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Vanadium-based monoatomic catalyst for directly oxidizing benzene to prepare phenol, and preparation method thereof

A catalyst, a direct technology, applied in the direction of catalyst activation/preparation, preparation of organic compounds, physical/chemical process catalysts, etc., can solve problems such as design and synthesis research that have not been reported yet

Active Publication Date: 2019-08-16
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To date, metal-organic framework-based NH 2 -The design, synthesis, and application of MIL-101(V)-derived single-atom V-based catalysts to the hydroxylation of benzene have not been reported yet

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Prepare a mixture of vanadium chloride, 2-aminoterephthalic acid, and DMF at a molar ratio of 1:1:1000: weigh 0.208g of VCl 3 and 0.24g of 2-aminoterephthalic acid were added into 100mL of DMF, and a mixed solution was obtained after ultrasonication for 10min. Seal the mixed solution in a 100mL polytetrafluoroethylene-lined reaction kettle, put it in an oven at 180°C for a constant temperature reaction for 36 hours, and cool it down to room temperature, then wash it with DMF and methanol, and dry it in vacuum at 120°C Overnight, get NH 2 -MIL-101(V) solid powder, the obtained NH 2 -MIL-101(V) solid powder in N 2 Under the atmosphere, heat treatment at 900 °C for 5 h at a heating rate of 5 °C / min, cool to room temperature, and add the obtained black powder to 1M H 2 SO 4 Submerge the material completely in the solution, stir at a constant temperature of 80°C for 48 hours, wash until neutral, and dry the precipitate in a vacuum oven. The obtained black powder is the ...

Embodiment 2

[0019] Prepare a mixture of vanadium chloride, 2-aminoterephthalic acid, and DMF at a molar ratio of 1:1:200: weigh 0.208g of VCl 3 and 0.24g of 2-aminoterephthalic acid were added into 20mL of DMF, and after ultrasonication for 10min, a mixed solution was obtained. Seal the mixed solution in a 100mL polytetrafluoroethylene-lined reaction kettle, put it into an oven at 90°C for a constant temperature reaction for 16h, and cool it to room temperature, then wash it with DMF and methanol, and dry it in vacuum at 90°C. overnight. get NH 2 -MIL-101(V) solid powder, the obtained NH 2 -MIL-101(V) solid powder in N 2 Under atmosphere, heat treatment at 500°C for 5h at a heating rate of 5°C / min, cool to room temperature, add the obtained black powder to 1MH 2 SO 4 Submerge the material completely in the solution, stir at a constant temperature of 20°C for 12 hours, wash until neutral, and dry the precipitate in a vacuum oven. The obtained black powder is the V SAs / N-C catalyst, w...

Embodiment 3

[0022] Prepare a mixture of vanadium chloride, 2-aminoterephthalic acid, and DMF at a molar ratio of 1:1:600: weigh 0.208g of VCl 3 and 0.24g of 2-aminoterephthalic acid were added into 60mL of DMF, and after ultrasonication for 10min, a mixed solution was obtained. Seal the mixed solution in a 100mL polytetrafluoroethylene-lined reaction kettle, put it into an oven at 135°C for a constant temperature reaction for 26h to obtain a solid substance, after cooling to room temperature, wash with DMF and methanol in turn, and vacuum-dry at 120°C Get NH overnight 2 - MIL-101(V) solid powder. Will get NH 2 -MIL-101(V) solid powder in N 2 Under atmosphere, heat treatment at 700°C for 5h at a heating rate of 5°C / min. After cooling to room temperature, the resulting black powder was added to 0.5M H 2 SO 4 Submerge the material completely in the solution, stir at a constant temperature of 50°C for 30 hours, wash until neutral, and dry the precipitate in a vacuum oven. The obtained ...

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PUM

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Abstract

The invention discloses a vanadium-based monoatomic catalyst for directly oxidizing benzene to prepare phenol, and a preparation method thereof. The catalyst comprises a monoatomic vanadium species derived from a metal-organic framework material NH2-MIL-101 (V), and N-doped amorphous carbon, and the monoatomic vanadium species accounts for 0.1-3% of the weight of the catalyst. The preparation method comprises the following steps: preparing the NH2-MIL-101 (V) from vanadium chloride, 2-aminoterephthalic acid and N,N-dimethylformamide, carrying out high temperature treatment in a N2 atmosphere,and carrying out treatment by using a dilute acid to obtain the vanadium-based monoatomic catalyst V SAs / N-C. The catalyst has an excellent catalytic activity and an excellent reusability when used for directly oxidizing benzene to prepare phenol.

Description

technical field [0001] The invention relates to a heterogeneous catalyst and a preparation method thereof, in particular to a vanadium-based single-atom catalyst used for the direct oxidation of benzene to phenol and a preparation method thereof. Background technique [0002] Phenol is an important organic chemical raw material, widely used in dyes, polymers, plastics, medicine, pesticides and other fields. At present, the industrial production method of phenol is mainly the cumene method, but the process flow is complicated, the reaction steps are many, and its development is restricted by the parallel product acetone. In recent years, due to the popularization of the concept of green chemistry, based on the sustainable development strategy, people have gradually shifted their attention to the direct catalytic hydroxylation of benzene to prepare phenol from the aspects of improving atom economy, energy conservation and environmental protection. The direct catalyzed hydroxy...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/08B01J37/34B01J37/06C07C37/60C07C39/04
CPCB01J27/24B01J37/082B01J37/343B01J37/06C07C37/60C07C39/04Y02P20/52
Inventor 张富民徐琼皓方莉涂高美朱伟东
Owner ZHEJIANG NORMAL UNIVERSITY
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