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Preparation method of ordered mesoporous silica microspheres with hollow structures

A technology of mesoporous silica and hollow structure, applied in the direction of silica, silicon oxide, nanotechnology for materials and surface science, etc., can solve the problems of time-consuming preparation process, high cost, unsuitable for expanding production, etc. Achieve the effects of uniform spherical shape and size, low equipment requirements, and good polar solvent dispersion performance

Inactive Publication Date: 2012-10-10
NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the preparation and removal of sacrificial hard templates often involve multiple complex reaction processes, the preparation process is time-consuming, and the cost is relatively high, which is not suitable for industrialized and commercialized scale-up production

Method used

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  • Preparation method of ordered mesoporous silica microspheres with hollow structures
  • Preparation method of ordered mesoporous silica microspheres with hollow structures
  • Preparation method of ordered mesoporous silica microspheres with hollow structures

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Dissolve 0.08 g of cetyltrimethylammonium bromide in a mixed solution of 30 ml of ethanol and 50 ml of water, and mix 1 ml of concentrated ammonia water (the concentrated ammonia water contains Ammonia NH 3 The mass percentage concentration is 25~28%) and 1 ml tetraethyl orthosilicate were added to the mixed solution, and reacted for 12 h to obtain white solid silica microspheres ( figure 1 );

[0034] (2) The silica obtained in step (1) was centrifuged and washed with water, transferred to water to prepare a silica dispersion (2 mg / ml), and stirred at 50 °C for 20 h;

[0035] (3) The reaction product obtained in step (2) was centrifuged, washed with water, and dried; calcined at 550 °C for 6 h to obtain ordered mesoporous silica microspheres with a hollow structure (see figure 2 ).

[0036]The silica obtained through step (1) is a solid sphere with spherical morphology. The obtained ordered mesoporous silica microspheres with a hollow structure have a particle...

Embodiment 2

[0038] (1) Dissolve 0.08 g of dodecyltrimethylammonium bromide in a mixed solution of 15 ml of ethanol and 100 ml of water, and mix 0.5 ml of concentrated ammonia water (the concentrated ammonia water contains Ammonia NH 3 The mass percentage concentration is 25~28%) and 0.5 ml tetraethyl orthosilicate were added to the mixed solution, and reacted for 24 h to obtain white solid silica microspheres;

[0039] (2) Centrifuge and wash the silica obtained in step (1), transfer it to water to prepare a silica dispersion (0.1 mg / ml), and stir at 20 °C for 1 h;

[0040] (3) The reaction product obtained in step (2) was centrifuged, washed with water, and dried; calcined at 500 °C for 6 h to obtain ordered mesoporous silica microspheres with a hollow structure.

[0041] The obtained ordered mesoporous silica microspheres with a hollow structure have a particle size of 210 nm, a hollow structure, and a shell thickness of about 40 nm; the mesoporous channels are radial and have a hexago...

Embodiment 3

[0043] (1) Dissolve 0.08 g of cetyltrimethylammonium bromide in a mixed solution of 60 ml of ethanol and 25 ml of water, and mix 1.9 ml of concentrated ammonia water (the concentrated ammonia water contains Ammonia NH 3 The mass percent concentration is 25~28%) and 1.9 ml tetraethyl orthosilicate were added to the mixed solution, reacted for 3 h, and white solid silica microspheres were obtained;

[0044] (2) The silica obtained in step (1) was centrifuged and washed with water, transferred to water to prepare a silica dispersion (5 mg / ml), and stirred at 90 °C for 120 h;

[0045] (3) The reaction product obtained in step (2) was centrifuged, washed with water, and dried; calcined at 600 °C for 7 h to obtain ordered mesoporous silica microspheres with a hollow structure.

[0046] The obtained ordered mesoporous silica microspheres with a hollow structure have a particle size of 780 nm, a hollow structure, and a shell thickness of about 60 nm; the mesoporous channels are radia...

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Abstract

The invention discloses a preparation method of ordered mesoporous silica microspheres with hollow structures. The preparation method comprises the following steps: firstly, dissolving a cationic surface active agent in mixed solution of ethanol and water, sequentially adding ammonia water and a silicon source in the mixed solution under the conditions of heating and mixing, and reacting for a period of time to obtain solid silica microspheres; washing the obtained silica, transferring the silica into water for etching, and reacting for a period of time to obtain hollow silica microspheres; and finally, collecting the hollow silica, and obtaining products of ordered mesoporous silica microspheres with hollow structures by drying and roasting. In the preparation method, a sacrificial hard template or an emulsion template does not need to be prepared in advance. The preparation method has the characteristics of simple technological process, mild reaction conditions, low cost, and environmental friendliness; and the prepared hollow mesoporous silica microspheres have great application potential in ultrasonic imaging, drug delivery and other biomedical fields.

Description

technical field [0001] The invention relates to a method for preparing ordered mesoporous silica microspheres with a hollow structure, belonging to the field of preparation of inorganic materials. Background technique [0002] Using surfactants as templates to synthesize mesoporous materials with high specific surface area and uniform pore size has become a research hotspot in materials science. These mesoporous materials have been widely used in the fields of physics, chemistry and biomedicine. A variety of mesoporous materials with advanced structures and special morphologies can be synthesized by controlling the reaction conditions, such as films, fibers, spheres, hollow spheres, etc. Among them, mesoporous silica microspheres with a hollow structure have attracted widespread attention due to their special structure and function. Initially, researchers used oil-in-water emulsions, supercritical CO 2 and microcapsules as hollow templates to successfully prepare mesoporo...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y30/00
Inventor 滕兆刚卢光明陈国韬田聪聪孙晶王昕王春艳刘莹黄小银
Owner NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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