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Preparation method of mesoporous silicone balls having regular morphology

A technology of mesoporous silicon spheres and mesoporous silica, applied in the directions of silicon oxide, silicon dioxide, etc., can solve the problems of difficult to have good morphology and high synthesis price of synthetic products, and achieve the effect of facilitating industrial application and reducing fluid resistance.

Inactive Publication Date: 2016-06-29
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is to overcome the defects in the prior art that the synthesis price is expensive and the synthesis product is difficult to have the good shape and particle size required by the industry, and provide a low-cost preparation with good properties. Preparation method of mesoporous silica sphere

Method used

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  • Preparation method of mesoporous silicone balls having regular morphology
  • Preparation method of mesoporous silicone balls having regular morphology

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Wash and dry 50g (1-3mm) silica balls, then place them in a muffle furnace and raise the temperature to 550°C at a rate of 5°C / min and keep for 30min, then cool down and take them out for use.

[0028] (2) Dissolve 7.5g of cetyltrimethylammonium bromide (CTAB) in 151ml of deionized water, add 0.3g of NaOH, 38ml of absolute ethanol, and stir for 30min until the solution is clear to obtain a reaction solution.

[0029] (3) Add 4.5 g of pretreated silicon spheres to the reaction solution in (2), stir for 30 min, transfer the mixture to a hydrothermal reaction kettle for crystallization at 110°C for 48 h;

[0030] (4) Filter the solution in (3) to obtain a composite sphere, add 189ml of deionized water and place it in a hydrothermal reaction kettle to react at 110°C for 48h for hydrothermal post-treatment.

[0031] (5) The composite spheres obtained after hydrothermal post-treatment are washed and dried at 50°C for 12 hours; then the dried composite spheres containing t...

Embodiment 2

[0034] (1) Wash and dry 50g (0.5-1.5mm) of silica balls, then place them in a muffle furnace and raise the temperature to 350°C at a rate of 6°C / min and keep for 50min, then cool down and take them out for use.

[0035] (2) Dissolve 7.0g of dodecyltrimethylammonium bromide in 189ml of deionized water, add 0.3g of NaOH, and stir for 45min until the solution is clear to obtain a reaction solution.

[0036] (3) Add 4.5 g of pretreated silicon spheres to the reaction solution in (2), stir for 45 min, and transfer the mixture to a hydrothermal reactor for crystallization at 80°C for 40 h.

[0037] (4) Filter the solution in (3) to obtain a composite sphere, add 189ml of deionized water and place it in a hydrothermal reaction kettle to react at 80°C for 40h for hydrothermal post-treatment.

[0038] (5) The composite spheres obtained after hydrothermal post-treatment are washed and dried at 45°C for 12 hours; then the dried composite spheres containing the template agent are roasted,...

Embodiment 3

[0041] (1) Wash and dry 50g (3-5mm) of silica balls, then place them in a muffle furnace and raise the temperature to 450°C at a rate of 7°C / min and keep for 40min, then cool down and take them out for use.

[0042] (2) 15g tetradecyltrimethylammonium bromide (C 14TAB) was dissolved in 303ml of deionized water, added with 0.6g of NaOH and 75ml of absolute ethanol, and stirred for 30min until the solution became clear to obtain a reaction solution.

[0043] (3) Add 9 g of pretreated silicon spheres to the reaction solution in (2), stir for 30 min, and transfer the mixture to a hydrothermal reaction kettle for crystallization at 100°C for 35 h.

[0044] (4) Filter the solution in (3), save the filtrate for reuse, and obtain a composite sphere, add 189ml of deionized water and place it in a hydrothermal reactor for 35 hours at 100°C for hydrothermal post-treatment.

[0045] (5) The composite spheres obtained after hydrothermal post-treatment are washed and dried at 45°C for 12 h...

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Abstract

The invention relates to a preparation method of mesoporous silicone balls having regular morphology and belongs to the technical field of mesoporous material preparation. The preparation method includes: utilizing low-cost large-particle commercial silicone balls (0.5-8 mm) as cue balls; adding alkaline substance and template agent and controlling dissolution and polymerization rate in reaction; synthesizing through hydrothermal reaction before hydrothermal aftertreatment; filtering, drying and calcining for 3-5 h at 350-550 DEG C to obtain the mesoporous silica balls regular in morphology. Experiments prove that a reaction solution can be used many times. Mesoporous silica obtained by the method has regular spherical morphology, and nitrogen adsorption and desorption representation shows that the mesoporous silicone balls have the advantages of large specific surface area and regular mesoporous pore structure. By using the method, the low-cost advantage of industrial silicone balls is utilized, and macro morphology and mechanical strength of particles are maintained, so that the disadvantage that a silicone source is high in price in the synthesis process of conventional mesoporous materials is overcome, the problem of fluid resistance during catalysis and heavy metal adsorption of the mesoporous materials is solved, and experience is provided for application of the mesoporous silica balls having regular morphology in industrialization.

Description

technical field [0001] A method for preparing mesoporous silicon spheres with regular appearance belongs to the technical field of mesoporous material preparation. Background technique [0002] Mesoporous silica materials have great advantages and potential application value in macromolecular separation, catalysis, adsorption and other related industries due to their advantages of high specific surface area and relatively regular channels, especially the high specific surface area and The regular pore structure can increase the interaction area and efficiency with molecules, so that the adsorption and catalytic performance can be doubled. However, the current factors restricting the industrial application of mesoporous materials mainly include (1) high synthesis cost. Including expensive silicon source materials to be added in the traditional synthesis process and a large amount of acid and alkali materials required in the synthesis process. (2) For applications such as in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/18
CPCC01B33/18C01P2006/12C01P2006/16C01P2004/32
Inventor 朱文杰李曦同吴迪马文会罗永明韩彩芸
Owner KUNMING UNIV OF SCI & TECH