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Method for preparing mesoporous SBA-15 unstuck micro spheres

A microsphere and mesoporous technology, applied in the direction of silicon dioxide, silicon oxide, etc., can solve the problems of high adhesion and poor dispersibility of mesoporous SBA-15 microspheres, and achieve the effect of preventing adhesion and large pore size

Inactive Publication Date: 2012-06-27
LIAOCHENG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the mesoporous SBA-15 microspheres prepared by these methods have a high degree of adhesion and poor dispersion, so improving their dispersion and particle size uniformity has become a big challenge.

Method used

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  • Method for preparing mesoporous SBA-15 unstuck micro spheres
  • Method for preparing mesoporous SBA-15 unstuck micro spheres
  • Method for preparing mesoporous SBA-15 unstuck micro spheres

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Take 2.0 g of P123 and 1.5 g of KCl, add it to a 100 mL beaker filled with 72 g of 1.7 mol / L hydrochloric acid, heat to 40°C, and magnetically stir for 4 h until clarification;

[0026] (2) Then lower the temperature to 26°C, add 1.2 g of TMB, continue stirring for 10 h, add 4.2 g of TEOS dropwise, add 0.0 g of PVA, stop stirring after dissolving; raise the temperature to 40°C, and let stand for 20 hours;

[0027] (3) Transfer the above mixture to a 100 mL hydrothermal kettle (lined with polytetrafluoroethylene), add 0.025 g of NH 4 After F, seal the kettle, and conduct static hydrothermal crystallization at 100° C. for 24 hours. After cooling, the obtained product was filtered, washed with distilled water to remove soluble components, dried at 60°C for 4 h, and then calcined at 550°C for 6 hours to completely remove the template agent and the like to obtain mesoporous SBA-15 microspheres.

Embodiment 2

[0029] (1) Take 2.0 g of P123 and 1.5 g of KCl, add it to a 100 mL beaker filled with 72 g of 1.7 mol / L hydrochloric acid, heat to 40°C, and magnetically stir for 4 h until clarification;

[0030] (2) Then lower the temperature to 26°C, add 1.2 g of TMB, continue stirring for 10 h, add 4.2 g of TEOS dropwise, add 0.5 g of PVA, stop stirring after dissolving; raise the temperature to 40°C, and let stand for 20 hours;

[0031] (3) Transfer the above mixture to a 100 mL hydrothermal kettle (lined with polytetrafluoroethylene), add 0.025 g of NH 4 After F, seal the kettle, and conduct static hydrothermal crystallization at 100° C. for 24 hours. After cooling, the obtained product was filtered, washed with distilled water to remove soluble components, dried at 60°C for 4 h, and then calcined at 550°C for 6 hours to completely remove the template agent, etc., to obtain non-adhesive mesoporous SBA-15 microspheres.

Embodiment 3

[0033](1) Take 2.0 g of P123 and 1.5 g of KCl, add it to a 100 mL beaker filled with 72 g of 1.7 mol / L hydrochloric acid, heat to 40°C, and magnetically stir for 4 h until clarification;

[0034] (2) Then lower the temperature to 26°C, add 1.2 g of TMB, continue stirring for 10 h, add 4.2 g of TEOS dropwise, add 1.0 g of PVA, stop stirring after dissolving; raise the temperature to 40°C, and let stand for 20 hours;

[0035] (3) Transfer the above mixture to a 100 mL hydrothermal kettle (lined with polytetrafluoroethylene), add 0.025 g of NH 4 After F, seal the kettle, and conduct static hydrothermal crystallization at 100° C. for 24 hours. After cooling, the obtained product was filtered, washed with distilled water to remove soluble components, dried at 60°C for 4 h, and then calcined at 550°C for 6 hours to completely remove the template agent, etc., to obtain non-adhesive mesoporous SBA-15 microspheres.

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Abstract

The invention relates to a method for preparing mesoporous SBA-15 unstuck micro spheres, in particular a method for preparing mesoporous SBA-15 unstuck micro spheres for high-efficiency liquid chromatography. According to the method, a three-block copolymer P123 is used as a template agent, tetraethoxysilane, hydrochloric acid, potassium chloride, mesitylene, ammonium fluoride and polyvinyl alcohol are used as raw materials, and the dispersity of the mesoporous silica spheres can be regulated by adding polyvinyl alcohol. The mesoporous micro spheres prepared by the method are smooth and unstuck basically, and the addition of poly(vinyl acetate) (PVA) prevents the sticking of the micro spheres without influencing the specific surface area and mesoporous aperture obviously.

Description

technical field [0001] The invention relates to a preparation method of mesoporous silicon dioxide microspheres, in particular to a preparation method of mesoporous SBA-15 non-adhesion microspheres which can be used for high performance liquid chromatography. Background technique [0002] Since Zhao Dongyuan et al. synthesized the ordered mesoporous silica material SBA-15 using the triblock copolymer P123 as a template in 1998, SBA-15 is one of the ordered mesoporous materials because of its high specific surface area. In addition to the advantages of mesoporous materials such as narrow pore size distribution, controllable pore size and a large number of silanol groups, it has larger pore size, thicker pore wall and higher stability than MCM-41. Therefore, it has shown attractive application prospects in the fields of catalysis, adsorption, separation, biosensors, nanomaterial reactors and drug sustained release. Especially the development of monodisperse SBA-15 micron sphe...

Claims

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Application Information

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IPC IPC(8): C01B33/12
Inventor 李文智杜明霞王利平赵挥
Owner LIAOCHENG UNIV
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