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Preparation method of titanium oxide nano pore molecular sieve film

A technology of nanopores and molecular sieves, applied in the direction of titanium dioxide, molecular sieve compounds, chemical instruments and methods, etc., can solve the problems of long period of mesoporous materials, destroying the ordered structure of materials, and long preparation period, etc., and achieve the improvement of the order degree of material structure , Improving the structural order and shortening the preparation cycle

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

In the past few literatures or patents on titanium oxide nanoporous materials, the reported materials are often not highly ordered, the preparation process is cumbersome, and the preparation cycle is long, which has become a "bottleneck" in the application of titanium oxide nanoporous materials.
affect its scope of application
[0004] It is worth mentioning that there are certain defects in the traditional synthesis method of transition metal oxide (titanium oxide) in non-aqueous phase: (1), previously only anhydrous chloride inorganic salt was used as precursor, which will A large amount of HCl is released, and the acidity of the solution is extremely high, making TiO 2 Dissolution, thus resulting in a very long period for the preparation of mesoporous materials, generally ranging from one to two weeks, and the quality of the product is also poor
(2) The synthesis of most transition metal mesoporous oxides is generally achieved by the coordination between surfactants and inorganic precursors. In a highly acidic environment, this coordination will be greatly reduced, destroying the ordered structure of materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Add 1 g of Polyglycol B50-1500 (EO 75 BO 45 ) Dissolve in 15 grams of tetrahydrofuran, add 3.4 grams of TiCl 4 (Very small amount) and Ti(OC 4 H 9 ) 4 The mass ratio of the two is 1:20, and the pH value of the solution is controlled between 2-3. After stirring the mother liquor for 2 hours, transfer it to a petri dish and volatilize to form a film. After 2-4 hours, the film is taken out and calcined in a muffle furnace at 350°C to remove the surfactant. The specific surface area of ​​the material is 210m 2 / g, the pore volume is 0.5cm 3 / g, the pore size is 5.2 nanometers. The material is a three-dimensional cubic structure (space group is 1m-3m).

Embodiment 2

[0016] Add 1 g of Polyglycol B50-6600 (EO 39 BO 47 EO 39 ) Dissolve in 15 grams of ethanol and add 3.4 grams of TiCl 4 (Very small amount) and Ti(OC 4 H 9 ) 4 The mass ratio of the two is 1:18, and the pH value of the solution is controlled between 2-3. After stirring the mother liquor for 2 hours, transfer it to a petri dish and volatilize to form a film. After 2-4 hours, the film is taken out and calcined in a muffle furnace at 350°C to remove the surfactant. The specific surface area of ​​the material is 250m 2 / g, the pore volume is 0.5cm 3 / g, the pore size is 7.5 nanometers. The material is a three-dimensional cubic structure (space group is 1m-3m).

Embodiment 3

[0018] Add 0.7 grams of polyoxyethylene alkylamine (H(C 2 H 4 O) x (R)N(C 2 H 4 O) y H(x+y>5)) is dissolved in 15 g of tetrahydrofuran, and 3.2 g of TiCl is added 4 (Very small amount) and Ti(OC 3 H 7 ) 4 The mass ratio of the two is 1:10, and the pH value of the solution is controlled between 2-3. After stirring the mother liquor for 2 hours, transfer it to a petri dish and volatilize to form a film. After 2-4 hours, the film is taken out and calcined in a muffle furnace at 350°C to remove the surfactant. The specific surface area of ​​the material is 230m 2 / g, the pore volume is 0.5cm 3 / g, the pore size is 2.5 nanometers.

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PUM

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Abstract

The preparation method of titanium oxide nanometer porous molecular sieve film is characterized by that it adopts mixed inorganic source method, and includes the following steps: firstly, mixing prehydrolyzed mixed inorganic precursor, surfactant, volatile non-aqueous solvent, 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 film material. After said film material is undergone the processes of ageing and high-temp. calcination, said film material can be formed into the invented titanium oxide nanometer porous molecular sieve film with large specific surface and high porosity. Said molecular sieve film possesses extensive application in the fields of catalysis, separation and sensor, etc.

Description

Technical field [0001] The invention belongs to the technical field of inorganic nano materials, and specifically relates to a method for preparing a titanium oxide nanoporous molecular sieve film with a high degree of order and a large specific surface area. technical background [0002] The synthesis of ordered nanoporous materials with 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 higher specific surface, uniform pores, and orderly dimensions to the scientific and industrial circles. This material can be designed into a certain shape, such as film, sheet, fiber, ball, polyhedron, etc. Among them, nanoporous film materials are most widely used in laboratories and industrial production. Because of their large specific surface area, easy modification of the surface, and one-dimensional or three-dimensional connec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B33/145C01B33/155C01B37/00C01G23/047
Inventor 田博之刘晓英屠波赵东元
Owner FUDAN UNIV
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