CN111408369A - Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof - Google Patents
Nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and preparation method thereof Download PDFInfo
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- CN111408369A CN111408369A CN202010298288.0A CN202010298288A CN111408369A CN 111408369 A CN111408369 A CN 111408369A CN 202010298288 A CN202010298288 A CN 202010298288A CN 111408369 A CN111408369 A CN 111408369A
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- 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
- B01J23/48—Silver or gold
- B01J23/52—Gold
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- 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
- B01J23/42—Platinum
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
Abstract
The invention discloses a nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and a preparation method thereof. Preparing a nano gold-platinum bimetal @ carbon material oxygen reaction catalyst by using a carbon material as a carrier and using an organic ligand-terminated nano gold-platinum bimetal as an active center through a one-step reduction method; the carbon material is one or more of carbon nano tube, graphene and carbon black, and the end-capping reagent is one or more of tetrakis hydroxymethyl phosphonium chloride, mercaptosuccinic acid and triphenylphosphine. The average grain diameter of the nano-Au-Pt bimetal is 2.8-3.2 nm, the loading capacity of the nano-Au-Pt bimetal is 10-15 wt.%, and the molar ratio of Au to Pt is 0.5-1.7. The catalyst has the advantages of controllable structure, mild reaction conditions, simple operation and low cost; compared with commercial 20wt.% Pt/C, the prepared nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst has better oxygen reduction and oxygen evolution catalytic activity and stability.
Description
Technical Field
The invention relates to the field of oxygen reaction catalysis, in particular to a nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst and a preparation method thereof.
Background
The development in the field of electric vehicles has placed higher demands on the energy density of batteries (> 300 Wh/kg). The theoretical energy density of the lithium ion battery widely used at present is low, and is only 150-200Wh/kg, which can not meet the endurance requirement of the electric automobile. The metal air battery, such as a zinc air battery, a magnesium air battery, an aluminum air battery, a lithium air battery and the like, has high energy density and can meet the development requirements of electric automobiles. The metal-air battery positive electrode relates to oxygen reduction reaction and oxygen evolution reaction, but the oxygen electrode reaction kinetics is slow, and the energy efficiency of the metal-air battery is reduced.
The oxygen electrode reaction kinetics can be improved by adopting the catalyst, the current commercial platinum-carbon catalyst (20 wt.% Pt/C) has higher catalytic activity on the oxygen reaction, but the cost of the metal-air battery is increased due to high price of the catalyst because platinum resources are scarce. Moreover, platinum may dissolve or fall off during the battery cycle process, and the stability of the catalyst is poor, which is not favorable for maintaining high energy efficiency of the battery in long-term operation. Therefore, the development of a high catalytic activity, high stability, and low cost oxygen reaction catalyst is a problem to be solved.
Disclosure of Invention
In view of the above, the present invention aims to provide a nano-gold-platinum bimetallic @ carbon material oxygen reaction catalyst and a preparation method thereof.
The invention relates to a nano gold platinum bimetal @ carbon material oxygen reaction catalyst, which takes nano gold platinum bimetal with a carbon material as a carrier and an organic ligand as a capping reagent as an active center. The average grain diameter of the nano-Au-Pt bimetal is 2.8-3.2 nm, the loading capacity of the nano-Au-Pt bimetal is 10-15 wt.%, and the molar ratio of Au to Pt is 0.5-1.7.
The preparation method of the nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst comprises the following specific steps:
(1) placing 40-80 mg of carbon material into a 150 m L conical flask, and adding 100 m L deionized water.
(2) Preserving the heat of the product obtained in the step (1) in a super constant temperature water bath at the temperature of 60-95 ℃ for 5 minutes, and then adding 0.5-1.5 m L with the concentration of 2.0 × 10-4~ 3.0×10-4The concentration of chloroauric acid in mol/L and 0.6-1.9 m L is 2.0 × 10-4~ 3.0×10-4And (3) chloroplatinic acid of mol/L, stirring and carrying out ultrasonic treatment to obtain a stable dispersion liquid with constant temperature.
(3) And (3) adding an alkali source with the concentration of 1 mol/L and the end-capping reagent with the concentration of 50 mmol/L of 1.9-2.4 m L into the stable dispersion liquid with the constant temperature obtained in the step (2) to obtain an alkaline mixed solution, and adding sodium borohydride with the concentration of 50 mmol/L of 3.8-4.8 m L if the end-capping reagent is mercaptosuccinic acid.
(4) Stirring the product obtained in the step (3) in a constant-temperature water bath for reaction for 3 hours to obtain a mixed solution of reaction products; and immediately placing the conical flask into an ice-water bath to stop reaction after the reaction is finished, then taking out the conical flask, standing the conical flask overnight at an air temperature, centrifuging the conical flask at 8000 rpm to be neutral, drying the conical flask, and fully grinding the conical flask to obtain the nano gold-platinum bimetallic @ carbon nano tube oxygen reaction catalyst powder.
The carbon material is one or more of commercially available carbon nanotubes, graphene and carbon black.
The alkali source is sodium hydroxide or potassium hydroxide.
The end-capping reagent is one or more of commercial tetrakis hydroxymethyl phosphonium chloride, mercaptosuccinic acid and triphenylphosphine, wherein the tetrakis hydroxymethyl phosphonium chloride is oxidized in the reaction of step (3) to generate trihydroxy phosphonium oxide.
The invention has no special requirements on ultrasonic power and ultrasonic time, and can produce uniform mixed liquid.
The invention has no special requirements on the type of the super constant temperature water bath, and can be realized by adopting a commercial instrument well known in the field.
The invention has no special requirement on the stirring speed, and only needs to uniformly mix the liquid; the invention has no special requirement on the stirring time as long as the constant temperature can be reached.
The method of centrifugation is not particularly required in the present invention, and the product can be centrifuged by a method well known in the art.
The invention has no special requirement on the washing times, and can clean the solid obtained by centrifugation.
The invention has no special requirements on the drying temperature and time, and can ensure that the water of the washed solid is removed.
The carbon material is used as a carrier of the catalyst, so that the catalyst is prevented from agglomerating, and a conductive network is provided for the catalyst. Because the organic ligand end capping agent is coordinated and complexed with the nano gold and the nano platinum, the nano gold and the nano platinum are tightly combined to form nano gold platinum bimetal, but not nano gold platinum alloy. The organic ligand end capping agent can prevent the growth of the nano gold-platinum bimetallic crystal and is beneficial to providing more active sites. The nano gold and the nano platinum can be used as oxygen reaction active sites, and the activity of the nano gold-platinum bimetal is higher than that of single nano gold or nano platinum due to the synergistic effect of the nano gold and the nano platinum. The combination of the nano gold and the nano platinum can inhibit the dissolution and precipitation of the nano platinum, so that the stability of the nano gold-platinum bimetal is good.
The method takes the carbon material as a matrix, the organic ligand end capping agent and the one-step reduction method to prepare the nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst, the catalyst structure is controllable, the reaction condition is mild, the operation is simple and the cost is low; compared with commercial 20wt.% Pt/C, the prepared nano gold-platinum bimetallic @ carbon material oxygen reaction catalyst has better oxygen reduction and oxygen evolution catalytic activity and stability.
Drawings
FIG. 1 is a transmission electron micrograph of example 1.
FIG. 2 is a graph showing a particle size distribution in example 1.
FIG. 3 is a high-resolution TEM image of example 1.
FIG. 4 is an X-ray diffraction chart of example 1.
FIG. 5 is a diagram showing the distribution of gold, platinum and carbon elements in the nano-Au-Pt bimetal of example 1.
Fig. 6 is a graph comparing catalytic activity of oxygen reduction reaction of example 2, with a commercial platinum/carbon catalyst in dotted line and a nano-gold platinum bimetallic @ carbon material catalyst in solid line.
Fig. 7 is a graph comparing the catalytic activity of the oxygen evolution reaction of example 2 with a commercial platinum/carbon catalyst in dashed lines and a nano-gold-platinum bimetallic @ carbon material catalyst in solid lines.
FIG. 8 is a stability control curve for example 2 with the dashed line for the commercial platinum/carbon catalyst and the solid line for the nano-gold platinum bimetallic @ carbon material catalyst.
Fig. 9 is a graph comparing the catalytic activity of the oxygen reduction reaction of example 3, with a commercial platinum/carbon catalyst in dashed lines and a nano-gold-platinum bimetallic @ carbon material catalyst in solid lines.
FIG. 10 is a graph of the catalytic activity of the oxygen evolution reaction versus example 3 with the dashed line for the commercial platinum/carbon catalyst and the solid line for the nano-gold platinum bimetallic @ carbon material catalyst.
FIG. 11 is a stability control curve for example 3 with the dashed line for the commercial platinum/carbon catalyst and the solid line for the nano-gold platinum bimetallic @ carbon material catalyst.
Detailed Description
Example 1:
(1) 45 mg of commercially available carbon nanotubes were placed in a 150 m L conical flask and 100 m L of deionized water was added.
(2) The product obtained in step (1) was incubated for 5 minutes in a super thermostatic water bath at 70 ℃ and subsequently 1.5 m L was added to the flask at a concentration of 2.43 × 10-4Chloroauric acid in mol/L and a concentration of 0.625 m L of 2.0 × 10-4And (3) chloroplatinic acid of mol/L, stirring and carrying out ultrasonic treatment to obtain a stable dispersion liquid with constant temperature.
(3) To the stable dispersion liquid obtained in step (2) at a constant temperature, 550. mu. L sodium hydroxide of 1 mol/L and 1.9 m L tetrakis hydroxymethyl phosphonium chloride of 50 mmol/L were added to obtain an alkaline mixed liquid.
(4) Stirring the product obtained in the step (3) in a constant-temperature water bath for reaction for 3 hours to obtain a mixed solution of reaction products; and immediately placing the conical flask into an ice-water bath to stop reaction after the reaction is finished, then taking out the conical flask, standing the conical flask overnight at an air temperature, centrifuging the conical flask at 8000 rpm to be neutral, drying the conical flask, and fully grinding the conical flask to obtain the nano gold-platinum bimetallic @ carbon nano tube oxygen reaction catalyst powder.
The TEM of the nano-gold-platinum bimetallic @ carbon nanotube prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that the nano-gold-platinum bimetallic is uniformly distributed on the carbon nanotube. The particle size distribution of the nano-Au-Pt bimetal of the present example is shown in FIG. 2, and it can be seen from FIG. 2 that the average size of the nano-Au-Pt bimetal is 3.02 nm. The morphology of the high-resolution transmission electron microscope of the nano-gold-platinum bimetal of the embodiment is shown in fig. 3, and as can be seen from fig. 3, nano-gold (111) is located at an interplanar spacing of 0.236 nm, nano-platinum (111) is located at an interplanar spacing of 0.225 nm, and the nano-gold and the nano-platinum are combined together, but do not form an alloy. In this example, XRD is shown in fig. 4, XRD diffraction peaks of nano-gold and nano-platinum are respectively at 38.1 °, 44.3 °, 64.5 ° and 39.5 °, 45.9 °, 67.0 °, which proves that nano-gold and nano-platinum do not form an alloy. The distribution of gold and platinum elements of the nano gold-platinum bimetal of the embodiment is shown in fig. 5, and the gold and platinum elements are overlapped together, which proves that the nano gold and the nano platinum are combined together.
Example 2:
(1) 50 mg of commercially available carbon nanotubes were placed in a 150 m L conical flask and 100 m L of deionized water was added.
(2) The product obtained in step (1) was incubated for 5 minutes in a super thermostatic water bath at 75 ℃ and subsequently 1m L, 2.43 × 10 concentration was added to the bottle-4Chloroauric acid in mol/L and a concentration of 1.25 m L of 2.0 × 10-4And (3) chloroplatinic acid of mol/L, stirring and carrying out ultrasonic treatment to obtain a stable dispersion liquid with constant temperature.
(3) 600 mu L sodium hydroxide with a concentration of 1 mol/L and 2.1m L tetrakis hydroxymethyl phosphonium chloride with a concentration of 50 mmol/L were added to the stable dispersion obtained in step (2) at a constant temperature to obtain an alkaline mixture.
(4) Stirring the product obtained in the step (3) in a constant-temperature water bath for reaction for 3 hours to obtain a mixed solution of reaction products; and immediately placing the conical flask into an ice-water bath to stop reaction after the reaction is finished, then taking out the conical flask, standing the conical flask overnight at an air temperature, centrifuging the conical flask at 8000 rpm to be neutral, drying the conical flask, and fully grinding the conical flask to obtain the nano gold-platinum bimetallic @ carbon nano tube oxygen reaction catalyst powder.
The nano-gold platinum bimetallic @ carbon nanotubes (designated as AuPt-1/MWNTs) prepared in this example were tested for catalytic performance of oxygen reduction reaction, catalytic performance of oxygen evolution reaction, and stability, respectively, using a commercial platinum/carbon catalyst (20 wt.% Pt/C) as a control, and the test results are shown in fig. 6, fig. 7, and fig. 8. The dashed line in FIG. 6 represents 20wt.% Pt/C, and the solid line represents AuPt-1/MWNTs; as can be seen from FIG. 6, the oxygen reduction catalytic activity of AuPt-1/MWNTs is comparable to 20wt.% Pt/C. The dashed line in FIG. 7 represents 20wt.% Pt/C, and the solid line represents AuPt-1/MWNTs; as can be seen from FIG. 7, the oxygen evolution catalytic activity of AuPt-1/MWNTs is comparable to 20wt.% Pt/C. The dashed line in FIG. 8 represents 20wt.% Pt/C, and the solid line represents AuPt-1/MWNTs; as can be seen from FIG. 8, the stability of AuPt-1/MWNTs is comparable to 20wt.% Pt/C.
Example 3:
(1) 55 mg of commercially available carbon nanotubes were placed in a 150 m L conical flask and 100 m L of deionized water was added.
(2) The product obtained in step (1) was incubated for 5 minutes in a super thermostatic water bath at 80 ℃ and subsequently 0.5 m L was added to the flask at a concentration of 2.43 × 10-4The concentration of chloroauric acid and 1.875 m L in mol/L is 2.0 × 10-4And (3) chloroplatinic acid of mol/L, stirring and carrying out ultrasonic treatment to obtain a stable dispersion liquid with constant temperature.
(3) Adding 650 mu L sodium hydroxide with concentration of 1 mol/L and 2.3 m L mercaptosuccinic acid with concentration of 50 mmol/L into the stable dispersion liquid with constant temperature obtained in the step (2), and adding 4.6 m L sodium borohydride with concentration of 50 mmol/L to obtain alkaline mixed liquid.
(4) Stirring the product obtained in the step (3) in a constant-temperature water bath for reaction for 3 hours to obtain a mixed solution of reaction products; and immediately placing the conical flask into an ice-water bath to stop reaction after the reaction is finished, then taking out the conical flask, standing the conical flask overnight at an air temperature, centrifuging the conical flask at 8000 rpm to be neutral, drying the conical flask, and fully grinding the conical flask to obtain the nano gold-platinum bimetallic @ carbon nano tube oxygen reaction catalyst powder.
The nano-gold platinum bimetallic @ carbon nanotubes (designated as AuPt-2/MWNTs) prepared in this example were tested for catalytic performance of oxygen reduction reaction, catalytic performance of oxygen evolution reaction, and stability, respectively, using a commercial platinum/carbon catalyst (20 wt.% Pt/C) as a control, and the test results are shown in fig. 9, fig. 10, and fig. 11. The dashed line in FIG. 9 represents 20wt.% Pt/C, and the solid line represents AuPt-2/MWNTs; as can be seen from FIG. 9, the oxygen reduction catalytic activity of AuPt-2/MWNTs is comparable to 20wt.% Pt/C. The dashed line in FIG. 10 represents 20wt.% Pt/C, and the solid line represents AuPt-2/MWNTs; as can be seen from FIG. 10, the oxygen evolution catalytic activity of AuPt-2/MWNTs is comparable to 20wt.% Pt/C. The dashed line in FIG. 11 represents 20wt.% Pt/C, and the solid line represents AuPt-2/MWNTs; as can be seen from FIG. 11, the stability of AuPt-2/MWNTs is comparable to that of 20wt.% Pt/C.
Claims (2)
1. A nanometer gold platinum bimetal @ carbon material oxygen reaction catalyst is characterized in that the nanometer gold platinum bimetal @ carbon material oxygen reaction catalyst takes a carbon material as a matrix, and nanometer gold platinum bimetal with an organic ligand as a capping reagent as an oxygen reaction catalyst with an active center;
the carbon material is one or more of commercially available carbon nanotubes, graphene and carbon black;
the end-capping reagent is one or more of market-available tetrakis (hydroxymethyl) phosphonium chloride, mercaptosuccinic acid and triphenylphosphine, wherein the tetrakis (hydroxymethyl) phosphonium chloride is oxidized to generate trihydroxy phosphonium oxide;
the average grain diameter of the nano-Au-Pt bimetal is 2.8-3.2 nm, the loading capacity of the nano-Au-Pt bimetal is 10-15 wt.%, and the gold/Pt molar ratio is 0.5-1.7.
2. The preparation method of the nano-Au-Pt bimetallic @ carbon material oxygen reaction catalyst as claimed in claim 1, is characterized by comprising the following specific steps:
(1) putting 40-80 mg of carbon material into a 150 m L conical flask, and adding 100 m L deionized water;
(2) preserving the heat of the product obtained in the step (1) in a super constant temperature water bath at the temperature of 60-95 ℃ for 5 minutes, and then adding 0.5-1.5 m L with the concentration of 2.0 × 10-4~ 3.0×10-4The concentration of chloroauric acid in mol/L and 0.6-1.9 m L is 2.0 × 10-4~3.0×10-4Stirring and ultrasonically treating chloroplatinic acid of mol/L to obtain stable dispersion liquid with constant temperature;
(3) adding an alkali source with the concentration of 1 mol/L and an end-capping reagent with the concentration of 50 mmol/L of 1.9-2.4 m L into the stable dispersion liquid with the constant temperature obtained in the step (2) to obtain an alkaline mixed solution, and adding sodium borohydride with the concentration of 50 mmol/L of 3.8-4.8 m L if the end-capping reagent is mercaptosuccinic acid;
(4) stirring the product obtained in the step (3) in a constant-temperature water bath for reaction for 3 hours to obtain a mixed solution of reaction products; immediately placing the conical flask into an ice-water bath to stop reaction after the reaction is finished, then taking out the conical flask, standing the conical flask overnight at an air temperature, centrifuging the conical flask at 8000 rpm to be neutral, drying the conical flask, and fully grinding the conical flask to obtain nano gold-platinum bimetallic @ carbon nanotube oxygen reaction catalyst powder;
the carbon material is one or more of commercially available carbon nanotubes, graphene and carbon black;
the alkali source is sodium hydroxide or potassium hydroxide;
the end-capping reagent is one or more of commercial tetrakis hydroxymethyl phosphonium chloride, mercaptosuccinic acid and triphenylphosphine, wherein the tetrakis hydroxymethyl phosphonium chloride is oxidized in the reaction of the step (3) to generate trihydroxy phosphonium oxide.
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