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Method for synthesizing phosphotungstic acid-titanium dioxide composite spherical nanomaterials by one-step sol-gel method

A technology of titanium dioxide and synthesis methods, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, nanotechnology, etc., can solve the problems of complex preparation methods and unresolved energy consumption, and achieve simple preparation methods , less equipment energy consumption, and the effect of simplifying the experimental process

Inactive Publication Date: 2016-03-30
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

Therefore, the preparation method is complicated and the energy consumption problem is still unresolved

Method used

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  • Method for synthesizing phosphotungstic acid-titanium dioxide composite spherical nanomaterials by one-step sol-gel method
  • Method for synthesizing phosphotungstic acid-titanium dioxide composite spherical nanomaterials by one-step sol-gel method
  • Method for synthesizing phosphotungstic acid-titanium dioxide composite spherical nanomaterials by one-step sol-gel method

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Experimental program
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Effect test

Embodiment 1

[0017] 1) 0.6g tetrabutyl titanate ([C 4 h 9 0] 4 Ti) drop into 50mL absolute ethanol, stir vigorously;

[0018] 2) Add 1 mL of absolute ethanol solution containing 0.135 g of phosphotungstic acid drop by drop;

[0019] 3) Continue to stir and add 1ml of a mixed solution of water and ethanol (v / v=1:5) dropwise, and continue to stir and react at room temperature for 4h;

[0020] 4) Centrifuge to obtain a white precipitate, wash it twice with water and ethanol respectively, dry it in an oven at 70°C for 4 hours, and then dry it in a muffle furnace at 150°C for 3 hours to obtain a composite spherical nanomaterial of phosphotungstic acid-titanium dioxide. It has a spherical cluster structure, and the mass ratio of phosphotungstic acid and titanium dioxide is 1:10.

[0021] Prepare 20 mL of DBT n-octane solution with a sulfur content of 350 ppm, add it to a 100 mL three-necked round-bottom flask, add 20 mL of acetonitrile as an extraction agent, and weigh 70 mg of the prepared ...

Embodiment 2

[0023] 1) 0.6g tetrabutyl titanate ([C 4 h 9 0] 4 Ti) drop into 50mL absolute ethanol, stir vigorously;

[0024] 2) Add 1 mL of absolute ethanol solution containing 0.653 g of phosphotungstic acid drop by drop;

[0025] 3) Continue to stir and add 1ml of a mixed solution of water and ethanol (v / v=1:5) dropwise, and continue to stir and react at room temperature for 4h;

[0026] 4) Centrifuge to obtain a white precipitate, wash it twice with a small amount of water and ethanol, dry it in an oven at 70°C for 4 hours, and then dry it in a muffle furnace at 150°C for 3 hours to obtain phosphotungstic acid-titanium dioxide composite spherical nanomaterials. The material has a spherical cluster structure, and the mass ratio of phosphotungstic acid and titanium dioxide is 3:10.

[0027] Prepare 20 mL of DBT n-octane solution with a sulfur content of 350 ppm, add it to a 100 mL three-necked round-bottom flask, add 20 mL of acetonitrile as an extraction agent, and weigh 70 mg of th...

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Abstract

The invention discloses a method for synthesizing a phosphotungstic acid-titanium dioxide composite spherical nanometer material by a one-step sol-gel method and belongs to the technical field of preparation of functional nanometer materials. The method avoids complex experimental steps and high energy consumption of solvent-induced self-assembly and hydrothermal methods and greatly simplifies the experimental flow. The shape and size of the prepared phosphotungstic acid-titanium dioxide composite spherical nanometer material are controllable. The material with the spherical-like nanometer structure has high sulphur removal efficiency and is applied to a sulphur removal reaction by extraction combined with catalytic oxidation. DBT simulated oil with sulphur content being 350ppm can be degraded to reach the sulphur content of 4.8ppm by 70mg of catalyst within 2h. The novel preparation method of the nanometer catalyst is simple, has the characteristics of good thermal stability, less energy consumption of equipment and environmental friendliness, and is expected to be actually developed in and applied to the sulphur removal industry production.

Description

technical field [0001] The invention belongs to the technical field of preparation of functional nanometer materials, and specifically relates to a method for synthesizing a phosphotungstic acid-titanium dioxide composite spherical nanometer material with high-efficiency sulfur removal performance by using a one-step sol-gel method. Background technique [0002] In recent years, polyoxometalates (referred to as polyacids) have attracted widespread attention as a "green" industrial catalyst. Polyacids have stimulated scientific research in many fields due to their adjustable chemical properties and high oxidation selectivity. Research, for example, catalysis, materials, structural chemistry and medicine. Polyacids have been intensively studied as catalysts in the catalytic oxidation of sulfur removal. Polyacid catalysts have shown high catalytic activity in the oxidation of benzothiophenes (BTs) and dibenzothiophenes (DBTs), but the difficulty of separation and reuse of thes...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38B01J35/08C10G27/00B82Y30/00B82Y40/00
Inventor 周云山雷寰张立娟秦立波
Owner BEIJING UNIV OF CHEM TECH
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