CN111682222A - Preparation method and catalytic application of Pt-CdS-nitrogen doped graphene quantum dot composite material - Google Patents
Preparation method and catalytic application of Pt-CdS-nitrogen doped graphene quantum dot composite material Download PDFInfo
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Abstract
The invention discloses a preparation method and catalytic application of a Pt-CdS-nitrogen doped graphene quantum dot composite material. The Pt-CdS-nitrogen doped graphene quantum dot composite material is prepared from soluble cadmium salt, thiourea, citric acid and urea serving as raw materials by a solvothermal method, is in a nanowire shape, is uniform in particle size distribution, has the advantages of being simple and convenient in process, low in cost, environment-friendly and free of pollution, and can be used for catalytic oxidation of alcohols.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a preparation method and catalytic application of a Pt-CdS-nitrogen doped graphene quantum dot composite material.
Background
With the continuous consumption of fossil fuels worldwide, excessive shortage of energy and deterioration of the environment will become key problems in the coming years. Therefore, it is a concern to seek an ideal alternative fuel and develop a new energy conversion device. Fuel cells, particularly Direct Alcohol Fuel Cells (DAFCs), have important values in solving the two problems of rational utilization of resources and environmental pollution control, which plague the sustainable development of national economy, due to the advantages of high energy density, low pollution emission, high energy conversion efficiency, and the like. Platinum-based catalysts are among the most effective catalysts recognized for electrocatalytic alcohol oxidation. However, the disadvantages of high price and susceptibility to intermediate poisoning limit their use. Typically, semiconductor materials are used as supports for depositing Pt to achieve high performance electrocatalysts. In addition, rational design and combination of semiconductors can efficiently facilitate Photoelectrochemical (PEC) catalytic processes. By means of light irradiation, the semiconductor is excited and electron-hole pairs are generated, thereby significantly improving the catalytic activity of the metal/semiconductor catalyst and the oxidizing ability of the alcohol. Cadmium sulfide (CdS) nanowires are typical one-dimensional (1D) semiconductor materials with large surface areas, have excellent electron transmission capacity and narrow band gaps, and are widely used for photoelectrocatalytic oxidation of alcohol. However, the application of pure cadmium sulfide nanowires is severely hampered by the rapid recombination of electron-hole pairs and poor resistance to photo-corrosion. Therefore, the metal-free carbon material and CdS are used as a support of the noble metal to improve the catalytic performance. Graphene Quantum Dots (GQDs) are a novel zero-dimensional (0D) carbon nanomaterial consisting of several layers of graphene having small dimensions, and are mainly used as photosensitizers integrated with semiconductors, and can improve photoresponse by reducing photocatalytic intensity. Since GQDs have excellent conductivity, it can be used not only as a photoelectron sensitizer but also as an electron transfer mediator, allowing rapid electron transfer and causing efficient electron-hole separation, thereby improving catalytic performance. Therefore, the development of CdS/N-GQDs nano-structure to support Pt NPs to construct Pt-CdS/N-GQDs electrode material for the catalytic oxidation of alcohols has become one of the hot points of research.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a Pt-CdS-nitrogen doped carbon quantum dot composite material with simple and convenient operation process, low cost, environmental protection, no pollution and photoresponse and application of the Pt-CdS-nitrogen doped carbon quantum dot composite material in catalytic oxidation of ethylene glycol.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a Pt-CdS-nitrogen doped carbon quantum dot composite material specifically comprises the following steps:
(1) weighing a proper amount of cadmium acetate and thiourea, ultrasonically dispersing the cadmium acetate and the thiourea in ethylenediamine to obtain a mixture solution, transferring the mixture solution to a 50mL high-pressure reaction kettle, reacting for 24-72 h at 150-200 ℃, naturally cooling to room temperature, centrifuging to separate precipitates, alternately washing the precipitates with ethanol and deionized water for three times, and carrying out vacuum drying on the precipitate sample in an oven overnight at 60 ℃ to obtain CdS nanowires;
(2) weighing a proper amount of Citric Acid (CA) and urea, dissolving the Citric Acid (CA) and the urea in 10mL of distilled water, stirring until a clear solution is obtained, transferring the clear solution to a 20mL high-pressure reaction kettle, reacting for 48 hours at 180 ℃, cooling to room temperature, adding absolute ethyl alcohol to generate a precipitate, centrifugally separating the precipitate, washing the precipitate for 3 times by using the absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain nitrogen-doped graphene quantum dots (N-GQDs), wherein the N-GQDs is abbreviated as N-GQDs, and an N-GQDs aqueous solution with the concentration of 5mg/mL is prepared for later use;
(3) weighing a proper amount of CdS nanowires prepared in the step (1), ultrasonically dispersing the CdS nanowires in distilled water, adding a proper amount of N-GQDs aqueous solution of 5mg/mL prepared in the step (2) in the ultrasonic dispersion process, magnetically stirring the solution for 0.5 to 2 hours to obtain a mixed solution, transferring the mixed solution to a reaction kettle for reacting for 2 to 8 hours at 180 to 200 ℃, cooling the mixed solution to room temperature, centrifugally separating and precipitating the mixed solution, and drying the mixed solution in vacuum at 70 ℃ to obtain a CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as CdS/N-GQD;
(4) ultrasonically dispersing a proper amount of the CdS/N-GQDs composite material prepared in the step (3) in a mixed solvent of ethanol and water in a volume ratio of 1:1, adding a proper amount of chloroplatinic acid, ultrasonically treating for 30-60 min, transferring the mixture solution into a high-pressure reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, centrifugally separating and precipitating, and then performing vacuum drying at 60 ℃ to obtain a Pt-CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as Pt-CdS/N-GQDs composite material.
The chemical formula of the cadmium acetate is C4H6CdO4·H2O; the chemical formula of the thiourea is CH4N2S；
The chemical formula of the chloroplatinic acid is H2PtCl6；
The substances or solvents involved in the reaction are all chemically pure.
Furthermore, the invention also provides the application of the Pt-CdS-nitrogen doped graphene quantum dot composite material, and the composite material is used as a working electrode and has good electrocatalytic activity on ethylene glycol.
Compared with the prior art, the invention has the following advantages:
the Pt-CdS/N-GQDs composite material is successfully constructed by a solvothermal method; the shape of the composite material prepared by the method is in a nano-line shape, and the particle size distribution is uniform; cheap soluble cadmium salt, thiourea, citric acid and urea are used as raw materials, so that the use amount and cost of noble metal are reduced; the method has the advantages of simple and convenient operation process, low cost, environmental protection and no pollution, and can be used for the research of the catalytic oxidation of alcohols.
Drawings
FIG. 1 is a TEM image of N-GQDs obtained in example 1 of the present invention.
FIG. 2 is a TEM image of CdS/N-GQDs composite material prepared by example 1 of the present invention.
FIG. 3 is a TEM image of the Pt-CdS/N-GQDs composite material prepared by example 1 of the present invention.
FIG. 4 shows diffraction peaks of CdS/N-GQDs composite material and Pt-CdS/N-GQDs composite material prepared in example 1.
FIG. 5 is a cyclic voltammetry curve of the Pt-CdS/N-GQDs composite material prepared in example 1 of the present invention as a working electrode in a 1.0M ethylene glycol +1.0M potassium hydroxide solution.
Detailed Description
The present invention is further described in detail with reference to the following examples, and the technical solution of the present invention is not limited to the specific embodiments listed below, but includes any combination of the specific embodiments.
Example 1
(1) 2.0mmol (0.497g) of cadmium acetate (C) was weighed4H6CdO4·H2O) and 2.0mmol (0.152g) of thiourea (CH)4N2S), ultrasonically dispersing the solution in 40mL of ethylenediamine to obtain a mixture solution, transferring the mixture solution to a 50mL high-pressure reaction kettle, reacting for 72 hours at 180 ℃, naturally cooling to room temperature, centrifugally separating precipitates, alternately washing with ethanol and deionized water for three times, and carrying out vacuum drying on the precipitate sample in an oven at 60 ℃ overnight to obtain CdS nanowires;
(2) 2.0mmol (0.384g) of Citric Acid (Citric Acid is abbreviated as CA and the molecular formula is C6H8O7) And 6.0mmol (0.36g) of Urea (CH)4N2O) dissolving in 10mL of deionized water, stirring for 30min to obtain a clear solution, transferring the solution to a 20mL high-pressure reaction kettle, reacting for 48h at 180 ℃, cooling to room temperature, adding absolute ethyl alcohol to generate a precipitate, centrifugally separating the precipitate, washing the precipitate for 3 times by using the absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain nitrogen-doped graphene quantum dots (N-GQDs), and preparing an N-GQDs aqueous solution with the concentration of 5mg/mL for later use;
(3) weighing 50mg of CdS nanowires prepared in the step (1), dispersing into 10mL of deionized water, performing ultrasonic treatment for 30min, adding 10mL of N-GQDs aqueous solution with the concentration of 5mg/mL prepared in the step (2), continuously stirring for 30min to obtain a mixture solution, transferring the mixture solution into a 50mL high-pressure reaction kettle, heating and reacting for 8h at 180 ℃, cooling to room temperature, performing centrifugal separation and precipitation, and performing vacuum drying on a precipitation sample in an oven at 70 ℃ to obtain a CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as CdS/N-GQDs;
(4) ultrasonically dispersing 20mg of the CdS/N-GQDs composite material prepared in the step (3) into 20mL of mixed solvent of ethanol and water with the volume ratio of 1:1, and then adding 0.66mL of mixed solvent with the concentration of 3.8 × 10-2H of M2PtCl6Ultrasonically stirring the aqueous solution for 1h, transferring the mixture solution into a 25mL high-pressure reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, centrifugally separating the precipitate, and drying in vacuum at 60 DEG CAnd drying to obtain the Pt-CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as Pt-CdS/N-GQDs.
The morphology of the N-GQDs of the nitrogen-doped graphene quantum dots prepared in the example 1 is observed by using a TEM (transmission electron microscope), and the result shows that the prepared quantum dots are uniform in size (figure 1); the appearance of the CdS/N-GQDs composite material prepared in the example 1 is observed by using a TEM (transmission electron microscope), and the result shows that CdS is in a nano-line shape (figure 2); the morphology of the Pt-CdS/N-GQDs composite material is observed by using a TEM (transmission electron microscope), and the result shows that Pt nano particles are uniformly dispersed on the surface of a CdS nano wire (figure 3); the composition structure of the prepared composite material is tested by X-ray powder diffraction (XRD), in figure 4, a is the diffraction peak of CdS/N-GQDs composite material, and b is the diffraction peak of Pt-CdS/N-GQDs composite material.
Catalytic Oxidation study of ethylene glycol Using the Compound prepared in example 1
Weighing 2mg of prepared Pt-CdS-nitrogen doped graphene quantum dot composite material, adding the Pt-CdS-nitrogen doped graphene quantum dot composite material into a mixed solution (5 wt%) of 0.5mL of ethanol, 0.5mL of distilled water and 20 mu L of perfluorosulfonic acid, performing ultrasonic treatment for 1h to form a uniform dispersion liquid, coating the dispersion liquid on the surface of a pre-polished glassy carbon electrode (L-GCE), and drying to obtain an electrode with the surface attached with the Pt-CdS-nitrogen doped graphene quantum dot composite material, namely a Pt-CdS-nitrogen doped graphene quantum dot composite material electrode, which is abbreviated as a Pt-CdS/N-GQDs electrode; preparing a Pt-CdS electrode by the same method;
FIG. 5 is a cyclic voltammetry curve of the prepared Pt-CdS/N-GQDs composite material as a working electrode for catalytic oxidation of ethylene glycol in a 1.0M ethylene glycol +1.0M potassium hydroxide solution.
The specific experimental steps are as follows: in a three-electrode system, a platinum wire electrode is used as a counter electrode, a calomel electrode is used as a reference electrode, a prepared Pt-CdS/N-GQDs electrode or Pt-CdS electrode is used as a working electrode, a 1.0M glycol +1.0M KOH solution is used as a supporting electrolyte solution, an electrochemical workstation is used as a detection instrument, and current-voltage scanning is carried out by means of cyclic voltammetry, wherein the parameters of the cyclic voltammetry are as follows: the potential range is-0.7V to 0.2V, and the scanning rate is 50mV s-1. The cyclic voltammogram shown in fig. 5 was obtained based on the above procedure.
From FIG. 5, two characteristic oxidation peaks of ethylene glycol were observed in the forward scan curve (about-0.2V) and the reverse scan curve (about-0.3V). The positive sweep is due to the direct oxidation of ethylene glycol to carbon dioxide and water, and its peak current density (i) is usedp) To evaluate the catalytic performance of the electrode on ethylene glycol, a larger peak current density indicates a higher catalytic activity. Peak Current Density ip (1053mA mg of GQDs) for Pt-CdS/N-GQDs electrodes under dark conditions-1) The peak current density is obviously higher than that of the Pt-CdS electrode under the dark condition (179mA mg)-1) It shows that the Pt-CdS/N-GQDs electrode has high electrocatalytic activity. Under the condition of visible light irradiation, the peak current density of the Pt-CdS/N-GQDs electrode is 2415mA mg-1Is 8.1 times the peak current density of the Pt-CdS electrode. Experimental test results show that the Pt-CdS/N-GQDs composite material has good electrocatalytic activity on ethylene glycol as a working electrode, and has wide application in the aspect of catalytic oxidation of ethylene glycol.
Example 2
(1) 1.0mmol (0.248g) of cadmium acetate (C) was weighed4H6CdO4·H2O) and 1.0mmol (0.076g) of thiourea (CH)4N2S), ultrasonically dispersing the solution in 40mL of ethylenediamine to obtain a mixture solution, transferring the mixture solution to a 50mL high-pressure reaction kettle, reacting for 24 hours at 200 ℃, naturally cooling to room temperature, centrifugally separating precipitates, alternately washing with ethanol and deionized water for three times, and carrying out vacuum drying on the precipitate sample in an oven at 60 ℃ overnight to obtain CdS nanowires;
(2) dissolving 1.0mmol (0.192g) of citric acid and 3.0mmol (0.18g) of urea in 10mL of deionized water, stirring for 30min to obtain a clear solution, transferring the solution to a 20mL high-pressure reaction kettle, reacting for 48h at 180 ℃, cooling to room temperature, adding absolute ethyl alcohol to generate precipitate, centrifugally separating the precipitate, washing the precipitate for 3 times with absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain nitrogen-doped graphene quantum dots, which are abbreviated as N-GQDs, and preparing an N-GQDs aqueous solution with the concentration of 5mg/mL for later use;
(3) weighing 50mg of CdS nanowires prepared in the step (1), dispersing into 10mL of deionized water, performing ultrasonic treatment for 30min, adding 10mL of N-GQDs aqueous solution with the concentration of 5mg/mL prepared in the step (2), continuously stirring for 2h to obtain a mixed solution, transferring the mixed solution into a 50mL high-pressure reaction kettle, heating to react for 2h at 200 ℃, cooling to room temperature, performing centrifugal separation on precipitates, and performing vacuum drying on the precipitate sample in an oven at 70 ℃ to obtain a CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as CdS/N-GQDs;
(4) ultrasonically dispersing 20mg of the CdS/N-GQDs composite material prepared in the step (3) into 20mL of mixed solvent of ethanol and water with the volume ratio of 1:1, and then adding 0.66mL of mixed solvent with the concentration of 3.8 × 10-2H of M2PtCl6And ultrasonically stirring the aqueous solution for 30min, transferring the mixture solution into a 25mL high-pressure reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, centrifugally separating and precipitating, and drying in vacuum at 60 ℃ to obtain the Pt-CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as Pt-CdS/N-GQDs composite material.
Observing the appearance of the prepared nitrogen-doped graphene quantum dots N-GQDs by using a TEM (transmission electron microscope); observing the appearance of the prepared CdS/N-GQDs composite material by using a TEM; observing the appearance of the Pt-CdS/N-GQDs composite material by using a TEM; the compositional structure of the prepared composite was tested by X-ray powder diffraction (XRD). The prepared Pt-CdS/N-GQDs composite material is used as a working electrode to perform an experimental test of catalytic oxidation of ethylene glycol.
Example 3
(1) 2.0mmol (0.497g) of cadmium acetate (C) was weighed4H6CdO4·H2O) and 2.0mmol (0.152g) of thiourea (CH)4N2S), ultrasonically dispersing the solution in 40mL of ethylenediamine to obtain a mixture solution, transferring the mixture solution to a 50mL high-pressure reaction kettle, reacting for 60 hours at 150 ℃, naturally cooling to room temperature, centrifugally separating precipitates, alternately washing with ethanol and deionized water for three times, and carrying out vacuum drying on the precipitate sample in an oven at 60 ℃ overnight to obtain the CdS nanowire;
(2) dissolving 2.0mmol (0.384g) of citric acid and 6.0mmol (0.36g) of urea in 10mL of deionized water, stirring for 30min to obtain a clear solution, transferring the solution to a 20mL high-pressure reaction kettle, reacting at 180 ℃ for 48h, cooling to room temperature, adding absolute ethyl alcohol to generate precipitate, centrifugally separating the precipitate, washing the precipitate for 3 times with absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain nitrogen-doped graphene quantum dots, which are abbreviated as N-GQDs, and preparing an N-GQDs aqueous solution with the concentration of 5mg/mL for later use;
(3) weighing 50mg of CdS nanowires prepared in the step (1), dispersing into 10mL of deionized water, performing ultrasonic treatment for 30min, adding 10mL of N-GQDs aqueous solution with the concentration of 5mg/mL prepared in the step (2), continuously stirring for 60min to obtain a mixed solution, transferring the mixed solution into a 50mL high-pressure reaction kettle, heating to react for 4h at 190 ℃, cooling to room temperature, performing centrifugal separation on precipitates, and performing vacuum drying on the precipitate sample in an oven at 70 ℃ to obtain a CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as CdS/N-GQDs;
(4) ultrasonically dispersing 20mg of the CdS/N-GQDs composite material prepared in the step (3) into 20mL of mixed solvent of ethanol and water with the volume ratio of 1:1, and then adding 0.66mL of mixed solvent with the concentration of 3.8 × 10-2H of M2PtCl6And ultrasonically stirring the aqueous solution for 45min, transferring the mixture solution into a 25mL high-pressure reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, centrifugally separating and precipitating, and drying in vacuum at 60 ℃ to obtain the Pt-CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as Pt-CdS/N-GQDs composite material.
Observing the appearance of the prepared nitrogen-doped graphene quantum dots N-GQDs by using a TEM (transmission electron microscope); observing the appearance of the prepared CdS/N-GQDs composite material by using a TEM; observing the appearance of the Pt-CdS/N-GQDs composite material by using a TEM; the compositional structure of the prepared composite was tested by X-ray powder diffraction (XRD). The prepared Pt-CdS/N-GQDs composite material is used as a working electrode to perform an experimental test of catalytic oxidation of ethylene glycol.
Claims (2)
1. A preparation method of a Pt-CdS-nitrogen doped graphene quantum dot composite material is characterized by comprising the following steps of:
(1) weighing proper amount of cadmium acetate (C)4H6CdO4·H2O) and thiourea (CH)4N2S), ultrasonically dispersing in ethylenediamine to obtain a mixtureTransferring the mixture solution into a 50mL high-pressure reaction kettle, reacting for 24-72 h at 150-200 ℃, naturally cooling to room temperature, centrifugally separating precipitates, alternately washing the precipitates with ethanol and deionized water for three times, and carrying out vacuum drying on the precipitate sample in an oven at 60 ℃ overnight to obtain CdS nanowires;
(2) weighing a proper amount of citric acid and urea, dissolving the citric acid and urea in 10mL of distilled water, stirring to obtain a clear solution, transferring the clear solution to a 20mL high-pressure reaction kettle, reacting for 48 hours at 180 ℃, cooling to room temperature, adding absolute ethyl alcohol to generate a precipitate, centrifugally separating the precipitate, washing the precipitate for 3 times by using the absolute ethyl alcohol, and drying in vacuum at 80 ℃ to obtain nitrogen-doped graphene quantum dots (N-GQDs), wherein the N-GQDs are abbreviated as N-GQDs, and preparing an N-GQDs aqueous solution with the concentration of 5mg/mL for later use;
(3) weighing a proper amount of CdS nanowires prepared in the step (1), ultrasonically dispersing the CdS nanowires in distilled water, adding a proper amount of N-GQDs aqueous solution of 5mg/mL prepared in the step (2) in the ultrasonic dispersion process, magnetically stirring the solution for 0.5 to 2 hours to obtain a mixture solution, transferring the mixture solution to a reaction kettle for reaction at 180 to 200 ℃ for 2 to 8 hours, cooling the mixture solution to room temperature, centrifugally separating and precipitating the mixture solution, and drying the mixture solution in vacuum at 70 ℃ to obtain a CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as CdS/N-GQD composite material;
(4) ultrasonically dispersing a proper amount of the CdS/N-GQDs composite material prepared in the step (3) into a mixed solvent of ethanol and water with the volume ratio of 1:1, and then adding a proper amount of chloroplatinic acid (H)2PtCl6) And after ultrasonic treatment is carried out for 30-60 min, transferring the mixture solution into a high-pressure reaction kettle, reacting for 4h at 140 ℃, naturally cooling to room temperature, carrying out centrifugal separation and precipitation, and then carrying out vacuum drying at 60 ℃ to obtain the Pt-CdS-nitrogen doped graphene quantum dot composite material, which is abbreviated as Pt-CdS/N-GQDs composite material.
2. The catalytic use of the Pt-CdS-nitrogen doped graphene quantum dot composite material according to claim 1, wherein the composite material has good electrocatalytic activity on ethylene glycol as a working electrode.
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| CN113422055A (en) * | 2021-05-27 | 2021-09-21 | 复旦大学 | Lithium-philic graphene quantum dot/lithium composite material and preparation method and application thereof |
| CN114749149A (en) * | 2022-04-20 | 2022-07-15 | 广州全高环保科技有限公司 | Carbon material for formaldehyde purification and preparation method thereof |
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