CN112169809B - Preparation method of flexible nano Pd/CuO particle@foam Cu catalyst - Google Patents
Preparation method of flexible nano Pd/CuO particle@foam Cu catalyst Download PDFInfo
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- 239000003054 catalyst Substances 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 238000005520 cutting process Methods 0.000 claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 17
- 230000008018 melting Effects 0.000 claims abstract description 17
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910002528 Cu-Pd Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012300 argon atmosphere Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 abstract description 9
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 22
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 4
- 238000007747 plating Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 229910002668 Pd-Cu Inorganic materials 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 239000006260 foam Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 238000010314 arc-melting process Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8926—Copper and noble metals
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- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
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Abstract
The invention discloses a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which comprises the following steps: placing Al wires, cu wires and Pd wires in an acetone solution, ultrasonically cleaning with alcohol, drying, placing the Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting into slices by a cutting machine; and finally, soaking the thin sheet in KOH solution with a certain pH value, washing with deionized water, and drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst. The flexible nano Pd/CuO particle@foam Cu catalyst prepared by the method has good conductivity, high flexibility and large specific surface area, can be installed in reactors of different shapes after being cut, and has large active reaction site area, rapid reaction kinetics and high catalytic activity and stability.
Description
Technical Field
The invention belongs to the technical field of catalyst preparation, and particularly relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst.
Background
Pd catalyst shows good activity for coupling reaction, hydrogenation, oxidation, dehydrogenation, hydrogenation decomposition reaction and the like, and has very good application. In view of the rapid development of flexible power supply devices in recent years, the development of flexible Pd catalysts has attracted a great deal of attention.
The flexible Pd catalyst has the multiple effects of good toughness, foldability, easy cutting, easy recovery and the like on the basis of keeping good catalytic performance, and the main preparation methods comprise chemical plating, electroplating, dipping method, sol-gel method and the like, wherein noble metal Pd is loaded and electroplated on the surface of a flexible substrate, so that the flexible Pd catalyst is a macroscopic flexible material with catalytic activity. However, the plating thickness is difficult to be uniform and consistent in both chemical plating and electroplating, the process is complex, and the cost is high; the impregnation method and the gel sol method can accurately regulate and control the Pd loading capacity, but have poor dispersibility, are easy to agglomerate, and have weak binding force between the substrate and Pd, so that Pd particles are easy to fall off.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which solves the problem of weak bonding force between an active substance and a flexible substrate in the prior art.
The technical scheme adopted by the invention is that the preparation method of the flexible nano Pd/CuO particle@foam Cu catalyst is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
The present invention is also characterized in that,
in the step 1, the ultrasonic cleaning time is 30min.
In the step 2, the content of Al wires is 30-70 at%; the Cu wire content is 30-70 at%; pd filament content is 0.1-5at.%.
In step 2, the thickness of the sheet is 1mm-1cm.
In step 2, arc melting process parameters: the current is 90-120A, and the heating temperature is 850-1000 ℃.
In the step 3, the pH value of the KOH solution is 9-14; the soaking time is 0.5-4h.
The invention has the advantages that,
the flexible nano Pd/CuO particle@foam Cu catalyst prepared by the method has good conductivity, high flexibility and large specific surface area, can be installed in reactors of different shapes after being cut, has large active reaction site area, rapid reaction dynamics and high catalytic activity and stability, is simple in preparation process, can be accurately regulated and controlled in components, can be produced in a large amount, and effectively reduces the production cost under the condition of keeping high catalytic performance.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein the Al wire content is 30-70 at%; the Cu wire content is 30-70 at%; pd filament content is 0.1-5 at%; the thickness of the thin sheet is 1mm-1cm;
technological parameters of arc melting: the current is 90-120A, and the heating temperature is 850-1000 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 9-14; the soaking time is 0.5-4h.
The preparation method of the flexible nano Pd/CuO particle@foam Cu catalyst adopts an arc melting method to prepare an Al-Pd-Cu alloy ingot, cuts the Al-Pd-Cu alloy ingot into slices, places the slices into KOH solution with a certain pH value for a period of time at room temperature, and then uses deionized water for cleaning and drying to directly obtain the flexible nano Pd/CuO particle@foam Cu catalyst. The simple preparation method perfectly combines the active metal Pd, two cocatalysts (CuO and Cu) and the foam structure with light weight, large specific surface area and good toughness, thereby effectively improving the activity of Pd catalyst, reducing the cost and widening the application of Pd catalyst in the field of flexible devices.
Example 1
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein, the Al content is 28 at%; the Cu content was 70at.%; pd content is 2at.%; the thickness of the slice is 0.5cm; technological parameters of arc melting: the current is 90A, and the heating temperature is 850 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 10; the soaking time is 4 hours.
Example 2
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein, the Al content is 31 at%; the Cu content was 65at.%; pd content is 4at.%; the thickness of the slice is 1cm; technological parameters of arc melting: the current is 100A, and the heating temperature is 900 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 11; the soaking time is 4 hours.
Example 3
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein, the Al content is 35 at%; cu content is 60at.%; pd content 5at.%; the thickness of the slice is 1cm; technological parameters of arc melting: the current is 120A, and the heating temperature is 1000 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 13; the soaking time is 3 hours.
Example 4
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein, the Al content is 45 at%; cu content 50at.%; pd content 5at.%; the thickness of the slice is 0.5cm; technological parameters of arc melting: the current is 110A, and the heating temperature is 850 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 14; the soaking time is 1h.
Example 5
The invention relates to a preparation method of a flexible nano Pd/CuO particle@foam Cu catalyst, which is implemented according to the following steps:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
wherein, the Al content is 60 at%; the Cu content was 35at.%; pd content 5at.%; the thickness of the thin sheet is 0.5mm; technological parameters of arc melting: the current is 100A, and the heating temperature is 950 ℃;
and 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle@foam Cu catalyst.
Wherein the pH value of the KOH solution is 9; the soaking time is 4 hours.
The flexible nano Pd/CuO particle @ foam Cu catalyst prepared in the examples 1-5 is placed in alkali liquor to perform electrocatalytic oxidation of methanol, and the catalytic activity data are shown in the table 1, so that the catalyst prepared by the method has higher activity in the process of catalytically oxidizing methanol.
TABLE 1 catalytic Activity data for electrocatalytically oxidizing methanol in alkaline solution for samples
The flexible nano Pd/CuO particle@foam Cu catalyst adopts a one-step dealloying technology to simultaneously grow active nano Pd particles and nano CuO particles serving as cocatalysts on a foam Cu carrier which has good conductivity, high flexibility and large specific surface area and can play a role in promoting catalysis. The preparation method has low cost, simple process, accurate regulation and control of components and mass production. The prepared flexible catalyst material has uniform components, strong binding force between Pd and CuO and a matrix, no easy falling phenomenon, good toughness, large active reaction site area, quick dynamic reaction, high catalytic activity and stability, and can be installed in reactors of different shapes after cutting.
Claims (1)
1. The preparation method of the flexible nano Pd/CuO particle@foam Cu catalyst is characterized by comprising the following steps of:
step 1, placing Al wires, cu wires and Pd wires in an acetone solution together, ultrasonically cleaning to remove oil stains on the surface, ultrasonically cleaning with alcohol, and drying for later use; the ultrasonic cleaning time is 30min;
step 2, placing Al wires, cu wires and Pd wires in a crucible according to a certain proportion, repeatedly carrying out arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the ternary precursor alloy ingot into thin slices with a certain thickness by a cutting machine;
the Al filament content was 45at.%; the Cu wire content was 50at%; pd filament content 5at.%; the thickness of the slice is 0.5cm; technological parameters of arc melting: the current is 110A, and the heating temperature is 850 ℃;
step 3, soaking the sheet obtained in the step 2 in KOH solution with a certain pH value at room temperature, washing with deionized water, and naturally drying at room temperature to obtain a flexible nano Pd/CuO particle@foam Cu catalyst;
the pH of the KOH solution was 14; the soaking time is 1h.
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| US7259124B2 (en) * | 2005-02-07 | 2007-08-21 | Industrial Technology Research Institiute | Hydrogen storage composite and preparation thereof |
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| TW200704786A (en) * | 2006-08-04 | 2007-02-01 | Univ Nat Central | Casting production process of smelting vaporization with constant temperature |
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