Graded-hole gold-copper alloy monolithic catalyst and preparation method thereof

A monolithic catalyst, gold-copper alloy technology, applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, carbon-based compound preparation, etc., can solve the problem of poor catalyst dispersion and lack of effective carrier , poor mass and heat transfer capabilities, etc., to achieve the effect of easy recycling, good mass and heat transfer and electrical conductivity, and no loss of precious metals

Inactive Publication Date: 2013-01-02
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the existing reports, the preparation methods of graded pores or composite pores mostly use template method or repeated alloying / dealloying method. These methods are complicated in process and easy to pollute the catalyst.
In addition, the porous metal catalysts prepared in the existing reports lack effective supports during the catalytic reaction process, the dispersion of the catalysts is not good, the mass transfer and heat transfer capabilities are poor, the catalytic efficiency is reduced, and it is difficult to recycle.
[0005] The gold-copper alloy monolithic catalyst with nano-micron hierarchical pores prepared on the surface of alloy wire by alloying / de-alloying method, especially one-step dealloying method, has not been reported after searching

Method used

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  • Graded-hole gold-copper alloy monolithic catalyst and preparation method thereof
  • Graded-hole gold-copper alloy monolithic catalyst and preparation method thereof
  • Graded-hole gold-copper alloy monolithic catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The method for preparing the graded pore gold-copper alloy monolithic catalyst includes the following steps:

[0046] (1) At 0.5mol / L CuSO 4 And 0.2mol / L H 2 SO 4 In the mixed solution of, add -0.2V bias voltage for 400s to electrodeposit copper on the surface of the gold-copper alloy wire, the length of the gold-copper alloy is 5cm;

[0047] (2) Anneal the alloy wire processed in step (1) in a nitrogen atmosphere at 500°C for 6 hours;

[0048] (3) Place the alloy wire in 68wt.% concentrated nitric acid in a constant temperature water bath of 30°C for free corrosion for 9h;

[0049] (4) Collect the corroded alloy wire, wash it repeatedly with ultrapure water 10 times, use a wide pH test paper to test that the washed water is neutral, and then dry it in air at 25°C to obtain a graded pore gold-copper alloy monolithic catalyst.

[0050] The above preparation method produces a graded-porous gold-copper alloy monolithic catalyst, which consists of a gold-copper alloy core and a grade...

Embodiment 2

[0053] The method for preparing the graded pore gold-copper alloy monolithic catalyst includes the following steps:

[0054] (1) At 0.5mol / L CuSO 4 And 0.2mol / L H 2 SO 4 In the mixed solution of, add -0.2V bias voltage for 400s to electrodeposit copper on the surface of the gold-copper alloy wire, the size of the gold-copper alloy wire is 5cm;

[0055] (2) Anneal the alloy wire treated in step (1) in a nitrogen atmosphere at 500°C for 6 hours;

[0056] (3) Place the alloy wire in 68wt.% concentrated nitric acid in a constant temperature water bath at 30°C for free corrosion for 24h;

[0057] (4) Collect the corroded alloy wire, wash it repeatedly with ultrapure water 10 times, use a wide pH test paper to test that the washed water is neutral, and then dry it in air at 25°C to obtain a graded pore gold-copper alloy monolithic catalyst.

[0058] The above preparation method produces a graded-porous gold-copper alloy monolithic catalyst, which is composed of a gold-copper alloy core and a ...

Embodiment 3

[0061] The method for preparing the graded pore gold-copper alloy monolithic catalyst includes the following steps:

[0062] (1) At 0.5mol / L CuSO 4 And 0.2mol / L H 2 SO 4 In the mixed solution of, add -0.2V bias voltage for 400s to electrodeposit copper on the surface of the gold-copper alloy wire, the size of the gold-copper alloy wire is 5cm;

[0063] (2) Anneal the alloy wire treated in step (1) in a nitrogen atmosphere at 500°C for 6 hours;

[0064] (3) Put the alloy wire in 0.5mol / L sulfuric acid in a water bath with a constant temperature of 30℃, and use a gold-copper alloy as the working electrode, platinum as the counter electrode and calomel electrode as the reference under the condition of a constant temperature of 30℃. Electrode, add bias voltage 0.1~2V for corrosion treatment, corrosion for 0.1h;

[0065] (4) Collect the corroded alloy wire, repeatedly wash it with ultrapure water 15 times, use a wide pH test paper to test that the rinsed water is neutral, and then dry it i...

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Abstract

The invention relates to a graded-hole gold-copper alloy monolithic catalyst and a preparation method thereof, belonging to the technical field of chemical catalysts. The graded-hole gold-copper alloy monolithic catalyst consists of a gold-copper alloy core and a graded-hole gold-copper alloy membrane covering the surface of the gold-copper alloy core; the thickness of the graded-hole gold-copperalloy membrane is 0.01-20 microns, the copper content of the graded-hole gold-copper alloy membrane is 10-90 at.%, and the gold content of the graded-hole gold-copper alloy membrane is 90-10 at.%; big holes with the pore diameter of 0.1-10 microns are fully distributed on the graded-hole gold-copper alloy membrane, and the space among the big holes is 0.1-10 microns; and small holes with the porediameter of 1-500 nm are fully distributed on the hole walls of the big holes, and the space among the small holes is 1-500 nm. In the preparation method of the graded-hole gold-copper alloy monolithic catalyst provided by the invention, the gold-copper alloy membrane which has uniform distribution, uniform pore size and a graded-hole structure that the small holes penetrate the hole walls of thebig holes is obtained through a one-step dealloying method; and the prepared graded-hole gold-copper alloy monolithic catalyst macroscopically and independently exists, has good mass-and-heat transfer and conductivity, and is easy to be recycled and reused.

Description

Technical field [0001] The invention relates to a graded pore gold-copper alloy monolithic catalyst and a preparation method thereof, in particular to a graded pore with adjustable structure and composition that can be used in the selective oxidation of alcohols, CO oxidation, and electrocatalytic oxidation of methanol and formic acid. A gold-copper alloy monolithic catalyst and a preparation method thereof belong to the technical field of chemical catalysts. Background technique [0002] Dealloying is a common corrosion process, that is, under certain conditions, components with high electrochemical activity are selectively dissolved. At present, most of the objects that use this method to prepare porous materials are binary alloy solid solutions. In the process of relatively active metal dissolution, a nanoporous sponge structure with relatively inert metals in the alloy as the main skeleton is gradually formed. [0003] In recent years, researchers have begun to use dealloying ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J35/10B01J37/34C07C47/54C07C45/38
CPCY02P20/584
Inventor 许效红邢新峰
Owner SHANDONG UNIV
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