres

A monodisperse silica microsphere, silica technology, applied in the direction of silica, silica, etc., can solve the problems of being limited in the laboratory, difficult to achieve the scale of mass production, etc., to achieve easy operation of the process and experimental conditions. Mild, easy-to-industrial effect

Inactive Publication Date: 2011-03-30
纪志勇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although people have a systematic and in-depth understanding of the monodisperse silica system, because the formation process of the monodisperse system is very sensitive to conditions, the rate relationship of the two main reactions in the process, hydrolysis and condensation, is constantly changing with the change of reaction conditions. , and the growth rate of microspheres also changes with hydrolysis and condensation, so the preparation of monodisperse silica microspheres is still limited to the laboratory, and it is difficult to reach the scale of mass production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] (1) Use the Stober method to synthesize monodisperse silica microsphere seeds: add 120ml of n-propanol, 10.4ml of water and 9.5ml of ammonia water into a clean 250ml four-neck flask, start the mechanical stirring, and control the speed at 450r / pm , control the temperature at 10°C, slowly add 26ml of 0.23mol / L TEOS-n-propanol solution dropwise, and react for 25 minutes to obtain monodisperse silica microsphere seeds;

[0018] (2) Using the seed growth method, prepare silica microspheres with the above silica microsphere seeds: add 20ml of the silica microsphere seed suspension prepared in (1) to a clean 500ml four-neck flask, 100ml of n-propanol, 23ml of water and 16ml of ammonia water make the concentration of 10 15 A / L silica seed solution, start stirring and control the speed to be 450rpm. At 25°C, slowly add 2.0mol / L ammonia water-n-propanol solution and 0.23mol / L TEOS-n-propanol solution dropwise at the same time, the silicon dioxide formed by hydrolysis of TEOS gr...

Embodiment 2

[0020] (1) Using the Stober method to synthesize monodisperse silica microsphere seeds: add 130ml of ethanol, 11.6ml of water and 9.8ml of ammonia water to a clean 250ml four-neck flask, turn on mechanical stirring, control the speed at 450r / pm, and control The temperature is 20°C, slowly drop 31ml of 0.21mol / L TEOS-ethanol solution for 25 minutes, and react to obtain monodisperse silica microsphere seeds;

[0021] (2) Using the seed growth method, prepare silica microspheres with the above silica microsphere seeds: add 20ml of the silica microsphere seed suspension prepared in (1) to a clean 500ml four-neck flask, 120ml of ethanol, 20ml of water and 15ml of ammonia water make up the concentration of 10 15 A / L silica seed solution, start stirring and control the speed to be 450rpm. At 35°C, 0.5 mol / L ammonia-ethanol solution and 0.1 mol / L TEOS-ethanol solution were slowly added dropwise at the same time, and the silicon dioxide generated by hydrolysis of TEOS grew on the oute...

Embodiment 3

[0023] (1) Synthesize monodisperse silica microsphere seeds by the Stober method: add 125ml of ethanol, 10.6ml of water and 8.8ml of ammonia water into a clean 250ml four-neck flask, turn on the mechanical stirring, control the speed at 450r / pm, and control The temperature is 40°C, slowly add 27ml of 0.31mol / L TEOS-ethanol solution dropwise for 25 minutes, and react to obtain monodisperse silica microsphere seeds;

[0024] (2) Using the seed growth method, prepare silica microspheres with the above silica microsphere seeds: add 20ml of the silica microsphere seed suspension prepared in (1) to a clean 500ml four-neck flask, 140ml of ethanol, 30ml of water and 21ml of ammonia water make up the concentration of 10 15 A / L silica seed solution, start stirring and control the speed to be 450rpm. At 40°C, 4 mol / L ammonia-ethanol solution and 3 mol / L TEOS-ethanol solution were slowly added dropwise at the same time, and the silicon dioxide produced by hydrolysis of TEOS grew on the o...

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Abstract

The invention discloses a preparation method of mono-disperse silicon dioxide micro-spheres, which comprises the following steps of: (1) synthesizing mono-disperse silicon dioxide micro-sphere seeds by using a Stober method, namely at a reaction temperature of 10 to 60 DEG C, and in a solvent system of alcohol, water and ammonia, adding tetraethoxysilane alcoholic solution of which the concentration is 0.1 to 0.5 mol / L to react so as to obtain the mono-disperse silicon dioxide micro-sphere seeds; and (2) preparing the silicon dioxide micro-spheres from the silicon dioxide micro-sphere seeds by using a seed growth method, namely preparing silicon dioxide seed solution of which the concentration is 1,015 to 1,017 seeds / L by using the silicon dioxide micro-sphere seeds, the ammonia and the alcohol, and at the reaction temperature of 10 to 60 DEG C, adding ammonia-alcohol solution of which the concentration is 0.5 to 5.0 mol / L and tetraethoxy-silicane alkanol solution of which the concentration is 0.1 to 5.0 mol / L to react so as to obtain a suspension of the mono-disperse silicon dioxide micro-spheres.

Description

technical field [0001] The invention relates to a method for preparing monodisperse silica microspheres, in particular to a method for preparing monodisperse silica microspheres with a particle size distribution of 100-800nm. Background technique [0002] Monodisperse silica microspheres (SiO 2 ) Due to its superior stability, reinforcement, thixotropy, single composition and easy surface functionalization, it has great potential in the fields of rubber, plastics, coatings, pigments, catalysts, chromatographic fillers, high-performance ceramics and other materials science. Wide range of applications; in addition, because it does not swell in organic solvents and is not susceptible to bacterial erosion, it has good biocompatibility and can be widely used in molecular biology, including biological cell separation and medical engineering, cosmetics, drugs, medical diagnosis and immunoassays, etc. In recent years, what has aroused people's research interest is the self-assembl...

Claims

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Application Information

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IPC IPC(8): C01B33/12
Inventor 纪志勇吴建才陈胜利
Owner 纪志勇
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