A kind of method for preparing mesoporous silica core-shell microspheres

A technology of mesoporous silica and core-shell microspheres, applied in the direction of silica, silica, etc., can solve the problems of reducing the effective surface area of ​​chromatographic applications, prone to agglomeration, and affecting separation efficiency, so as to achieve easy control and amplification, The effect of simple preparation process and mild conditions

Inactive Publication Date: 2018-04-24
NORTHWEST UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Ma Y et al. [Y. Ma , L. Qi, J. Ma, Colloid. Surfaces. A, 229(2003) 1-8] used triblock polymer as pore forming agent and CTAB as surfactant to prepare a pore diameter of 9nm core-shell microspheres, but the pore structure is non-open, which greatly reduces the effective surface area in chromatography applications, affects the separation efficiency, and is prone to agglomeration during the preparation process

Method used

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  • A kind of method for preparing mesoporous silica core-shell microspheres
  • A kind of method for preparing mesoporous silica core-shell microspheres
  • A kind of method for preparing mesoporous silica core-shell microspheres

Examples

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Embodiment 1

[0038] Example 1 Preparation of micron-sized surface porous silica core-shell microspheres ( figure 1 )

[0039] (1) Preparation of solid silica microspheres

[0040] According to the reference [H. Nakabayashi, A. Yamada, M. Noba, Y. Kobayashi, M. Konno, D. Nagao, Langmuir 26 (2010) 7512-7515] to prepare micron-sized silica solid microspheres, a typical method Preparation of solution A: Take a clean reagent bottle, add 200-300 mL of absolute ethanol, an appropriate amount of water and ammonia, and an appropriate amount of electrolytes to make a 300 mL mixed solution, ultrasonic for 10 minutes for use.

[0041] Preparation of solution B: Add an appropriate amount of TEOS to a certain amount of absolute ethanol to make a diluted solution, and ultrasonicate for 10 minutes for use.

[0042] Add liquid A to a 1000 mL three-necked flask, control the dropping rate to be less than 0.8 mL / min, slowly add liquid B, and react at an appropriate temperature with a certain stirring speed. After the...

Embodiment 2

[0047] Disperse 0.1 g of solid silica gel microspheres in Example 1 into 40 mL of deionized water for ultrasonic dispersion, and then disperse 0.74 g of cetyltrimethylammonium bromide (CTAB) and 0.46 g of trioctylmethylammonium bromide (TOMAB). ) Template is dispersed into a mixture of 80 mL ethanol and water (V water :V Ethanol =1:1), ultrasonically disperse uniformly, then add to the silicon core suspension, stir for 30 min, add 1 mL of ammonia (25 wt%) dropwise at room temperature, stir for 30 min, add 20 drops at a rate of 0.2 mL / min mL of TEOS solution (1-5% ethanol solution), react for 6 h at room temperature after the addition is complete. After the reaction, the obtained product was washed repeatedly with deionized water and ethanol. Finally, the resulting product was dried at 60°C for 6 hours, and then the resulting product was placed in a muffle furnace and calcined at 600°C for 10 hours. The obtained core-shell microspheres have an average pore diameter of 10.60 n...

Embodiment 3

[0050] Disperse 0.1 g of solid silica gel microspheres in Example 1 into 40 mL of deionized water for ultrasonic dispersion, and then mix 0.54 g of cetyltrimethylammonium bromide (CTAB) and 0.66 g of trioctylmethylammonium bromide (TOMAB). ) Is dispersed into a mixture of 80 mL of ethanol and water (V water :V Ethanol =1:1), disperse uniformly by ultrasonic, then add to the silicon core suspension, stir for 30 min, add 1 mL of ammonia (25 wt%) dropwise at room temperature, stir for 30 min, add 20 drops at a rate of 0.2 mL / min mL of TEOS solution (1-5% ethanol solution) was added dropwise and reacted at room temperature for 6 hours. After the reaction, the obtained product was washed repeatedly with deionized water and ethanol. Finally, the resulting product was dried at 60°C for 6 hours, and then the resulting product was placed in a muffle furnace and calcined at 600°C for 10 hours. The average pore size is 6.37 nm.

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Abstract

The invention discloses a method for preparing surface mesoporous silica core-shell microspheres, which uses 1-3 μm monodispersed non-porous silica gel microspheres, and disperses quaternary ammonium salt B and quaternary ammonium salt A dispersants into an ethanol aqueous solution. , disperse the silica gel microspheres into water, add mixed surfactant solution, adjust the pH value to 7.5-10 with ammonia water, then add tetraethoxysilane and / or tetramethoxysilane solution, wash, dry, and calcine to remove the template agent Surface mesoporous silica core-shell microspheres were obtained. The present invention uses two quaternary ammonium salts with different carbon chain lengths as co-templates to prepare core-shell microspheres with larger radioactive mesoporous structures. By adjusting the ratio of the two quaternary ammonium salt templates, the mesopore diameter is within 4 It is controllable within the range of ~20nm, and the resulting radioactive mesoporous structure increases the effective specific surface area of ​​the microspheres and improves their applications in adsorption, catalysis, and separation analysis.

Description

Technical field [0001] The invention relates to a method for preparing silica core-shell microspheres, in particular to a method for preparing silica core-shell microspheres with a surface mesoporous structure. Background technique [0002] With the development of modern society and science and technology, the requirements for the separation and analysis of complex samples are getting higher and higher, especially in the fields of food safety, environmental monitoring, drug development, and life sciences. Efficient and fast separation analysis is always the goal pursued by chromatographers. The development history of chromatographic technology shows that the change of chromatographic filler particles from large to small is the main driving force to achieve this goal. In recent years, the development of ultra-high pressure liquid chromatography technology based on sub-2μm fillers and rapid separation technology based on core-shell fillers has brought liquid chromatography technol...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/14
CPCC01B33/14C01P2004/03C01P2004/04C01P2004/84C01P2006/17
Inventor 白泉夏红军
Owner NORTHWEST UNIV
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