CN114406278A - Preparation method of palladium nano cubic particles - Google Patents

Preparation method of palladium nano cubic particles Download PDF

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Publication number
CN114406278A
CN114406278A CN202111507672.8A CN202111507672A CN114406278A CN 114406278 A CN114406278 A CN 114406278A CN 202111507672 A CN202111507672 A CN 202111507672A CN 114406278 A CN114406278 A CN 114406278A
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palladium
mixed solution
aminophenol
group
nanocube
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黄远福
李尊华
王洪林
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Shenzhen Baiao Biotechnology Co ltd
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Shenzhen Baiao Biotechnology Co ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B22CASTING; POWDER METALLURGY
    • B22FWORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00Making metallic powder or suspensions thereof
    • B22F9/16Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions

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  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Catalysts (AREA)
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Abstract

The invention discloses a preparation method of palladium nanocubes, which adopts aminophenol as a reducing agent to reduce palladium (II) salt into nanocubes, and controls the appearance of the palladium nanocubes by adjusting the temperature and the reaction time of a reaction solution. The method has the advantages of simple process, convenient operation and good repeatability, and the prepared palladium nano cubic particles have good dispersibility and uniform particle size.

Description

Preparation method of palladium nano cubic particles
Technical Field
The invention belongs to the field of synthesis of inorganic metal nano materials, and particularly relates to a preparation method of palladium nano cubic particles.
Background
Research on the preparation method of the nano noble metal catalyst has been receiving wide attention, because the activity of the supported nano noble metal catalyst (such as Pd, Ru, Au, etc.) has a very close relationship with the preparation method. The existing methods for preparing the nano noble metal catalyst mainly comprise two types: physical methods and chemical methods. The physical method comprises microwave irradiation, ultrasonic method, pulse laser ablation, ray radiation, and plasma method. The nano noble metal catalyst prepared by the physical method has the advantages of simplicity, convenience, narrow noble metal particle size distribution, environmental protection and the like, but the price of required instruments is high. Therefore, at present, the main emphasis is on researching the chemical method for preparing the nano noble metal catalyst. The commonly used methods include a dipping method, a coprecipitation method, a deposition-precipitation method, an ion exchange method, an adsorption method, a chemical vapor deposition method, a photochemical method, a microemulsion method, a surface functionalization method, and the like. Among them, the most commonly used are impregnation, coprecipitation and deposition-precipitation methods, but the conventional impregnation method is liable to cause a large amount of particles to be aggregated during the roasting and reduction processes of the prepared catalyst, and a high-activity Pd catalyst cannot be obtained.
In recent years, with the progress of technology, some more novel and environmentally friendly preparation methods are gradually reported. Several methods have been proposed to explain the growth of metal nanostructures, such as particle coalescence, Ostwald ripening and directed attachment. For example, both Pd worm-like nanowires and Pt mesoporous nanocubes are grown by adsorption, and their unique morphology leads to their excellent performance in catalytic applications.
Despite the extremely attractive features of the non-classical growth pathway, the ability to achieve specific shapes or morphologies remains very limited due to the lack of a profound understanding of the mechanisms that control the growth process. In general, many parameters, including reduction kinetics, surface coverage, adatom diffusion, particle attachment and fusion, affect the growth mode and thus the shape or morphology of the final product.
Although much work has been devoted to studying these factors, the interactions between them are still not well defined and need to be explored further. To fully appreciate these potential factors, the present application is directed to improving the manufacturing process and producing defined nanostructures of metal having desired shapes and properties.
Disclosure of Invention
The present invention aims to provide a method for preparing palladium nanocube particles, so as to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of palladium nano cubic particles comprises the following steps:
step (1), adding polyvinylpyrrolidone into deionized water, and uniformly stirring to obtain a transparent solution;
adding Br ions into the transparent solution obtained in the step (1), and uniformly stirring to obtain a mixed solution A;
step (3), adding palladium salt into the mixed solution A obtained in the step (2), and uniformly stirring to obtain a mixed solution B;
adding reducing agent aminophenol into the mixed solution B obtained in the step (3), and stirring at constant temperature to enable the mixed solution B to react fully;
and (5) centrifuging the reaction liquid obtained in the step (4) to obtain a precipitate, washing the precipitate, and dispersing to obtain the palladium nano cubic particles.
As a further scheme of the invention: in the step (1), the concentration of the transparent solution is 5-20 mg/mL.
As a further scheme of the invention: in the step (2), the Br ions are sodium bromide or potassium bromide, and the concentration is 0.5-4.0 mM.
As a further scheme of the invention: in the step (3), the palladium salt is potassium tetrachloropalladate or sodium tetrachloropalladate, and the concentration is 0.5-4.0 mM.
As a further scheme of the invention: in the step (4), the reducing agent aminophenol is one or a mixture of more of o-aminophenol, m-aminophenol, p-aminophenol, o-acetaminophen, p-methylamino phenol and p-dimethylamino phenol, and the concentration of the reducing agent is 1.0-6.0 mM.
As a further scheme of the invention: the reaction condition temperature of the step (4) is 20-100 ℃, and the time is 20-48 h.
As a further scheme of the invention: in the step (5), the precipitate is washed and dispersed with deionized water, and the number of washing times is 3-5.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts aminophenol as a reducing agent to reduce palladium (II) salt into nano cube particles, and controls the appearance of the palladium nano cube by adjusting the temperature and the reaction time of reaction liquid. The method has the advantages of simple process, convenient operation and good repeatability, and the prepared palladium nano cubic particles have good dispersibility and uniform particle size.
Drawings
FIG. 1 is a scanning electron microscope photograph of palladium nanocube particles prepared in example 1;
FIG. 2 is a scanning electron micrograph of palladium nanocube particles prepared in example 2;
FIG. 3 is a scanning electron micrograph of palladium nanocube particles prepared in example 3;
fig. 4 is a scanning electron microscope photograph of palladium nanocube particles prepared in example 4.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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
In this embodiment, a method for preparing palladium nanocube particles includes the following steps:
adding 1.00g of polyvinylpyrrolidone (PVP) into 100mL of deionized water, and uniformly stirring to obtain a transparent solution I;
adding 0.15mmol KBr into the solution I, and uniformly stirring to obtain a mixed solution II;
adding 0.15mmol of K2PdCl4 into the mixed solution II, and uniformly stirring to obtain a mixed solution III;
adding 0.30mmol of o-aminophenol into the mixed solution, stirring, and reacting at constant temperature of 20 ℃ for 24 hours to obtain reaction liquid.
And centrifuging the reaction solution for 20min at the rotation speed of 13000rpm to obtain a precipitate, washing the precipitate for 3-5 times by using deionized water, and dispersing the precipitate by using the deionized water to obtain the palladium nano cubic particles.
Example 2
In this embodiment, a method for preparing palladium nanocube particles includes the following steps:
adding 1.00g of PVP into 100mL of deionized water, and uniformly stirring to obtain a transparent solution I;
adding 0.15mmol KBr into the solution I, and uniformly stirring to obtain a mixed solution II;
adding 0.15mmol of K2PdCl4 into the mixed solution II, and uniformly stirring to obtain a mixed solution III;
adding 0.30mmol of o-aminophenol into the mixed solution, stirring, and reacting at constant temperature of 40 ℃ for 24 hours to obtain reaction liquid.
And centrifuging the reaction solution for 20min at the rotation speed of 13000rpm to obtain a precipitate, washing the precipitate for 3-5 times by using deionized water, and dispersing the precipitate by using the deionized water to obtain the palladium nano cubic particles.
Example 3
In this embodiment, a method for preparing palladium nanocube particles includes the following steps:
adding 1.00g of PVP into 100mL of deionized water, and uniformly stirring to obtain a transparent solution I;
adding 0.15mmol KBr into the solution I, and uniformly stirring to obtain a mixed solution II;
adding 0.15mmol of K2Adding PdCl4 into the mixed solution II, and stirring and uniformly mixing to obtain a mixed solution III;
adding 0.30mmol of m-aminophenol into the mixed solution, stirring, and reacting at the constant temperature of 60 ℃ for 24 hours to obtain reaction liquid.
And centrifuging the reaction solution for 20min at the rotation speed of 13000rpm to obtain a precipitate, washing the precipitate for 3-5 times by using deionized water, and dispersing the precipitate by using the deionized water to obtain the palladium nano cubic particles.
Example 4
In this embodiment, a method for preparing palladium nanocube particles includes the following steps:
adding 1.00g of PVP into 100mL of deionized water, and uniformly stirring to obtain a transparent solution I;
adding 0.15mmol KBr into the solution I, and uniformly stirring to obtain a mixed solution II;
adding 0.15mmol of K2PdCl4 into the mixed solution II, and uniformly stirring to obtain a mixed solution III;
adding 0.30mmol of m-aminophenol into the mixed solution, stirring, and reacting at the constant temperature of 80 ℃ for 24 hours to obtain reaction liquid.
And centrifuging the reaction solution for 20min at the rotation speed of 13000rpm to obtain a precipitate, washing the precipitate for 3-5 times by using deionized water, and dispersing the precipitate by using the deionized water to obtain the palladium nano cubic particles.
Scanning the palladium nano cubic particles prepared in the embodiment by an electron microscope to obtain electron micrographs as shown in figures 1-4, and thus, the prepared palladium nano cubic particles are uniform in size and particle diameter and good in dispersibility.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: the method comprises the following steps:
step (1), adding polyvinylpyrrolidone into deionized water, and uniformly stirring to obtain a transparent solution;
adding Br ions into the transparent solution obtained in the step (1), and uniformly stirring to obtain a mixed solution A;
step (3), adding palladium salt into the mixed solution A obtained in the step (2), and uniformly stirring to obtain a mixed solution B;
adding reducing agent aminophenol into the mixed solution B obtained in the step (3), and stirring at constant temperature to enable the mixed solution B to react fully;
and (5) centrifuging the reaction liquid obtained in the step (4) to obtain a precipitate, washing the precipitate, and dispersing to obtain the palladium nano cubic particles.
2. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: in the step (1), the concentration of the transparent solution is 5-20 mg/mL.
3. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: in the step (2), the Br ions are sodium bromide or potassium bromide, and the concentration is 0.5-4.0 mM.
4. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: in the step (3), the palladium salt is potassium tetrachloropalladate or sodium tetrachloropalladate, and the concentration is 0.5-4.0 mM.
5. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: in the step (4), the reducing agent aminophenol is one or a mixture of more of o-aminophenol, m-aminophenol, p-aminophenol, o-acetaminophen, p-methylamino phenol and p-dimethylamino phenol, and the concentration of the reducing agent is 1.0-6.0 mM.
6. The method of claim 1 or 5, wherein the palladium nanocube is selected from the group consisting of: the reaction condition temperature of the step (4) is 20-100 ℃, and the time is 20-48 h.
7. The method of claim 1, wherein the palladium nanocube is selected from the group consisting of: in the step (5), the precipitate is washed and dispersed with deionized water, and the number of washing times is 3-5.
CN202111507672.8A 2021-12-10 2021-12-10 Preparation method of palladium nano cubic particles Withdrawn CN114406278A (en)

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CN104493153A (en) * 2014-12-08 2015-04-08 中国科学院深圳先进技术研究院 Palladium nanoparticles and preparation method thereof
KR20150138623A (en) * 2014-06-02 2015-12-10 고려대학교 산학협력단 Direct synthesis of hydrogen peroxide from hydrogen and oxygen using shape controlled Pd nanoparticle supported catalysts
CN109355677A (en) * 2018-11-15 2019-02-19 江苏科技大学 Palladium cubic nanometer crystalline substance of surface doping P elements and its preparation method and application
CN110302777A (en) * 2018-03-20 2019-10-08 天津大学 Palladium nano-particles-absorbent charcoal composite material and its application in carbon dioxide electro-catalysis reduction
CN110511745A (en) * 2019-08-26 2019-11-29 河南师范大学 A kind of preparation method of water soluble fluorescence silicon quantum dot and its application in selective enumeration method paranitrophenol
CN113477936A (en) * 2021-06-30 2021-10-08 海南深远海新能源科技有限公司 Method and device for preparing palladium and palladium alloy nanocrystals

Patent Citations (8)

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US20090263496A1 (en) * 2006-04-15 2009-10-22 Bayer Technology Services Gmbh Method for producing metal particles, metal particles produced thereby, and the use thereof
US20140299821A1 (en) * 2011-11-03 2014-10-09 Bayer Intellectual Property Gmbh Method for producing a metal nanoparticle dispersion, metal nanoparticle dispersion, and use of said metal nanoparticle dispersion
KR20150138623A (en) * 2014-06-02 2015-12-10 고려대학교 산학협력단 Direct synthesis of hydrogen peroxide from hydrogen and oxygen using shape controlled Pd nanoparticle supported catalysts
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CN110302777A (en) * 2018-03-20 2019-10-08 天津大学 Palladium nano-particles-absorbent charcoal composite material and its application in carbon dioxide electro-catalysis reduction
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CN110511745A (en) * 2019-08-26 2019-11-29 河南师范大学 A kind of preparation method of water soluble fluorescence silicon quantum dot and its application in selective enumeration method paranitrophenol
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Application publication date: 20220429