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Preparation method of mono-disperse silica mesoporous sphere material

A silicon dioxide, monodisperse technology, applied in the direction of silicon dioxide, silicon oxide, nanostructure manufacturing, etc., can solve the problem of not uniform particle size of spherical materials, etc.

Inactive Publication Date: 2010-02-24
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The synthetic methods proposed in these two documents obtain spherical materials with insufficient particle size, and the implementation method is quite special.

Method used

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  • Preparation method of mono-disperse silica mesoporous sphere material
  • Preparation method of mono-disperse silica mesoporous sphere material
  • Preparation method of mono-disperse silica mesoporous sphere material

Examples

Experimental program
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Effect test

Embodiment 1

[0024] Such as figure 1 As shown, the 0.11g C 18 h 37 NBr(CH 3 ) 2 CH 2 CH 2 CH 2 N(CH 3 ) 3 Dissolve Br in 38g of deionized water, then add 9.2g of ethanol, and add 6.5g of 0.1mol / l sodium hydroxide to the aqueous solution of the surfactant under stirring at 80°C, and add 0.8g of tetraethoxylate to the system base silane; the system was stirred for 10 minutes, left to react at 80°C for 48 hours, filtered, washed, dried, and calcined at 550°C for 6 hours to obtain a monodisperse silica mesoporous spherical material from which organic templates and functional groups were removed.

[0025] The material was characterized by transmission electron microscope, X-ray diffraction, scanning electron microscope and nitrogen adsorption instrument. figure 2 and image 3 They are electron micrographs, X-ray diffraction patterns and nitrogen adsorption isotherms of the mesoporous material, respectively. From figure 2 It can be seen that the silica mesoporous spherical material...

Embodiment 2

[0027] Such as figure 1 As shown, 0.04g C 18 h 37 NCl(CH 3 ) 2 CH 2 CH 2 CH 2 N(CH 3 ) 3 Cl was dissolved in 38g of deionized water, then 13.8g of ethanol was added, and under stirring at 50°C, 6.5g of 0.1mol / l sodium hydroxide was added to the aqueous solution of the surfactant, and 0.15g of tetramethoxyl was added to the system base silane; the system was stirred for 10 minutes, left to react at 50°C for 48 hours, filtered, washed, dried, and calcined at 550°C for 6 hours to obtain a monodisperse silica mesoporous spherical material from which organic templates and functional groups were removed.

[0028] The material was characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption and transmission electron microscopy. The average particle diameter of the material is 280nm, the relative standard deviation of particle diameter is 8.9%, the unit cell parameter is 4.4nm, the pore diameter is 2.5nm, and the pore wall thickness is calculated to b...

Embodiment 3

[0030] Such as figure 1 As shown, the 0.11g C 18 h 37 NBr(CH 3 ) 2 CH 2 CH 2 CH 2 N(CH 3 ) 3 Dissolve Br in 38g of deionized water, then add 13.8g of ethanol, under stirring at 80°C, add 6.5g of 0.1mol / l sodium hydroxide to the aqueous solution of the surfactant, and add 0.8g of tetraethoxylate to the system base silane; the system was stirred for 10 minutes, left to react at 80°C for 48 hours, filtered, washed, dried, and calcined at 550°C for 6 hours to obtain a monodisperse silica mesoporous spherical material from which organic templates and functional groups were removed.

[0031] The material was characterized by X-ray diffraction, scanning electron microscopy, nitrogen adsorption and transmission electron microscopy. The average particle diameter of the material is 460nm, the relative standard deviation of particle diameter is 3.9%, the unit cell parameter is 4.0nm, the pore diameter is 2.5nm, and the pore wall thickness is calculated to be 1.0nm.

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Abstract

The invention discloses a preparation method of a mono-disperse silica mesoporous sphere material in the technical field of inorganic materials, comprising the following steps: taking quaternary ammonium salt gemini surfactant as a template, organic solvent as an auxiliary solvent and organosiloxane as a silica resource, adjusting solution alkalinity and preparing the silica mesoporous sphere material with a structure in which pore canals are arranged to disperse from the centre of the sphere to the outer surface of the sphere. The silica mesoporous sphere material has single dispersed sphereappearance, with the relative standard deviation of the diameter being lower than 10 percent and the diameter of 70490 nm.

Description

technical field [0001] The invention relates to a preparation method in the technical field of inorganic materials, in particular to a preparation method of a monodisperse silica mesoporous spherical material. Background technique [0002] Inorganic mesoporous materials have large specific surface area and pore volume, adjustable pore structure, adjustable pore size, surface properties that can be modified and appearance that can be controlled; mesoporous silica spherical materials with monodisperse particle size It has great application potential in the fields of chromatographic columns, cosmetics, and photonic crystals. [0003] Found through the document retrieval to prior art, Yano, K etc. have published " Particlesize control of mono-dispersed super-microporous silica spheres in " Journal of MaterialsChemistry " (Material Chemistry Journal) 2003 the 13th phase 2577-2581 pages "(Particle size control of monodisperse ultra-microporous silica spheres), it is mentioned in ...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82B3/00
Inventor 陈茜茹车顺爱
Owner SHANGHAI JIAO TONG UNIV