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Preparation method of niobium oxide nano pore molecular sieve film

A molecular sieve thin film and nanopore technology, which is applied in molecular sieve compounds, chemical instruments and methods, niobium compounds, etc., can solve the problems of long preparation cycle, damage to the ordered structure of materials, and poor product quality, and achieve the order degree of material structure The effect of improving and improving the structural order and shortening the synthesis 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 niobium 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 niobium 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 (niobium oxide) in the non-aqueous phase: (1), previously only anhydrous chloride inorganic salt was used as the precursor, which will A large amount of HCl is released, and the acidity of the solution is extremely high, making Nb 2 o 5 Dissolution, thus resulting in a very long period for the preparation of mesoporous materials, generally ranging from three days to one week, and the quality of the products 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

[0013] Embodiment 1, with 1 gram of Pluronic P123 (EO 20 PO 70 EO 20 ) was dissolved in 15 grams of tetrahydrofuran, and 2.7 grams of NbCl were added 5 After one hour of stirring and reacting, turn on the heating device, evaporate the solution to 1 / 3 of the original volume at 80° C., and supplement the solvent to the original volume. Repeat the above steps until the pH value of the solution is between 0-1. After continuing to stir the mother liquor for 2 hours, transfer it to a petri dish, volatilize to form a film, take out the film after 3-4 hours, and bake it in a muffle furnace at 400°C to remove the surfactant. The specific surface area of ​​the material is 250m 2 / g, the pore volume is 0.6cm 3 / g, the pore size is 7.2 nm. The material is a two-dimensional hexagonal structure (space group p6mm).

Embodiment 2

[0014] Example 2, 1 gram of Polyglycol B50-1500 (EO 75 BO 45 ) was dissolved in 15 grams of tetrahydrofuran, and 2.7 grams of NbCl were added 5 After one hour of stirring and reacting, turn on the heating device, evaporate the solution to 1 / 3 of the original volume at 90° C., and supplement the solvent to the original volume. Repeat the above steps until the pH value of the solution is between 0-1. After continuing to stir the mother liquor for 2 hours, transfer it to a petri dish, volatilize to form a film, take out the film after 2-4 hours, and bake it in a muffle furnace at 450°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 5.1 nm. The material is a two-dimensional hexagonal structure (space group p6mm).

Embodiment 3

[0015] Embodiment 3, 1 gram of Polyglycol B50-6600 (EO 39 BO 47 EO 39 ) was dissolved in 15 grams of ethanol, and 2.7 grams of NbCl was added 5 After one hour of stirring and reacting, turn on the heating device, evaporate the solution to 1 / 3 of the original volume at 75° C., and supplement the solvent to the original volume. Repeat the above steps until the pH value of the solution is between 0-1. After continuing to stir the mother liquor for 2 hours, transfer it to a petri dish, volatilize to form a film, take out the film after 2-4 hours, and bake it in a muffle furnace at 400°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 7.8 nm. The material is a three-dimensional cubic structure (space group 1m-3m).

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Abstract

The preparation method of niobium oxide nanometer porous molecular sieve film material is characterized by that it adopts a stepwise dilution method, and includes the following steps: mixing inorganic precursor, surfactant and volatile non-aqueous solvent firstly, stirring them and making them produce reaction, then using said non-aqueous solvent to stepwise dilute the reaction solution, controlling solution pH value, then utilizing quick volatilization of solvent and 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, it can be formed into the invented niobium 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 nanomaterials, in particular to a niobium oxide (Nb) with high order degree and large specific surface area. 2 o 5 ) A method for preparing a nanoporous molecular sieve film. 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 its large specific surface area, easy surface modification, and one-dimensional or three-dimensional connectivity ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B37/00C01G33/00
Inventor 田博之刘晓英屠波赵东元
Owner FUDAN UNIV
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