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Method for preparing nanoscale mesoporous silica spheres

A mesoporous silica, nano-scale technology, applied in the preparation of mesoporous silica spheres, particle size control and preparation of nano-scale mesoporous silica spheres, can solve the problem of long synthesis time and synthesis process Complicated, non-adjustable particle size and other issues

Inactive Publication Date: 2009-10-21
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, its particle size cannot be adjusted, the synthesis process is complex (the pH value of the easy to change needs to be changed many times during the synthesis process), and the synthesis takes a long time (6 months).
However, a method that can control the diameter of mesoporous silica spheres in the nanoscale range and has a narrow particle size distribution has not been reported yet.

Method used

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  • Method for preparing nanoscale mesoporous silica spheres
  • Method for preparing nanoscale mesoporous silica spheres
  • Method for preparing nanoscale mesoporous silica spheres

Examples

Experimental program
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example 1

[0022] Dissolve 1.0g cetyltrimethylammonium bromide (CTAB) in 192ml deionized water, stir until clear, add 1.0ml 1mol / L NaOH solution dropwise, stir the above solution at 80°C, add 5.68ml Tetraethyl orthosilicate was kept under the above conditions and stirred for 2 hours to obtain a reaction solution containing a white precipitate. Then the mixed solution was filtered and dried at room temperature to obtain a white solid powder. The powder was put into a muffle furnace at 550° C. and roasted for 1 hour with nitrogen gas, and then with air for 4 hours to obtain the medium after the template agent was burned. Porous silica, analyzed and tested by XRD, HRSEM, BET, HRTEM, particle size distribution, etc., shows that its microscopic shape is spherical, the average particle size is 49nm, the particle size distribution range is 40-55nm, and the specific surface is 803m 2 / g, the pore size is 2.2nm, its XRD, FE-SEM, HRTEM and particle size distribution are as follows Figure 1-a , 1-...

example 2

[0024] Operate with embodiment 1, only change the amount of NaOH, drop the NaOH solution of 2.0ml 1mol / L, the average particle diameter of the sample obtained by reaction is 180nm, specific surface is 747m 2 / g, the pore size is 2.6nm.

example 3

[0026] The ratio of the reactants and the reaction conditions are the same as in Example 2, the template agent is changed to octaalkyltrimethylammonium bromide, the average particle diameter of the sample obtained from the reaction is 380nm, and the specific surface is: 971m 2 / g, the pore size is 1.9nm.

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Abstract

The invention relates to a method for preparing nanoscale mesoporous silica spheres, and the method belongs to the technical field of preparation of inorganic porous materials. The invention specifically relates to the synthesis of a series of mesoporous silica with different sphere diameters. The method takes quaternary ammonium salt cationic surfactants with different carbon chain lengths, which are taken as template agents and adopts the sol-gel method for synthesis under alkaline conditions. The method is characterized in that mesoporous silica material particles are spherical, the sphere diameter is adjustable within the range of 40-400nm; the specific surface area is large, the particle size distribution is narrow; and the hole diameter is adjustable within the range of 1.9-4.0nm. The materials are widely applied in catalysis, separation, sensors, nano-reactors, optical materials and other aspects.

Description

technical field [0001] The invention belongs to the field of preparation of inorganic porous materials, and relates to the preparation of a series of nanometer-sized mesoporous silica spheres. In particular, it relates to a particle size control and preparation method of nanoscale mesoporous silica spheres. technical background [0002] In 1992, Mobil Corporation of the United States reported a method for synthesizing M41S series mesoporous silica under alkaline conditions using surfactants as templates. This type of material has regular and orderly periodic pores, highly uniform pore size, extremely high specific surface area, and good thermal stability, making it highly promising in the fields of catalysis, adsorption and separation, semiconductors, optoelectronic devices, and sensors. Theoretical research and practical application value. However, the particle size of traditional mesoporous silica is generally between micrometers and centimeters, and the shape is not uni...

Claims

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Application Information

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IPC IPC(8): C01B33/18B82B3/00
Inventor 孔岩杜军孙鹏刘安康吕忆农王军
Owner NANJING UNIV OF TECH
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