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Method for preparing surface porous silicon dioxide microspheres based on long-chain alkyl ionic liquid as pore-foaming agent

An ionic liquid and long-chain alkyl technology, which is applied in the field of preparation of surface porous silica microspheres, can solve the problems of limited pore structure regulation, small pore size, and limitations

Pending Publication Date: 2021-06-11
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, currently used porogens are mainly cationic quaternary ammonium salts represented by cetyl ammonium bromide (CTAB), which have a single type and structure, limited regulation of pore structure and size, and small pore size, which limits It affects the application range of superficially porous silica microspheres

Method used

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  • Method for preparing surface porous silicon dioxide microspheres based on long-chain alkyl ionic liquid as pore-foaming agent
  • Method for preparing surface porous silicon dioxide microspheres based on long-chain alkyl ionic liquid as pore-foaming agent
  • Method for preparing surface porous silicon dioxide microspheres based on long-chain alkyl ionic liquid as pore-foaming agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 0.435 g of 1-octadecyl-3-methylimidazolium bromide porogen and 0.5 g of non-porous silica (particle size 1.8 μm) as the inner core into 30 ml of deionized water, and ultrasonically disperse to obtain an aqueous phase solution ; Subsequently, 0.5 ml of tetraethyl orthosilicate is used as a silicon source and 2 ml of acetonitrile is added as a cosolvent into 30 ml of n-hexane solution to disperse evenly to obtain an oil phase solution; React at a reaction temperature of 70 °C and a rotational speed of 300 r / min for 17 h. The obtained product was washed with deionized water and an organic solvent repeatedly to remove impurities. The obtained solid was dried and placed in a muffle furnace, and calcined at 500 °C for 3 h to obtain Crude product; the crude product is washed with water and absolute ethanol to remove impurities, and the surface porous silica microspheres with regular shape, uniform size and obvious core-shell structure are obtained (see figure 1 , figure ...

Embodiment 2

[0030] Add 0.446 g of 1-octadecyl-3-vinylimidazolium bromide porogen and 0.5 g of non-porous silica (particle size 1.8 μm) as the inner core into 30 ml of deionized water, and ultrasonically disperse to obtain an aqueous phase solution ; Subsequently, 0.5 ml of tetraethyl orthosilicate is used as a silicon source and 2 ml of acetonitrile is added as a cosolvent into 30 ml of n-hexane solution to disperse evenly to obtain an oil phase solution; React at a reaction temperature of 70 °C and a rotational speed of 300 r / min for 17 h. The obtained product was washed with deionized water and organic solvent repeatedly to remove impurities. The obtained solid was dried and placed in a muffle furnace, and calcined at 500 °C for 3 h. A crude product is obtained; the crude product is washed with water and absolute ethanol to remove impurities, and the surface porous silica microspheres with regular shape, uniform size and obvious core-shell structure are obtained. The characterization re...

Embodiment 3

[0032]Add 0.435 g of 1-octadecyl-3-methylimidazolium bromide porogen and 0.5 g of non-porous silica (particle size 1.8 μm) as the inner core into 30 ml of deionized water, and ultrasonically disperse to obtain an aqueous phase solution ; Then add 0.5 ml tetraethyl orthosilicate as a silicon source and 0.46 ml isopropanol as a cosolvent into 30 ml n-hexane solution to disperse evenly to obtain an oil phase solution; then mix the obtained water phase solution and oil phase solution , reacted at a reaction temperature of 70 °C and a rotational speed of 300 r / min for 17 h, washed the obtained product with deionized water and organic solvent repeatedly to remove impurities, dried the obtained solid, placed it in a muffle furnace, and calcined at 500 °C After 3 hours, the crude product was obtained; the crude product was washed with water and absolute ethanol to remove impurities, and superficially porous silica microspheres with regular shape, uniform size and obvious core-shell str...

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Abstract

The invention discloses a method for preparing surface porous silicon dioxide based on a long-chain alkyl ionic liquid as a pore-foaming agent. The method comprises the following steps: ultrasonically dispersing the long-chain alkyl ionic liquid, urea and compact non-porous silicon dioxide in water to obtain a water-phase solution; adding tetraethyl orthosilicate and a cosolvent into an organic solvent, and uniformly dispersing to obtain an oil-phase solution; mixing the water-phase solution and the oil-phase solution, and stirring and reacting at 40-120 DEG C for 10-40 hours; centrifuging, washing, drying and calcining the obtained product to obtain a crude product; and washing the crude product with water and absolute ethyl alcohol to remove impurities so as to obtain silicon dioxide microspheres with porous surfaces. The structural characteristics of the surface porous silicon dioxide are jointly determined by the types of the long-chain ionic liquid, the types of the organic phases, the reaction time, the stirring speed and the like, so that the pore structure of the surface porous silicon dioxide can be controlled by selecting the types of the long-chain ionic liquid and the types of the organic phases and regulating and controlling a reaction system and reaction conditions.

Description

technical field [0001] The invention relates to the preparation of a surface porous silica microsphere, in particular to a method for preparing a surface porous silica microsphere based on a long-chain ionic liquid as a porogen, and belongs to the field of composite materials and chromatographic stationary phase materials. Background technique [0002] Superficially porous silica microspheres are a new type of chromatographic stationary phase matrix filler composed of a dense non-porous silicon core and a porous silica shell covering the solid core. When used as a stationary phase, the separation only occurs in the surface porous layer, which can significantly shorten the mass transfer path of the analyte, and also has the advantages of low back pressure and high column efficiency. Therefore, superficially porous silica packing is considered to be a real alternative to fully porous silica packing and has become an ideal tool for ultrafast analysis in liquid chromatography. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2004/03C01P2004/04C01P2004/32C01P2006/16C01P2006/12
Inventor 邱洪灯全凯军刘钟山陈佳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI