CN111715244A - Preparation method and application of pseudo-enzyme catalyst - Google Patents
Preparation method and application of pseudo-enzyme catalyst Download PDFInfo
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- CN111715244A CN111715244A CN202010721456.2A CN202010721456A CN111715244A CN 111715244 A CN111715244 A CN 111715244A CN 202010721456 A CN202010721456 A CN 202010721456A CN 111715244 A CN111715244 A CN 111715244A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 47
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 47
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 37
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 230000000694 effects Effects 0.000 claims abstract description 14
- 230000003197 catalytic effect Effects 0.000 claims abstract description 10
- 230000007547 defect Effects 0.000 claims abstract description 8
- 239000002135 nanosheet Substances 0.000 claims abstract description 7
- 230000002789 catalaselike Effects 0.000 claims abstract description 4
- 239000006185 dispersion Substances 0.000 claims description 27
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- ZKKLPDLKUGTPME-UHFFFAOYSA-N diazanium;bis(sulfanylidene)molybdenum;sulfanide Chemical compound [NH4+].[NH4+].[SH-].[SH-].S=[Mo]=S ZKKLPDLKUGTPME-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 102000004190 Enzymes Human genes 0.000 claims description 5
- 108090000790 Enzymes Proteins 0.000 claims description 5
- 230000003278 mimic effect Effects 0.000 claims description 2
- 239000002055 nanoplate Substances 0.000 claims 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 10
- 239000000463 material Substances 0.000 abstract description 7
- 238000000034 method Methods 0.000 abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 230000001954 sterilising effect Effects 0.000 abstract description 2
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 24
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 6
- 230000001580 bacterial effect Effects 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 102000016938 Catalase Human genes 0.000 description 2
- 108010053835 Catalase Proteins 0.000 description 2
- 239000002054 inoculum Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- UAIUNKRWKOVEES-UHFFFAOYSA-N 3,3',5,5'-tetramethylbenzidine Chemical compound CC1=C(N)C(C)=CC(C=2C=C(C)C(N)=C(C)C=2)=C1 UAIUNKRWKOVEES-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 238000002965 ELISA Methods 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 230000002255 enzymatic effect Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000003307 slaughter Methods 0.000 description 1
- 239000007974 sodium acetate buffer Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/02—Sulfur; Selenium; Tellurium; Compounds thereof
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- B01J35/40—
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
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Abstract
The invention discloses a molybdenum disulfide/graphene composite material enzyme-like catalyst and a preparation method thereof. The catalyst is prepared by a microwave hydrothermal method, and molybdenum disulfide nanosheets vertically grow on the surface of graphene to form a molybdenum disulfide/graphene vertical heterostructure. According to the invention, more active sites can be exposed by vertically growing the molybdenum disulfide nanosheets on the graphene nanosheets, and the molybdenum disulfide synthesized by the microwave method has more defects, stronger pseudo-enzyme activity, catalase-like activity, peroxidase-like activity and oxidase-like activity, and can be used for antibacterial materials, antibacterial preparations and the like. The preparation method provided by the invention is simple and convenient, the preparation time is short, and the prepared composite material has more defects, exposes more active sites, has higher pseudoenzyme catalytic activity and improves the sterilization efficiency.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a molybdenum disulfide/graphene vertical heterostructure enzyme mimetic catalytic material, and a preparation method and application thereof.
Background
Molybdenum disulfide (MoS2) is a typical graphene-like two-dimensional Transition Metal Sulfide (TMDs), and has unique physicochemical properties, thereby having wide applications in the fields of catalysis, batteries, photoelectric devices, and the like. The application of the nano MoS2 in the biomedical field is also of great interest, which is mainly attributed to the fact that the molybdenum disulfide has a pseudoenzyme activity, especially a high catalase-like activity, and can catalyze hydrogen peroxide into hydroxyl radicals with oxidizing capability.
The existing research shows that the enzymatic activity of the molybdenum disulfide comes from the lattice defect, and the edge of the nanosheet is the active site. Therefore, the design of molybdenum disulfide with high defect and exposed edge area has been the research focus. Molybdenum disulfide, however, tends to agglomerate, which results in a reduction in its surface defects, and its edge active sites are easily buried. Currently, some reports have reported that molybdenum disulfide with exposed high-activity sites is prepared by using a vapor deposition method, but the molybdenum disulfide needs to be prepared on a substrate, is not beneficial to subsequent biological application research, and has complex preparation method and expensive required equipment.
Disclosure of Invention
In order to solve the above problems, an object of the present invention is to provide a method for rapidly preparing a molybdenum disulfide/graphene vertical heterostructure rich in defects and exposed edge active sites, and a method for preparing the same.
The invention is characterized in that: the catalyst is vertically grown on graphene by molybdenum disulfide nanosheets, wherein the diameter of the molybdenum disulfide nanosheets is 50-150 nm.
The molybdenum disulfide/graphene mimic enzyme catalyst is prepared by the following method:
(1) dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion solution, then adding 0.5-5mL of 1mg/mL graphene oxide solution into the dispersion solution, and uniformly stirring;
(2) adding the dispersion into a reactor, heating the dispersion to 200 +/-20 ℃ by using a microwave reactor under the condition of stirring, and reacting for 10 +/-6 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
The molybdenum disulfide/graphene composite structure related by the invention has three types of enzyme mimetic activities: catalase-like activity, peroxidase-like activity and oxidase-like activity
The molybdenum disulfide/graphene composite structure provided by the invention obviously improves the antibacterial performance on the basis of keeping the characteristics of the original nano material, has an excellent bacterial killing effect, can be used in antibacterial materials and antibacterial preparations, and expands the types and applications of the antibacterial materials and the antibacterial preparations. The preparation method provided by the invention is a microwave hydrothermal synthesis method, is simple and convenient to operate, and can shorten the preparation time.
Drawings
Fig. 1 is a Scanning Electron Microscope (SEM) image of the molybdenum disulfide/graphene composite structure prepared in example 1 of the present invention.
Fig. 2 is (a) a Transmission Electron Microscope (TEM) image and (b) a high-resolution transmission electron microscope (HRTEM) image of the molybdenum disulfide/graphene composite structure prepared in example 1 of the present invention.
FIG. 3 is a catalase activity test of the molybdenum disulfide/graphene composite structure prepared in example 1 of the present invention.
Fig. 4 is a graph showing the sterilization effect of the molybdenum disulfide/graphene composite structure prepared in example 1, the pure molybdenum disulfide synthesized by microwave synthesis prepared in comparative example 1, the molybdenum disulfide/graphene composite structure hydrothermally synthesized by the oven prepared in comparative example 2, and the pure molybdenum disulfide synthesized by the oven hydrothermal method prepared in comparative example 3.
Detailed Description
The present invention will be described in more detail and fully with reference to the following examples, which are not intended to limit the scope of the invention.
Example 1
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion solution, then adding 1mL of 1mg/mL graphene oxide solution into the dispersion solution, and uniformly stirring;
(2) adding the dispersion into a reactor, heating the dispersion to 200 ℃ by using a microwave reactor under the condition of stirring, and reacting for 10 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Comparative example 1
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion liquid;
(2) adding the dispersion into a reactor, heating the dispersion to 200 ℃ by using a microwave reactor under the condition of stirring, and reacting for 10 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Comparative example 2
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion solution, then adding 1mL of 1mg/mL graphene oxide solution into the dispersion solution, and uniformly stirring;
(2) adding the dispersion into a reaction kettle, putting the reaction kettle into an oven, heating the reaction kettle to 200 ℃, and reacting for 10 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Comparative example 3
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion liquid;
(2) adding the dispersion into a reaction kettle, putting the reaction kettle into an oven, heating the reaction kettle to 200 ℃, and reacting for 10 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Example 2
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion solution, then adding 0.5mL of 1mg/mL graphene oxide solution into the dispersion solution, and uniformly stirring;
(2) adding the dispersion into a reactor, heating the dispersion to 190 ℃ by using a microwave reactor under the condition of stirring, and reacting for 6 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Example 3
(1) Dissolving 260mg of ammonium tetrathiomolybdate in 15mL of dimethylformamide to obtain a dispersion solution, then adding 5mL of 1mg/mL graphene oxide solution into the dispersion solution, and uniformly stirring;
(2) adding the dispersion into a reactor, heating the dispersion to 200 ℃ by using a microwave reactor under the condition of stirring, and reacting for 10 hours;
(3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate. Thus obtaining the molybdenum disulfide/graphene composite catalyst with high-efficiency pseudo-enzyme catalytic activity.
Test example 1
Observation by a Scanning Electron Microscope (SEM).
As shown in fig. 1, nano-sized molybdenum disulfide is vertically grown on micro-sized graphene sheets.
Test example 2
Observation with a Transmission Electron Microscope (TEM).
As shown in fig. 2, the molybdenum disulfide/graphene vertical heterostructure is shown in the diagrams (a) and (b) under different magnifications, the molybdenum disulfide grows vertically on the graphene from the diagram (a), the active sites exposed at the edge of the molybdenum disulfide are exposed in the composite material, and the molybdenum disulfide has a large number of defect sites from the diagram (b).
Test example 3
And (3) testing the catalase activity of the molybdenum disulfide/graphene vertical heterostructure. Adding 20 microgram of 800 microgram 3,3',5,5' -tetramethylbenzidine of a material into a sodium acetate buffer solution with the pH value of 3.6, adding different amounts of hydrogen peroxide, shaking up, rapidly placing the mixture under an ultraviolet visible spectrophotometer, detecting the absorbance at 652nm, and calculating the reaction rate according to the absorbance. As shown in fig. 3, it can be seen that the reaction rate gradually increases as the hydrogen peroxide concentration increases.
Test example 4
And the antibacterial effect of the molybdenum disulfide/graphene vertical heterostructure.
The antibacterial effect was determined by plate counting. The shaken bacterial solution was placed in a test tube, centrifuged (4000rpm, 5min), the supernatant was discarded, washed three times with 10mL of PBS, centrifuged (4000rpm, 5min), and the supernatant was discarded. 10mL of PBS was added to the tube and the bacteria were redispersed. And (4) taking 200 mu L of the redispersed bacterial liquid, placing the bacterial liquid in a 96-well plate, and measuring an absorbance value (the absorbance value of escherichia coli is 0.15) at a position of 600nm on an enzyme-linked immunosorbent assay. Diluting the bacterial liquid in gradient 104After doubling, 400. mu.L of the inoculum was incubated with 25. mu.g/mL of the test material (prepared in examples and comparative examples) for 20min, 100. mu.L of the inoculum was applied to a slaughter plate, incubated at 37 ℃ for 18h on a shaker at 200rpm, and counted. FIG. 4 shows the statistical results of the plate counting method. The antibacterial effect of the molybdenum disulfide is most obvious through comparison of different materials.
Unless otherwise defined, all terms used herein have the meanings commonly understood by those skilled in the art.
Claims (4)
1. The enzyme simulating catalyst is characterized by comprising graphene micron sheets and molybdenum disulfide nano sheets vertically grown on graphene, wherein the mass ratio of the graphene to the molybdenum disulfide in the catalyst is (0.5-5): 100.
2. the pseudoenzyme catalyst of claim 1, wherein the molybdenum disulfide nanoplates are in the size range of 50-150 nm.
3. The composite catalyst of claim 1, wherein: the composite catalyst is rich in defects and exposes more active sites, and simultaneously has three pseudoenzyme activities: catalase-like activity, peroxidase-like activity, and oxidase-like activity.
4. A preparation method of a mimic enzyme catalyst is characterized by comprising the following steps:
(1) 260mg of ammonium tetrathiomolybdate is dissolved in 15mL of dimethylformamide to obtain a dispersion, and then 0.5-5mL of 1mg/mL graphene oxide solution is added to the dispersion and stirred uniformly.
(2) The dispersion was charged into a reactor and heated to 200. + -. 20 ℃ with stirring using a microwave reactor for 10. + -. 6 hours.
(3) And (3) filtering the solution reacted in the step (2), washing the generated precipitate with deionized water and ethanol, and drying the separated precipitate to obtain the molybdenum disulfide/graphene vertical heterostructure with high-efficiency pseudoenzyme catalytic activity.
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| CN113769768A (en) * | 2021-09-08 | 2021-12-10 | 中国科学院海洋研究所 | Double-function composite nano material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113769768A (en) * | 2021-09-08 | 2021-12-10 | 中国科学院海洋研究所 | Double-function composite nano material and preparation method and application thereof |
| CN113769768B (en) * | 2021-09-08 | 2023-05-26 | 中国科学院海洋研究所 | Double-function composite nano material and preparation method and application thereof |
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Application publication date: 20200929 |