CN114950411B - Noble metal monoatomic catalyst, preparation method thereof and application thereof in detection of ascorbic acid - Google Patents
Noble metal monoatomic catalyst, preparation method thereof and application thereof in detection of ascorbic acid Download PDFInfo
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Abstract
The application provides a noble metal single-atom catalyst, which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in the form of cationic species. Compared with commercial conductive carbon black, the noble metal monoatomic catalyst provided by the application has the advantages of obviously improved detection effect on ascorbic acid, high sensitivity, low detection limit, good selectivity and the like, and can meet the direct or indirect quantitative monitoring in biological sensing.
Description
Technical Field
The application belongs to the technical field of electrochemical sensing, and particularly relates to a noble metal monoatomic catalyst, a preparation method thereof and application thereof in detecting ascorbic acid.
Background
Ascorbic acid is an essential compound for normal operation of the organism, and can cause various diseases such as scurvy, osteoporosis, anorexia and the like when the content of the ascorbic acid is insufficient through diet intake, so that the detection of the content of the ascorbic acid in foods, medicines and even physiological environments of human bodies is particularly important. There are many effective means for detecting ascorbic acid reported at present, and spectrophotometry, fluorescence, capillary electrophoresis, high performance liquid chromatography, amperometric detection and the like are commonly used, wherein electrochemical methods are widely used due to the advantages of sensitive detection, simple equipment, strong portability, mild conditions and the like.
Under the condition of not depending on biomolecules such as enzymes, the electrochemical sensing technology still has the problems of narrow detection range, poor selectivity and the like, and the targeted design and development of a high-efficiency catalyst are important ways for coping with the challenges. The single-atom catalyst has high activity, high selectivity and 100% metal atom utilization rate, and has great application potential in the aspect of improving the biosensing performance. Meanwhile, with the gradual and deep research of the monoatomic catalyst, a universal synthesis method and a macro preparation process are reported, and support is provided for the expansion of practical application.
Disclosure of Invention
In view of the above, the technical problem to be solved by the present application is to provide a noble metal monoatomic catalyst, a preparation method thereof and an application thereof in detecting ascorbic acid, wherein the noble metal monoatomic catalyst provided by the present application can be used for electrode modification and exhibits excellent electrochemical sensing performance on ascorbic acid.
The application provides a noble metal single-atom catalyst, which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in the form of cationic species.
Preferably, the carbon support is selected from conductive carbon blacks.
Preferably, the conductive carbon black is selected from one of KJ600, BP2000, XC72 and N326.
Preferably, the noble metal element is selected from one of Ru, pd, au and Pt.
Preferably, the mass ratio of the noble metal element to the conductive carbon black is (1 to 1.5): 100.
The application also provides a preparation method of the noble metal monoatomic catalyst, which comprises the following steps:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
the conductive carbon black is ground, a noble metal solution is dropwise added into the conductive carbon black, and the solvent is volatilized after full grinding to obtain solid powder;
and carrying out heat treatment on the solid powder to obtain the noble metal monoatomic catalyst.
Preferably, the noble metal compound is selected from one of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid and platinum acetylacetonate;
the low-boiling point low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone;
the concentration of the noble metal compound when dissolved in the low-boiling point low-polarity solvent is 8-16 mg/mL.
Preferably, the heat treatment is performed under the inert atmosphere condition, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling point low-polarity solvent, and the time of the heat treatment is 12-16 h.
The application also provides application of the noble metal monoatomic catalyst in ascorbic acid detection.
Compared with the prior art, the application provides a noble metal single-atom catalyst which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are atomically dispersed on the surface of the carbon carrier in the form of cationic species. Compared with commercial conductive carbon black, the noble metal monoatomic catalyst provided by the application has the advantages of obviously improved detection effect on ascorbic acid, high sensitivity, low detection limit, good selectivity and the like, and can meet the direct or indirect quantitative monitoring in biological sensing.
Drawings
FIG. 1 is a scanning and transmission electron microscope image of Ru monoatoms, pd monoatoms, au monoatoms, pt monoatoms catalysts prepared in examples 1-4 of the present application;
FIG. 2 is an X-ray diffraction pattern of Ru monoatomic and Pd monoatomic catalysts prepared in examples 1-2 of the present application;
FIG. 3 is a spherical aberration correcting high angle annular dark field scanning transmission electron microscope image of the Ru monoatomic catalyst prepared according to example 1 of the present application;
FIG. 4 is an X-ray near side absorption structure spectrum and an extended side X-ray absorption fine structure spectrum of Ru monoatomic catalyst and Pd monoatomic catalyst prepared in examples 1-2 of the present application;
FIG. 5 is a graph showing the comparison of the performance of the Ru monoatomic and Pd monoatomic catalysts prepared in examples 1-2 of the present application with the performance of the original commercial conductive carbon black for detecting ascorbic acid;
FIG. 6 shows the selectivity of the Ru monoatomic and Pd monoatomic catalysts prepared in examples 1-2 of the present application to ascorbic acid and interfering substances.
Detailed Description
The application provides a noble metal single-atom catalyst, which consists of a carbon carrier and noble metal elements, wherein noble metal atoms are dispersed on the surface of the carbon carrier in the form of cationic species.
Wherein the carbon support is selected from conductive carbon black. The conductive carbon black is a commercial conductive carbon black. In some embodiments of the application, the conductive carbon black is selected from one of KJ600, BP2000, XC72, and N326.
The noble metal element is selected from one of Ru, pd, au and Pt, preferably one of Ru and Pd.
The mass ratio of the noble metal element to the conductive carbon black is (1-1.5): 100, preferably 1:100, 1.1:100, 1.2:100, 1.3:100, 1.4:100, 1.5:100, or any value between (1-1.5): 100.
The application also provides a preparation method of the noble metal monoatomic catalyst, which comprises the following steps:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
the conductive carbon black is ground, a noble metal solution is dropwise added into the conductive carbon black, and the solvent is volatilized after full grinding to obtain solid powder;
and carrying out heat treatment on the solid powder to obtain the noble metal monoatomic catalyst.
Specifically, the application dissolves noble metal compound in low-boiling point low-polarity solvent to obtain noble metal solution.
The noble metal compound is selected from one of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid and platinum acetylacetonate, preferably ruthenium acetylacetonate or palladium acetylacetonate;
the low-boiling point low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone, and is preferably acetone;
the concentration of the noble metal compound when dissolved in the low-boiling point low-polarity solvent is 8 to 16mg/mL, preferably 8, 10, 12, 14, 16, or any value between 8 and 16mg/mL.
Then, while grinding the conductive carbon black, a small amount of noble metal solution is added dropwise into the conductive carbon black, and the solvent is basically volatilized after full grinding, so as to obtain solid powder. Wherein the mass ratio of the noble metal element to the conductive carbon black in the noble metal compound is (1-1.5): 100, preferably 1:100, 1.1:100, 1.2:100, 1.3:100, 1.4:100, 1.5:100, or any value between (1-1.5): 100.
Finally, carrying out heat treatment on the solid powder to obtain the noble metal monoatomic catalyst. The heat treatment is carried out under inert atmosphere conditions, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling point low-polarity solvent, and the time of the heat treatment is 12-16 h, preferably 12, 13, 14, 15, 16 or any value between 12 and 16h.
In the present application, the inert atmosphere condition is preferably argon. In a specific embodiment, the solid powder is heat treated in a tube furnace to sufficiently remove the solvent, and mild drying conditions are effective to prevent aggregation of metal atoms.
The noble metal monoatomic catalyst provided by the application is obtained by impregnating and adsorbing a noble metal precursor by using commercial conductive carbon black and drying, wherein the wettability of an impregnating solution on a carbon carrier is increased, and the effective anchoring of monoatomic dispersed metal species is promoted by combining mild drying conditions. The application utilizes an impregnation method and utilizes the action of a low-boiling point, low-polarity solvent to cause the noble metal atoms to be dispersed on the surface of the carbon carrier in the form of cationic species.
The application also provides application of the noble metal monoatomic catalyst in ascorbic acid detection.
The application of the noble metal monoatomic catalyst means that the catalyst has a catalytic effect on the oxidation of ascorbic acid under a certain potential after the electrode is modified, and the generated current signal is linearly related to the concentration of ascorbic acid molecules. Electrochemical biosensors based on this promise to meet the need for in vivo and in vitro ascorbic acid content analysis and monitoring. In the specific embodiment of the application, compared with commercial conductive carbon black, the noble metal monoatomic catalyst has the advantages of obviously improved detection effect on ascorbic acid, high sensitivity, low detection limit, good selectivity and the like.
The preparation method of the noble metal monoatomic catalyst provided by the application is simple and easy to implement, has universality, has the potential of macro-synthesis and further application in the fields of electrode printing, electrochemical test paper production, microelectrode modification and the like, and provides support for developing more efficient and practical sensing devices and detection products.
In order to further understand the present application, the noble metal monoatomic catalyst, the preparation method thereof and the application thereof in detecting ascorbic acid provided by the present application are described below with reference to examples, and the scope of the present application is not limited by the following examples.
Example 1
Preparation of Ru monoatomic catalyst:
(1) Preparing 270 mu L of an acetone solution of 16mg/mL ruthenium acetylacetonate, dropwise adding the acetone solution into 100mg of conductive carbon black while grinding, and continuously grinding for 30min after the dripping is finished, until the solvent is basically volatilized, so as to obtain solid powder;
(2) Putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing and introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16 hours, naturally cooling to room temperature, taking out to obtain the Ru monoatomic catalyst, wherein the morphology of the material is shown in figure 1, a is a scanning and transmission electron microscope image of the Ru monoatomic catalyst of the embodiment 1, b is a scanning and transmission electron microscope image of the Pd monoatomic catalyst of the embodiment 2, c is a scanning and transmission electron microscope image of the Au monoatomic catalyst of the embodiment 3, and d is a scanning and transmission electron microscope image of the Pt monoatomic catalyst of the embodiment 4; as shown in fig. 2, a is an X-ray diffraction pattern of a Ru monoatomic catalyst and a standard pattern of Ru metal, b is an X-ray diffraction pattern of a Pd monoatomic catalyst and a standard pattern of Pd metal, and it can be seen that no diffraction peak of Ru is shown in the X-ray diffraction pattern; as shown in fig. 3, a is a low power, b is a spherical aberration correcting high angle annular dark field scanning transmission electron microscope image of the Ru single-atom catalyst, the Ru single atoms are observed to be uniformly distributed on the carbon carrier under the spherical aberration correcting transmission electron microscope, meanwhile, the Ru-Ru bond is not present in the material as can be seen from fig. 4, which further illustrates that the Ru-Ru bond is a single-atom dispersing catalyst. In fig. 4, a and b are respectively an X-ray near-side absorption structure spectrum and an extended-side X-ray absorption fine structure spectrum of the Ru monoatomic catalyst, and c and d are respectively an X-ray near-side absorption structure spectrum and an extended-side X-ray absorption fine structure spectrum of the Pd monoatomic catalyst.
Example 2
Preparation of Pd monoatomic catalyst:
(1) Preparing 270 mu L of an acetone solution of 16mg/mL palladium acetylacetonate, dropwise adding the acetone solution into 100mg of conductive carbon black while grinding, and continuously grinding for 30min after the dripping is finished, until the solvent is basically volatilized, so as to obtain solid powder;
(2) Putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing and introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16 hours, naturally cooling to room temperature, and taking out to obtain a Pd monoatomic catalyst, wherein the morphology of the material is shown in the attached figure 1; as shown in fig. 2, the X-ray diffraction pattern does not show diffraction peaks of Pd; as shown in FIG. 4, pd-Pd bonds were not present in the material, further illustrating that it is a monoatomically dispersed catalyst.
Example 3
Preparation of Au monoatomic catalyst:
(1) Preparing 270 mu L of acetone solution of 8mg/mL chloroauric acid, dropwise adding the acetone solution into 100mg of conductive carbon black while grinding, and continuously grinding for 30min after the dripping is finished, until the solvent is basically volatilized, so as to obtain solid powder;
(2) And (3) putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing, introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16 hours, naturally cooling to room temperature, and taking out to obtain the Au monoatomic catalyst, wherein the appearance of the material is shown in the figure 1.
Example 4
Preparation of Pt monoatomic catalyst:
(1) Preparing 270 mu L of an acetone solution of 10mg/mL of platinum acetylacetonate, dropwise adding the acetone solution into 100mg of conductive carbon black while grinding, and continuously grinding for 30min after the dripping is finished, until the solvent is basically volatilized, so as to obtain solid powder;
(2) And (3) putting the obtained solid powder into a porcelain boat, then putting the porcelain boat into a tube furnace, sealing, introducing argon, heating to 65 ℃ under the argon atmosphere, keeping for 16 hours, naturally cooling to room temperature, and taking out to obtain the Pt single-atom catalyst, wherein the appearance of the material is shown in the attached figure 1.
Example 5
Ascorbic acid sensing performance test was performed on the Ru and Pd monoatomic catalysts prepared in preparation examples 1 to 2:
10. Mu.L of a catalyst dispersion consisting of 2mg of noble metal monoatomic catalyst, 1mL of ethanol/water (v/v=1:1) and 10. Mu.L of Nafion D-521 dispersion was added dropwise to a clean glassy carbon electrode as a working electrode.
The test was performed using a three electrode system, the reference electrode was an Ag/AgCl electrode, the counter electrode was Pt wire, and the electrolyte was a 1 XPBS buffer solution.
The three electrode system was placed in a 1 XPBS buffer solution and ascorbic acid was added continuously to the solution such that the concentration of ascorbic acid in the solution was 1. Mu.M, 3. Mu.M, 10. Mu.M, 30. Mu.M, 0.1mM, 0.3mM, 1mM, 3mM, 10mM, 30mM in this order, giving a continuous Ampere-time response curve as shown in FIG. 5 a. And a corresponding current versus ascorbic acid concentration curve was obtained as shown in figure 5 b. As can be seen from FIG. 5c, the detection limit of the Pd monoatomic catalyst for ascorbic acid was 1. Mu.M, while the detection limit of the commercial conductive carbon black was 3. Mu.M. From the results, it can be seen that the noble metal single-atom catalyst shows good detection effect, and has obvious advantages over commercial conductive carbon black in sensitivity and detection limit due to high activity and high selectivity of single-atom metal center. The three electrode system was placed in a 1×pbs buffer solution and ascorbic acid, glucose, glycine, L-glutamic acid were sequentially added to the solution to evaluate the selectivity of Ru monoatomic, pd monoatomic catalysts for ascorbic acid and interfering substances, as shown in fig. 6. Both Ru monoatomic and Pd monoatomic catalysts showed little response to interfering species, exhibiting excellent selectivity.
The foregoing is merely a preferred embodiment of the present application and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present application, which are intended to be comprehended within the scope of the present application.
Claims (5)
1. The application of a noble metal monoatomic catalyst in ascorbic acid detection is characterized in that the noble metal monoatomic catalyst consists of a carbon carrier and noble metal elements, and the noble metal atoms are atomically dispersed on the surface of the carbon carrier in the form of cationic species;
the preparation method of the noble metal monoatomic catalyst comprises the following steps:
dissolving a noble metal compound in a low-boiling-point low-polarity solvent to obtain a noble metal solution;
the conductive carbon black is ground, a noble metal solution is dropwise added into the conductive carbon black, and the solvent is volatilized after full grinding to obtain solid powder;
carrying out heat treatment on the solid powder to obtain a noble metal monoatomic catalyst, wherein the heat treatment is carried out under the inert atmosphere condition, the temperature of the heat treatment is 5-10 ℃ higher than the boiling point of the low-boiling point low-polarity solvent, and the heat treatment time is 12-16 h;
the low-boiling point low-polarity solvent is selected from one of acetone, tetrahydrofuran and 2-butanone.
2. The use according to claim 1, wherein the conductive carbon black is selected from one of KJ600, BP2000, XC72 and N326.
3. The use according to claim 1, wherein the noble metal element is selected from one of Ru, pd, au and Pt.
4. The use according to claim 1, wherein the mass ratio of the noble metal element to the conductive carbon black is (1-1.5): 100.
5. The use according to claim 1, wherein the noble metal compound is selected from one of ruthenium acetylacetonate, palladium acetylacetonate, chloroauric acid and platinum acetylacetonate;
the concentration of the noble metal compound when dissolved in the low-boiling point low-polarity solvent is 8-16 mg/mL.
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