CN104907557A - Flower-like gold palladium heterogeneous nano particle with good electro-catalytic property and preparing method thereof - Google Patents
Flower-like gold palladium heterogeneous nano particle with good electro-catalytic property and preparing method thereof Download PDFInfo
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Abstract
The invention relates to a flower-like gold palladium heterogeneous nano particle with a good electro-catalytic property and a preparing method thereof. The preparing method of the particle includes the following steps that firstly, under the condition of magnetic force stirring, ascorbic acid (AA), sodium citrate, dehydrate (C6H5Na3O7.2H2O), an aurum (Au) decahedron colloidal solution and a disodium tetrachloropalladate (Na2PdC14) water solution are added to an ethylene glycol solution in sequence; secondly, a reaction polymeric precursor solution is placed at the reaction temperature of 25-75 DEG C for 0.2-1 hour, and then centrifuging is conducted for 15-50 minutes under the condition of the rotation speed of 5000-15000 turns per minute; thirdly, solvent ultrasonic is used for cleaning dark blue precipitate products, and therefore the flower-like gold palladium heterogeneous nano particle is prepared. The flower-like gold palladium heterogeneous nano particle has important application value in the aspects of direct alcohol fuel batteries, surface enhanced Raman scattering (SERS), chemical and biological sensors and the like.
Description
Technical field
The present invention relates to a kind of heterogeneous nano particle of flower-shaped golden palladium with good electric catalytic performance and preparation method thereof.
Background technology
Gold palladium bimetal nano material directly prepares the fields such as hydrogen peroxide at the hydrochlorination of the synthesis of the catalytic oxidation of the low-temperature oxidation of CO, alcohol, vinyl acetate, alkynes, alkene epoxidation and hydrogen and oxygen important application.In addition, the oxidation of synergy on alcohols of golden palladium has significant impact.Such as, by benzyl alcohol oxidation to benzaldehyde, when utilizing the nano particle ratio of golden core palladium shell to be used alone golden nanometer particle or Pd nano particle, conversion rate can improve 10 to 100 times.Therefore, the bimetal nano particles of golden palladium composition becomes study hotspot at catalytic field.At present, synthesis size golden palladium bimetal nano particles that is homogeneous, morphology controllable achieves very much progress, synthetic method according to bibliographical information gold palladium bimetal nano particles can be divided into two large classes, i.e. co-reducing process and seed mediated growth method, it is bar-shaped, dendritic and have the golden palladium bimetal nano material of the patterns such as polyhedron that people have utilized said method to synthesize.Research shows, the catalytic reaction of metal nanoparticle generally occurs in the outer surface of particle, but has continuous print shell structurre with the golden palladium composite nanoparticle that current method is synthesized, and can not give full play to the synergy of golden core and palladium shell.Compared with the golden palladium bimetal nano particles with continuous shell structurre, the heterogeneous nano particle of flower-shaped golden palladium more can give full play to its catalytic performance.But the heterogeneous nano particle of the Environment friendly technology flower-shaped golden palladium of synthesis still faces lot of challenges, and its synthesis technique rarely has report.
Summary of the invention
The technical problem to be solved in the present invention is overcome the weak point in the heterogeneous nano particle technology of preparing of existing flower-shaped golden palladium, there is provided a kind of simple and practical preparation method with universality, and the heterogeneous nano particle of flower-shaped golden palladium utilizing the method to prepare has excellent catalytic performance.
In the present invention, the heterogeneous nano particle exemplary synthesis of flower-shaped golden palladium adopts seed mediated growth method to heat under ambiance and uniform temperature condition containing ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), golden decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) mixed solution.
The preparation method of the described heterogeneous nano particle of flower-shaped golden palladium, comprises following concrete steps:
(1) add successively in ethylene glycol solution under the condition of magnetic agitation, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0001-0.001 mol/L, 0.00025-0.001 mol/L, 0.00015-0.001 mol/L, 0.00025-0.001 mol/L;
(1) subsequently, 0.2-1 hour is reacted under precursor solution being placed in 25-75 degree Celsius of reaction temperature, obtain navy blue colloidal solution, after naturally cooling to room temperature, with supercentrifuge under 5000-15000 rev/min of speed conditions after centrifugal 15-50 minute, remove colourless solution in centrifuge tube, obtain dark blue precipitate product;
(2) with deionized water ultrasonic cleaning dark blue precipitate product, obtained product as shown in Figure 2, this product is the heterogeneous nano particle of flower-shaped golden palladium.
Beneficial effect of the present invention:
(1) product that prepared by the method is the heterogeneous nano particle of flower-shaped golden palladium, and particle scale is even, good dispersion;
(2) the heterogeneous nano particle of flower-shaped golden palladium has extraordinary dispersiveness and stability in the solution such as water or ethylene glycol, can preserve for a long time and deformation does not occur or precipitation of reuniting under room temperature, ambient atmosphere conditions;
(3) preparation of the present invention only needs general conventional equipment, and does not need special equipment, and technical process is simple to operation;
(4) of the present invention raw materials used abundant, pollution-free and cheap and easy to get, be particularly suitable in enormous quantities, the low cost preparation of the heterogeneous nano particle of flower-shaped golden palladium, be not only applicable to industrialized large-scale production, be also easy to business-like application;
(5) used in the present invention method has universality, can prepare the heterogeneous nano particle of flower-shaped golden palladium with the gold seeds of different-shape;
(6) catalytic oxidation of the heterogeneous nano particle of flower-shaped golden palladium to ethanol synthesized in the present invention shows excellent catalytic performance.
Accompanying drawing explanation
Fig. 1 visually observes to obtained gold (Au) nanometer decahedron colloidal solution and flower-shaped golden palladium heterogeneous nanometer particle colloid solution the optical photograph that rear camera takes, Fig. 1 a is gold (Au) nanometer decahedron colloidal solution, solution colour is rose, Fig. 1 b is the colloidal solution of product, and solution colour is navy blue;
Fig. 2 is the schematic diagram of golden decahedron and the heterogeneous nano particle of flower-shaped golden palladium, and wherein Fig. 2 a is golden decahedral schematic diagram, and figure b is the schematic diagram of the heterogeneous nano particle of flower-shaped golden palladium;
Fig. 3 be in multiple transmission electron microscopes (TEM) photo taken after obtained flower-shaped golden palladium heterogeneous nano particle JEOL-1400 transmission electron microscope observing one of, wherein, Fig. 3 a is low power TEM image, Fig. 3 b is high power TEM image, scale in Fig. 3 a, 3b is respectively 100 nanometers and 50 nanometers, can be seen by Fig. 3 a and Fig. 3 b, product is that yardstick is even, the heterogeneous nano particle of the flower-shaped golden palladium of productive rate;
Fig. 4 is the X-ray energy spectrum figure (EDS) obtained flower-shaped golden palladium heterogeneous nano particle Oxford type X-ray energy spectrometer being tested to rear acquisition, and wherein, ordinate is intensity, and abscissa is energy.From EDS collection of illustrative plates, obtaining product component is gold, palladium element (copper is from Electronic Speculum copper mesh);
Fig. 5 be multiple transmission electron microscopes (TEM) photo taken after the flower-shaped golden palladium heterogeneous nano particle JEOL-1400 transmission electron microscope observing of different golden palladium ratio one of, wherein, Fig. 5 a gold palladium ratio is the heterogeneous nano particle of flower-shaped golden palladium of 1:1, the heterogeneous nano particle of flower-shaped golden palladium of Fig. 5 b to be golden palladium ratio be 1:2, the heterogeneous nano particle of flower-shaped golden palladium of Fig. 5 c to be golden palladium ratio be 1:3, the heterogeneous nano particle of flower-shaped golden palladium of Fig. 5 d to be golden palladium ratio be 1:4.Fig. 5 a, Fig. 5 b, Fig. 5 c, Fig. 5 d can find out, the method can prepare the heterogeneous nano particle of flower-shaped golden palladium of different golden palladium ratio;
Fig. 6 is the cyclic voltammetry curve with the Catalytic oxidation of ethanol measured by 760D in the morning electrochemical workstation of Shanghai.Wherein, Fig. 6 a is with the cyclic voltammetry curve of golden decahedron nano particle as the Catalytic oxidation of ethanol measured by catalyst, Fig. 6 b is with the cyclic voltammetry curve of the golden palladium ratio heterogeneous nano particle of flower-shaped golden palladium that is 1:1 as the Catalytic oxidation of ethanol measured by catalyst, Fig. 6 c is with the cyclic voltammetry curve of the golden palladium ratio heterogeneous nano particle of flower-shaped golden palladium that is 1:2 as the Catalytic oxidation of ethanol measured by catalyst, Fig. 6 d is with the cyclic voltammetry curve of the golden palladium ratio heterogeneous nano particle of flower-shaped golden palladium that is 1:3 as the Catalytic oxidation of ethanol measured by catalyst, Fig. 6 e is with the cyclic voltammetry curve of the golden palladium ratio heterogeneous nano particle of flower-shaped golden palladium that is 1:4 as the Catalytic oxidation of ethanol measured by catalyst.Known by curve, the heterogeneous nano particle of flower-shaped golden palladium prepared in the present invention shows excellent catalytic activity in the catalytic oxidation of ethanol.
Detailed description of the invention
First diallyl dimethyl ammoniumchloride (PDDA, Mw=100000-200000, the 20 wt%) aqueous solution, ethylene glycol solvent, gold chloride (HAuCl that the present invention uses is bought from market
4), silver nitrate (AgNO
3); Then with 18 megaohm deionized water preparation gold chloride (HAuCl
4), silver nitrate (AgNO
3) aqueous solution, gold chloride (HAuCl
4), silver nitrate (AgNO
3) concentration of aqueous solution is respectively 0.01 mol/L, 0.0001 mol/L.
Golden decahedron nanometer particle colloid solution is prepared: first in diallyl dimethyl ammoniumchloride (PDDA) ethylene glycol solution, add gold chloride (HAuCl successively with polyol reduction method
4), silver nitrate (AgNO
3) and a small amount of ferric trichloride (FeCl
3) aqueous solution, obtain reaction precursor liquid solution, then it is reacted 1-4 hour under 220 degrees Celsius of reaction temperatures, naturally cool to room temperature, obtain the redness gold decahedron nanometer particle colloid solution that yardstick is 30 nanometers.
Below in conjunction with concrete embodiment, content of the present invention is described in further detail, but the invention is not restricted to the following specific examples enumerated.
embodiment 1
the preparation of flower-shaped golden palladium (golden palladium ratio is 1:1) heterogeneous nano particle
Add successively in ethylene glycol solution under magnetic agitation condition, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0005 mol/L, 0.00075 mol/L, 0.00025 mol/L, 0.00025 mol/L; Subsequently, react 0.5 hour under precursor solution being placed in 75 degrees Celsius of reaction temperatures, the heterogeneous nanometer particle colloid solution of flower-shaped golden palladium obtained, as shown in Figure 1 b, use supercentrifuge centrifugation, under rotating speed 10000 revs/min of conditions after centrifugal 30 minutes, remove colourless solution in centrifuge tube, obtain dark blue precipitate product; By deionized water to the ultrasonic cleaning of dark blue precipitate product, the obtained approximate heterogeneous nano particle of flower-shaped golden palladium as shown in Figure 5 a.
embodiment 2
the preparation of flower-shaped golden palladium (golden palladium ratio is 1:2) heterogeneous nano particle
Add successively in ethylene glycol solution under magnetic agitation condition, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0005 mol/L, 0.00075 mol/L, 0.00025 mol/L, 0.0005 mol/L; Subsequently, react 0.5 hour under precursor solution being placed in 75 degrees Celsius of reaction temperatures, the heterogeneous nanometer particle colloid solution of flower-shaped golden palladium obtained, as shown in Figure 1 b, use supercentrifuge centrifugation, under rotating speed 10000 revs/min of conditions after centrifugal 30 minutes, remove colourless solution in centrifuge tube, obtain dark blue precipitate product; By deionized water to the ultrasonic cleaning of dark blue precipitate product, the obtained approximate heterogeneous nano particle of flower-shaped golden palladium as shown in Figure 5 b.
embodiment 3
the preparation of flower-shaped golden palladium (golden palladium ratio is 1:3) heterogeneous nano particle
Add successively in ethylene glycol solution under magnetic agitation condition, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0005 mol/L, 0.00075 mol/L, 0.00025 mol/L, 0.00075 mol/L; Subsequently, react 0.5 hour under precursor solution being placed in 75 degrees Celsius of reaction temperatures, the heterogeneous nanometer particle colloid solution of flower-shaped golden palladium obtained, as shown in Figure 1 b, use supercentrifuge centrifugation, under rotating speed 10000 revs/min of conditions after centrifugal 30 minutes, remove colourless solution in centrifuge tube, obtain dark blue precipitate product; By deionized water to the ultrasonic cleaning of dark blue precipitate product, the obtained approximate heterogeneous nano particle of flower-shaped golden palladium as shown in Figure 5 c.
embodiment 4
the preparation of flower-shaped golden palladium (golden palladium ratio is 1:4) heterogeneous nano particle
Add successively in ethylene glycol solution under magnetic agitation condition, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0005 mol/L, 0.00075 mol/L, 0.00025 mol/L, 0.001 mol/L; Subsequently, react 0.5 hour under precursor solution being placed in 75 degrees Celsius of reaction temperatures, the heterogeneous nanometer particle colloid solution of flower-shaped golden palladium obtained, as shown in Figure 1 b, use supercentrifuge centrifugation, under rotating speed 10000 revs/min of conditions after centrifugal 30 minutes, remove colourless solution in centrifuge tube, obtain dark blue precipitate product; By deionized water to the ultrasonic cleaning of dark blue precipitate product, the obtained approximate heterogeneous nano particle of flower-shaped golden palladium as shown in Fig. 3, Fig. 5 d.
Claims (8)
1. the heterogeneous nano particle of flower-shaped golden palladium, is characterized in that:
(1) the heterogeneous nano particle of said flower-shaped golden palladium is nucleocapsid structure, and particle scale is even, good dispersion;
(2) the heterogeneous nano particle of flower-shaped golden palladium has good dispersiveness and stability in the solution such as water or ethylene glycol, preserves for a long time and deformation does not occur or precipitation of reuniting under room temperature, ambient atmosphere conditions;
(3) synthetic method of the heterogeneous nano particle of flower-shaped golden palladium has universality, can prepare the heterogeneous nano particle of flower-shaped golden palladium with the gold seeds of different-shape;
(4) catalytic oxidation of the heterogeneous nano particle of flower-shaped golden palladium to ethanol synthesized in the present invention shows excellent catalytic performance.
2. a preparation method for the heterogeneous nano particle of flower-shaped golden palladium according to claim 1, comprises the following steps:
Add successively in ethylene glycol solution under the condition of magnetic agitation, ascorbic acid (AA), two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron colloidal solution, tetrachloro-palladium acid sodium (Na
2pdCl
4) aqueous solution, wherein ascorbic acid (AA), two citric acid monohydrate trisodium (C in reaction precursor liquid solution
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0001-0.001 mol/L, 0.00025-0.001 mol/L, 0.00015-0.001 mol/L, 0.00025-0.001 mol/L;
(2) subsequently, 0.2-1 hour is reacted under precursor solution being placed in 25-75 degree Celsius, obtain navy blue colloidal solution, supercentrifuge centrifugal 15-50 minute under 5000-15000 rev/min of rotating speed is used after naturally cooling to room temperature, remove colourless solution in centrifuge tube, obtain dark blue precipitate product;
(3) with deionized water ultrasonic cleaning dark blue precipitate product, the heterogeneous nano particle of golden palladium as shown in Fig. 3, Fig. 5, Fig. 7 is obtained.
3. preparation method according to claim 2, is characterized in that employing that manipulation is convenient, the ascorbic acid of environmental protection with low cost and two citric acid monohydrate trisodiums is as reducing agent.
4. preparation method according to claim 2, is characterized in that ascorbic acid (AA) in reaction precursor liquid solution, two citric acid monohydrate trisodium (C
6h
5na
3o
7 .2H
2o), gold (Au) nanometer decahedron, tetrachloro-palladium acid sodium (Na
2pdCl
4) concentration be respectively 0.0001-0.001 mol/L, 0.00025-0.001 mol/L, 0.00015-0.001 mol/L, 0.00025-0.001 mol/L.
5. the heterogeneous nano particle preparation method of flower-shaped golden palladium according to claim 2, is characterized in that reaction temperature is 25-75 degree Celsius.
6. preparation method according to claim 2, is characterized in that the solvent of washing and precipitating product is deionized water or distilled water.
7. preparation method according to claim 2, has universality, can prepare the heterogeneous nano particle of flower-shaped golden palladium with the gold seeds of different-shape.
8. the catalytic oxidation of the heterogeneous nano particle of flower-shaped golden palladium to ethanol according to claim 2, synthesized in the present invention shows excellent catalytic performance.
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| CN106825608A (en) * | 2017-03-02 | 2017-06-13 | 济南大学 | A kind of method that single dispersing gold decahedron nano-particle is prepared in ethylene glycol |
| CN106944613A (en) * | 2017-03-08 | 2017-07-14 | 济南大学 | A kind of method that fast accurate prepares the heterogeneous nanometer rods of silver-colored@gold@silver with multiple absorbing properties |
| CN108311712A (en) * | 2018-05-03 | 2018-07-24 | 济南大学 | A kind of preparation method of high catalytic performance polyhedral gold-palldium alloy nano material |
| CN111659899A (en) * | 2020-04-21 | 2020-09-15 | 华南师范大学 | Flower-like palladium oxide-gold nano composite material and preparation method and application thereof |
| CN113560592A (en) * | 2021-07-16 | 2021-10-29 | 山西医科大学 | Micro-morphology control method of gold-palladium nano heterostructure material |
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