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A kind of preparation method of the au catalyst that is used to prepare ka oil

A technology for catalysts and preparation steps, applied in the field of preparation of self-supporting two-dimensional nano-Au catalysts, to achieve the effect of saving production costs

Active Publication Date: 2017-03-15
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, with the continuous research on Au catalysts, the conversion rate of the reaction is below 20%.

Method used

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  • A kind of preparation method of the au catalyst that is used to prepare ka oil
  • A kind of preparation method of the au catalyst that is used to prepare ka oil
  • A kind of preparation method of the au catalyst that is used to prepare ka oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) SrTiO 3 (111) The single crystal is placed in a quartz burning boat, and the burning boat and SrTiO 3 Put the single wafer into the annealing furnace, heat the furnace temperature to 800°C at a speed of 10°C / min, keep it for 6h, and then cool it to room temperature with the furnace. 3 The surface is crystallized;

[0026] 2) The crystallized SrTiO 3 Clean the surface by ultrasonication for 10 minutes in 5% NaOH dilute solution and absolute alcohol respectively;

[0027] 3) The purified SrTiO 3 Put it into the chamber of the magnetron sputtering coating machine, pump the chamber to 6×10 - 4 Pa, the gas sputtering pressure is 0.6Pa, the reverse sputtering power is 30W, the reverse sputtering time is 30min, the sputtering power is 10W, the deposition temperature is 100°C, and the thickness of the Au film is controlled at 10nm by a film thickness meter. In its XRD pattern, It shows only the existence of Au (111) diffraction peak, and the Phi scan pattern shows the ...

Embodiment 2

[0029] 1) SrTiO 3 (111) The single crystal is placed in a quartz burning boat, and the burning boat and SrTiO 3 Put the single wafer into the annealing furnace, heat the furnace temperature to 850°C at a rate of 10°C / min, keep it for 8h, and then cool it to room temperature with the furnace. 3 The surface is crystallized;

[0030] 2) The crystallized SrTiO 3 Clean the surface by ultrasonication for 10 minutes in 2% NaOH dilute solution and alcohol respectively;

[0031] 3) The purified SrTiO 3 Put it into the chamber of the magnetron sputtering coating machine, pump the chamber to 8×10 - 4 Pa, gas sputtering pressure 0.6Pa, reverse sputtering power 30W, reverse sputtering time 50min, sputtering power 5W, deposition at 100°C, the thickness of the Au film was controlled at 10nm by a film thickness meter, XRD and Phi scanning patterns and implementation The spectrum of Example 1 is consistent, which indicates that the deposited Au film is a single crystal film with (111) or...

Embodiment 3

[0033] 1) SrTiO 3 (111) The single crystal is placed in a quartz burning boat, and the burning boat and SrTiO 3 Put the single wafer into the annealing furnace, heat the furnace temperature to 900°C at a speed of 15°C / min, keep it for 6h, and then cool it to room temperature with the furnace. 3 The surface is crystallized;

[0034] 2) The crystallized SrTiO 3 Clean the surface by ultrasonicating in 5% NaOH dilute solution and alcohol for 10 minutes respectively;

[0035] 3) The purified SrTiO 3 Put it into the chamber of the magnetron sputtering coating machine, pump the chamber to 6×10 - 4 Pa, gas sputtering pressure 1.2Pa, reverse sputtering power 50W, reverse sputtering time 30min, sputtering power 8W, deposition temperature 80°C, the thickness of the Au film was controlled at 10nm by a film thickness meter, and it was found that only Au(111) The existence of diffraction peaks, XRD and Phi scan patterns are consistent with the patterns of Example 1.

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Abstract

The invention relates to a preparation method of a self-supporting nano-Au catalyst used for preparing KA oil. According to the method, SrTiO3 (111) oriented monocrystalline is subjected to a surface crystallization treatment and a surface cleaning treatment; a monocrystalline Au film with a (111) orientation is deposited on the surface of the SrTiO3 substrate under a relatively low sputtering power of 5-10W and a deposition temperature of 80-100 DEG C; with an electrochemical hydrogen stripping method, the Au film is stripped from the substrate; and evaporation drying is carried out, such that the self-supporting two-dimensional nano-Au catalyst is obtained. With hydrogen peroxide as a catalyst, the catalyst shows catalytic activity in a cyclohexane liquid-phase oxidation reaction system, and cyclohexane liquid-phase oxidation reaction conversion rate is substantially improved. Under the conditions with a conventional distillation device, a standard atmospheric pressure and a temperature of 70 DEG C, a KA oil conversion rate can be higher than 40%.

Description

technical field [0001] The invention relates to a preparation method of a nano-Au catalyst, in particular to a preparation method of a self-supporting two-dimensional nano-Au catalyst with (111) orientation, which exhibits catalytic performance in the liquid-phase oxidation reaction of cyclohexane. Background technique [0002] Nano-Au supported on metal oxides has become a research hotspot in the field of catalysis due to its excellent catalytic activity in the CO oxidation reaction at room temperature or low temperature. This kind of nano-Au catalyst with high catalytic activity at lower temperature is widely used in the fields of automobile exhaust gas treatment, petrochemical industry, liquid phase oxidation, etc., replacing many applications of precious metals such as Pt and Pd. [0003] At present, the Au catalyst for the preparation of KA oil (a mixture of cyclohexanol and cyclohexanone) by the liquid-phase oxidation of cyclohexane is usually supported on Fe 2 o 3 、...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/52C07C27/16C07C49/403C07C35/08C07C45/28C07C29/48
Inventor 曹江利高时庄杨穆张欢黄亚丽向青云王捷
Owner UNIV OF SCI & TECH BEIJING