CN112169809A - 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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- CN112169809A CN112169809A CN202011206991.0A CN202011206991A CN112169809A CN 112169809 A CN112169809 A CN 112169809A CN 202011206991 A CN202011206991 A CN 202011206991A CN 112169809 A CN112169809 A CN 112169809A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000005520 cutting process Methods 0.000 claims abstract description 19
- 238000000034 method 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
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 18
- 239000000956 alloy Substances 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000002844 melting Methods 0.000 claims abstract description 18
- 230000008018 melting Effects 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 17
- 238000010891 electric arc Methods 0.000 claims abstract description 15
- 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
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 24
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000003197 catalytic effect Effects 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000004140 cleaning Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 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
- 239000000126 substance Substances 0.000 description 2
- 229910002668 Pd-Cu Inorganic materials 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 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
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000011068 loading method Methods 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
- 238000011084 recovery Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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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
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or 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 the Al wire, the Cu wire and the Pd wire in an acetone solution, ultrasonically cleaning by using alcohol, drying, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting into slices by using a cutting machine; and finally, soaking the sheet in a 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 the advantages of good conductivity, high flexibility, large specific surface area, large active reaction site area, rapid reaction kinetics, high catalytic activity and stability, and can be installed in reactors of different shapes after being cut.
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
The 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 much attention.
The flexible Pd catalyst needs to have multiple effects of good toughness, folding, 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 substrate presents a macroscopic flexible material with catalytic activity. But the plating layer thickness is difficult to be uniform no matter the chemical plating or the electroplating, the process is more complex and the cost is high; the impregnation method and the gel sol method can accurately regulate and control the loading capacity of Pd, but the Pd particles are easy to fall off due to poor dispersibility and low bonding force between the base material and the Pd, and the Pd particles are easy to agglomerate.
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 that the binding force between an active substance and a flexible substrate is weak 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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 step 1, the ultrasonic cleaning time is 30 min.
In the step 2, the content of Al filaments is 30-70 at.%; cu wire content 30-70 at.%; the Pd filament content is 0.1-5 at.%.
In step 2, the thickness of the slice is 1mm-1 cm.
In step 2, the process parameters of arc melting are as follows: 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 0.5-4 h.
The beneficial effect of the invention is that,
the flexible nano Pd/CuO particle @ foam Cu catalyst prepared by the method has the advantages of good conductivity, high flexibility, large specific surface area, large active reaction site area, rapid reaction kinetics, high catalytic activity and stability, simple preparation process, accurate regulation and control of components, mass production and effective reduction of production cost under the condition of keeping high catalytic performance, and can be installed in reactors of different shapes after being cut.
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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein, the content of Al filaments is 30-70 at.%; cu wire content 30-70 at.%; pd filament content is 0.1-5 at.%; the thickness of the slice is 1mm-1 cm;
the process parameters of the electric arc melting are as follows: the current is 90-120A, and the heating temperature is 850-1000 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 0.5-4 h.
The invention relates to a preparation method of a flexible nano Pd/CuO particle @ foam Cu catalyst, which is characterized in that an Al-Pd-Cu alloy ingot is prepared by adopting an arc melting method, is cut into slices, is placed in a KOH solution with a certain pH value for a period of time at room temperature, and is washed and dried by deionized water, so that the flexible nano Pd/CuO particle @ foam Cu catalyst is directly obtained. The simple preparation method perfectly combines the active metal Pd, two promoters (CuO and Cu) and a foam structure with light weight, large specific surface area and good toughness, effectively improves the activity of the Pd catalyst, reduces the cost and widens the application of the 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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein, the Al content is 28 at.%; cu content 70 at.%; pd content 2 at.%; the thickness of the thin slice is 0.5 cm; the process parameters of the electric arc melting are as follows: the current is 90A, and the heating temperature is 850 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 h.
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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein, the Al content is 31 at.%; cu content 65 at.%; pd content 4 at.%; the thickness of the slice is 1 cm; the process parameters of the electric arc melting are as follows: the current is 100A, and the heating temperature is 900 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 h.
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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein, the Al content is 35 at.%; cu content 60 at.%; pd content 5 at.%; the thickness of the slice is 1 cm; the process parameters of the electric arc melting are as follows: the current is 120A, and the heating temperature is 1000 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 h.
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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein the Al content is 45 at.%; cu content 50 at.%; pd content 5 at.%; the thickness of the thin slice is 0.5 cm; the process parameters of the electric arc melting are as follows: the current is 110A, and the heating temperature is 850 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 1 h.
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 an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
wherein the ultrasonic cleaning time is 30 min;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
wherein, the Al content is 60 at.%; cu content 35 at.%; pd content 5 at.%; the thickness of the thin slice is 0.5 mm; the process parameters of the electric arc melting are as follows: the current is 100A, and the heating temperature is 950 ℃;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally 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 h.
The flexible nano Pd/CuO particles @ foam Cu catalyst prepared in the examples 1-5 is placed in an alkali solution to be subjected to electrocatalytic oxidation of methanol, and the catalytic activity data of the catalyst is shown in Table 1.
TABLE 1 data of the catalytic activity of the electrocatalytic oxidation of methanol in alkaline solution of the samples
The flexible nano Pd/CuO particle @ foam Cu catalyst adopts a one-step dealloying technology to simultaneously grow the active nano Pd particles and the nano CuO particles serving as the cocatalyst on the foam Cu carrier which has good conductivity, high flexibility and large specific surface area and can play a role of cocatalyst in situ. The preparation method has the advantages of low cost, simple process, accurate regulation of components and large-scale production. The prepared flexible catalyst material has uniform components, strong binding force between Pd and CuO and a substrate, no easy shedding phenomenon, large active reaction site area, fast dynamic reaction, high catalytic activity and stability due to good toughness, and can be installed in reactors with different shapes after being cut.
Claims (6)
1. The preparation method of the flexible nano Pd/CuO particle @ foam Cu catalyst is characterized by comprising the following steps:
step 1, placing an Al wire, a Cu wire and a Pd wire in an acetone solution together, carrying out ultrasonic cleaning, removing oil stains on the surface, then carrying out ultrasonic cleaning by using alcohol, and drying for later use;
step 2, placing the Al wire, the Cu wire and the Pd wire in a crucible according to a certain proportion, repeatedly carrying out electric arc melting under the protection of argon atmosphere to form an Al-Cu-Pd ternary precursor alloy ingot, and then cutting the precursor alloy ingot into slices with a certain thickness by using a cutting machine;
and 3, soaking the slice obtained in the step 2 in a KOH solution with a certain pH value at room temperature, finally washing with deionized water, and naturally drying at room temperature to obtain the flexible nano Pd/CuO particle @ foam Cu catalyst.
2. The preparation method of the flexible nano Pd/CuO particles @ foam Cu catalyst as claimed in claim 1, wherein the ultrasonic cleaning time in step 1 is 30 min.
3. The method for preparing flexible nano Pd/CuO particles @ foamy Cu catalyst as claimed in claim 1, wherein in said step 2, the Al filament content is 30-70 at.%; cu wire content 30-70 at.%; the Pd filament content is 0.1-5 at.%.
4. The method for preparing flexible nano Pd/CuO particles @ foam Cu catalyst as claimed in claim 1, wherein in the step 2, the thickness of the sheet is 1mm-1 cm.
5. The method for preparing the flexible nano Pd/CuO particles @ foam Cu catalyst as claimed in claim 1, wherein in the step 2, the process parameters of arc melting are as follows: the current is 90-120A, and the heating temperature is 850-1000 ℃.
6. The method for preparing flexible nano Pd/CuO particles @ foam Cu catalyst as claimed in claim 1, wherein in the step 3, the pH value of KOH solution is 9-14; the soaking time is 0.5-4 h.
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| CN103406128A (en) * | 2013-08-13 | 2013-11-27 | 山东大学 | Preparation method of nano-particles with nano-grade porous structure |
| CN104475125A (en) * | 2014-11-06 | 2015-04-01 | 天津大学 | Method for preparing Pd/CuO composite nanometer porous material by using amorphous alloy for dealloying |
| CN104624200A (en) * | 2014-12-30 | 2015-05-20 | 西安交通大学 | Preparation method of nano porous copper oxide loaded precious metal catalytic material |
| CN108091886A (en) * | 2016-11-23 | 2018-05-29 | 天津大学 | A kind of nano-porous structure composite material and preparation method thereof and alcohols catalytic performance application |
| CN107507986A (en) * | 2017-08-31 | 2017-12-22 | 天津大学 | A kind of PdSn CuO composites of nano-porous structure prepare and application |
| CN110241438A (en) * | 2018-03-08 | 2019-09-17 | 天津大学 | Foam copper supports palladium-copper alloy nanocages catalyst and preparation method thereof |
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