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A controllable aspect ratio and channel-functionalized silica nanorod and preparation method thereof

A technology of silica and aspect ratio, applied in the direction of silica, silica, chemical instruments and methods, etc., can solve the problems of cumbersome process and the inability to fully utilize the high specific surface of mesoporous silica, and achieve The effect of simple synthesis steps, good porosity, and large specific surface area

Active Publication Date: 2018-10-02
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this type of synthesis method, at least two steps are required to synthesize surface-functionalized nano-silica, and the process is cumbersome, and the surface-functionalized nano-silica obtained by the step-by-step synthesis method has a part of the pores blocked and the pores The channel is rarely functionalized, so that the high specific surface of mesoporous silica cannot be fully utilized

Method used

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  • A controllable aspect ratio and channel-functionalized silica nanorod and preparation method thereof
  • A controllable aspect ratio and channel-functionalized silica nanorod and preparation method thereof
  • A controllable aspect ratio and channel-functionalized silica nanorod and preparation method thereof

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Effect test

Embodiment 1

[0044] Add 0.652g of surfactant cetyltrimethylammonium bromide to 315mL of water, stir to fully dissolve the surfactant in the water; then add 12.45mL of 28% concentrated ammonia water to the solution, stir for 1h to form a colorless and transparent Solution A; then, a mixed solution B of 1.8 mL of ethyl orthosilicate and 0.9 mL of 3-aminopropyltriethoxysilane (APTES) was added dropwise to solution A at a rate of 23 mL / h, and stirred at 25°C 4h. The obtained product solution was centrifuged to collect the solid, washed with water and centrifuged to neutrality, then the obtained solid product was added to 1 g / L ammonium nitrate-ethanol solution for reflux, repeated the reflux step, and the solid product was collected by centrifugation. -NH 2group of silica nanorods with L=980nm, D=980nm, AR=1, specific surface=1145.3m 2 / g, see the SEM image figure 1 , and its infrared spectrum can be seen in Figure 5 .

Embodiment 2

[0046] Add 0.873g of surfactant cetyltrimethylammonium chloride to 210mL of water, stir to fully dissolve the surfactant in the water; then add 8.3mL of 28% concentrated ammonia water to the solution, stir for 1h to form colorless and transparent solution; then a mixed solution of 2.5 mL of ethyl orthosilicate and 1.25 mL of 3-aminopropyltriethoxysilane (APTES) was added dropwise to the solution at a rate of 23 mL / h, and stirred at 5° C. for 120 h. The obtained product solution was centrifuged to collect the solids, washed with water and centrifuged to neutrality, then the obtained solids were added to 6g / L ammonium nitrate-methanol solution for reflux, the refluxing step was repeated, the solid products were collected by centrifugation, washed and dried to obtain a -NH 2 group of silica nanorods with L=695nm, D=371nm, AR=1.9, specific surface=851.2m 2 / g.

Embodiment 3

[0048] Add 0.873g of surfactant octadecyltrimethylammonium bromide to 210mL of water, stir to fully dissolve the surfactant in the water; then add 8.3mL of 28% concentrated ammonia into the solution, stir for 1h to form colorless and transparent solution; then a mixed solution of 2.5 mL of ethyl orthosilicate and 1.25 mL of 3-chloropropyltrimethoxysilane was added dropwise to the solution at a rate of 30 mL / h, and stirred at 25° C. for 4 h. The obtained product solution was centrifuged to collect the solid, washed with water and centrifuged to neutrality, then the obtained solid product was added to 2 g / L ammonium nitrate-ethanol solution for reflux, the reflux step was repeated, the solid product was collected by centrifugation, washed and dried to obtain a Silica nanorods with chloropropyl group, L=658nm, D=319nm, AR=2, specific surface area=911.4m 2 / g.

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Abstract

The invention belongs to the field of nano material preparation, and particularly relates to a silica nanorod controllable in length-diameter ratio and functionalized in pore. The silica nanorod is porous, the inside of the pore is uniformly modified by functional groups, length L of the silica nanorod is 50-4300 nm while diameter D of the same is 50-700 nm, and the length-diameter ratio AR is 1-20. A silica nano material with the functionalized pore is obtained by adopting a one-pot method to enable ortho-silicate ester and siloxane containing the functional groups to be in hydrolysis copolymerization. Effective regulation of different length-diameter ratios of nano silica can be realized by controlling dropwise-adding speed and concentration of a surfactant. An ion exchange method is adopted to effectively remove the surfactant in an alcohol solution, so that troublesome removal steps like high-temperature calcining are omitted. The silica nanorod has high monodispersity and high specific surface area, and the surface of the pore is effectively functionalized.

Description

technical field [0001] The invention belongs to the field of nanomaterial preparation, and mainly relates to the preparation of mesoporous nanomaterials with different shapes, in particular to the preparation of silicon dioxide nanorods with controllable aspect ratios and pore channels. Background technique [0002] Due to its large specific surface area and pore volume, easy large-scale preparation, easy modification of other functional groups on the surface, and good mechanical properties, mesoporous silica materials are widely used in chemical and chemical catalysis, sensors, advanced coatings and It has a wide range of potential applications in fields such as early diagnosis. The microstructure of silica has a very important influence on its physical and chemical properties and its application. For example, silica with different morphologies has an important influence on the activity and behavior of cells in organisms. It is very important to screen out nano-silica mate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/12B82Y40/00
CPCC01B33/126C01P2002/82C01P2004/03C01P2004/16C01P2004/54C01P2004/61C01P2004/62C01P2004/64C01P2006/12
Inventor 李国良王军鹏张绘齐涛
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI