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High amino content ordered mesoporous silicon dioxide film and its preparation method and application

A technology of mesoporous silica and silica, applied in the directions of silica, silica, chemical instruments and methods, etc., can solve the problem of difficulty in obtaining order, small film pore size, mesoporous pore size and pore volume. and other problems, to achieve the effects of excellent assembly and fixation performance, orderly pore structure, and smooth and continuous surface.

Inactive Publication Date: 2008-07-09
NAT UNIV OF DEFENSE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has several disadvantages: (a) many organic functional groups are grafted on the surface of mesoporous channels, which will lead to smaller pore size and pore volume of mesoporous channels; (b) the density of surface-active organosilanes is low, and organic functional groups (c) post-grafting is a time-consuming process, which includes two steps of preparation of parent pure silicon mesoporous film and silanization treatment; (d) grafting of organic groups in mesoporous channels Branch efficiency and average distribution are difficult to control
However, few researchers have discussed in detail the influence of organic groups and sol aging on the assembly of organic functionalized mesoporous films, especially when the initial sol contains a relatively high concentration of organosilanes, it is difficult to obtain mesoporous membranes with good order. film
In addition, all the mesoporous films reported above mostly use small-molecule surfactants, and the pore size of the prepared films is small, which cannot meet the needs of large-scale molecular assembly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] An ordered mesoporous silica film with high amino content, the mass content of amino groups in the film is 9%, and the specific surface area is 690m 2 / g, the distribution of organic groups on the surface of the mesoporous film is 4.8 amino groups / nm 2 , The mesopore diameter is 2.1nm. This silicon dioxide thin film is made by following method:

[0020] Mix 4.47mL tetraethyl orthosilicate (TEOS), 8.7mL absolute ethanol (EtOH), 0.025mL dilute hydrochloric acid (0.1mol / L), and 0.9mL deionized water. Meet: 0.4TEOS: 3C 2 h 5 OH: 5×10 -5 HCl:1H 2 O; after stirring evenly, heat to 60°C for reflux hydrolysis for 60 minutes to obtain clear, partially hydrolyzed silica sol; after the silica sol is cooled, add 0.45mL deionized water and 3.15mL concentrated hydrochloric acid (mass concentration is 36%), stir After 10 minutes, add 35 mL of absolute ethanol to dilute the mixed sol, and slowly add 7 mL of 3-aminopropyltriethoxysilane (APTES) dropwise to the diluted sol in an ic...

Embodiment 2

[0022] An ordered mesoporous silica film with high amino content, the mass content of amino in the film is 7.5%, and the specific surface area is 705m 2 / g, the distribution of organic groups on the surface of the mesoporous film is 4 amino groups / nm 2 , Mesopore diameter is 3.2nm. This silicon dioxide thin film is made by following method:

[0023] Mix 5.58mL tetraethyl orthosilicate (TEOS), 8.7mL absolute ethanol (EtOH), 0.025mL dilute hydrochloric acid (0.1mol / L), and 0.9mL deionized water. Meet: 0.5TEOS: 3C2 h 5 OH: 5×10 -5 HCl:1H 2 O, after stirring evenly, heat to 60°C for reflux hydrolysis for 60 minutes to obtain clear, partially hydrolyzed silica sol; after the silica sol is cooled, add 0.95mL deionized water and 2.65mL concentrated hydrochloric acid (mass concentration is 36%), stir After 10 minutes, add 30 mL of absolute ethanol to dilute the mixed sol, and slowly add 5.84 mL of 3-aminopropyltriethoxysilane (APTES) dropwise to the diluted sol in an ice-water ba...

Embodiment 3

[0025] An ordered mesoporous silica film with high amino content, the mass content of amino in the film is 6%, and the specific surface area is 680m 2 / g, the distribution of organic groups on the surface of the mesoporous film is 3.2 amino groups / nm 2 , The mesopore diameter is 8.4nm. This silicon dioxide thin film is made by following method:

[0026] Mix 6.7mL tetraethyl orthosilicate (TEOS), 8.7mL absolute ethanol (EtOH), 0.025mL dilute hydrochloric acid (0.1mol / L), and 0.9mL deionized water. Meet: 0.6TEOS: 3C 2 h 5 OH: 5×10 -5 HCl:1H 2 O, after stirring evenly, heat to 60°C for reflux and hydrolyze for 60 minutes to obtain clear, partially hydrolyzed silica sol; after the silica sol is cooled, add 1.45mL deionized water and 2.15mL concentrated hydrochloric acid (mass concentration is 36%), stir After 10 minutes, add 25 mL of absolute ethanol to dilute the mixed sol, slowly add 4.67 mL of 3-aminopropyltriethoxysilane (APTES) dropwise to the diluted solution in an ice...

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PUM

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Abstract

The invention relates to a preparing process and application sequential mesoporous silicon dioxide film with high amino content. The preparing process of the invention takes various surface active agent as template, takes tetraethyl ortho-silicate and 3-3-aminopropyl triethoxysilane as the silicon source, utilizing sol-gel manner, leading the amino silane to take the molar percentage of the whole silane of 30-60 by introducing amino silane directly part of silica sol, after forming homogeneous solution, relying on the synergy of the silane and organic templates, forming films by dip-coating on the clear substrate, finally forming functional sequential silicon dioxide film with different meso-structure and high amino content. The silicon dioxide mesoporous film of the invention has perfect assembly and fixing property to organic molecules, inorganic anions, protein, enzyme molecule and the like object materials.

Description

technical field [0001] The invention relates to a mesoporous silicon dioxide film, in particular to an ordered mesoporous silicon dioxide film with high amino content and its preparation method and application. Background technique [0002] At present, the biggest application prospect of mesoporous silica film is as the main material, using the ordered pores in the film layer to assemble various functional active molecules in it. Early studies found that very low loading rates were caused by the lack of interaction between mesoporous host materials and guest molecules. Organically functionalized mesoporous materials can solve this problem, because the surface organically functionalized mesoporous materials can increase the force between the guest molecules (van der Waals force, hydrogen bond, electrostatic force, etc.), or between the two form ionic and covalent bonds. Therefore, in recent years, many researchers have begun to pay attention to the preparation of functional...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B33/14C01B33/157C09K9/00
Inventor 王建方张学骜吴文健满亚辉胡碧茹
Owner NAT UNIV OF DEFENSE TECH
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