CN113492214B - Pt nano particle and preparation method thereof - Google Patents
Pt nano particle and preparation method thereof Download PDFInfo
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- CN113492214B CN113492214B CN202010263465.1A CN202010263465A CN113492214B CN 113492214 B CN113492214 B CN 113492214B CN 202010263465 A CN202010263465 A CN 202010263465A CN 113492214 B CN113492214 B CN 113492214B
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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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- 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
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
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Abstract
The invention discloses Pt nano particles and a preparation method thereof, which solve the problems of complex operation, high cost and unfriendly environment for preparing the Pt nano particles in the prior art. According to the preparation method of the Pt nano particles, ethylene glycol is used as a reducing agent and a protecting agent, and a solvent thermal synthesis method is adopted to reduce chloroplatinic acid, so that nano-scale Pt particles are obtained. The method has the advantages of simple process, convenient operation and low requirements on raw materials and equipment, adopts the simple solvothermal synthesis process, adopts ethylene glycol to reduce chloroplatinic acid, can obtain nano-scale Pt particles without a stabilizer, has uniform size of the Pt particles and size of 1-2nm, and provides a new idea for simplifying the preparation of the nano-scale Pt particles.
Description
Technical Field
The invention relates to the technical field of nano metals, in particular to Pt nano particles and a preparation method thereof.
Background
The nano material has many physical and chemical properties which are not possessed by the traditional solid due to the small size, and is mainly represented by the surface effect, the volume effect, the quantum size effect, the macroscopic quantum tunneling effect and the like of the nano particles. Meanwhile, the nano particles have small size, the surface atoms occupy a large proportion, the specific surface area is high, and the surface atoms have high activity due to insufficient coordination. In addition, the Pt nano particles have excellent catalytic performance and have wide application in the fields of hydrogenation, dehydrogenation, methane conversion, photocatalysis, proton exchange membrane fuel cells and the like. The prior art carries out a great deal of research on reducing the particle size of Pt particles, improving the dispersity of the Pt particles and the like.
At present, a chemical reduction method is mainly adopted to prepare Pt nano particles. Luo Yangming et al employ cetyltrimethylammonium bromide/n-octanol/water (CTAB/C 8 H 17 OH/H 2 The microemulsion of O) and hydrazine hydrate are taken as reducing agents, and Pt particles with the particle size of 6-8 nm are prepared at normal temperature. Li Gan and the like adopt a hydrothermal method to synthesize petal-shaped platinum nano particles with uniform size and good dispersibility by taking potassium chloroplatinate as a precursor and polyvinylpyrrolidone (PVP) as a stabilizer and a reducing agent in the presence of a proper amount of KBr; adopts a solvothermal method, takes chloroplatinic acid as a precursor, methylamine (40%) as a reducing agent, N, N-Dimethylformamide (DMF) as a solvent, PVP as a stabilizer, and synthesizes the chorine-shaped platinum nano particles with uniform size and good dispersibility in the presence of a proper amount of KI. Chen Wei and the like dissolve H with methanol and water 2 PtCl 6 ·6H 2 And O, adopting polyvinylpyrrolidone (PVP) as a stabilizer, and dropwise adding NaOH solution under vigorous stirring to prepare the Pt metal nano particles. Jiang Peng and the like adopt polyethylene glycol (PEG) with the average molecular weight of 300 as a stabilizer, methanol is used as a reducing agent to prepare nano Pt, and the nano Pt catalyst with the particle size distribution of 2.5-3.0 nm is obtained.
In the preparation process of Pt particles, the prepared Pt particles are required to be small in particle size, high in dispersity, uniform in distribution and the like, and the complexity of the preparation process, the preparation cost, the environmental friendliness and the like are also required to be comprehensively considered. In the prior preparation method, a stabilizer and a reducing agent are required, a dispersing agent is sometimes required to be introduced, and a large amount of organic matters are used, and even some organic matters which are not friendly to the environment, such as hydrazine hydrate, methylamine, formaldehyde and the like are required. Therefore, the preparation method of the Pt nano particles is simple, is easy and convenient to operate, is environment-friendly, and is a problem to be solved by the person skilled in the art.
Disclosure of Invention
The invention solves the technical problems that: the preparation method of the Pt nano particles solves the problems that in the prior art, the operation for preparing the Pt nano particles is complex, the cost is high, the preparation method is not friendly to the environment and the like.
The invention also provides Pt nano particles prepared by the preparation method.
The technical scheme adopted by the invention is as follows:
according to the preparation method of the Pt nano particles, ethylene glycol is used as a reducing agent and a protecting agent, and a solvent thermal synthesis method is adopted to reduce chloroplatinic acid, so that nano-scale Pt particles are obtained.
The preparation method only adopts ethylene glycol and chloroplatinic acid, does not adopt other reducing agents, stabilizing agents and the like, and has the advantages of simple operation, low production cost and environmental friendliness.
In the technical scheme of the invention, the preparation method comprises the following steps: and adding the chloroplatinic acid solution into ethylene glycol, dispersing, adjusting the pH value of the mixed solution, and then heating for reaction to obtain nano-scale Pt particles.
Specifically, the concentration of the chloroplatinic acid solution is 0.01mol/l to 0.1mol/l.
Specifically, 0.1 to 10ml of chloroplatinic acid solution is taken and added into 8 to 20ml of ethylene glycol. .
As some examples of the invention, chloroplatinic acid solution was dispersed with ethylene glycol under ultrasonic conditions.
It should be noted that the chloroplatinic acid solution and the ethylene glycol may be dispersed by a method in the prior art, such as magnetic stirring and dispersing.
Specifically, the ultrasonic dispersion time is 15-60min.
In the invention, the mixed solution can react in an alkaline environment to exert the reducibility of glycol.
As some examples of the present invention, the pH of the mixture was adjusted to 9 to 10.
The pH value of the adjusting mixture in the invention can be adjusted before the dispersion, during the dispersion process or after the dispersion is completed. Preferably the pH is adjusted during the dispersion.
As some examples of the present invention, the pH-adjusted dispersed mixed solution is poured into a high-pressure reaction vessel, and then the high-pressure reaction vessel is placed in an oven to heat for reaction.
As some embodiments of the invention, the reaction kettle is placed in an oven with the temperature of 150-190 ℃ and heated for reaction for 30-120 min.
The preparation method of the Pt nano particles comprises the following steps:
step 1, preparing a chloroplatinic acid solution: weighing a proper amount of chloroplatinic acid crystals, adding the chloroplatinic acid crystals into a proper amount of ultrapure water, stirring until the chloroplatinic acid crystals are completely dissolved, preparing a chloroplatinic acid solution with the concentration of 0.01mol/l to 0.1mol/l, and filling the solution into a brown bottle for standby;
step 2, measuring chloroplatinic acid solution, putting the chloroplatinic acid solution into a measured ethylene glycol container, and putting the container with two liquids into an ultrasonic cleaner for ultrasonic dispersion;
step 3, gradually dripping sodium hydroxide solution into the ultrasonic dispersion mixed solution, and adjusting the pH value of the mixed solution to 9-10;
step 4, pouring the dispersed mixed solution with the pH value adjusted into a high-pressure reaction kettle, and placing the mixed solution into an oven for heating reaction;
and 5, stopping the reaction, taking out the reaction kettle, and naturally cooling to room temperature.
The Pt nano particles prepared by the preparation method are prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method has the advantages of simple process, convenient operation and low requirements on raw materials and equipment, adopts the simple solvothermal synthesis process, adopts ethylene glycol to reduce chloroplatinic acid, can obtain nano-scale Pt particles without a stabilizer, has uniform size of the Pt particles and size of 1-2nm, and provides a new idea for simplifying the preparation of the nano-scale Pt particles.
(2) The invention has high cost performance, strong practicability, good repeatability and selectivity, has very good application prospect, and is suitable for popularization and application in the fields of catalysts, membranes, fuel cells and the like.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2-1 is a TEM image of Pt particles synthesized in example 1 of the present invention, and FIG. 2-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 1.
FIG. 3-1 is a TEM image of Pt particles synthesized in example 2 of the present invention, and FIG. 3-2 is a distribution diagram of the particle size of Pt particles synthesized in example 2.
FIG. 4-1 is a TEM image of Pt particles synthesized in example 3 of the present invention, and FIG. 4-2 is a distribution diagram of the particle size of Pt particles synthesized in example 3.
FIG. 5-1 is a TEM image of Pt particles synthesized in example 4 of the present invention, and FIG. 5-2 is a distribution diagram of the particle size of Pt particles synthesized in example 4.
FIG. 6-1 is a TEM image of Pt particles synthesized in example 5 of the present invention, and FIG. 6-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 5.
FIG. 7-1 is a TEM image of Pt particles synthesized in example 6 of the present invention, and FIG. 7-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 6.
Fig. 8 is a TEM image of Pt particles synthesized in example 7 of the present invention.
Fig. 9 is a TEM image of Pt particles synthesized in example 8 of the present invention.
Fig. 10 is a TEM image of Pt particles synthesized in example 9 of the present invention.
FIG. 11-1 is a TEM image of Pt particles synthesized in example 10 of the present invention, and FIG. 11-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 10.
FIG. 12-1 is a TEM image of Pt particles synthesized in example 11 of the present invention, and FIG. 12-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 11.
FIG. 13-1 is a TEM image of Pt particles synthesized in example 12 of the present invention, and FIG. 13-2 is a distribution diagram of the particle diameters of Pt particles synthesized in example 12.
Detailed Description
The invention will be further illustrated by the following description and examples, which include but are not limited to the following examples.
As shown in figure 1, the invention provides a preparation method of Pt nano particles, which uses glycol as a reducing agent and adopts a solvothermal synthesis method to reduce chloroplatinic acid to obtain nano-scale Pt particles.
The preparation method comprises the following steps: and adding the chloroplatinic acid solution into ethylene glycol, performing ultrasonic dispersion, adjusting the pH value of the mixed solution, and then performing heating reaction to obtain nano-scale Pt particles.
The concentration of the chloroplatinic acid solution is 0.01mol/l to 0.1mol/l.
Specifically, 0.01mmol of chloroplatinic acid solution is taken and added to 8-20 ml of ethylene glycol.
Dispersing chloroplatinic acid solution and ethylene glycol under ultrasonic condition.
The ultrasonic dispersion time is 15-60min.
The PH value of the mixed solution is regulated to 9-10.
And pouring the dispersed mixed solution with the pH value adjusted into a high-pressure reaction kettle, and then placing the high-pressure reaction kettle into an oven for heating reaction.
The reaction kettle is placed in an oven with the temperature of 150-190 ℃ and heated for reaction for 30-120 min.
The preparation method of the Pt nano particles comprises the following steps:
step 1, preparing a chloroplatinic acid solution: weighing a proper amount of chloroplatinic acid crystals, adding the chloroplatinic acid crystals into a proper amount of ultrapure water, stirring until the chloroplatinic acid crystals are completely dissolved, preparing a chloroplatinic acid solution with the concentration of 0.01mol/l to 0.1mol/l, and filling the solution into a brown bottle for standby;
step 2, measuring a chloroplatinic acid solution, putting the chloroplatinic acid solution into a container with measured ethylene glycol, and putting the container with two liquids into an ultrasonic cleaner for ultrasonic dispersion;
step 3, gradually dripping sodium hydroxide solution into the ultrasonic dispersion mixed solution, and adjusting the pH value of the mixed solution to 9-10;
step 4, pouring the dispersed mixed solution with the pH value adjusted into a high-pressure reaction kettle, and placing the mixed solution into an oven for heating reaction;
and 5, stopping the reaction, taking out the reaction kettle, and naturally cooling to room temperature.
The Pt nano particles prepared by the preparation method are prepared by the preparation method.
The technical effects of the invention are illustrated below in several test cases. The test cases used chloroplatinic acid solutions with concentrations of 0.02mol/l and 0.05 mol/l. The same applies to the use of a chloroplatinic acid solution having a concentration of 0.01mol/l to 0.1mol/l.
Example 1
The embodiment discloses a preparation method of Pt nano particles, which comprises the following steps:
preparing a chloroplatinic acid solution: preparing a chloroplatinic acid solution by chloroplatinic acid crystals and deionized water, weighing 2.0g chloroplatinic acid crystals and 192.6ml deionized water, preparing 0.02mol/l chloroplatinic acid solution, and filling the prepared chloroplatinic acid solution in a brown bottle for later use.
Mixing and dispersing chloroplatinic acid and ethylene glycol solution: weighing 12ml of ethylene glycol solution, and pouring into a glass container; measuring 0.5ml of chloroplatinic acid solution with the concentration of 0.02mol/l by a liquid-transferring gun, and pouring the solution into the same glass container; placing the glass container with the two liquids into an ultrasonic cleaner for ultrasonic dispersion for 30min; in the ultrasonic dispersion process, 1mol/l sodium hydroxide solution is added dropwise into the mixed solution, and the pH value of the mixed solution is regulated to be about 10.
Solvothermal synthesis of Pt nanoparticles: pouring the ultrasonic dispersion mixed solution with the pH value adjusted into a high-pressure reaction kettle, screwing the reaction kettle, and placing the reaction kettle in a 180 ℃ oven for reaction; stopping the reaction after 30min, taking out the reaction kettle, and naturally cooling to room temperature.
The liquid after synthesis was measured by a pipette, and then 1ml of absolute ethanol was added, and after mixing, the mixture was subjected to ultrasonic dispersion for 10 minutes, and a small amount of the dispersed liquid was dropped on an ultra-thin carbon film dedicated to transmission electron microscope analysis, and after air-drying, the analysis was performed, and the results of the partial analysis were shown in fig. 2. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.06nm.
Examples 2-12 disclose a method of preparing Pt nanoparticles, differing from example 1 in that: the concentration and the dosage of the chloroplatinic acid solution are different, the dosage of the ethylene glycol is different, and the heating temperature and the heating time are different; the remaining conditions were the same.
Example 2
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 14ml; the reaction was carried out in an oven at 180℃for 30min.
The results of a part of the analysis of this example are shown in fig. 3. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.31nm.
Example 3
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 170℃for 30min.
The results of a part of the analysis of this example are shown in fig. 4. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.48nm.
Example 4
The concentration of the chloroplatinic acid solution is 0.05mol/l, and the dosage is 0.2ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 180℃for 30min.
The results of a part of the analysis of this example are shown in fig. 5. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.29nm.
Example 5
The concentration of the chloroplatinic acid solution is 0.1mol/l, and the dosage is 0.1ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 180℃for 30min.
The results of a part of the analysis of this example are shown in fig. 6. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.28nm.
Example 6
The concentration of the chloroplatinic acid solution is 0.001mol/l, and the dosage is 10ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 180℃for 30min.
The results of a part of the analysis of this example are shown in fig. 7. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.47nm.
Example 7
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 8ml; the reaction was carried out in an oven at 180℃for 30min.
The results of a part of the analysis of this example are shown in fig. 8. It can be seen that the Pt nanoparticles thermally synthesized using ethylene glycol to reduce chloroplatinic acid solvent were 1-2nm in size.
Example 8
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 20ml; the reaction was carried out in an oven at 180℃for 30min.
The results of partial analysis of this example are shown in fig. 9. It can be seen that the Pt nanoparticles thermally synthesized using ethylene glycol to reduce chloroplatinic acid solvent were 1-2nm in size.
Example 9
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 150℃for 30min.
The results of partial analysis of this example are shown in fig. 10. It can be seen that the Pt nanoparticles thermally synthesized using ethylene glycol to reduce chloroplatinic acid solvent were 1-2nm in size.
Example 10
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 190℃for 30min.
The results of partial analysis of this example are shown in fig. 11. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.27nm.
Example 11
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 180℃for 60min.
The results of partial analysis of this example are shown in fig. 12. It can be seen that the Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent were 1-1.27nm in size.
Example 12
The concentration of the chloroplatinic acid solution is 0.02mol/l, and the dosage is 0.5ml; the dosage of the glycol solution is 12ml; the reaction was carried out in an oven at 180℃for 120min.
The results of partial analysis of this example are shown in fig. 13. It can be seen that the average size of Pt nanoparticles thermally synthesized using ethylene glycol reduced chloroplatinic acid solvent was 1.54nm.
According to the invention, nano-scale Pt particles can be obtained through reactions of chloroplatinic acid solutions with different concentrations and dosages, ethylene glycol with different volumes, different temperatures and different times. The method has the advantages of simple operation, low requirements on raw materials and equipment, environmental friendliness and good repeatability and selectivity, and is particularly suitable for preparing the nano noble metal catalyst.
The above embodiment is only one of the preferred embodiments of the present invention, and should not be used to limit the scope of the present invention, and all the modifications or color changes that are not significant in the spirit and scope of the main body design of the present invention are still consistent with the present invention.
Claims (2)
1. The preparation method of the Pt nano particle is characterized in that ethylene glycol is used as a reducing agent and a protecting agent, and a solvent thermal synthesis method is adopted to reduce chloroplatinic acid, so that Pt particles with the size of 1-2nm are obtained; the method comprises the following steps:
step 1, preparing a chloroplatinic acid solution: weighing a proper amount of chloroplatinic acid crystals, adding the chloroplatinic acid crystals into a proper amount of ultrapure water, stirring until the chloroplatinic acid crystals are completely dissolved, preparing a chloroplatinic acid solution with the concentration of 0.01mol/l to 0.1mol/l, and filling the solution into a brown bottle for standby;
step 2, measuring chloroplatinic acid solution, putting the chloroplatinic acid solution into a measured ethylene glycol container, and putting the container with two liquids into an ultrasonic cleaner for ultrasonic dispersion;
step 3, gradually dripping sodium hydroxide solution into the ultrasonic dispersion mixed solution, and adjusting the pH value of the mixed solution to 9-10;
step 4, pouring the dispersed mixed solution with the pH value adjusted into a high-pressure reaction kettle, and placing the mixed solution into an oven for heating reaction;
stopping the reaction, taking out the reaction kettle, and naturally cooling to room temperature;
adding 0.1-10 ml of chloroplatinic acid solution into 8-20 ml ethylene glycol;
and placing the reaction kettle in an oven at 150-190 ℃ for heating reaction for 30-120 min.
2. Pt nanoparticles produced by the method of claim 1.
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| CN101269417A (en) * | 2008-05-08 | 2008-09-24 | 郴州高鑫铂业有限公司 | Method for manufacturing nano-platinum powder |
| CN108817416A (en) * | 2018-07-06 | 2018-11-16 | 中国科学院大连化学物理研究所 | A kind of preparation method and application of Pt nanoparticle |
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| DE10037071A1 (en) * | 2000-07-29 | 2002-02-21 | Omg Ag & Co Kg | Precious metal nanoparticles, process for their production and use |
| US6686308B2 (en) * | 2001-12-03 | 2004-02-03 | 3M Innovative Properties Company | Supported nanoparticle catalyst |
| TWI298646B (en) * | 2005-12-28 | 2008-07-11 | Ind Tech Res Inst | Process for preparing platinum based electrode catalyst for use in direct methanol fuel cell |
| CN101497134A (en) * | 2008-01-30 | 2009-08-05 | 中国中化集团公司 | Method for preparing precious metal nanoparticle |
| US9550170B2 (en) * | 2012-04-10 | 2017-01-24 | Brookhaven Sciecne Associates, LLC | Synthesis of nanoparticles using ethanol |
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| CN101269417A (en) * | 2008-05-08 | 2008-09-24 | 郴州高鑫铂业有限公司 | Method for manufacturing nano-platinum powder |
| CN108817416A (en) * | 2018-07-06 | 2018-11-16 | 中国科学院大连化学物理研究所 | A kind of preparation method and application of Pt nanoparticle |
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