Mesoporous silica with yolk-shell structure and preparation method thereof

A technology of mesoporous silica and eggshell, which is applied in the field of mesoporous silica with egg yolk-eggshell structure and its preparation, can solve the problems of increased preparation cost, environmental pollution, high temperature heating, etc., and achieve low cost and environmental protection. Friendly, low-equipment-requiring effect

Active Publication Date: 2013-07-10
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

Such a preparation process usually requires strict control of reaction conditions, and the tedious preparation process is time-consuming and labor-intensive.
On the other hand, the removal of the intermediate layer often requires high temperature h...

Method used

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  • Mesoporous silica with yolk-shell structure and preparation method thereof
  • Mesoporous silica with yolk-shell structure and preparation method thereof
  • Mesoporous silica with yolk-shell structure and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Mix 1ml of concentrated ammonia water (the mass percent concentration of NH3 contained in the concentrated ammonia water is 25%) with 30ml of ethanol and 75ml of water, and then dissolve 0.16g of dodecyltrimethylammonium bromide in the mixed solution , 0.25ml tetraethyl orthosilicate and 0.25ml 1,2-bis(triethoxysilyl)ethane were added to the aqueous alcohol solution at 30°C and stirred at 500rpm, and reacted for 12h to obtain white di Silica precipitation;

[0032] (2) Centrifuge the silicon dioxide obtained in step (1), wash it with water, transfer it to water to prepare a silicon dioxide dispersion (2 mg / ml), and place it at 70°C for 20 hours;

[0033] (3) The reaction product obtained in step (2) was centrifuged, washed with water, transferred to a mixed solution of 50 μl concentrated hydrochloric acid and 100ml ethanol, heated at 40°C for 1 hour to remove the surfactant, and finally obtained the egg yolk-eggshell structure medium Porous silica, such as figure 1 ...

Embodiment 2

[0036] (1) Mix 1ml of concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percentage concentration is 28%) mixed with 30ml ethanol and 75ml water, then 0.16g tetradecyltrimethylammonium bromide was dissolved in the mixed solution, and 0.5ml orthosilicon Acetate tetraethyl ester and 0.5ml 1,2-bis(triethoxysilyl)ethane were added to the mixed solution, reacted for 24h, and white silica precipitate was obtained;

[0037] (2) Centrifuge and wash the silica obtained in step (1), transfer it to water to prepare a silica dispersion (0.1 mg / ml), and place it at 50°C for 12 hours;

[0038] (3) The reaction product obtained in step (2) was centrifuged, washed with water, transferred to a mixed solution of 100 μl concentrated hydrochloric acid and 200ml ethanol, heated at 50°C for 10 hours to remove the surfactant, and finally obtained the egg yolk-eggshell structure medium Porous silica.

[0039] The mesoporous silica with egg yolk-eggshell struct...

Embodiment 3

[0041] (1) Mix 1ml of concentrated ammonia water (the NH contained in the concentrated ammonia water 3 The mass percent concentration is 26%) mixed with 30ml ethanol and 75ml water, then 0.64g hexadecyltrimethylammonium bromide was dissolved in the mixed solution, and 0.25ml orthosilicon Acetate tetraethyl ester and 0.25ml 1,2-bis(triethoxysilyl)ethane were added to the mixed solution, reacted for 3h, and white silica precipitate was obtained;

[0042] (2) Centrifuge and wash the silica obtained in step (1), transfer it to water to prepare a silica dispersion (5mg / ml), and place it at 20°C for 150h;

[0043] (3) The reaction product obtained in step (2) was centrifuged, washed with water, transferred to a mixed solution of 200 μl concentrated hydrochloric acid and 400ml ethanol, heated at 60°C for 5 hours to remove the surfactant, and finally obtained the egg yolk-eggshell structure medium Porous silica.

[0044] The mesoporous silica with egg yolk-eggshell structure obtaine...

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Abstract

The invention discloses mesoporous silica with a yolk-shell structure and a preparation method thereof. The morphology of the mesoporous silica is of spherical bodies. The spherical body has a mesoporous core and a mesoporous shell. A cavity structure is between the mesoporous core and the mesoporous shell. Mesoporous silica balls have high specific surface area, uniform and adjustable particle size and uniform pore size. The preparation method of the mesoporous silica includes: dissolving a surface active agent in a mixed solution of ethanol, ammonia and water, adding two silica precursors into the mixed solution under heating and stirring conditions, transferring the obtained spherical silica into water after reacting for a period, etching to remove intermediate loose layers of silica balls, finally removing the surface active agent to obtain mesoporous silica products having the yolk-shell structure. The preparation method of the present invention has the characteristics of simple process, low cost, and environmental protection. The prepared mesoporous silica has great application potential in medical imaging, drug delivery and other fields.

Description

technical field [0001] The invention relates to a core-shell structure nano material in the field of inorganic materials and a preparation method thereof, in particular to an egg yolk-eggshell structure mesoporous silica and a preparation method thereof. Background technique [0002] In recent years, the application of core-shell nanomaterials in the fields of catalysis and biomedicine has become more and more in-depth and extensive. As a special core-shell structure, the yolk-eggshell structure with a large gap layer between the core and the shell has attracted more attention. Among many nanomaterials, the egg yolk-eggshell structure with mesoporous silica shell has good biocompatibility, high specific surface area, uniform pore size and large cavity in drug delivery, medical imaging, etc. Show great application potential. For example, Shi Jianlin and his collaborators used pre-prepared gold nanoparticles or ferric oxide particles as the core, and obtained mesoporous sili...

Claims

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Application Information

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IPC IPC(8): C01B33/12B82Y40/00
Inventor 滕兆刚卢光明陈国韬刘莹唐玉霞朱飞鹏杨楠楠卢楠谢媛赵艳娥曹新志
Owner NANJING GENERAL HOSPITAL NANJING MILLITARY COMMAND P L A
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