CN115286039A - Preparation method of molybdenum oxide-graphene antibacterial material - Google Patents
Preparation method of molybdenum oxide-graphene antibacterial material Download PDFInfo
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- CN115286039A CN115286039A CN202211020444.2A CN202211020444A CN115286039A CN 115286039 A CN115286039 A CN 115286039A CN 202211020444 A CN202211020444 A CN 202211020444A CN 115286039 A CN115286039 A CN 115286039A
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- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 86
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 71
- 239000000463 material Substances 0.000 title claims abstract description 69
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 229910052750 molybdenum Inorganic materials 0.000 title claims abstract description 58
- 239000011733 molybdenum Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000011888 foil Substances 0.000 claims abstract description 48
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 48
- 239000010439 graphite Substances 0.000 claims abstract description 48
- MEFBJEMVZONFCJ-UHFFFAOYSA-N molybdate Chemical compound [O-][Mo]([O-])(=O)=O MEFBJEMVZONFCJ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000003792 electrolyte Substances 0.000 claims abstract description 27
- 239000000376 reactant Substances 0.000 claims abstract description 26
- 239000007787 solid Substances 0.000 claims abstract description 26
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 238000000967 suction filtration Methods 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 25
- 235000015393 sodium molybdate Nutrition 0.000 claims description 15
- 239000011684 sodium molybdate Substances 0.000 claims description 15
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 15
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 14
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 14
- 239000011609 ammonium molybdate Substances 0.000 claims description 14
- 229940010552 ammonium molybdate Drugs 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 5
- NMHMDUCCVHOJQI-UHFFFAOYSA-N lithium molybdate Chemical compound [Li+].[Li+].[O-][Mo]([O-])(=O)=O NMHMDUCCVHOJQI-UHFFFAOYSA-N 0.000 claims description 5
- MODMKKOKHKJFHJ-UHFFFAOYSA-N magnesium;dioxido(dioxo)molybdenum Chemical compound [Mg+2].[O-][Mo]([O-])(=O)=O MODMKKOKHKJFHJ-UHFFFAOYSA-N 0.000 claims description 5
- 229910052748 manganese Inorganic materials 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 5
- XAEWLETZEZXLHR-UHFFFAOYSA-N zinc;dioxido(dioxo)molybdenum Chemical compound [Zn+2].[O-][Mo]([O-])(=O)=O XAEWLETZEZXLHR-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000002994 raw material Substances 0.000 abstract description 7
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 description 9
- 241000894006 Bacteria Species 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 6
- 230000035484 reaction time Effects 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 231100000331 toxic Toxicity 0.000 description 3
- 230000002588 toxic effect Effects 0.000 description 3
- XOJVVFBFDXDTEG-UHFFFAOYSA-N Norphytane Natural products CC(C)CCCC(C)CCCC(C)CCCC(C)C XOJVVFBFDXDTEG-UHFFFAOYSA-N 0.000 description 2
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 229940088710 antibiotic agent Drugs 0.000 description 2
- 239000004599 antimicrobial Substances 0.000 description 2
- 208000022362 bacterial infectious disease Diseases 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000002848 electrochemical method Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- 231100001261 hazardous Toxicity 0.000 description 2
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 2
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 2
- 150000002926 oxygen Chemical class 0.000 description 2
- 230000007847 structural defect Effects 0.000 description 2
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 206010034133 Pathogen resistance Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
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- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
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- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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Abstract
The invention provides a preparation method of a molybdenum oxide-graphene antibacterial material, which comprises the following steps: providing a molybdate; dissolving molybdate in deionized water to form an electrolyte; putting a double graphite foil electrode into the electrolyte, and connecting the double graphite foil electrode with a direct current stabilized voltage power supply to obtain a suspension after reaction; carrying out suction filtration on the suspension to obtain a solid reactant; and cleaning the solid reactant to obtain the molybdenum oxide-graphene antibacterial material. According to the invention, molybdate is used as a raw material, and double graphite foils are respectively used as a positive electrode and a negative electrode, so that the use of noble metal electrodes is reduced, the cost is effectively reduced, and in the preparation process, the graphite foil electrode is connected to a direct current stabilized voltage power supply, the graphite foil of the negative electrode can be used as an electrode only but does not participate in the reaction, and the graphite foil of the positive electrode participates in the reaction, so that the required molybdenum oxide-graphene antibacterial material is obtained, and a complex graphene preparation process is not required.
Description
Technical Field
The invention relates to the technical field of preparation of antibacterial composite materials, in particular to a preparation method of a molybdenum oxide-graphene antibacterial material.
Background
Graphene-based materials are considered to be an antimicrobial material with great potential. However, in the traditional preparation method of the graphene-based composite material, the graphene oxide is mostly adopted as a raw material to be compounded with other composite materials, and the problem of serious environmental pollution caused by complex compounding steps exists. When the graphene-based composite material is prepared, reducing graphene oxide by a thermal or chemical method; these processes are complex and time consuming, energy intensive, and require hazardous reducing agents and high temperatures. In addition, certain properties of graphene-based composites are limited due to structural defects in the graphene that is reduced using high temperature heat or chemistry, and the electrical conductivity of the reduced graphene is lower than that of the original graphene. These preparation methods require complicated steps and long reaction times. These requirements may further limit the practical application of molybdenum oxide grown on pristine graphene, and thus the desired molybdenum oxide-graphene antibacterial material cannot be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of a molybdenum oxide-graphene antibacterial material, which is used for solving the problem that the required molybdenum oxide-graphene antibacterial material cannot be obtained due to complicated manufacturing steps, long reaction time, low production efficiency and high cost commonly existing in the existing preparation method of graphene in the prior art.
In order to solve the technical problem, the invention provides a preparation method of a molybdenum oxide-graphene antibacterial material, which comprises the following steps:
providing a molybdate;
dissolving the molybdate in deionized water to form an electrolyte;
putting a double graphite foil electrode into the electrolyte, and connecting the double graphite foil electrode with a direct current stabilized voltage power supply to enable the electrolyte to react to obtain a reacted suspension;
carrying out suction filtration on the suspension to obtain a solid reactant;
and cleaning the solid reactant to obtain the molybdenum oxide-graphene antibacterial material.
Optionally, the molarity of the molybdate in the electrolyte is greater than or equal to 0.05mol/L.
Optionally, the molybdate comprises at least one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate, and manganese molybdate.
Optionally, the molybdate is dissolved in 50 to 500mL of deionized water to form the electrolyte.
Optionally, the length of the graphite foil electrode is 3-8 cm, the width of the graphite foil electrode is 3-10 cm, and the thickness of the graphite foil electrode is less than or equal to 0.3mm.
Optionally, the voltage of the power supply is 6-20V.
Optionally, the solid reactant is repeatedly washed a plurality of times with absolute ethanol and deionized water.
Optionally, after the solid reactant is washed, before the molybdenum oxide-graphene antibacterial material is obtained, the method further includes: and drying the washed solid reactant.
Optionally, the washed solid reactant is placed in a vacuum drying oven for drying, and the drying temperature is 40-70 ℃.
As described above, the preparation method of the molybdenum oxide-graphene antibacterial material of the present invention has the following beneficial effects: the invention takes molybdate as raw material, is relatively common in industry and has low price; the method has the advantages that the double graphite foils are used as the positive electrode and the negative electrode respectively, so that the use of noble metal electrodes is reduced, the cost is effectively reduced, the graphite foils are directly used as the electrodes, in the preparation process, the graphite foil electrodes are connected to a direct current stabilized voltage power supply based on the graphite foils and the electrolyte of molybdate, the graphite foil electrodes are connected with the direct current stabilized voltage power supply, the graphite foil electrodes of the negative electrode can be used as the electrodes only but do not participate in the reaction, the graphite foil electrodes of the positive electrode participate in the reaction, and therefore the required molybdenum oxide-graphene antibacterial material is obtained without a complex graphene preparation process; the preparation method of the molybdenum oxide-graphene antibacterial material adopts an electrochemical method for preparation, and has the advantages of simple process steps, short operation reaction time, convenient operation, high production efficiency, low production cost, high conversion rate, no by-product, no toxic or harmful gas, and environmental protection.
Drawings
Fig. 1 is a flowchart of a method for preparing a molybdenum oxide-graphene antibacterial material according to the present invention;
fig. 2 is an XRD pattern of the molybdenum oxide-graphene antibacterial material prepared from ammonium molybdate according to the method for preparing the molybdenum oxide-graphene antibacterial material of the present invention;
fig. 3 is an XRD chart of the molybdenum oxide-graphene antibacterial material prepared from sodium molybdate as a raw material in the preparation method of the molybdenum oxide-graphene antibacterial material of the present invention.
Fig. 4 shows the antibacterial performance of the molybdenum oxide-graphene antibacterial material prepared from ammonium molybdate in the preparation method of the molybdenum oxide-graphene antibacterial material of the present invention.
Fig. 5 illustrates the antibacterial performance of the molybdenum oxide-graphene antibacterial material prepared from sodium molybdate according to the method for preparing the molybdenum oxide-graphene antibacterial material of the present invention.
Description of reference numerals: 11. selecting ammonium molybdate as molybdate to obtain a molybdenum oxide-graphene antibacterial material; 12. graphene; 13. and selecting sodium molybdate as molybdate to obtain the molybdenum oxide-graphene antibacterial material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The preferred embodiments described below are by way of example only, and other obvious variations will occur to those skilled in the art. The underlying principles of the invention, as defined in the following description, may be applied to other embodiments, variations, modifications, equivalents, and other technical solutions without departing from the spirit and scope of the invention.
It will be understood by those skilled in the art that in the present disclosure, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced devices or components must be constructed and operated in a particular orientation and thus are not to be considered limiting.
In recent years, bacterial infectious diseases have seriously endangered human health, and although the emergence of traditional antibiotics has saved many patients with bacterial infections, the problem of bacterial resistance is becoming serious due to the long-term use and abuse of antibiotics, and therefore, the development of novel antibacterial agents is particularly important. At present, inorganic antibacterial materials mainly comprise two major classes of antibacterial materials based on a heavy metal ion (such as Ag +) dissolution mechanism and semiconductor antibacterial materials. The semiconductor antibacterial material can generate active oxygen clusters with antibacterial effect under illumination, and the active oxygen clusters with strong oxidizing capability can not only generate oxidation-reduction reaction with organic substances forming bacteria to kill the bacteria, but also can directly degrade the dead remains of the bacteria, so that the semiconductor antibacterial material is far stronger than an inorganic antibacterial material containing Ag + in antibacterial effect, and has application potential as an antibacterial material.
Graphene-based materials are considered to be an antimicrobial material with great potential. However, in the traditional preparation method of the graphene-based composite material, the graphene oxide is mostly adopted as a raw material to be compounded with other composite materials, and the problem of serious environmental pollution caused by complex compounding steps exists. When preparing the graphene-based composite material, reducing graphene oxide by a thermal or chemical method; these processes are complex and time consuming, energy intensive, and require hazardous reducing agents and high temperatures. In addition, since graphene reduced using high temperature heat or chemistry has structural defects, and the electrical conductivity of the reduced graphene is lower than that of the original graphene, some properties of the graphene-based composite material are limited. These preparation methods require complicated steps and long reaction times. These requirements may further limit the practical application of molybdenum oxide grown on pristine graphene, and thus the desired molybdenum oxide-graphene antibacterial material cannot be obtained.
Example one
Referring to fig. 1, the present invention provides a preparation method of a molybdenum oxide-graphene antibacterial material, including:
s1: providing a molybdate;
s2: dissolving the molybdate in deionized water to form an electrolyte;
s3: putting a double graphite foil electrode into the electrolyte, and connecting the double graphite foil electrode with a direct current stabilized voltage power supply to enable the electrolyte to react to obtain a reacted suspension;
s4: carrying out suction filtration on the suspension to obtain a solid reactant;
s5: and cleaning the solid reactant to obtain the molybdenum oxide-graphene antibacterial material.
The invention takes molybdate as raw material, is relatively common in industry and has low price; the method has the advantages that the double graphite foils are used as the positive electrode and the negative electrode respectively, so that the use of noble metal electrodes is reduced, the cost is effectively reduced, the graphite foils are directly used as the electrodes, in the preparation process, the graphite foil electrodes are connected to a direct current stabilized voltage power supply based on the graphite foils and the electrolyte of molybdate, the graphite foil electrodes are connected with the direct current stabilized voltage power supply, the graphite foil of the negative electrode can be used as the electrodes only and does not participate in the reaction, the graphite foil of the positive electrode participates in the reaction, and therefore the required molybdenum oxide-graphene antibacterial material is obtained, and a complex graphene preparation process is not needed; the preparation method of the molybdenum oxide-graphene antibacterial material adopts an electrochemical method for preparation, and has the advantages of simple process steps, short operation reaction time, convenient operation, high production efficiency, low production cost, high conversion rate, no by-product, no toxic or harmful gas, and environmental protection.
In step S1, a molybdate is provided.
By way of example, the molybdate may include, but is not limited to, at least one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate, and manganese molybdate.
Specifically, the molybdate may be any one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate, and the molybdate may also be any two or a combination of more than two of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate.
In step S2, the molybdate is dissolved in deionized water to form an electrolyte.
For example, the molarity of the molybdate in the electrolyte may be set according to actual requirements, and in this embodiment, the molarity of the molybdate is not less than 0.05mol/L. Specifically, in the electrolyte, the molarity of the molybdate may be 0.05mol/L, 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.5mol/L, 0.7mol/L, 1mol/L or 5mol/L, and the like.
As an example, the molybdate is dissolved in 50 to 500mL of deionized water to form the electrolyte.
Specifically, the molybdate may be dissolved in 50mL, 100mL, 200mL, 400mL, or 500mL of deionized water to form the electrolyte.
As an example, the molybdate may be placed in a beaker or a glass ware, and then the deionized water is added into the beaker or the glass ware and then stirred, so as to obtain the electrolyte. Of course, the electrolyte may also be obtained by adding the deionized water to a beaker or a glass ware, then adding the molybdate to the deionized water, and then stirring.
In step S3, a double graphite foil electrode is placed in the electrolyte, and the double graphite foil electrode is connected to a dc regulated power supply, so that the electrolyte reacts to obtain a reacted suspension.
As an example, the length, width and thickness of the graphite foil electrode can be set according to actual needs; in this embodiment, the length of the graphite foil electrode may be, but is not limited to, 3 to 8cm, the width of the graphite foil electrode may be, but is not limited to, 3 to 10cm, and the thickness of the graphite foil electrode may be 0.3mm or less.
Specifically, the length of the graphite foil electrode may be 3cm, 5cm, 7cm, 8cm, or the like, the width of the graphite foil electrode may be 3cm, 5cm, 7cm, 9cm, 10cm, or the like, and the thickness of the graphite foil electrode may be 0.1mm, 0.2mm, 0.3mm, or the like.
As an example, the voltage of the DC regulated power supply may be 6-20V.
Specifically, the voltage of the dc regulated power supply may be 6V, 10V, 15V, 20V, or the like.
In step S4, the suspension is suction filtered to obtain a solid reactant.
Specifically, any one of the existing suction filtration methods may be adopted to perform suction filtration on the suspension to obtain the solid reactant.
In step S5, the solid reactant is washed to obtain the molybdenum oxide-graphene antibacterial material.
As an example, the solid reactant may be repeatedly washed several times using absolute ethanol and deionized water. Specifically, the solid reactant may be alternately and repeatedly washed with the absolute ethyl alcohol and the deionized water several times.
As an example, after the solid reactant is washed, before the molybdenum oxide-graphene antibacterial material is obtained, the method further includes: and drying the washed solid reactant.
As an example, the solid reactant after washing may be dried in a vacuum drying oven.
Specifically, the drying temperature for drying the solid reactant may be, but is not limited to, 40 to 70 ℃.
Specifically, the drying temperature for drying the washed solid reactant in a vacuum drying oven can be 40 ℃, 50 ℃, 60 ℃ or 70 ℃ and the like.
Further, when ammonium molybdate is used as the molybdate, an XRD pattern of the finally obtained molybdenum oxide-graphene antibacterial material is shown in fig. 2, and when sodium molybdate is used as the molybdate, an XRD pattern of the finally obtained molybdenum oxide-graphene antibacterial material is shown in fig. 3. As can be seen from fig. 2 and 3, the molybdenum oxide-graphene antibacterial material can be obtained by using either ammonium molybdate or sodium molybdate as the molybdate, and the molybdenum oxide-graphene antibacterial material obtained by using sodium molybdate as the molybdate has high purity and good crystallinity. Meanwhile, as shown in fig. 4 and 5, the molybdenum oxide-graphene antibacterial material prepared from ammonium molybdate or sodium molybdate has good antibacterial performance. Specifically, as shown in fig. 4, when the molybdenum oxide-graphene antibacterial material 11 and the graphene 12 obtained by using ammonium molybdate as molybdate are respectively dropped into the culture medium, it can be found that bacteria around the molybdenum oxide-graphene antibacterial material 11 obtained by using ammonium molybdate as molybdate are killed (i.e., a circle of light-colored region formed by removing bacteria around the molybdenum oxide-graphene antibacterial material 11 obtained by using ammonium molybdate as shown in fig. 4); as shown in fig. 5, when the molybdenum oxide-graphene antibacterial material 13 obtained by using sodium molybdate as molybdate and the graphene 12 were dropped into the culture medium, respectively, it was found that the bacteria around the molybdenum oxide-graphene antibacterial material 13 obtained by using sodium molybdate as molybdate were all killed (i.e., a circle of lighter area formed by the bacteria removed around the molybdenum oxide-graphene antibacterial material 13 obtained by using sodium molybdate as shown in fig. 5).
The invention provides a preparation method of a molybdenum oxide-graphene antibacterial material, wherein double graphite foils are used as a positive electrode and a negative electrode respectively, so that the use cost of a noble metal electrode is reduced effectively, the graphite foils are directly used as the electrodes, in the preparation process, the graphite foil electrodes are connected to a direct current stabilized voltage power supply based on the graphite foils and an electrolyte of molybdate, the graphite foil electrodes are connected with the direct current stabilized voltage power supply, the graphite foil of the negative electrode can be used as the electrode only but not participate in reaction, and the graphite foil of the positive electrode can participate in the reaction, so that the required molybdenum oxide-graphene antibacterial material is obtained, and a complex preparation process of graphene is not needed. The device of the invention can be implemented simply in a common beaker or glass ware, and the molybdate selected as the raw material is relatively common in industry and low in price. The molybdenum oxide-graphene antibacterial material can be prepared by a one-step method, the electrochemical operation time is short, the process is simple, the operation is convenient, the conversion rate is high, no by-product is generated, no toxic or harmful gas is generated, and the method is green and environment-friendly.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (9)
1. A preparation method of a molybdenum oxide-graphene antibacterial material is characterized by comprising the following steps:
providing a molybdate;
dissolving the molybdate in deionized water to form an electrolyte;
putting a double graphite foil electrode into the electrolyte, and connecting the double graphite foil electrode with a direct current stabilized voltage power supply to enable the electrolyte to react to obtain a reacted suspension;
carrying out suction filtration on the suspension to obtain a solid reactant;
and cleaning the solid reactant to obtain the molybdenum oxide-graphene antibacterial material.
2. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 1, wherein the molarity of the molybdate in the electrolyte is not less than 0.05mol/L.
3. The method of preparing a molybdenum oxide-graphene antibacterial material according to claim 1, wherein the molybdate includes at least one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate, and manganese molybdate.
4. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 1, wherein the molybdate is dissolved in 50 to 500mL of deionized water to form the electrolyte.
5. The preparation method of the molybdenum oxide-graphene antibacterial material according to claim 1, wherein the length of the graphite foil electrode is 3-8 cm, the width of the graphite foil electrode is 3-10 cm, and the thickness of the graphite foil electrode is not more than 0.3mm.
6. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 1, wherein the voltage of the power supply is 6-20V.
7. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 1, wherein the solid reactant is repeatedly washed a plurality of times using absolute ethanol and deionized water.
8. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 1, wherein after the solid reactant is washed and before the molybdenum oxide-graphene antibacterial material is obtained, the method further comprises: and drying the washed solid reactant.
9. The method for preparing the molybdenum oxide-graphene antibacterial material according to claim 8, wherein the washed solid reactant is dried in a vacuum drying oven at a temperature of 40-70 ℃.
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