Monodisperse hollow mesoporous silicon oxide microsphere material and double-surfactant induced assembly preparation method thereof

A mesoporous silica and surfactant technology, applied in the direction of microsphere preparation, microcapsule preparation, etc., can solve the problem that it is difficult to prepare monodisperse mesoporous silica microsphere materials, achieve good monodispersity, and can The effect of strong control and uniform particle size

Inactive Publication Date: 2019-04-26
元颉新材料科技(浙江)有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation methods of hollow silica microsphere materials currently developed mainly include the template method and the microemulsion method, but because the silicon source precursor is hydrolyzed and cross-linked too fast in an aqueous solvent, it is usually difficult to prepare large-scale adjustable silica microspheres. Monodisperse mesoporous silica microsphere material, the preparation of large-scale controllable and monodisperse mesoporous silica microspheres still has great technical challenges

Method used

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  • Monodisperse hollow mesoporous silicon oxide microsphere material and double-surfactant induced assembly preparation method thereof
  • Monodisperse hollow mesoporous silicon oxide microsphere material and double-surfactant induced assembly preparation method thereof
  • Monodisperse hollow mesoporous silicon oxide microsphere material and double-surfactant induced assembly preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Dissolve a certain amount of Pluronic F127 and CTAB with 200ml of ethanol and water mixed solution under stirring condition, add 10ml of tetraethyl silicate deionized water after dissolving, and continue mechanical stirring. After stirring for 5 minutes, 5ml of ammonia water was added dropwise to the above mixed solution, and stirring was continued for 10 hours. The obtained white gel mixed solution was centrifuged at 12000rpm for 10 minutes to separate the white gel precipitate product, then washed with ethanol three times, and then washed with water three times, and the obtained white precipitate was dried in air at 60°C for 12 hours, Dispersed in 100ml of water, heat-treated in solvent at 150°C for 6 hours, and then calcined at 600°C for 4 hours, the mesoporous silica microspheres with a diameter of 500nm and a monodisperse hollow structure can be obtained. Its shape and properties are shown in Figure 1-Figure 5 shown. What is prepared is a silica microsphere mate...

Embodiment 2

[0034] Dissolve a certain amount of Pluronic F127 and dodecyltrimethylammonium chloride with 200ml of ethanol and water mixed solution with stirring, add 10ml of tetraethyl silicate deionized water after dissolution, and continue mechanical stirring. After stirring for 5 minutes, 5ml of ammonia water was added dropwise to the above mixed solution, and stirring was continued for 10 hours. The obtained white gel mixed solution was centrifuged at 12000rpm for 10 minutes to separate the white gel precipitate product, then washed with ethanol three times, and then washed with water three times, and the obtained white precipitate was dried in air at 60°C for 12 hours, Dispersed in 100ml of water, heat-treated in solvent at 150°C for 6 hours, and then calcined at 600°C for 4 hours, the mesoporous silica microspheres with a diameter of 550nm and a monodisperse hollow structure can be obtained.

Embodiment 3

[0036] Dissolve a certain amount of Pluronic F127 and CTAB with 200ml of ethanol and water mixed solution under stirring condition, add 10ml of tetraethyl silicate deionized water after dissolving, and continue mechanical stirring. Compared with Example 1, the ratio of ethanol and water in the mixed solution was changed, and after stirring for 5 minutes, 5ml of ammonia water was added dropwise to the above mixed solution, and the stirring was continued for 10 hours. The obtained white gel mixed solution was centrifuged at 12000rpm for 10 minutes to separate the white gel precipitate product, then washed with ethanol three times, and then washed with water three times, and the obtained white precipitate was dried in air at 60°C for 12 hours, Dispersed into 100ml of water, heat-treated in solvent at 150°C for 6 hours, and then calcined at 600°C for 4 hours, the mesoporous silica microspheres with a diameter of 300nm and a monodisperse hollow structure can be obtained.

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Abstract

The invention relates to a monodisperse hollow mesoporous silicon oxide microsphere material and a double-surfactant induced assembly preparation method thereof. The monodisperse hollow mesoporous silicon oxide microsphere material has a hollow microsphere morphology, the microsphere diameter size is 200-1000nm, the hollow size of 50-700nm, an outer shell adopts a mesoporous structure, the shell thickness is 50-500nm, the mesoporous size is 2-20nm, the specific surface area of the microspheres is 700-1200m<2>/g, and the pore volume is 0.3-0.85cm<3>/g. During preparation, an induced self-assembly method under mutual assistance of two surfactants, namely a nonionic amphiphilic triblock polymer surfactant and an ionic organic surfactant, is adopted, and in a simple mixed solvent of alcohol and water, in a sol-gel way of dropwise adding a silicon source precursor, centrifuging, washing and calcinating treatment is performed to obtain the size-controllable, monodisperse, mesoporous, high-specific surface area and large-pore volume silicon oxide microsphere material. Compared with the prior art, the invention has the advantages of simple operation, good repeatability, easy obtainment ofraw materials, low cost, capability of achieving industrial preparation and the like.

Description

technical field [0001] The invention belongs to the technical field of material preparation, and in particular relates to a monodisperse hollow structure mesoporous silicon oxide microsphere material and a preparation method for its double-surfactant-induced assembly. Background technique [0002] Hollow-structured nano-mesoporous materials have been widely used in many fields, including electronics industry, environmental protection, cosmetics industry, and medical science, due to their special physical and chemical structures and their available internal cavities and external mesoporous structures. , but it is often dispersed in a certain system during use, which means that the dispersion of the material in the system plays a very critical role in the performance of the material, which affects the monodispersity and size of the particles in the material Higher requirements have been put forward, and more and more researchers have paid more and more attention to the prepara...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/02
CPCB01J13/02
Inventor 朱洪伟赵东元
Owner 元颉新材料科技(浙江)有限公司
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