CN111068663A - Nano palladium catalyst and preparation method thereof - Google Patents
Nano palladium catalyst and preparation method thereof Download PDFInfo
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- CN111068663A CN111068663A CN201811221991.0A CN201811221991A CN111068663A CN 111068663 A CN111068663 A CN 111068663A CN 201811221991 A CN201811221991 A CN 201811221991A CN 111068663 A CN111068663 A CN 111068663A
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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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
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Abstract
The invention provides a nano palladium catalyst and a preparation method thereof, relating to the technical field of catalyst processing. The nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, and the loading capacity of nano palladium is 1.2-2.4% of the carrier. The preparation method mainly comprises the following steps: carrying out nitric acid treatment on a carrier, performing ultrasonic oscillation, treating by using a high-voltage pulse electric field, mixing and stirring, performing vacuum drying, performing helium protection and high-temperature reduction, and the like. The invention overcomes the defects of the prior art, improves the stability of the traditional nano palladium, and has the advantages of good catalytic reaction effect, good recovery effect, low production and use cost, high comprehensive utilization value and the like.
Description
Technical Field
The invention relates to the technical field of catalyst processing, in particular to a nano palladium catalyst and a preparation method thereof.
Background
With the development and consumption of natural resources such as petroleum, coal, natural gas and the like, the human society faces serious problems such as energy shortage, deterioration of living environment and the like. The automobile, as a symbol of civilization in human society, consumes a large amount of petroleum, brings convenience to human beings and also seriously pollutes the environment. Researchers have been looking for clean and sustainable energy sources to develop new energy vehicles for decades. The fuel cell is the most ideal power source of new energy automobiles, however, the research of the key material, namely the oxygen reduction reaction electrocatalyst, used by the anode of the fuel cell cannot meet the requirement of large-scale popularization. Particularly, the oxygen reduction reaction catalysts with good performance developed at present are molybdenum-based catalysts, namely Pt and alloys thereof, and the application and development of fuel cells are severely restricted because Pt belongs to precious and scarce metals, is expensive and has insufficient resources.
The nano palladium and the compound thereof have surface effect, quantum size effect, optical effect and other performances different from those of the bulk metal, so that the nano palladium and the compound thereof have wide potential application prospects in various aspects such as industrial catalysis, biomedicine, bioanalytical chemistry, sensors and the like. However, the preparation and application of the nano palladium particles are severely limited because the nano palladium particles are very unstable due to the extremely large specific surface area and are easy to agglomerate and inactivate.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the nano palladium catalyst and the preparation method thereof, which improve the stability of the traditional nano palladium and have the advantages of good catalytic reaction effect, good recovery effect, low production and use cost, high comprehensive utilization value and the like.
In order to achieve the above purpose, the technical scheme of the invention is realized by the following technical scheme:
the nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, and the loading capacity of nano palladium is 1.2-2.4% of the carrier.
Preferably, the carrier is one or more of silicon dioxide, aluminum oxide, magnesium oxide, titanium oxide, activated carbon, montmorillonite and kaolin.
The preparation method of the nano palladium catalyst comprises the following steps:
(1) adding nitric acid into the carrier for treating for a period of time, taking out and washing the carrier, adding deionized water, stirring at a high speed and mixing uniformly to obtain slurry for later use;
(2) adding soluble palladium salt into deionized water, and carrying out heat preservation, vibration and homogenization in an ultrasonic vibration instrument to obtain a homogeneous solution for later use;
(3) pretreating the homogeneous liquid by adopting a high-voltage pulse electric field, adding the slurry obtained in the step (1), and mixing and stirring uniformly to obtain a mixed liquid for later use;
(4) filtering the mixed solution, and then drying in vacuum to obtain a catalyst precursor for later use;
(5) and carrying out high-temperature reduction treatment on the catalyst precursor for 20-24h under the protection of helium to obtain the nano palladium catalyst.
Preferably, the time for treating the carrier in the nitric acid is 4-6h, and the rotating speed for adding the deionized water and stirring at a high speed is 600-800 r/min.
Preferably, the power of the mixing ultrasonic oscillation of the soluble palladium salt and the deionized water is 400-500W, the oscillation mode is that the mixture is kept stand for 20-30min every 10-15min of oscillation, the oscillation is repeated for 3-5 times, and the oscillation temperature is 30-40 ℃.
Preferably, the frequency of the pulse electric field of the mean solution in the high-voltage pulse electric field is 10Hz, the processing time is 400 mus, the electric field strength is 20kV/cm, the rotating speed of mixing and stirring with the slurry is 400-.
Preferably, the temperature of the vacuum drying after the filtration of the mixed solution is 60-80 ℃.
Preferably, the temperature of the high-temperature reduction treatment of the catalyst precursor is 200-250 ℃.
The invention provides a nano palladium catalyst and a preparation method thereof, and compared with the prior art, the nano palladium catalyst has the advantages that:
(1) the invention adopts a high-speed stirring mode aiming at the characteristics of the nano-palladium, so that nano-palladium particles can be effectively combined with a carrier, the loss of components during metal activity is prevented, and the stability of a product is enhanced.
(2) The invention adopts high-voltage pulse electric field treatment for the palladium salt solution, can effectively increase the acting force among palladium particles, enables the palladium particles to be more easily compounded with a carrier, enhances the magnetism of palladium metal and facilitates the later recovery of the catalyst.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, the loading amount of nano palladium is 1.2% of the carrier, and the carrier is one or more of silicon dioxide, aluminum oxide, magnesium oxide, titanium oxide, activated carbon, montmorillonite and kaolin.
The preparation method of the nano palladium catalyst comprises the following steps:
(1) adding nitric acid into the carrier for treating for a period of time, taking out and washing the carrier, adding deionized water, stirring at a high speed and mixing uniformly to obtain slurry for later use;
(2) adding soluble palladium salt into deionized water, and carrying out heat preservation, vibration and homogenization in an ultrasonic vibration instrument to obtain a homogeneous solution for later use;
(3) pretreating the homogeneous liquid by adopting a high-voltage pulse electric field, adding the slurry obtained in the step (1), and mixing and stirring uniformly to obtain a mixed liquid for later use;
(4) filtering the mixed solution, and then drying in vacuum to obtain a catalyst precursor for later use;
(5) and carrying out high-temperature reduction treatment on the catalyst precursor for 20-24h under the protection of helium to obtain the nano palladium catalyst.
Wherein the treatment time of the carrier in nitric acid is 4-6h, and the rotating speed of adding deionized water and stirring at high speed is 600 r/min; the power of the mixed ultrasonic oscillation of the soluble palladium salt and the deionized water is 400W, the oscillation mode is that the mixed ultrasonic oscillation is kept for 20min every 10min, the mixed ultrasonic oscillation is repeated for 3 times, and the oscillation temperature is 30 ℃; the frequency of a pulse electric field of the mean solution in a high-voltage pulse electric field is 10Hz, the processing time is 400 mus, the electric field strength is 20kV/cm, the rotating speed of mixing and stirring with the slurry is 400r/min, and the stirring time is 3 min; the temperature of vacuum drying after filtering the mixed solution is 60 ℃; the temperature of the catalyst precursor high-temperature reduction treatment is 200 ℃.
Example 2:
the nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, the loading amount of nano palladium is 2.4% of the carrier, and the carrier is one or more of silicon dioxide, aluminum oxide, magnesium oxide, titanium oxide, activated carbon, montmorillonite and kaolin.
The preparation method of the nano palladium catalyst comprises the following steps:
(1) adding nitric acid into the carrier for treating for a period of time, taking out and washing the carrier, adding deionized water, stirring at a high speed and mixing uniformly to obtain slurry for later use;
(2) adding soluble palladium salt into deionized water, and carrying out heat preservation, vibration and homogenization in an ultrasonic vibration instrument to obtain a homogeneous solution for later use;
(3) pretreating the homogeneous liquid by adopting a high-voltage pulse electric field, adding the slurry obtained in the step (1), and mixing and stirring uniformly to obtain a mixed liquid for later use;
(4) filtering the mixed solution, and then drying in vacuum to obtain a catalyst precursor for later use;
(5) and carrying out high-temperature reduction treatment on the catalyst precursor for 20-24h under the protection of helium to obtain the nano palladium catalyst.
Wherein the treatment time of the carrier in nitric acid is 4-6h, and the rotating speed of adding deionized water and stirring at high speed is 800 r/min; the power of the mixed ultrasonic oscillation of the soluble palladium salt and the deionized water is 500W, the oscillation mode is that the mixed ultrasonic oscillation is kept for 30min every 15min, the mixed ultrasonic oscillation is repeated for 5 times, and the oscillation temperature is 40 ℃; the frequency of a pulse electric field of the mean solution in a high-voltage pulse electric field is 10Hz, the processing time is 400 mus, the electric field strength is 20kV/cm, the rotating speed of mixing and stirring the mean solution with the slurry is 600r/min, and the stirring time is 5 min; the temperature of vacuum drying after filtering the mixed solution is 80 ℃; the temperature of the catalyst precursor high-temperature reduction treatment is 250 ℃.
Example 3:
the nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, the loading amount of nano palladium is 1.8% of the carrier, and the carrier is one or more of silicon dioxide, aluminum oxide, magnesium oxide, titanium oxide, activated carbon, montmorillonite and kaolin.
The preparation method of the nano palladium catalyst comprises the following steps:
(1) adding nitric acid into the carrier for treating for a period of time, taking out and washing the carrier, adding deionized water, stirring at a high speed and mixing uniformly to obtain slurry for later use;
(2) adding soluble palladium salt into deionized water, and carrying out heat preservation, vibration and homogenization in an ultrasonic vibration instrument to obtain a homogeneous solution for later use;
(3) pretreating the homogeneous liquid by adopting a high-voltage pulse electric field, adding the slurry obtained in the step (1), and mixing and stirring uniformly to obtain a mixed liquid for later use;
(4) filtering the mixed solution, and then drying in vacuum to obtain a catalyst precursor for later use;
(5) and carrying out high-temperature reduction treatment on the catalyst precursor for 20-24h under the protection of helium to obtain the nano palladium catalyst.
Wherein the treatment time of the carrier in nitric acid is 4-6h, and the rotating speed of adding deionized water and stirring at high speed is 700 r/min; the power of the mixed ultrasonic oscillation of the soluble palladium salt and the deionized water is 450W, the oscillation mode is that the mixed ultrasonic oscillation is kept for 25min every 12min of oscillation and is repeatedly oscillated for 4 times, and the oscillation temperature is 35 ℃; the frequency of a pulse electric field of the mean solution in a high-voltage pulse electric field is 10Hz, the processing time is 400 mus, the electric field strength is 20kV/cm, the rotating speed of mixing and stirring the mean solution with the slurry is 500r/min, and the stirring time is 4 min; the temperature of vacuum drying after filtering the mixed solution is 70 ℃; the temperature of the catalyst precursor high-temperature reduction treatment is 220 ℃.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. A nano-palladium catalyst characterized by: the nano palladium catalyst comprises active palladium nano particles and a carrier, wherein the particle size of the active palladium nano particles is 5-20nm, the particle size of the carrier is 60-100nm, and the loading capacity of nano palladium is 1.2-2.4% of the carrier.
2. The nano-palladium catalyst according to claim 1, wherein: the carrier is one or more of silicon dioxide, aluminum oxide, magnesium oxide, titanium oxide, active carbon, montmorillonite and kaolin.
3. A preparation method of a nano palladium catalyst is characterized by comprising the following steps: the preparation method of the nano palladium catalyst comprises the following steps:
(1) adding nitric acid into the carrier for treating for a period of time, taking out and washing the carrier, adding deionized water, stirring at a high speed and mixing uniformly to obtain slurry for later use;
(2) adding soluble palladium salt into deionized water, and carrying out heat preservation, vibration and homogenization in an ultrasonic vibration instrument to obtain a homogeneous solution for later use;
(3) pretreating the homogeneous liquid by adopting a high-voltage pulse electric field, adding the slurry obtained in the step (1), and mixing and stirring uniformly to obtain a mixed liquid for later use;
(4) filtering the mixed solution, and then drying in vacuum to obtain a catalyst precursor for later use;
(5) and carrying out high-temperature reduction treatment on the catalyst precursor for 20-24h under the protection of helium to obtain the nano palladium catalyst.
4. The method for preparing a nano-palladium catalyst according to claim 3, wherein: the treatment time of the carrier in the nitric acid is 4-6h, and the high-speed stirring speed of adding the deionized water is 600-800 r/min.
5. The method for preparing a nano-palladium catalyst according to claim 3, wherein: the power of the mixing ultrasonic oscillation of the soluble palladium salt and the deionized water is 400-500W, the oscillation mode is that the mixture is kept stand for 20-30min every 10-15min of oscillation, the oscillation is repeated for 3-5 times, and the oscillation temperature is 30-40 ℃.
6. The method for preparing a nano-palladium catalyst according to claim 3, wherein: the frequency of the pulse electric field of the mean solution in the high-voltage pulse electric field is 10Hz, the processing time is 400 mus, the electric field strength is 20kV/cm, the rotating speed of mixing and stirring the mean solution with the slurry is 400-600r/min, and the stirring time is 3-5 min.
7. The method for preparing a nano-palladium catalyst according to claim 3, wherein: the temperature of vacuum drying after filtering the mixed solution is 60-80 ℃.
8. The method for preparing a nano-palladium catalyst according to claim 3, wherein: the temperature of the high-temperature reduction treatment of the catalyst precursor is 200-250 ℃.
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| CN201811221991.0A CN111068663A (en) | 2018-10-19 | 2018-10-19 | Nano palladium catalyst and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546620A (en) * | 2021-07-22 | 2021-10-26 | 山西大学 | Palladium oxide supported zinc-based catalyst and preparation method and application thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113546620A (en) * | 2021-07-22 | 2021-10-26 | 山西大学 | Palladium oxide supported zinc-based catalyst and preparation method and application thereof |
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Application publication date: 20200428 |