CN103397387A - Preparation method of rhodium-palladium alloy nano dendrite and rhodium-palladium alloy nano dendrite prepared by same - Google Patents
Preparation method of rhodium-palladium alloy nano dendrite and rhodium-palladium alloy nano dendrite prepared by same Download PDFInfo
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Abstract
The invention discloses a preparation method of a rhodium-palladium alloy nano dendrite, which comprises the following steps: dissolving oil-soluble rhodium salt and palladium salt in oleylamine to obtain a first solution; dissolving cetyl trimethyl ammonium bromide and tri-n-octyl phosphine oxide in oleylamine to obtain a second solution; heating the second solution to 160-200 DEG C while stirring, injecting the first solution into the second solution with a pipette, and reacting at 140-200 DEG C for 1-24 hours; and centrifuging the obtained product to obtain the rhodium-palladium alloy nano dendrite. According to the invention, the reaction is carried out at certain temperature by using the oil-soluble palladium salt and rhodium salt as metal sources and oleylamine as a solvent, reducer, modifier and stabilizer; and thus, the preparation method is simple, and the reagents are non-toxic and harmless. The invention also discloses a rhodium-palladium alloy nano dendrite prepared by the method. The rhodium-palladium alloy nano dendrite is echinoid with exposed high-index crystal face, and has the advantages of uniform size, favorable dispersity and adjustable composition.
Description
Technical field
The invention belongs to field of nanometer material technology, relate in particular to a kind of rothenio-palladium nanodendrites and preparation method thereof.
Background technology
Noble metal nanocrystalline mainly refers to precious metal (as gold and silver, rhodium, platinum, the palladium) single crystal particle of size between 1-100nm, in recent years, noble metal nanocrystalline, due to its widespread use in fields such as catalysis, air-sensitive, biomedicine and stored energy conversions, has been subject to investigator's extensive concern.Wherein rhodium nanocrystalline as catalyzer vehicle exhaust process and organic reaction catalysis aspect be widely applied, as hydrogenation reaction, hydroformylation reaction, alkylation reaction etc., therefore improving the nanocrystalline catalytic performance of rhodium has important practical significance.In numerous research methods, synthetic rhodium-base alloy is nanocrystalline is a kind of important channel of improving its catalytic performance.
Synthetic rothenio-palladium is nanocrystalline mainly contains following some advantage: (1), rhodium, palladium are all the metals of face-centred cubic structure, and both lattice parameter difference is less, so both are easier to form alloy; (2), palladium is also a kind of precious metal with catalytic performance, when the rhodium palladium formed alloy, intermetallic coupling can improve catalytic performance; (3), with respect to rhodium, the price of palladium is comparatively cheap, can reduce costs.
According to domestic and international present Research, as can be known: the nanocrystalline pattern of the rothenio-palladium of delivering after deliberation is mainly irregular nano particle (J.Am.Chem.Soc., 2012,134,12390-12393; Catalysis Communications, 2010,11,919 – 922).Nanocrystalline than these irregular rothenio-palladiums of having prepared, the nanodendrites of sea urchin shape is a kind of more difficult synthetic, good, costly nanocrystalline pattern of performance.
Therefore, a kind of novel method for preparing sea urchin shape rothenio-palladium nanodendrites of invention has very important scientific research and realistic meaning.
Summary of the invention
The object of the invention is to the abundant existing nanocrystalline research of rothenio-palladium, a kind of preparation method of sea urchin shape rothenio-palladium nanodendrites is provided, the rothenio-palladium nanodendrites size of the method preparation evenly, good dispersity, composition be controlled.
For achieving the above object, the present invention takes following technical scheme:
A kind of preparation method of rothenio-palladium nanodendrites comprises the following steps:
(1) palladium salt, rhodium salt are dissolved in oleyl amine and obtain the first solution; Cetyl trimethylammonium bromide and trioctylphosphine are dissolved in oleyl amine to obtain the second solution;
(2) be heated to 140-220 ° of C in the time of with the second solution stirring, with liquid-transfering gun, the first solution injected above-mentioned the second solution, reaction 1-24 hour under 140-220 ° of C;
(3) the product centrifugation that step (2) is obtained, obtain the rothenio-palladium nanodendrites.
In above-mentioned preparation process, too much rhodium salt makes product form irregular branched structure; And too much palladium salt will cause forming nanodendrites, but the nano particle that obtains reuniting.As preferably, in step (1), the concentration of palladium salt is 0.002～0.02mol/L, and the mol ratio of palladium salt and rhodium salt is 9:1～1:9.
Further preferred, in step (1), the concentration of palladium salt is 0.005～0.01mol/L.
The present invention prepares the rothenio-palladium nanodendrites in oil phase, so the selection of raw material must be oil-soluble, as preferably, in step (1), palladium salt is palladium acetylacetonate or acid chloride; Rhodium salt is trifluoracetic acid rhodium dimer or methyl ethyl diketone rhodium.
In the present invention, cetyl trimethylammonium bromide has played the effect of modifier, and wherein the bromide anion selective adsorption makes nanocrystalline formation pine-tree structure; And that trioctylphosphine makes two kinds of metals obtain rothenio-palladium through the coreduction processes by complexing action is nanocrystalline.As preferably, in step (1), the volumetric molar concentration of cetyl trimethylammonium bromide and trioctylphosphine is respectively 0.01～0.2mol/L and 0.03～0.5mol/L.
As preferably, the first solution of step (1) and the volume ratio of the second solution are 1:3～1:1.
The rothenio-palladium nanodendrites that the present invention also provides aforesaid method to prepare.
The present invention, take oil-soluble palladium salt and rhodium salt as source metal, is used oleyl amine as solvent, reductive agent, modifier and stablizer, reacts under certain temperature, prepares the sea urchin shape rothenio-palladium nanodendrites that high miller index surface exposes.
Agents useful for same of the present invention is comparatively simple, nontoxic, the preparation method is simple and easy; The rothenio-palladium nanodendrites for preparing size homogeneous, good dispersity, composition is adjustable.The novel method for preparing sea urchin shape rothenio-palladium nanodendrites provided by the invention, have more important academic significance and realistic meaning.
Description of drawings
Fig. 1 is the pattern photo of the rothenio-palladium nanodendrites that obtains of embodiment 1;
Fig. 2 is high resolution transmission electron microscopy (HRTEM) photo (angle) of the rothenio-palladium nanodendrites that obtains of embodiment 1;
Fig. 3 is high resolution transmission electron microscopy (HRTEM) photo (another angle) of the rothenio-palladium nanodendrites that obtains of embodiment 1;
Fig. 4 is scanning transmission electron microscope power spectrum (STEM-EDX) distribution plan of the rothenio-palladium nanodendrites that obtains of embodiment 1.
Embodiment
The invention will be further described below by specific embodiment, but protection scope of the present invention is not limited to following examples.
Embodiment 1
At first 9mg palladium acetylacetonate and 20mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.01mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.02mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 300mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then with cetyl trimethylammonium bromide, the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, test result as shown in Figure 1, wherein in Fig. 1, a is partly transmission electron microscope under 54000 multiplying powers (TEM) picture, b is partly scanning transmission electron microscope under 54000 multiplying powers (STEM) picture, be the rothenio-palladium nanodendrites by its pattern of electron microscopic observation, Fig. 2 and Fig. 3 are high resolution transmission electron microscopy (HRTEM) photo of rothenio-palladium nanodendrites, in Fig. 4, a is partly the spectral distribution figure of rothenio-palladium nanodendrites under 72000 multiplying powers, in Fig. 4, b is partly the spectral distribution figure of rothenio-palladium nanodendrites under 180000 multiplying powers.
The rhodium palladium nano-crystal that can find out preparation by TEM and the STEM photo of Fig. 1 is by the sea urchin shape nanodendrites structure of reuniting; The high-resolution-ration transmission electric-lens photo of Fig. 2 and Fig. 3 can find out that nanodendrites has single crystal structure, and it exposes crystal face partly for high miller index surface (311), and more defect and ledge structure are arranged; In the power spectrum distribution diagram of element of Fig. 4, rhodium element and palladium element are distributed in whole nanodendrites uniformly, have confirmed the alloy structure of nanodendrites.
At first 3mg palladium acetylacetonate and 30mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.0033mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.03mol/L) in the 3mL oleyl amine.Simultaneously 300mg cetyl trimethylammonium bromide and 300mg trioctylphosphine are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then the 5mL mixing solutions of cetyl trimethylammonium bromide and trioctylphosphine and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 3
At first 5mg palladium acetylacetonate and 27mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.0055mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.027mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 300mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then with cetyl trimethylammonium bromide, the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 4
At first 15mg palladium acetylacetonate and 10mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.016mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.01mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 300mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then with cetyl trimethylammonium bromide, the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 5
At first 18mg palladium acetylacetonate and 4mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.02mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.004mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 300mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then with cetyl trimethylammonium bromide, the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 6
At first 9mg palladium acetylacetonate and 20mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.01mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.02mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 600mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.3mol/L) in the 5ml oleyl amine.Then the 5mL mixing solutions of cetyl trimethylammonium bromide and oleyl amine is positioned in well heater, be heated to 220 ° of C when stirring, the 3mL mixing solutions of palladium acetylacetonate, trifluoracetic acid rhodium dimer and oleyl amine is injected in the 5mL mixing solutions of cetyl trimethylammonium bromide and oleyl amine with liquid-transfering gun, react stopped heating after 1 hour, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 7
At first 4.5mg palladium acetylacetonate and 10mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.01mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.002mol/L) in the 1.5mL oleyl amine.Simultaneously, 150mg cetyl trimethylammonium bromide and 150mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 2.5ml oleyl amine.then with cetyl trimethylammonium bromide, the 2.5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 1.5mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 2.5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 7
At first 7mg acid chloride and 12mg methyl ethyl diketone rhodium are dissolved in (concentration of acid chloride is 0.01mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.012mol/L) in the 3mL oleyl amine.Simultaneously, 300mg cetyl trimethylammonium bromide and 300mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 5ml oleyl amine.then with cetyl trimethylammonium bromide, the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 3mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 5mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Embodiment 8
At first 18mg palladium acetylacetonate and 40mg trifluoracetic acid rhodium dimer are dissolved in (concentration of palladium acetylacetonate is 0.01mol/L, and the dimeric concentration of trifluoracetic acid rhodium is 0.02mol/L) in the 6mL oleyl amine.Simultaneously 600mg cetyl trimethylammonium bromide and 600mg three n-octyl oxygen phosphorus are joined (cetyl trimethylammonium bromide concentration is 0.15mol/L, and three n-octyl oxygen phosphorus concentrations are 0.15mol/L) in the 10ml oleyl amine.then with cetyl trimethylammonium bromide, the 10mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine is positioned in well heater, be heated to 200 ° of C when stirring, with liquid-transfering gun with palladium acetylacetonate, the 6mL mixing solutions of trifluoracetic acid rhodium dimer and oleyl amine is injected into cetyl trimethylammonium bromide, in the 10mL mixing solutions of three n-octyl oxygen phosphorus and oleyl amine, react stopped heating after 2 hours, the reacted solution that takes a morsel carries out centrifugal, preparation TEM sample, be sea urchin shape rothenio-palladium nanodendrites by its pattern of transmission electron microscope observing, its test result is similar to embodiment 1.
Claims (7)
1. the preparation method of a rothenio-palladium nanodendrites, is characterized in that, comprises the following steps:
(1) palladium salt, rhodium salt are dissolved in oleyl amine and obtain the first solution; Cetyl trimethylammonium bromide and trioctylphosphine are dissolved in oleyl amine to obtain the second solution;
(2) be heated to 140-220 ° of C in the time of with the second solution stirring, with liquid-transfering gun, the first solution injected above-mentioned the second solution, reaction 1-24 hour under 140-220 ° of C;
(3) the product centrifugation that step (2) is obtained, obtain the rothenio-palladium nanodendrites.
2. the preparation method of rothenio-palladium nanodendrites according to claim 1, is characterized in that, in step (1), the concentration of palladium salt is 0.002～0.02mol/L, and the mol ratio of palladium salt and rhodium salt is 9:1～1:9.
3. the preparation method of rothenio-palladium nanodendrites according to claim 2, is characterized in that, in step (1), the concentration of palladium salt is 0.005～0.01mol/L.
4. the preparation method of rothenio-palladium nanodendrites according to claim 1, is characterized in that, in step (1), palladium salt is palladium acetylacetonate or acid chloride; Rhodium salt is trifluoracetic acid rhodium dimer or methyl ethyl diketone rhodium.
5. the preparation method of rothenio-palladium nanodendrites according to claim 1, is characterized in that, in step (1), the volumetric molar concentration of cetyl trimethylammonium bromide and trioctylphosphine is respectively 0.01～0.2mol/L and 0.03～0.5mol/L.
6. the preparation method of rothenio-palladium nanodendrites according to claim 1, is characterized in that, the first solution of step (1) and the volume ratio of the second solution are 1:3～1:1.
7. the rothenio-palladium nanodendrites for preparing of according to claim 1～6 either method.
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| CN103397387B (en) | 2016-05-11 |
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