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Ordered mesoporous organosilica hollow sphere prepared by one-step method and preparation method thereof

A technology of organic silicon oxide and hollow spheres, applied in the direction of silicon oxide, silicon dioxide, etc., can solve the problems of limited loading of organic groups, hindering industrialization process, long production cycle, etc., and achieves simple and easy preparation process, Good prospects for industrial applications and the effect of increasing loading capacity

Active Publication Date: 2017-03-01
TSINGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method utilizes the hydrolysis of 1,2-bis(trimethoxysilyl)ethane silicon source to introduce C-C bonds into the inorganic silica framework, but because the etching process of this patent requires tetraethyl orthosilicate (RO) 4 Si is the silicon source, and the silicon source of this structure makes inorganic SiO exist in the product 2 structure, due to the existence of Si-O-Si bonds, the loading amount of organic groups in the prepared silica skeleton is limited, and the loading amount of organic groups in the skeleton will directly affect the adsorption, catalysis and drug absorption of organosilica. Slow release and controlled release performance, so increasing the loading of organic groups in the organosilica framework is also a technical problem to be solved urgently
At the same time, because the patent needs to synthesize silica spheres with a solid structure first, and then etch again to obtain mesoporous silica products with an egg yolk-eggshell structure, compared with the direct generation of core-shell or hollow silica spheres in one step. method, complex process, long production cycle, high energy consumption, which seriously hinders its industrialization process

Method used

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  • Ordered mesoporous organosilica hollow sphere prepared by one-step method and preparation method thereof
  • Ordered mesoporous organosilica hollow sphere prepared by one-step method and preparation method thereof
  • Ordered mesoporous organosilica hollow sphere prepared by one-step method and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Octadecyltrimethylammonium bromide, water and ethanol are mixed to form solution A, and the mass ratio of cetyltrimethylammonium bromide, water and ethanol is: 1:180:60;

[0038] (2) Dissolve 1,2-bis(triethoxysilyl)ethane in ethanol to form solution B, the concentration of 1,2-bis(triethoxysilyl)ethane in ethanol is: 0.05g / ml;

[0039] (3) Mix solution A and solution B and stir for 1 min to obtain solution C;

[0040] (4) Add ammonia water to solution C, stir or stand still for 0.25h at 25°C, and form positively charged ordered mesoporous organosilica hollow spheres in one step (such as figure 1 , figure 2 Shown), the concentration of ammoniacal liquor in solution C is 5mg / ml;

[0041] (5) After centrifugation, filtration, and water washing, the ordered mesoporous organosilica hollow spheres with positive charges on the surface are transferred to the surfactant extraction solution, and heated at 35°C for 6 hours to remove the cationic surfactant to obtain Orde...

Embodiment 2

[0044] (1) Mix octadecyltrimethylammonium bromide, water and ethanol to form solution A, the mass ratio of cetyltrimethylammonium bromide, water and ethanol is: 1:210:130;

[0045] (2) Dissolve 1,2-bis(trimethoxysilyl)ethane in ethanol to form solution B, the concentration of 1,2-bis(trimethoxysilyl)ethane in ethanol is: 0.01g / ml ;

[0046] (3) Mix solution A and solution B and stir for 1 min to form solution C;

[0047] (4) Add ammonia water to solution C, stir or stand still for 0.25h at 25°C, and form positively charged ordered mesoporous organosilica hollow spheres in one step (such as image 3 Shown), the concentration of ammoniacal liquor in solution C is 11mg / ml;

[0048] (5) After centrifugation, filtration, and water washing, the ordered mesoporous organosilica hollow spheres with positive charges on the surface are transferred to the surfactant extraction solution, and heated at 32°C for 8 hours to remove the cationic surfactant to obtain Ordered mesoporous organo...

Embodiment 3

[0051] (1) Tetradecyltrimethylammonium bromide, water and tert-butanol are mixed to form solution A, and the mass ratio of tetradecyltrimethylammonium bromide, water and tert-butanol is: 1:110: 150;

[0052] (2) Dissolve 1,2-bis(triethoxysilyl)ethane in tert-butanol to form solution B, 1,2-bis(triethoxysilyl)ethane in tert-butanol alcohol The concentration is: 0.08g / ml;

[0053] (3) Mix solution A and solution B and stir for 2 minutes to form solution C;

[0054] (4) Add ammonia water to solution C, stir or stand still for 0.25h at 25°C, and form positively charged ordered mesoporous organosilica hollow spheres in one step (such as Figure 4 Shown), the concentration of ammoniacal liquor in solution C is 6mg / ml;

[0055] (5) After centrifugation, filtration, and water washing, the ordered mesoporous organosilica hollow spheres with positive charges on the surface are transferred to the surfactant extraction solution, and heated at 55°C for 3 hours to remove the cationic sur...

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Abstract

The invention relates to an ordered mesoporous organic silicon oxide hollow ball prepared through a one-step method and a preparation method of the ordered mesoporous organic silicon oxide hollow ball. The prepared ordered mesoporous organic silicon oxide hollow ball has good spherical morphology. The ball grain size ranges from 50 nm to 100 nm. The ball grain size distribution is uniform. The ordered mesoporous organic silicon oxide hollow ball is high in monodispersity, strength and dispersibility. A spherical shell comprises ordered radial mesoporous ducts. The preparation method is simple and easy to implement and can be easily conducted in an industrial mode. The ordered mesoporous organic silicon oxide hollow ball can be prepared through one step without sacrificial template or postprocessing. The fastest preparation process lasts for only 0.25 h. By means of the structure, reaction molecules or medicine molecules can conveniently enter and leave the ordered mesoporous organic silicon oxide hollow ball, and the ordered mesoporous organic silicon oxide hollow ball has good application prospects in the fields of medicine slow release, release control, medical imaging, catalysis and the like.

Description

technical field [0001] The invention relates to the field of organic-inorganic composite materials, in particular to organic silicon oxide hollow spheres with ordered mesoporous channels and a preparation method thereof. Background technique [0002] Mesoporous silica spheres combine the dual advantages of mesoporous and spherical shapes, and their application research in the fields of catalysis, batteries, and biomedicine has attracted widespread attention, especially as an anticancer drug delivery system, which has become a new generation of Cancer drug carrier. However, due to the inherent inorganic characteristics of mesoporous silica spheres, compared with other organic supports, mesoporous silica spheres have lower biocompatibility and biosafety. Therefore, the organofunctionalization of silicon oxide—that is, the introduction of organic functional groups into the surface or pore walls of mesoporous molecular sieves to form organic-inorganic hybrid porous materials ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/18
Inventor 杨金龙马宁张月席小庆许杰王亚利张笑妍渠亚男
Owner TSINGHUA UNIV
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