Vanadium-potassium doped titanium nanotube catalyst, preparation method and application thereof

A titanium nanotube and potassium doping technology is applied in the field of preparation of vanadium potassium doped titanium nanotube catalysts, which can solve the problems of small carrier specific surface area, reducing the number of active vanadium species in a single layer on the catalyst surface, and limiting catalyst reaction activity. , to achieve high reactivity and selectivity, good industrial application prospects, and good stability.

Pending Publication Date: 2019-01-15
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disclosed KVTi catalysts mainly use amorphous TiO 2 Particles are carriers with a small specific surface area
However, the smaller specific surface area of ​​the carrier will reduce the number of active vanadium species on the surface of the catalyst, thereby limiting the reactivity of the catalyst.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 0.1 mol of tetrabutyl titanate, 1.5 mol of absolute ethanol and 0.15 mol of glacial acetic acid were prepared as mixed solution A. will be 1.9×10 -3 mol potassium nitrate and 0.19mol absolute ethanol are configured as mixed solution B. The solution A was slowly added dropwise to the solution B, stirred at room temperature for 2 hours, aged for 9 hours to obtain a transparent gel, dried at 150°C for 5 hours, and calcined at 600°C for 6 hours to obtain potassium-doped titanium nanotubes. will be 9.8×10 -3 mol of ammonium metavanadate and 0.123mol of absolute ethanol were prepared as mixed solution C, and the obtained potassium-doped titanium nanotubes were added to solution C, stirred and dried at 100°C, and calcined at 600°C for 6 hours to obtain vanadium-potassium doped titanium nanotube catalysts. The catalyst composition is K 2 The mass fraction of O is 1%, V 2 o 5 The mass fraction is 10%, and the rest is TiO 2 . The specific surface area of ​​the catalyst is...

Embodiment 2

[0026]0.1 mol of tetrabutyl titanate, 0.8 mol of absolute ethanol and 0.05 mol of glacial acetic acid were prepared as mixed solution A. Mix 0.001mol potassium citrate and 0.2mol absolute ethanol to form mixed solution B. The solution A was slowly added dropwise to the solution B, stirred at room temperature for 1 h, aged for 6 h to obtain a transparent gel, dried at 120° C. for 3 h, and calcined at 500° C. for 4 h to obtain potassium-doped titanium nanotubes. will be 7.2×10 -3 mol of vanadyl acetate and 0.18 mol of absolute ethanol were configured to form a mixed solution C, and the obtained potassium-doped titanium nanotubes were added to solution C, stirred and dried at 80°C, and calcined at 500°C for 6 hours to obtain vanadium-potassium-doped titanium nanotubes. Titanium nanotube catalyst. The catalyst composition is K 2 The mass fraction of O is 0.5%, V 2 o 5 The mass fraction is 7.5%, and the rest is TiO 2 . The specific surface area of ​​the catalyst is 570m 2 / ...

Embodiment 3

[0029] Pack 1 mL of the catalyst prepared in Example 2 into a fixed-bed reactor, calcinate for 2 hours at 300°C under a nitrogen atmosphere, then raise the temperature to a reaction temperature of 440°C, and switch to a reaction gas whose composition is the volume fraction of toluene vapor is 2%, the volume fraction of oxygen is 10%, the rest is nitrogen, and the space velocity of the reaction gas is 1×10 3 h -1 . Reactants and products were detected by gas chromatography. After reacting for 5 hours, the conversion rate of toluene was 40.6%, the selectivity of benzaldehyde was 53.1%, the yield of benzaldehyde was 21.6%, and the selectivity of carbon oxide was 10.9%.

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Abstract

The invention discloses a vanadium-potassium doped titanium nanotube catalyst for catalyzing gas phase oxidation of toluene to benzaldehyde. The catalyst comprises: 0-1% mass fraction of K2O, 1%-10% mass fraction of V2O5, and the balance TiO2. The catalyst has a specific surface area of 450-650m<2> / g, a pore volume of 0.5-0.8cm<3> / g and a pore size of 3-5nm. The preparation method of the catalystincludes: firstly preparing potassium doped titanium nanotubes by sol-gel process, and then loading vanadium to the potassium doped titanium nanotubes by impregnation process. The vanadium-potassium doped titanium nanotube catalyst provided by the invention has high reaction activity and selectivity, and good stability. After 5h of reaction, the selectivity of benzaldehyde can reach 79%, the yieldof benzaldehyde is up to 26%, and the selectivity of carbon oxide is less than 11%. Therefore, the vanadium-potassium doped titanium nanotube catalyst has good industrial application prospects.

Description

technical field [0001] The invention belongs to the technical field of preparation of titanium nanometer materials, and in particular relates to a titanium nanotube catalyst doped with vanadium and potassium, a preparation method and an application thereof. Background technique [0002] Benzaldehyde is an important fine chemical, which can be used in the fields of cosmetics, food, medicine, dyes and pesticides. Domestic benzaldehyde is mainly produced by chlorination and hydrolysis of toluene. Although this process can obtain a higher benzaldehyde yield, it consumes a large amount of chlorine gas, strong acid and strong alkali, which brings serious equipment corrosion and environmental pollution; and the synthesized benzaldehyde product contains trace chlorine, which cannot be applied in Cosmetics, food and medicine and other fields. At present, the commercial production process of chlorine-free benzaldehyde with market competitiveness in the world mainly uses liquid-phase...

Claims

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Application Information

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IPC IPC(8): B01J23/22C07C45/36C07C47/54
CPCC07C45/36B01J23/002B01J23/22B01J2523/00B01J35/617B01J35/615B01J35/635B01J35/647B01J2523/13B01J2523/47B01J2523/55C07C47/54
Inventor 李泽壮刘经伟杨爱武张诚柏基业方晓江刘丽娟王英武
Owner SINOPEC YANGZI PETROCHEM
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