Synthesis method of bimodal mesoporous silicon dioxide

A technology of mesoporous silica and silica, applied in the direction of silica, silica, etc., can solve the problems such as the decline of the order of the mesoporous structure of the material, shorten the preparation cycle, improve the preparation efficiency, and reduce the ionic strength Effect

Inactive Publication Date: 2015-01-07
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in these disclosed dual mesoporous silicas, the larger mesoporous pores are mostly caused by the interparticle gaps generated by the accumulation of nano-scale particles, and the range of the pore size distribution depends on the size of the nanoparticles and their packing methods, And with the decrease of the particle size, the order of the mesoporous structure of the material tends to decrease.

Method used

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  • Synthesis method of bimodal mesoporous silicon dioxide
  • Synthesis method of bimodal mesoporous silicon dioxide
  • Synthesis method of bimodal mesoporous silicon dioxide

Examples

Experimental program
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Embodiment approach 1

[0026] Mix 0.404 g STAB, 0.25 ml 85% phosphoric acid solution, 1.25 ml TEOS and 10 ml H 2 O Stir and mix successively at 25°C, and continue stirring at 25°C for 6 hours after the system is completely homogeneous, then directly add 1.22 grams of ammonium phosphate solid into the above reaction system under stirring, and continue stirring at 25°C for 24 Hours later, the separated precipitate was centrifuged, washed with deionized water, dried at 60°C, and then baked at 550°C for 6 hours at a heating rate of 2.5°C / min to remove the templating agent. Obtain double mesoporous silica, its XRD figure is shown in figure 1 , its N 2 Adsorption isotherms and corresponding pore size distribution curves are shown in figure 2 , its specific surface area is 1038.3m 2 / g, the pore volume is 0.96cm 3 / g, the skeleton mesopore diameters are 2.6nm and 3.3nm respectively.

Embodiment approach 2

[0028] Mix 0.375 g of CTAB, 0.25 ml of 85% phosphoric acid solution, 1.25 ml of TEOS and 10 ml of H 2 O Stir and mix successively at 25°C, and continue stirring at 25°C for 6 hours after the system is completely homogeneous, then directly add 1.22 grams of ammonium phosphate solid into the above reaction system under stirring, and continue stirring at 25°C for 24 Hours later, the separated precipitate was centrifuged, washed with deionized water, dried at 60°C, and then baked at 550°C for 6 hours at a heating rate of 2.5°C / min to remove the templating agent. Obtain double mesoporous silica, its XRD figure is shown in image 3 , its N2 Adsorption isotherms and corresponding pore size distribution curves are shown in Figure 4 , its specific surface area is 1131.6m 2 / g, the pore volume is 0.82cm 3 / g, the skeleton mesopore diameters are 2.3nm and 3.4nm respectively.

Embodiment approach 3

[0030] Mix 0.404 g STAB, 0.25 ml 85% phosphoric acid solution, 1.25 ml TEOS and 10 ml H 2 O Stir and mix at 25°C in turn, and continue stirring at 25°C for 6 hours after the system is completely homogeneous, then directly add 1.83 grams of ammonium phosphate solid into the above reaction system under stirring, and continue stirring at 25°C for 10 Minutes later, the precipitated precipitate was centrifuged, washed with deionized water, dried at 60°C, and then baked at 550°C for 6 hours at a heating rate of 2.5°C / min to remove the template agent. Obtain double mesoporous silica, its XRD figure is shown in Figure 5 .

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Abstract

The invention relates to a synthesis method of bimodal mesoporous silicon dioxide, belonging to the technical field of inorganic porous materials. The method is characterized in that by using a cationic quaternary ammonium salt surfactant as a template, a silicon source is subjected to prehydrolysis treatment in a phosphoric acid system incapable of easily forming ordered mesoporous phase, and a phosphate solid which is weakly alkaline after being dissolved is directly added to induce the synthesis of the bimodal mesoporous silicon dioxide, of which the specific area is 949.7-1181.8 m<2> / g, the pore volume is 0.68-1.05 cm<3> / g and the framework pore sizes are respectively 2.1-2.6nm and 3.3-3.9nm. The synthesis system and preparation conditions used by the method are beneficial to in-situ packaging of various metal ions in different mesoporous pore canals and also beneficial to in-situ coating and immobilization of bioactive guest molecules in different pore canals, so that the method has important application prospects in the field of development of novel commercial catalysts, biocatalysts, multistage porous complex function materials and the like.

Description

technical field [0001] The invention discloses a method for synthesizing double mesoporous silicon dioxide, which belongs to the technical field of inorganic porous materials, and specifically relates to a method for synthesizing double mesoporous distribution silicon dioxide with a skeleton under conditions of mild acidity and low ionic strength. Background technique [0002] Since mesoporous silica was successfully synthesized in the early 1990s (J.Am.Chem.Soc., 1992, 114, 10834), due to its large specific surface area, high pore volume and flexible and adjustable pore size, etc. It shows broad application prospects in many research fields such as catalysis, adsorption, separation, biomedicine, environmental protection, host-guest chemistry and new functional materials (Chem. Rev., 1997, 97, 2373). Especially in the field of development of new catalysts, since the pore size of mesoporous silica mostly has a single value distribution, it can well solve the problem of shape...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/12
Inventor 王晓钟白亚东刘瑜崔莹莹谢克昌
Owner TAIYUAN UNIV OF TECH
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