CN113664215A - Bi-Pd bimetal nanocrystal and preparation method thereof - Google Patents

Bi-Pd bimetal nanocrystal and preparation method thereof Download PDF

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CN113664215A
CN113664215A CN202110960470.2A CN202110960470A CN113664215A CN 113664215 A CN113664215 A CN 113664215A CN 202110960470 A CN202110960470 A CN 202110960470A CN 113664215 A CN113664215 A CN 113664215A
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oleylamine
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CN113664215B (en
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郑遗凡
周春静
刘宗健
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Zhejiang University of Technology ZJUT
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    • 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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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
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    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/56—Platinum group metals
    • B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/644—Arsenic, antimony or bismuth
    • B01J23/6447—Bismuth
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    • B01J35/51—
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention discloses a Bi-Pd bimetallic nanocrystal and a preparation method thereof, and the preparation method comprises the following steps: 1) taking oleylamine into a three-neck flask, heating and degassing, and dividing into two parts for later use after degassing is finished; 2) taking the first part of oleylamine degassed in the step 1), dissolving the Bi salt in a three-neck flask, adding the Pd salt after the Bi salt is completely dissolved, and transferring the mixture to a constant-pressure dropping funnel for later use after the Pd salt is completely dissolved; 3) heating the residual degassed oleylamine obtained in the step 1) to a reaction temperature, adding a surfactant, and stirring until the surfactant is dissolved; 4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for a period of time, and stopping heating; and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The preparation method is simple and convenient to operate, and can effectively regulate and control the size of the Bi-Pd bimetallic nanocrystal.

Description

Bi-Pd bimetal nanocrystal and preparation method thereof
Technical Field
The invention relates to the technical field of nano material preparation, in particular to Bi-Pd bimetallic nano crystal and a preparation method thereof.
Background
Catalysis is a key technology in chemical production. Wherein the supported catalyst occupies about 70% of the catalyst. The noble metal catalyst has the advantages of mild condition, excellent performance, high efficiency and the like, and is more widely applied. The supported noble metal catalyst usually adopts Pt, Pd, Ir, Ru, Os, Rh and the like as the active components of the catalyst, wherein the Pd has the advantages of high utilization rate due to high catalytic activity, difficult poisoning, stable chemical property, difficult oxidation and the like,
in many cases, the bimetallic catalyst has higher catalytic activity, selectivity and stability than a single noble metal catalyst, and the application range of the supported noble metal catalyst in catalytic hydrogenation is expanded. Due to the complexity of the components in supported bimetallic catalysts, their performance is not only dependent on the nature of the noble metal, but is also related to the amount of noble metal loading, the manner of loading and the nature of the support. Aiming at different catalytic hydrogenation systems, the continuous development of new supported double noble metal catalysts becomes a research hotspot.
Prepared bimetallic nanomaterials in combination with Pd typically have a composition of (1) Pd-Pt: in the catalytic hydrogenation reaction, the supported Pd-Pt catalyst has higher catalytic activity and selectivity than single metal Pd or Pt, is high-temperature resistant, oxidation resistant, corrosion resistant and easy to recycle, and becomes an important catalyst material. Rungisi adopts wet impregnation to prepare a Pd-Pt/MCM-41 catalyst, and uses the catalyst as a hydrogenation catalyst for preparing partially hydrogenated fatty acid methyl ester by using biodiesel using soybean oil as a raw material, and finds that the catalytic performance and the sulfur tolerance of the Pd-Pt/MCM-41 catalyst are closely related to the Pd/Pt mass ratio, and when the Pd/Pt mass ratio is 1, the catalyst performance is best (Rungisi AN, Lungarmmituechi A, Chollaoop N, et al]. Applied Catalysis A: General, 2020, 590.); (2) Pd-Ru: the metal Pd is added to modify the Ru/C catalyst, and the Pd-Ru is uniformly dispersed on the carrier AC and has small particle size, the electronic property of the Ru can be remarkably improved by adding the Pd, the existence state of Pd-Ru species can be influenced by adjusting different Ru/Pd atomic ratios, and the yield and the optical selectivity of the L-aminopropanol are further influenced. The catalyst shows the best catalytic performance when the Ru/Pd atomic ratio is 3:1, the yield of the L-aminopropanol and the optical selectivity of the product can reach 99.7 percent, the catalyst can be recycled for 20 times, and the catalytic performance is basically kept unchanged (Daiweiwei, Yaojiaolong, Schuosheng, and the like)]The journal of chemical engineering, 2018, 69 (6): 2503-; (3) Pd-Ag: in the supported Pd-Ag catalyst, the addition of Ag changes the distribution state and the electron cloud density of Pd on the surface of the catalyst, so that the selectivity of the catalyst is improved, and the catalyst shows good catalytic performance in selective hydrogenation reaction of alkyne and alkene. Korean jade incense and the like with TiO2The nano tube is used as a carrier, a photo-deposition method and an immersion method are respectively adopted to prepare bimetallic catalysts loaded with Pd and Ag, and the selective hydrogenation dechlorination behavior of the bimetallic catalysts to 1, 2-dichloroethane is examined. The characterization result shows that the catalyst prepared by the photo-deposition method has a more obvious Ag enrichment phenomenon than the catalyst prepared by the immersion method under the condition of similar Ag loading. The evaluation result of the catalyst on the activity of the 1, 2-dichloroethane shows that when the Ag loading capacity is similar, the catalyst prepared by the photo-deposition method has higher selectivity on ethylene, and the selectivity of the catalyst on the ethylene is gradually enhanced along with the increase of the Ag loading capacity (Korean jade fragrance, Shaoyu, Wanhaiqin, and the like2Selective hydrodechlorination [ J ] of 1, 2-dichloroethane by nanotube-supported Pd-Ag catalyst]Inorganic chemistry bulletin, 2014, 30(3): 481-.
Although there are many kinds of Pd-based bimetallic nanomaterials, these methods have many disadvantages. In particular, the price of noble metals is increasing, so that the development of a new process which is low in cost, easy to recover and suitable for large-scale industrialization has a great prospect.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a low-cost Bi-Pd bimetallic nanocrystal and a preparation method thereof, the prepared Bi-Pd bimetallic nanocrystal can regulate and control the particle size by changing the temperature, and the preparation method is simple and has mild reaction conditions.
The preparation method of the Bi-Pd bimetallic nanocrystalline is characterized by preparing the Bi-Pd bimetallic nanocrystalline by a chemical reduction method, and specifically comprises the following steps:
1) degassing oleylamine: taking oleylamine into a three-neck flask, heating and degassing, and dividing into two parts for later use after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: taking the first part of oleylamine degassed in the step 1), dissolving the Bi salt in a three-neck flask, adding the Pd salt after the Bi salt is completely dissolved, and transferring the mixture to a constant-pressure dropping funnel for later use after the Pd salt is completely dissolved;
3) heating the other part of residual oleylamine degassed in the step 1) to reaction temperature, then adding a surfactant, and stirring until the surfactant is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2) through a constant pressure dropping funnel to perform reaction; and cooling after the reaction is finished, finally performing centrifugal separation on the reaction liquid, and drying to obtain the product, namely the Bi-Pd bimetallic nanocrystal.
The preparation method of the Bi-Pd bimetallic nanocrystal is characterized in that the reaction temperature in the step 4) is 200-260 ℃, and preferably 230 ℃; the reaction time in the step 4) is 2-10 min, preferably 2-4 min.
The preparation method of the Bi-Pd bimetallic nanocrystalline is characterized in that the Bi salt in the step 2) is BiCl3The Pd salt is PdCl2。
The preparation method of the Bi-Pd bimetallic nanocrystalline is characterized in that in the step 2), the feeding molar ratio of Bi salt to Pd salt is 1: 0.03-0.07, preferably 1: 0.05; the volume of the first part of oleylamine in the step 2) accounts for 40-45% of the total volume of oleylamine in the step 1), and the ratio of the total molar amount of the Bi salt and the Pd salt to the total molar amount of oleylamine in the step 1) is 1: 71.8-143.6.
The preparation method of the Bi-Pd bimetallic nanocrystal is characterized in that in the step 3), the surfactant is polyvinylpyrrolidone, and the mass ratio of the polyvinylpyrrolidone to the total mass of the Bi salt and the Pd salt in the step 2) is 0.75-0.8: 1.
The preparation method of the Bi-Pd bimetallic nanocrystalline is characterized in that in the step 4), the centrifugal speed is 9000r/min, the drying temperature is 60-80 ℃, and the drying time is 8-12 h.
Bi-Pd bimetallic nanocrystalline prepared by any one of the above methods.
Compared with the prior art, the invention has the beneficial effects that:
1) by adopting the technical scheme of the invention, oleylamine is used as a solvent to dissolve Bi salt and Pd salt, and meanwhile, oleylamine is also a reducing agent and a surfactant of the whole reaction system.
2) The preparation method is simple, the Bi-Pd bimetallic nano-materials with different sizes and taking Bi as a main body can be prepared, and the prepared Bi-Pd bimetallic nano-crystal has excellent catalytic performance in the aspect of catalytic hydrodechlorination reaction.
Drawings
FIG. 1 is a high-resolution TEM image of Bi-Pd Bi-metal nanocrystals prepared in example 2;
FIG. 2 is a high-resolution TEM image of Bi-Pd Bi-metal nanocrystals prepared in example 3;
FIG. 3 is a high resolution TEM image of Bi-Pd Bi-metal nanocrystals prepared in example 4;
FIG. 4 is a high-resolution TEM image of the Bi-Pd Bi-metal nanocrystal prepared in example 5.
FIG. 5 is a high-resolution TEM image of the Bi-Pd Bi-metal nanocrystal prepared in example 6.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1
The reaction temperature is 210 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.05g, and the reaction time is 2 min:
1) degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml of oleylamine in the step 1) to 210 ℃, then adding 0.05g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystalline, wherein the morphology is not uniform and the product has a serious agglomeration phenomenon.
Example 2
The reaction temperature is 210 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2 min:
1) degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml of oleylamine in the step 1) to 210 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical and spheroidal particles; the size range is 10-100 nm; the agglomeration phenomenon is not obvious, and the dispersibility is better.
Example 3
The reaction temperature is 230 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2 min:
1) degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 230 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 10-30 nm; the agglomeration phenomenon is not obvious, and the dispersibility is very good.
Example 4
The reaction temperature is 240 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2 min:
1) degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 240 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 10-50 nm; the agglomeration phenomenon is not obvious, and the dispersibility is very good.
Example 5
The reaction temperature is 250 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2 min:
1) degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 250 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 20-100 nm; slightly agglomerating.
Example 6
The Bi-Pd bimetallic nanocrystal is prepared under the conditions that the reaction temperature is 260 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2min
1) Degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 260 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 50-2000 nm; the agglomeration phenomenon is obvious.
TEM images of the Bi-Pd bimetallic nanocrystals prepared in examples 2-6 are respectively shown in FIGS. 1-5, and the morphology and size of the Bi-Pd bimetallic nanocrystals can be seen from the TEM images.
Example 7
The Bi-Pd bimetallic nanocrystal is prepared under the conditions that the reaction temperature is 230 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 5min
1) Degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 230 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 5min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 10-40 nm; slightly agglomerating.
Example 8
The Bi-Pd bimetallic nanocrystal is prepared under the conditions that the reaction temperature is 230 ℃, the consumption of oleylamine is 12ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 10min
1) Degassing oleylamine: taking 12ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 7ml oleylamine in the step 1) to 230 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 10min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 10-40 nm; slightly agglomerating.
Example 9
The Bi-Pd bimetallic nanocrystal is prepared under the conditions that the reaction temperature is 230 ℃, the consumption of oleylamine is 10ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2min
1) Degassing oleylamine: taking 10ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the residual 5ml oleylamine of the step 1) to 230 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is spherical particles; the size range is 30-100 nm; there is an agglomeration phenomenon.
Example 10
The Bi-Pd bimetallic nanocrystal is prepared under the conditions that the reaction temperature is 230 ℃, the consumption of oleylamine is 20ml, the consumption of polyvinylpyrrolidone is 0.1g, and the reaction time is 2min
1) Degassing oleylamine: taking 20ml of oleylamine into a three-neck flask, heating and degassing, and transferring 5ml of oleylamine into another three-neck flask after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: 0.1263g of BiCl are initially introduced35ml of degassed oleylamine was dissolved in a three-necked flask, and after complete dissolution, 0.0040g of PdCl was added2After the materials are completely dissolved, transferring the materials into a constant-pressure dropping funnel for standby;
3) heating the 15ml of oleylamine remaining in the step 1) to 230 ℃, then adding 0.1g of PVP, and stirring until the PVP is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2), reacting for 2min, and stopping heating;
5) and centrifugally separating the reaction product, and drying to obtain the Bi-Pd bimetallic nanocrystal. The morphology is not spherical particles; the size range is 100-; the agglomeration phenomenon is severe.
Compared with the examples 1,2, 3, 4, 5, 6, 7, 8, 9 and 10, the Bi-Pd bimetallic nanocrystals prepared by different examples have different morphologies and sizes, and when the reaction temperature is 230 ℃; the consumption of the surface active agent PVP is 0.1 g; the molar ratio of the total molar amount of the Bi salt and the Pd salt to the reducing agent oleylamine is 1:86.2, and when the reaction time is 2min, the Bi-Pd bimetallic nano crystal has the best appearance and size and the best dispersity.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.

Claims (7)

1. A preparation method of Bi-Pd bimetallic nanocrystalline is characterized in that a chemical reduction method is used for preparing the Bi-Pd bimetallic nanocrystalline, and the preparation method specifically comprises the following steps:
1) degassing oleylamine: taking oleylamine into a three-neck flask, heating and degassing, and dividing into two parts for later use after degassing is finished;
2) preparing a Bi salt solution and a Pd salt solution: taking the first part of oleylamine degassed in the step 1), dissolving the Bi salt in a three-neck flask, adding the Pd salt after the Bi salt is completely dissolved, and transferring the mixture to a constant-pressure dropping funnel for later use after the Pd salt is completely dissolved;
3) heating the other part of residual oleylamine degassed in the step 1) to reaction temperature, then adding a surfactant, and stirring until the surfactant is dissolved;
4) after the surfactant is dissolved in the step 3), adding the oleylamine solution of the Bi salt-Pd salt prepared in the step 2) through a constant pressure dropping funnel to perform reaction; and cooling after the reaction is finished, finally performing centrifugal separation on the reaction liquid, and drying to obtain the product, namely the Bi-Pd bimetallic nanocrystal.
2. The method for preparing Bi-Pd Bi-metal nanocrystals as claimed in claim 1, wherein the reaction temperature in the step 4) is 200-260 ℃, preferably 230 ℃; the reaction time in the step 4) is 2-10 min, preferably 2-4 min.
3. The method according to claim 1, wherein the Bi salt in step 2) is BiCl3The Pd salt is PdCl2。
4. The method for preparing Bi-Pd Bi-metal nanocrystals according to claim 1, wherein the molar ratio of the Bi salt to the Pd salt in step 2) is 1:0.03 to 0.07, preferably 1: 0.05; the volume of the first part of oleylamine in the step 2) accounts for 40-45% of the total volume of oleylamine in the step 1), and the ratio of the total molar amount of the Bi salt and the Pd salt to the total molar amount of oleylamine in the step 1) is 1: 71.8-143.6.
5. The method of claim 1, wherein in step 3), the surfactant is polyvinylpyrrolidone, and the ratio of the mass of polyvinylpyrrolidone to the total mass of the Bi salt and the Pd salt in step 2) is 0.75-0.8: 1.
6. The method of claim 1, wherein in step 4), the centrifugation speed is 9000r/min, the drying temperature is 60-80 ℃, and the drying time is 8-12 h.
7. The Bi-Pd Bi-metal nanocrystal prepared by the method of any one of claims 1 to 6.
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Citations (5)

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