CN114406278A - Preparation method of palladium nano cubic particles - Google Patents
Preparation method of palladium nano cubic particles Download PDFInfo
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- 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
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- aminophenol
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- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 229910052763 palladium Inorganic materials 0.000 title claims abstract description 34
- 239000002245 particle Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 34
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims description 26
- 238000003756 stirring Methods 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 19
- 239000002244 precipitate Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 12
- CWLKGDAVCFYWJK-UHFFFAOYSA-N 3-aminophenol Chemical compound NC1=CC=CC(O)=C1 CWLKGDAVCFYWJK-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000012295 chemical reaction liquid Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 229940018563 3-aminophenol Drugs 0.000 claims description 4
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 claims description 4
- 150000002500 ions Chemical class 0.000 claims description 4
- 150000002940 palladium Chemical class 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- JVVRCYWZTJLJSG-UHFFFAOYSA-N 4-dimethylaminophenol Chemical compound CN(C)C1=CC=C(O)C=C1 JVVRCYWZTJLJSG-UHFFFAOYSA-N 0.000 claims description 2
- ZFIQGRISGKSVAG-UHFFFAOYSA-N 4-methylaminophenol Chemical compound CNC1=CC=C(O)C=C1 ZFIQGRISGKSVAG-UHFFFAOYSA-N 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical group [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 2
- 229910002094 inorganic tetrachloropalladate Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- -1 o-acetaminophen Chemical compound 0.000 claims description 2
- 229960005489 paracetamol Drugs 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 239000011591 potassium Substances 0.000 claims description 2
- ABKQFSYGIHQQLS-UHFFFAOYSA-J sodium tetrachloropalladate Chemical compound [Na+].[Na+].Cl[Pd+2](Cl)(Cl)Cl ABKQFSYGIHQQLS-UHFFFAOYSA-J 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 3
- MUJIDPITZJWBSW-UHFFFAOYSA-N palladium(2+) Chemical class [Pd+2] MUJIDPITZJWBSW-UHFFFAOYSA-N 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 7
- 229910000510 noble metal Inorganic materials 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 238000000053 physical method Methods 0.000 description 3
- 229910002093 potassium tetrachloropalladate(II) Inorganic materials 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000001016 Ostwald ripening Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 230000009629 growth pathway Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002070 nanowire Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 238000006557 surface reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making 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 & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Catalysts (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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
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.
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