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Ti2O nano tube supported V2O5 composite catalyst

A composite catalyst, nanotube technology, applied in physical/chemical process catalysts, organic chemistry, chemical instruments and methods, etc., can solve problems such as tedious water cleaning work

Inactive Publication Date: 2008-12-17
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

TiO reported in literature and patents 2 The maximum surface area of ​​nanotubes after calcination at 400°C is 300m 2 / g (Chemistry of Materials, volume 16 in 2004, pages 4352-4358), wherein TiO 2 The nanotubes were obtained by the hydrolysis of commercial titanium dioxide P25 under alkaline conditions, but the subsequent hydrochloric acid washing process of Cl - The introduction of the water cleaning has brought tedious work

Method used

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  • Ti2O nano tube supported V2O5 composite catalyst
  • Ti2O nano tube supported V2O5 composite catalyst
  • Ti2O nano tube supported V2O5 composite catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Take 0.9g commercial TiO of type P25 2 Add it to 32mL of 10mol / L NaOH solution, stir at room temperature for 30 minutes, transfer it to a polytetrafluoroethylene-lined autoclave with a filling degree of 80%, and keep it at 130°C for 24 hours. , 0.1mol / L dilute nitric acid, then washed once with 200mL, 0.05mol / L dilute nitric acid, and finally washed 3 times with deionized water, 500mL each time. Filter, dry the filter cake at 40°C for 24 hours, and roast at 400°C for 1 hour to obtain TiO 2 Nanotubes, whose surface area was measured to be 310m 2 / g, the pore diameter is 13.2nm, and the pore volume is 1.5mL / g. The TEM photos of the samples after firing are shown in the attached figure 1 As shown, the XRD pattern shows that the prepared TiO 2 The crystal phase is dominated by anatase with a small amount of TiO 2 -B structure (see attached figure 2 ).

Embodiment 2

[0022] 0.84g ammonium metavanadate and 1.68g oxalic acid are dissolved in 20mL water, obtain dark green solution, get the TiO prepared by 12.50g embodiment 1 2 Nanotubes were added into the solution, stirred into a paste, and dried at room temperature to obtain solid sample A. Dissolve 1.12g of titanium sulfate in 15mL of water, add the above solid sample A, stir to form a paste, dry at room temperature for 20 hours, and then roast at 400°C for 1 hour to obtain TiO 2 Nanotube loaded V 2 o 5 Composite catalyst. The vanadium content was determined to be 5.0% (in terms of vanadium pentoxide mass percentage), and the sulfur content was 4.8% (in terms of sulfate radical mass percentage). The prepared V 2 o 5 Composite catalyst tableting, sieve, get 20-40 order sample and pack in the U-shaped tube reactor of outer diameter 8mm, the ratio of the amount of substance is methanol 5%, O 2 15%, N 2 80% of the mixed gas was preheated to 120°C and passed into the reactor. The reactor...

Embodiment 3

[0031] 1.89g ammonium metavanadate and 3.78g oxalic acid were dissolved in 22mL water, and the TiO prepared in 13.21g embodiment 1 was taken 2 Nanotubes were added into the solution, stirred into a paste, and dried at room temperature for 40 hours to obtain solid sample A. Dissolve 1.26g of titanium sulfate in 15mL of water, add the above solid sample A, stir to form a paste, dry at room temperature for 30 hours, and then roast at 400°C for 1 hour to obtain TiO 2 Nanotube loaded V 2 o 5 The composite catalyst is determined to have a vanadium content of 10.1% (in terms of vanadium pentoxide mass percentage), and a sulfur content of 3.6% (in terms of sulfate radical mass percentage). The prepared V 2 o 5 The composite catalyst was pressed into tablets, sieved, and the 20-40 mesh sample was loaded into a U-shaped tube reactor with an outer diameter of 8mm, and the methanol oxidation reaction activity was measured at 140°C according to the method in Example 2: the conversion r...

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Abstract

The invention relates to a V2O5 catalyst loaded by a TiO2 nanotube with the vanadium content of 5 to 30 percent according to the mass of vanadic oxide and sulphur content of 0.6 to 6.0 percent according to the mass of sulfate radical. A carrier used, the TiO2 nanotube, is obtained by taking commercial titanium oxide P25 as a precursor to form pasty mass in acidic and hydrothermal condition and by carrying out acid cleaning, water cleaning, drying and roasting; the size and the surface of the TiO2 nanotube prepared are controllable. The catalyst of the invention is used for the production of methylal by the selective oxidation of methyl alcohol; the conversion ratio of methyl alcohol can reach 20 to 80 percent and the selectivity of methylal can reach 50 to 98 percent.

Description

1. Technical field [0001] The present invention relates to a kind of TiO 2 Nanotube loaded V 2 o 5 A composite catalyst and a preparation method thereof, the catalyst is used for synthesizing methylal by the reaction of methanol and oxygen. 2. Background technology [0002] TiO 2 It is an excellent semiconductor material, which has been widely valued by academia and industry because it can be used in catalyst carriers, photocatalysis, sensors, energy storage and other fields. With the emergence of one-dimensional carbon nanomaterials in the 1990s, material chemists also began to pay attention to TiO 2 Synthesis and properties of one-dimensional nanomaterials, such as TiO 2 Nanotubes, nanowires, nanorods and nanobelts have been discovered one after another, which has promoted the development of TiO 2 applications in more fields. TiO 2 The preparation of nanotubes mainly includes anodic oxidation electrochemical method, template method and hydrothermal synthesis under ...

Claims

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Application Information

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IPC IPC(8): B01J27/053B01J21/06C07C43/303C07C41/50
Inventor 沈俭一刘经伟傅玉川
Owner NANJING UNIV
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