Method for preparing mesoporous silica core-shell microspheres

A technology of mesoporous silica and core-shell microspheres, applied in silica, silica and other directions, can solve the problems of affecting separation efficiency, prone to agglomeration, and reducing the effective surface area of ​​chromatographic applications, and achieves a simple and easy preparation process. Controlled and amplified, mildly conditioned effects

Inactive Publication Date: 2017-01-04
NORTHWEST UNIV(CN)
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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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  • Method for preparing mesoporous silica core-shell microspheres
  • Method for preparing mesoporous silica core-shell microspheres
  • Method for preparing mesoporous silica core-shell microspheres

Examples

Experimental program
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Embodiment 1

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

[0039] (1) Preparation of solid silica microspheres

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

[0041] Preparation of solution B: add an appropriate amount of TEOS and a certain amount of absolute ethanol to make a diluted solution, and ultrasonically for 10 min for later use.

[0042] Add liquid A to a 1000 mL three-necked flask, slowly add liquid B dropwise at a controlled rate within 0.8 mL / min, and react at a certain temperature at a certain stirring speed. A...

Embodiment 2

[0047] Take 0.1 g of solid silica gel microspheres in Example 1 and disperse them into 40 mL of deionized water for ultrasonic dispersion, then mix 0.74 g of cetyltrimethylammonium bromide (CTAB) and 0.46 g of trioctylmethylammonium bromide (TOMAB ) template agent dispersed in 80 mL of ethanol and water mixture (V 水 :V 乙醇 =1:1), ultrasonically dispersed evenly, then added to the silicon nucleus suspension, stirred for 30 min, then added dropwise 1 mL of ammonia water (25 wt%), stirred at room temperature for 30 min, and added dropwise 20 at a rate of 0.2 mL / min mL of TEOS solution (1-5% ethanol solution), react at room temperature for 6 h after the dropwise addition. After the reaction, the obtained product was repeatedly washed with deionized water and ethanol. Finally, the obtained product was dried at 60 °C for 6 h, and then the obtained product was put into a muffle furnace and calcined at 600 °C for 10 h. The obtained core-shell microspheres had an average pore size of...

Embodiment 3

[0050] Take 0.1 g of solid silica gel microspheres in Example 1 and disperse them into 40 mL of deionized water for ultrasonic dispersion, then mix 0.54 g of cetyltrimethylammonium bromide (CTAB) and 0.66 g of trioctylmethylammonium bromide (TOMAB ) template agent dispersed in 80 mL of ethanol and water mixture (V 水 :V 乙醇 =1:1), ultrasonically dispersed evenly, then added to the silicon nucleus suspension, stirred for 30 min, then added dropwise 1 mL of ammonia water (25 wt%), stirred at room temperature for 30 min, and added dropwise 20 at a rate of 0.2 mL / min mL of TEOS solution (1-5% ethanol solution), react at room temperature for 6 h after the dropwise addition. After the reaction, the obtained product was repeatedly washed with deionized water and ethanol. Finally, the obtained product was dried at 60 °C for 6 h, and then the obtained product was put into a muffle furnace and calcined at 600 °C for 10 h. The average pore diameter is 6.37 nm.

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Abstract

The invention discloses a method for preparing surface mesoporous silica core-shell microspheres. The method comprises: selecting monodisperse non-porous silica microspheres with the particle size of 1 to 3 microns, dispersing quaternary ammonium salt B and quaternary ammonium salt A dispersing agents in ethanol water, dispersing the silica microspheres in water, adding a mixed surface active agent solution, regulating a pH value to be 7.5 to 10 by using ammonia water, adding tetraethoxysilane and/or tetramethoxysilane solution, washing, drying, calcining and removing a structure-directing agent, thereby obtaining the surface mesoporous silica core-shell microspheres. By utilizing the quaternary ammonium salt with two different carbon chain lengths as co-structure-directing agent, the core-shell microspheres with a relatively larger radioactive mesoporous structure are prepared; by regulating the proportion of two quaternary ammonium salt structure-directing agents, the mesoporous aperture is controllable in a range of 4 to 20 nm, the obtained radioactive mesoporous structure increases effective specific surface areas of the microspheres, and the application of the microspheres in adsorption, catalysis and separation analysis is improved.

Description

technical field [0001] The invention relates to a method for preparing silica core-shell microspheres, in particular to a method for preparing surface mesoporous silica core-shell microspheres. 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 rapid separation analysis is always the goal pursued by chromatographers. The history of chromatographic technology development shows that the change of chromatographic packing 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-2 μm packing and rapid separation technology based on core-shell packing has brought liquid chromatography technology into ...

Claims

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Application Information

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