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Preparation method of silicon oxide nano pore molecular sieve film

A technology of nanopores and molecular sieves, applied in molecular sieve compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as complex preparation methods, low structural order, and influence on the scope of application

Inactive Publication Date: 2003-07-09
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as a widely used silicon oxide nanoporous film material, the preparation method is relatively complicated, and the degree of structural order is not high, which affects its application range.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] A certain mass ratio of Pluronics P123 (EO 20 PO 70 EO 20 ) and Brij35 (C 12 EO 23 ) was dissolved in absolute ethanol, and TEOS, H 2 O, 2M HCl, and ethanol are mixed according to a certain ratio to prepare SiO 2 Sol. After two hours of stirring respectively, they were mixed, and the mixture was stirred for one hour, then transferred to a petri dish, and dried to form a film. After 2-5 days, the film was taken out and heated in water at 100°C for one day. Then place the product in a muffle furnace and heat it up to 550°C, and bake it at this temperature for 5 hours; or reflux in ethanol to remove the surfactant. The mass ratio of the mother liquor raw materials in the petri dish is as follows: P123: Brij35: TEOS: 2MCl: H 2 O: ethanol = 1.0:0.3:2.08:0.1:0.9:15. Analysis tests such as PXRD, BET and TEM prove that the film material is a high-quality silicon oxide film material with a two-dimensional hexagonal structure (space group p6mm). The specific surface are...

Embodiment 2

[0012] A certain mass ratio of PluronicsF127 (EO 106 PO 70 EO 106 ) and Brij78 (C 16 EO 20 ) was dissolved in absolute ethanol, and TMOS, H 2 O, 2M HCl, and ethanol are mixed according to a certain ratio to prepare SiO 2 Sol. After two hours of stirring respectively, they were mixed, and the mixture was stirred for one hour, then transferred to a petri dish, and dried to form a film. After 2-5 days, the film was taken out and heated in water at 100°C for one day. Then put the product in a muffle furnace and bake at 550°C for 5.5 hours; or reflux in ethanol to remove the surfactant. The mass ratio of the mother liquor raw materials in the petri dish is as follows: F127: Brij78: TMOS: 2MCl: H 2 O: ethanol = 0.7:0.1:1.52:0.1:0.9:15. Analysis tests such as PXRD, BET and TEM prove that the film material is a silicon oxide film material with a high-quality three-dimensional cubic structure (space group is Im-3m). The specific surface area of ​​the material is 620m 2 / g, t...

Embodiment 3

[0014] A certain mass ratio of Polyglycol B50-6600 (EO 39 BO 47 EO 39 ) and Brij35 were dissolved in absolute ethanol, and TEOS, H 2 O, 2M HCl, and ethanol are mixed according to a certain ratio to prepare SiO 2 Sol. After two hours of stirring respectively, they were mixed, and the mixture was stirred for one hour, then transferred to a petri dish, and dried to form a film. After 2-5 days, the film was taken out and heated in water at 100°C for one day. Then put the product in a muffle furnace and bake at 550°C for 5 hours; or reflux in ethanol to remove the surfactant. The mass ratio of the mother liquor raw materials in the petri dish is as follows: B50-6600: Brij35: TEOS: 2MCl: H 2 O: ethanol = 0.7:0.3:2.08:0.1:0.9:15. Analysis tests such as PXRD, BET and TEM prove that the film material is a silicon oxide film material with a high-quality three-dimensional cubic structure (space group 1m-3m). The specific surface area of ​​the material is 650m 2 / g, the pore volu...

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PUM

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Abstract

The preparation method of silicon oxide nanometer porous molecular sieve film is characterized by adopting mixed non-ionic surfactant as structural guide agent, mixing the prehydrolyzed inorganic precursor, surfactant, volatile non-aqueous solvent, proper quantity of water and hydrochloric acid, stirring them and making them produce reaction, then utilizing quick volatilization of solvent and utilizing sol-gel and liquid crystal template self-assembling process to form 2-D and 3-D high-ordered organic-inorganic composite silicon oxide film material. After the film material is undergone the processes of ageing, high-temp. calcination or ethyl alcohol extraction to remove surfactant, it can be formed into the silicon oxide molecular sieve film with large specific surface and high porosity. Said invented silicon oxide molecular sieve film possesses ectensive application in the fields of separation, catalysis and sensor, etc.

Description

technical field [0001] The invention belongs to the technical field of inorganic nanometer materials, and in particular relates to a preparation method of a silicon oxide nanoporous molecular sieve film with high order degree and large specific surface area. technical background [0002] Synthesis of ordered nanoporous materials using amphiphilic (hydrophilic, lipophilic) molecules as structure-directing agents and templates has an extremely important impact on materials science. This important discovery has introduced a new type of material with high specific surface, uniform pores and ordered dimensions to the scientific and industrial circles. This material can be designed into a certain shape, such as film, sheet, fiber, sphere, polyhedron, etc. Among them, nanoporous film materials are the most widely used in laboratory and industrial production. Because of their large specific surface area, easy surface modification, and one-dimensional or three-dimensional connectivi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/145C01B33/155C01B37/00
Inventor 田博之刘晓英屠波赵东元
Owner FUDAN UNIV