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Preparation method of molybdenum carbide-loaded carbon-coated iron catalyst and application thereof in selective hydroxylation reaction of benzene ring

An iron catalyst, molybdenum carbide technology, applied in the preparation of organic compounds, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problems of high chemical stability of aromatic rings, reduce reaction selectivity, etc., to improve yield and selectivity, promoting circulation, mild reaction conditions

Active Publication Date: 2021-09-17
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high chemical stability of the aromatic ring, the carbon-hydrogen bond on the ring is difficult to be activated, and the side chain group is more active, resulting in the side chain group being more easily oxidized during the hydroxylation process, thereby reducing the reaction rate. selectivity

Method used

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  • Preparation method of molybdenum carbide-loaded carbon-coated iron catalyst and application thereof in selective hydroxylation reaction of benzene ring
  • Preparation method of molybdenum carbide-loaded carbon-coated iron catalyst and application thereof in selective hydroxylation reaction of benzene ring
  • Preparation method of molybdenum carbide-loaded carbon-coated iron catalyst and application thereof in selective hydroxylation reaction of benzene ring

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Add 1 g MoCl 5 Dissolve in 10 mL of ethanol to form a green transparent solution, then add 2 g of urea and stir for 1 h. Then 1 g of glucose was added, the solvent was evaporated to dryness, and the sample was annealed in a tube furnace at 800 °C for 3 h under an argon atmosphere to obtain Mo 2 C@C.

[0028] (2) Add 0.6 g FeCl 3 ·6H 2 O and 1.2 g of dicyandiamide were dispersed in deionized water, stirred in a water bath at 80°C for 2 h to fully coordinate the two, and then 1 g of Mo was added. 2 C@C, continue heating and stirring for 2 h until the liquid evaporates to dryness. The obtained solid was ground, and programmed annealing in a tube furnace under an argon atmosphere. The annealing temperature of the first stage was 550 °C for 2 h, and the annealing temperature of the second stage was 700 °C for 2 h to obtain Fe@ C / Mo 2 C@C crude product. The sample was washed with 6 mol / L HCl solution for 24 h, centrifuged and dried in vacuum to obtain Fe@C / Mo 2 C@...

Embodiment 2

[0033] 0.6 g FeCl 3 ·6H 2 O and 1.2 g of dicyandiamide were dispersed in deionized water, stirred in a water bath at 80°C for 2 h to fully coordinate the two, and then 1 g of commercially available Mo was added. 2 C, continue heating and stirring for 2 h until the liquid evaporates to dryness. The obtained solid was ground, and programmed annealing in a tube furnace under an argon atmosphere. The annealing temperature of the first stage was 550 °C for 2 h, and the annealing temperature of the second stage was 700 °C for 2 h to obtain Fe@ C / Mo 2 C crude product. The sample was washed with 6 mol / L HCl solution for 24 h, centrifuged and dried in vacuum to obtain Fe@C / Mo 2 c.

Embodiment 3

[0035] (1) Prepare two solutions A and B, solution A is 1 g MoCl 5 Dissolve in 10 mL ethanol to form a green transparent solution, then add 2 g urea and stir for 1 h. Solution B is to dissolve 1.5 g of Pluronic F127 powder in 10 mL of ethanol. Solution B was added dropwise to solution A, and the solvent was removed after mixing and stirring for 4 h. The sample was annealed at 800 °C for 3 h in a tube furnace under an argon atmosphere to obtain porous Mo 2 C (Porous-Mo 2 C).

[0036] (2) Add 0.6 g FeCl 3 ·6H 2 O and 1.2 g of dicyandiamide were dispersed in deionized water, stirred in a water bath at 80 °C for 2 h to fully coordinate the two, and then 1 g of Porous-Mo 2 C, continue heating and stirring for 2 h until the liquid evaporates to dryness. The obtained solid was ground, and programmed annealing in a tube furnace under an argon atmosphere. The annealing temperature of the first stage was 550 °C for 2 h, and the annealing temperature of the second stage was 700 °C ...

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Abstract

The invention discloses a molybdenum carbide-loaded carbon-coated iron catalyst, a preparation method thereof and application of the molybdenum carbide-loaded carbon-coated iron catalyst in catalyzing hydroxylation of substituted benzene to prepare phenol, and the molybdenum carbide-loaded carbon-coated iron catalyst is prepared by mixing ferric chloride and dicyandiamide according to a certain proportion, then adding molybdenum carbide, and carrying out annealing treatment. Carbon-coated iron nano particles (Fe@C / Mo2C) are loaded on a molybdenum carbide substrate in-situ, so that carbon-hydrogen bonds of benzene rings can be activated by utilizing the characteristic that molybdenum carbide selectively adsorbs the benzene rings, the benzene rings are easier to oxidize than side chain groups, and the yield and selectivity of phenol or derivatives thereof in products are improved; and the electron-rich characteristic of molybdenum carbide can be utilized to promote the circulation of Fe (II) / Fe (III) in the Fenton reaction and improve the generation efficiency of hydroxyl radicals, so that the reaction efficiency is improved, and the method has a certain industrial application prospect.

Description

technical field [0001] The invention belongs to the technical field of heterogeneous catalysis and organic synthesis, and specifically relates to a molybdenum carbide-loaded carbon-coated iron catalyst and its preparation method and its application in catalyzing benzene or substituted benzene to prepare phenol and its derivatives. Background technique [0002] Phenol and its derivatives are an important class of basic organic chemical raw materials, widely used in the chemical industry. At present, the industrial production of phenolic compounds is still dominated by the cumene method, but it has problems such as low total yield, low atom utilization, high energy consumption, and serious pollution. Therefore, it is necessary to find a new synthetic method to replace the traditional industrial method. Using hydrogen peroxide as an oxidizing agent, one-step hydroxylation of benzene and substituted benzene to produce phenol and its derivatives has the characteristics of simple...

Claims

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Application Information

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IPC IPC(8): B01J27/22C07C37/58C07C39/07C07C39/06
CPCB01J27/22C07C37/58C07C39/07C07C39/06Y02P20/52
Inventor 张金水侯乙东余德熙阳灿卢尔君
Owner FUZHOU UNIVERSITY
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