CN110327919B - Pt/C catalyst and preparation method thereof - Google Patents
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Abstract
The invention discloses a Pt/C catalyst and a preparation method thereof, wherein the preparation method comprises the following steps: carrying out plasma treatment on the carbon nano tube to obtain a pretreated carbon nano tube; dispersing the obtained pretreated carbon nano tube in polydiallyldimethylammonium chloride and sodium chloride aqueous solution, ultrasonically dispersing, stirring and uniformly mixing, then washing with deionized water, and drying to obtain a functionalized carbon nano tube; adding the functionalized carbon nano tube into a dispersing agent to obtain a carbon nano tube dispersion liquid, performing ultrasonic dispersion, then adding chloroplatinic acid, and performing ultrasonic dispersion again to obtain a spray pyrolysis precursor dispersion liquid; and atomizing the obtained spray pyrolysis precursor dispersion liquid, and conveying the dispersion liquid to a pyrolysis furnace through carrier gas for thermal decomposition treatment to obtain Pt/C catalyst powder. The preparation method has the advantages of high process stability and repeatability, simple operation and automatic continuous large-scale production, and the obtained catalyst active component particles are uniformly distributed.
Description
Technical Field
The invention relates to the technical field of catalytic synthesis, in particular to a Pt/C catalyst and a preparation method thereof.
Background
A platinum-carbon catalyst (Pt/C) is a catalyst in which platinum is supported on a carbon support, and has been widely used in the fields of proton exchange membrane fuel cells, direct alcohol fuel cells, hydrogen production by electrolysis of water, catalytic hydrogenation/dehydrogenation reactions of various compounds, and the like.
Currently, the most effective and most commonly used catalyst in the above fields is still the Pt/C catalyst, and the preparation process thereof mainly includes the conventional chemical reduction method, the precipitation conversion method, the microwave method, and the like. On one hand, the method has the defects of complex process, poor repeatability of the catalyst, uneven distribution of active component particles of the prepared catalyst on a carrier and the like; on the other hand, the method has complex operation and long production period, and is difficult to realize large-scale mass production to a certain extent.
Therefore, it is very important to find a catalyst preparation method which has high process stability and repeatability, is simple to operate, can be produced automatically and continuously in large scale and has uniform active component particle distribution.
Disclosure of Invention
The invention mainly aims to provide a Pt/C catalyst and a preparation method thereof, the preparation method has high process stability and repeatability, is simple to operate, can realize automatic continuous large-scale production, and the obtained catalyst has uniform active component particle distribution.
In order to achieve the above object, according to one aspect of the present invention, there is provided a preparation method of a Pt/C catalyst, the preparation method including the steps of:
(1) carrying out plasma treatment on the carbon nano tube to obtain a pretreated carbon nano tube;
(2) dispersing the pretreated carbon nano tube obtained in the step (1) in polydiallyldimethylammonium chloride and sodium chloride aqueous solution, ultrasonically dispersing, stirring and uniformly mixing, then washing with deionized water, and drying to obtain a functionalized carbon nano tube;
(3) adding the functionalized carbon nano tube obtained in the step (2) into a dispersing agent to obtain a carbon nano tube dispersion liquid, performing ultrasonic dispersion, then adding chloroplatinic acid, and performing ultrasonic dispersion again to obtain a spray pyrolysis precursor dispersion liquid;
(4) and (4) atomizing the spray pyrolysis precursor dispersion liquid obtained in the step (3), and conveying the dispersion liquid to a pyrolysis furnace through carrier gas for thermal decomposition treatment to obtain Pt/C catalyst powder.
Further, in the step (1), the plasma treatment specifically means: the carbon nano tube is processed by plasma under the atmosphere of air or oxygen, wherein, the gas flow is 4-8sccm, the processing time is 20-40min, and the plasma processing power is 100-250W.
Further, in the step (1), the outer diameter of the carbon nanotube ranges from 10 nm to 100 nm.
Further, in the step (2), in the polydiallyldimethylammonium chloride and the sodium chloride aqueous solution, the mass percentage of the polydiallyldimethylammonium chloride is 0.05-0.10 wt%, the mass percentage of the sodium chloride is 0.05-0.10 wt%, and the molecular weight of the polydiallyldimethylammonium chloride is 100000-200000.
Further, in the step (2), the weight ratio of the pretreated carbon nano tubes to the polydiallyldimethylammonium chloride and sodium chloride aqueous solution is 1: 4.
further, in the step (3), the dispersing agent is one or more of deionized water, absolute ethyl alcohol, methanol and isopropanol; the content of the carbon nano-tube in the carbon nano-tube dispersion liquid is 0.20-0.80 mg/mL.
Further, in the step (3), the amount of chloroplatinic acid added relative to the dispersant was 0.00537-1.41 mg/mL.
Further, in the step (4), the atomization treatment is ultrasonic spray treatment or air compression spray treatment; the carrier gas used in the atomization treatment process is 5-10% hydrogen/argon mixed gas, and the partial pressure of the carrier gas is 0.10-0.14 MPa.
Further, in the step (4), the temperature range of the thermal decomposition treatment is 300-500 ℃, and the uniform heating rate is 5-10 ℃/min.
According to another aspect of the present invention, there is provided a Pt/C catalyst prepared by the above-described preparation method.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the preparation method, the carbon nano tube is subjected to plasma pretreatment, so that oxygen-containing functional groups on the surface of the carbon nano tube are increased, the carbon nano tube becomes more hydrophilic, and the complete morphology structure of the carbon nano tube is effectively reserved; the poly (diallyldimethylammonium chloride) can be wound on the surface of the carbon nanotube in a non-covalent manner through the charge effect, and the sodium chloride can promote the functionalization of the poly (diallyldimethylammonium chloride) on the carbon nanotube, so that the obtained carbon nanotube can be used for loading noble metal Pt more easily, and the dispersion uniformity of the Pt on the carbon nanotube is ensured;
(2) in the preparation method, all the raw materials react in a dispersion state, so that the uniformity of reaction components is ensured, and the utilization rate of the raw materials is high;
(3) the preparation method of the invention adopts the spray pyrolysis method to prepare the Pt/C catalyst, has simple and reliable process, does not need expensive large-scale instruments, saves the cost, has high production efficiency and is easy to realize automatic continuous large-scale production.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of a Pt/C catalyst prepared in example 1 of the present invention.
FIG. 2 is a Scanning Electron Micrograph (SEM) of a Pt/C catalyst prepared according to example 1 of the present invention.
FIG. 3 is a Transmission Electron Micrograph (TEM) of a Pt/C catalyst prepared according to example 1 of the present invention.
FIG. 4 is a high resolution transmission electron micrograph (HR-TEM) of a Pt/C catalyst prepared according to example 1 of the present invention.
FIG. 5 is an element distribution image (elementary mapping images) of the Pt/C catalyst prepared in example 1 of the present invention.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments described below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
a preparation method of the Pt/C catalyst comprises the following steps:
(1) weighing 200 parts by weight of carbon nano tube with the outer diameter of 20-40nm, and treating the carbon nano tube with oxygen plasma for 30min (the oxygen flow is 5sccm, and the power is 200W) to obtain a pretreated carbon nano tube;
(2) weighing 100 parts by weight of pretreated carbon nano tube, dispersing the carbon nano tube in 400 parts by weight of poly (diallyldimethylammonium chloride) and sodium chloride aqueous solution (wherein the molecular weight of the poly (diallyldimethylammonium chloride) is 100000-200000, the mass percentage content of the poly (diallyldimethylammonium chloride) is 0.05 wt%, and the mass percentage content of the sodium chloride is 0.10 wt%), dispersing the carbon nano tube for 60min by ultrasonic waves, stirring the mixture for 12h by using a magnetic stirrer, repeatedly washing the mixture for 6 times by using deionized water in a glass sand core funnel, and finally drying the mixture in a 60 ℃ vacuum drying box for 12h to obtain a functionalized carbon nano tube for later use;
(3) adding the functionalized carbon nano tube into 240000 parts by weight of absolute ethyl alcohol to obtain carbon nano tube dispersion liquid, ultrasonically dispersing the carbon nano tube dispersion liquid for 30min, and then adding 0.23mg/mL (relative to a dispersing agent) of chloroplatinic acid (H)2PtCl6·6H2O), ultrasonically dispersing for 30min to obtain a spray pyrolysis precursor dispersion liquid;
(4) and when the temperature of the pyrolysis furnace is uniformly increased to 400 ℃ (the temperature increase rate is 10 ℃/min), opening an atomization switch to atomize and spray the dispersion liquid of the spray pyrolysis precursor into the pyrolysis furnace, carrying out the spray pyrolysis process (the used carrier gas is 5% hydrogen/argon mixed gas by volume percentage, the partial pressure is 0.12MPa), and collecting the 20% Pt/C catalyst after the process is finished.
FIG. 1 is an X-ray diffraction pattern of the obtained Pt/C catalyst, from which it can be seen that the Pt/C catalyst was successfully prepared; FIG. 2 is a scanning electron micrograph of the Pt/C catalyst, from which it can be seen that the carbon nanotubes retain the intact morphology; FIG. 3 is a transmission electron micrograph of the Pt/C catalyst obtained, from which it can be seen that Pt nanoparticles are very uniformly distributed on the carbon nanotube support with an average size of 2-3 nm; FIG. 4 is a high resolution transmission electron micrograph of the Pt/C catalyst obtained, from which it can be seen that the surface lattice of the Pt nanoparticles corresponds to its 111 crystal plane; fig. 5 is an element distribution image of the obtained Pt/C catalyst, and it can be seen from the image that Pt nanoparticles are distributed on a carbon nanotube carrier very uniformly without agglomeration.
Example 2:
a preparation method of the Pt/C catalyst comprises the following steps:
(1) weighing 200 parts by weight of carbon nano tube with the outer diameter of 60-100nm, and treating the carbon nano tube for 20min by using oxygen plasma (the oxygen flow is 8sccm, and the power is 250W) to obtain a pretreated carbon nano tube;
(2) weighing 100 parts by weight of pretreated carbon nano tube, dispersing the carbon nano tube in 400 parts by weight of poly (diallyldimethylammonium chloride) and sodium chloride aqueous solution (wherein the molecular weight of the poly (diallyldimethylammonium chloride) is 100000-200000, the mass percentage content of the poly (diallyldimethylammonium chloride) is 0.06 wt%, and the mass percentage content of the sodium chloride is 0.07 wt%), dispersing the carbon nano tube for 60min by ultrasonic waves, stirring the mixture for 12h by using a magnetic stirrer, repeatedly washing the mixture for 7 times by using deionized water in a glass sand core funnel, and finally drying the mixture in a vacuum drying box at 60 ℃ for 12h to obtain a functionalized carbon nano tube for later;
(3) adding the functionalized carbon nano tube into 500000 parts by weight of deionized water to obtain carbon nano tube dispersion liquid, ultrasonically dispersing the carbon nano tube dispersion liquid for 30min, and then adding 0.13mg/mL (relative to a dispersing agent) of chloroplatinic acid (H)2PtCl6·6H2O), ultrasonically dispersing for 30min to obtain a spray pyrolysis precursor dispersion liquid;
(4) and when the temperature of the pyrolysis furnace is uniformly increased to 300 ℃ (the temperature increase rate is 5 ℃/min), opening an atomization switch to atomize and spray the dispersion liquid of the spray pyrolysis precursor into the pyrolysis furnace, carrying out the spray pyrolysis process (the used carrier gas is 10% hydrogen/argon mixed gas by volume percentage, the partial pressure is 0.14MPa), and collecting the 20% Pt/C catalyst after the process is finished.
Example 3:
a preparation method of the Pt/C catalyst comprises the following steps:
(1) weighing 200 parts by weight of carbon nano tube with the outer diameter of 40-60nm, and treating the carbon nano tube for 40min by using oxygen plasma (the oxygen flow is 7sccm, and the power is 150W) to obtain a pretreated carbon nano tube;
(2) weighing 100 parts by weight of pretreated carbon nano tube, dispersing the carbon nano tube in 400 parts by weight of poly (diallyldimethylammonium chloride) and sodium chloride aqueous solution (wherein the molecular weight of the poly (diallyldimethylammonium chloride) is 100000-200000, the mass percentage content of the poly (diallyldimethylammonium chloride) is 0.07 wt%, and the mass percentage content of the sodium chloride is 0.09 wt%), dispersing the carbon nano tube for 60min by ultrasonic waves, stirring the mixture for 12h by using a magnetic stirrer, repeatedly washing the mixture for 9 times by using deionized water in a glass sand core funnel, and finally drying the mixture for 12h in a vacuum drying box at 60 ℃ to obtain a functionalized carbon nano tube for later;
(3) adding the functionalized carbon nano tube into 133334 weight parts of anhydrous methanol to obtain carbon nano tube dispersion liquid, ultrasonically dispersing the carbon nano tube dispersion liquid for 30min, and then adding 1.06mg/mL (relative to a dispersing agent) of chloroplatinic acid (H)2PtCl6·6H2O), ultrasonically dispersing for 30min to obtain a spray pyrolysis precursor dispersion liquid;
(4) and when the temperature of the pyrolysis furnace is uniformly increased to 450 ℃ (the temperature increase rate is 10 ℃/min), opening an atomization switch to atomize and spray the dispersion liquid of the spray pyrolysis precursor into the pyrolysis furnace, carrying out the spray pyrolysis process (the used carrier gas is 5% hydrogen/argon mixed gas by volume percentage, the partial pressure is 0.13MPa), and collecting the catalyst with the concentration of 40% Pt/C after the process is finished.
Example 4:
a preparation method of the Pt/C catalyst comprises the following steps:
(1) weighing 200 parts by weight of carbon nano tube with the outer diameter of 10-20nm, and treating the carbon nano tube for 30min by using oxygen plasma (the oxygen flow is 4sccm, and the power is 100W) to obtain a pretreated carbon nano tube;
(2) weighing 100 parts by weight of pretreated carbon nano tube, dispersing the carbon nano tube in 400 parts by weight of poly (diallyldimethylammonium chloride) and sodium chloride aqueous solution (wherein the molecular weight of the poly (diallyldimethylammonium chloride) is 100000-200000, the mass percentage content of the poly (diallyldimethylammonium chloride) is 0.10 wt%, and the mass percentage content of the sodium chloride is 0.05 wt%), dispersing the carbon nano tube for 60min by ultrasonic waves, stirring the mixture for 12h by using a magnetic stirrer, repeatedly washing the mixture for 10 times by using deionized water in a glass sand core funnel, and finally drying the mixture for 12h in a vacuum drying box at 60 ℃ to obtain a functionalized carbon nano tube for later;
(3) the functionalized carbon nanotubes were added to 98188 parts by weight of isopropyl alcohol to obtain a carbon nanotube dispersion, which was ultrasonically dispersed for 30min, followed by addition of 1.41mg/mL (relative to the dispersant) of chloroplatinic acid (H)2PtCl6·6H2O), ultrasonic dispersion for 30min to obtain spray pyrolysis precursor dispersionLiquid;
(4) and when the temperature of the pyrolysis furnace is uniformly increased to 500 ℃ (the temperature increase rate is 5 ℃/min), opening an atomization switch to atomize and spray the dispersion liquid of the spray pyrolysis precursor into the pyrolysis furnace, carrying out the spray pyrolysis process (the used carrier gas is 10% hydrogen/argon mixed gas by volume percentage, the partial pressure is 0.10MPa), and collecting the catalyst with the concentration of 40% Pt/C after the process is finished.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A preparation method of a Pt/C catalyst is characterized by comprising the following steps:
(1) carrying out plasma treatment on the carbon nano tube to obtain a pretreated carbon nano tube;
(2) dispersing the pretreated carbon nano tube obtained in the step (1) in polydiallyldimethylammonium chloride and sodium chloride aqueous solution, ultrasonically dispersing, stirring and uniformly mixing, then washing with deionized water, and drying to obtain a functionalized carbon nano tube;
(3) adding the functionalized carbon nano tube obtained in the step (2) into a dispersing agent to obtain a carbon nano tube dispersion liquid, performing ultrasonic dispersion, then adding chloroplatinic acid, and performing ultrasonic dispersion again to obtain a spray pyrolysis precursor dispersion liquid;
(4) atomizing the spray pyrolysis precursor dispersion liquid obtained in the step (3), and conveying the dispersion liquid to a pyrolysis furnace through carrier gas for thermal decomposition treatment to obtain Pt/C catalyst powder;
in the step (1), the plasma treatment specifically includes:
carrying out plasma treatment on the carbon nano tube in the air or oxygen atmosphere, wherein the gas flow is 4-8sccm, the treatment time is 20-40min, and the plasma treatment power is 100-;
in the step (1), the outer diameter range of the carbon nano tube is 10-100 nm;
in the step (4), the atomization treatment is ultrasonic spray treatment or air compression spray treatment; the carrier gas used in the atomization treatment process is 5-10% hydrogen/argon mixed gas, and the partial pressure of the carrier gas is 0.10-0.14 MPa;
in the step (4), the temperature range of the thermal decomposition treatment is 300-.
2. The method for preparing a Pt/C catalyst according to claim 1, wherein in the step (2), the mass percentage of the poly (diallyldimethylammonium chloride) and the mass percentage of the sodium chloride in the aqueous solution of poly (diallyldimethylammonium chloride) are 0.05-0.10 wt%, the mass percentage of the sodium chloride is 0.05-0.10 wt%, and the molecular weight of the poly (diallyldimethylammonium chloride) is 100000-200000.
3. The method for preparing a Pt/C catalyst according to claim 1, wherein in the step (2), the weight ratio of the pretreated carbon nanotubes to the polydiallyldimethylammonium chloride and the aqueous sodium chloride solution is 1: 4.
4. the method for preparing the Pt/C catalyst according to claim 1, wherein in the step (3), the dispersant is one or more of deionized water, absolute ethyl alcohol, methanol and isopropanol; the content of the carbon nano-tube in the carbon nano-tube dispersion liquid is 0.20-0.80 mg/mL.
5. The method for preparing a Pt/C catalyst according to claim 1, wherein the chloroplatinic acid is added in an amount of 0.00537-1.41mg/mL with respect to the dispersant in the step (3).
6. A Pt/C catalyst prepared by the preparation method according to any one of claims 1 to 5.
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