CN115896801A - Preparation method of molybdenum oxide nanomaterial - Google Patents

Abstract

The invention provides a method for preparing molybdenum oxide nanomaterials, comprising: providing molybdate; dissolving the molybdate in deionized water to form an electrolyte; placing double electrodes in the electrolyte, and The electrode is connected to a power source to allow the electrolyte to react to obtain a reacted suspension; the electrode includes a graphite foil electrode or a metal foil electrode; the suspension is suction filtered to obtain a solid reaction The solid reactant is cleaned to obtain molybdenum oxide nanomaterials. The present invention uses molybdate as a raw material, which is relatively common in industry and low in price; graphite foil or metal foil is used as positive and negative electrodes respectively, which reduces the use of noble metal foil electrodes and effectively reduces costs; the present invention is prepared by an electrochemical method, The process steps are simple, the operation reaction time is short, the operation is convenient, the production efficiency is high, the production cost is low, the conversion rate is high, there is no by-product, no poisonous and harmful gas is produced, and it is green and environmentally friendly.

Description

Preparation method of molybdenum oxide nanomaterial

technical field

The invention relates to the technical field of nanomaterial preparation, in particular to a method for preparing a molybdenum oxide nanomaterial.

Background technique

At present, the preparation methods of molybdenum oxide mainly include hydrothermal method, chemical vapor deposition method, sol-gel method, spray pyrolysis method, sonochemical method and other preparation methods. The hydrothermal method is currently the most commonly used method for synthesizing nanomaterials. It has the advantages of simple synthesis process, easy control, and high repeatability. It can prepare nanomaterials with various morphologies. It is also one of the most commonly used synthesis methods for molybdenum oxide nanomaterials. The chemical vapor deposition method is a method of forming a thin film layer or a new nanomaterial on the surface of the substrate by heating the raw material into vapor deposition, and it is also a common method for synthesizing molybdenum oxide materials. The sol-gel method is to form a stable sol system by hydrolyzing metal salts and highly chemically active substances. The sol loses fluidity after aging and slowly polymerizes to form a gel. The gel can be dried and sintered to obtain nanostructured materials. The spray pyrolysis method is to spray the metal salt solution into a high-temperature atmosphere in the form of mist, causing the solvent to evaporate, and the metal salt is thermally decomposed at a high temperature to directly obtain a metal oxide film or powder on the substrate. However, all the above-mentioned methods require complex steps and long reaction time, and require high-temperature calcination, which consumes time and energy, has low production efficiency and high production cost, thus limiting the preparation of molybdenum trioxide.

Contents of the invention

The purpose of the present invention is to provide a method for preparing molybdenum oxide nanomaterials, which is used to solve the problems of complex process steps, long reaction time, low production efficiency and high production cost in the method of molybdenum oxide nanomaterials in the prior art.

In order to solve the above technical problems, the present invention provides a method for preparing molybdenum oxide nanomaterials, comprising:

Provide molybdate;

Dissolving the molybdate in deionized water to form an electrolyte;

Put double electrodes in the electrolyte, and connect the double electrodes with a power source, so that the electrolyte reacts to obtain a reacted suspension; the electrodes include graphite foil electrodes or metal foil electrodes ;

The suspension is suction filtered to obtain a solid reactant;

The solid reactant is cleaned to obtain molybdenum oxide nanometer material.

Optionally, in the electrolyte, the molar concentration of the molybdate is greater than or equal to 0.05 mol/L.

Optionally, the molybdate includes at least one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate.

Optionally, the molybdate is dissolved in 50-500 mL of deionized water to form the electrolyte.

Optionally, the length of the electrode is 3-8 cm, the width of the electrode is 3-10 cm, and the thickness of the electrode is less than or equal to 0.3 mm.

Optionally, when the electrode is a metal foil electrode, the material of the metal foil electrode includes at least one of iron, aluminum, nickel, copper, zinc and titanium.

Optionally, the power supply includes a square wave stabilized power supply, the voltage of the power supply is 6-20V, and the voltage conversion time of the power supply is 10-60s.

Optionally, the solid reactant is repeatedly washed with absolute ethanol and deionized water.

Optionally, after washing the solid reactant and before obtaining the molybdenum oxide nanomaterial, the method further includes: drying the washed solid reactant.

Optionally, the washed solid reactant is dried in a vacuum oven at a drying temperature of 40-70°C.

As mentioned above, the preparation method of molybdenum oxide nanomaterials of the present invention has the following beneficial effects: the present invention uses molybdate as a raw material, which is relatively common in industry and low in price; graphite foil or metal foil is used as positive and negative electrodes respectively, The use of noble metal foil electrodes is reduced, and the cost is effectively reduced; the preparation method of the molybdenum oxide nanomaterial of the present invention is prepared by an electrochemical method, the process steps are simple, the operation reaction time is short, the operation is convenient, the production efficiency is high, the production cost is low, and the conversion High efficiency and no by-products, no toxic and harmful gases, green and environmentally friendly.

Description of drawings

Fig. 1 is the flow chart of the preparation method of molybdenum oxide nanomaterial of the present invention;

Fig. 2 is in the preparation method of molybdenum oxide nano material of the present invention, is the XRD pattern of the molybdenum oxide nano material prepared as raw material with ammonium molybdate;

FIG. 3 is an XRD pattern of molybdenum oxide nanomaterials prepared with sodium molybdate as raw material in the preparation method of molybdenum oxide nanomaterials of the present invention.

Detailed ways

The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

The preferred embodiments described below are only examples, and those skilled in the art can devise other obvious variations. The basic principles of the present invention defined in the following description can be applied to other embodiments, variations, improvements, equivalents and other technical solutions without departing from the spirit and scope of the present invention.

Those skilled in the art should understand that in the disclosure of the present invention, the terms "vertical", "transverse", "upper", "lower", "front", "rear", "left", "right", " The orientation or positional relationship indicated by "vertical", "horizontal", "top", "bottom", "inner", "outer", etc. is based on the orientation or positional relationship shown in the drawings, which are only for the convenience of describing the present invention and The above terms should not be construed as limiting the present invention because the description is simplified rather than indicating or implying that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation.

Molybdenum oxide (e.g., molybdenum trioxide, MoO ₃ ) is a stable n-type semiconductor with a wide band gap of about 3.2 eV, and MoO ₃ is most commonly kinetically stable orthorhombic α-MoO ₃ and metastable single For oblique crystal β-MoO ₃ , the β phase will transform into a more stable α phase when the temperature is above 350°C. Orthorhombic α-MoO ₃ has a very ideal layered structure, which is a deformed planar crystal composed of double-layer MoO6 octahedra, and the double-layers are combined by weak van der Waals forces in the vertical direction [010], while the The interior is mainly composed of covalent bonds and ionic bonds. Due to the physicochemical properties resulting from this unique layered structure, molybdenum oxide materials have been extensively studied in various fields.

At present, the preparation methods of molybdenum oxide mainly include hydrothermal method, chemical vapor deposition method, sol-gel method, spray pyrolysis method, sonochemical method and other preparation methods. The hydrothermal method is currently the most commonly used method for synthesizing nanomaterials. It has the advantages of simple synthesis process, easy control, and high repeatability. It can prepare nanomaterials with various morphologies. It is also one of the most commonly used synthesis methods for molybdenum oxide nanomaterials. The chemical vapor deposition method is a method of forming a thin film layer or a new nanomaterial on the surface of the substrate by heating the raw material into vapor deposition, and it is also a common method for synthesizing molybdenum oxide materials. The sol-gel method is to form a stable sol system by hydrolyzing metal salts and highly chemically active substances. The sol loses fluidity after aging and slowly polymerizes to form a gel. The gel can be dried and sintered to obtain nanostructured materials. The spray pyrolysis method is to spray the metal salt solution into a high-temperature atmosphere in the form of mist, causing the solvent to evaporate, and the metal salt is thermally decomposed at a high temperature to directly obtain a metal oxide film or powder on the substrate. However, all the above-mentioned methods require complex steps and long reaction time, and require high-temperature calcination, which consumes time and energy, has low production efficiency and high production cost, thus limiting the preparation of molybdenum trioxide.

Embodiment one

Please refer to shown in Fig. 1, the present invention provides a kind of preparation method of molybdenum oxide nanomaterial, the preparation method of described molybdenum oxide nanomaterial comprises:

S1: Provide molybdate;

S2: dissolving the molybdate in deionized water to form an electrolyte;

S3: Put double electrodes in the electrolyte, and connect the electrodes to a power source, so that the electrolyte reacts to obtain a reacted suspension; the electrodes include graphite foil electrodes or metal foils electrode;

S4: Suction filtering the suspension to obtain a solid reactant;

S5: Washing the solid reactant to obtain molybdenum oxide nanomaterials.

The present invention uses molybdate as raw material, which is relatively common in industry and low in price; using graphite foil or metal foil as positive and negative electrodes respectively reduces the use of noble metal foil electrodes and effectively reduces costs; the molybdenum oxide nanomaterial of the present invention The preparation method is prepared by an electrochemical method, the process steps are simple, the operation reaction time is short, the operation is convenient, the production efficiency is high, the production cost is low, the conversion rate is high, there is no by-product, no toxic and harmful gas is produced, and it is green and environmentally friendly.

In step S1, molybdate is provided.

As an example, the molybdate may include but not limited to at least one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate.

Specifically, the molybdate can be any one of ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate, and the molybdate can also be ammonium molybdate , sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate any two or more combinations.

In step S2, the molybdate is dissolved in deionized water to form an electrolyte.

As an example, in the electrolyte, the molar concentration of the molybdate may be set according to actual needs. In this embodiment, the molar concentration of the molybdate is greater than or equal to 0.05 mol/L. Specifically, in the electrolyte, the molar concentration 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 so on.

As an example, the molybdate is dissolved in 50˜500 mL of deionized water to form the electrolyte.

Specifically, the molybdate may be dissolved in 50 mL, 100 mL, 200 mL, 400 mL or 500 mL of deionized water to form the electrolyte.

As an example, the molybdate may be first placed in a beaker or a glass vessel, and then the deionized water may be added into the beaker or glass vessel and then stirred to obtain the electrolyte solution. Certainly, the deionized water may also be added into a beaker or glassware first, and then the molybdate may be added into the deionized water and then stirred to obtain the electrolyte solution.

In step S3, double electrodes are placed in the electrolyte, and the electrodes are connected to a power source so that the electrolyte reacts to obtain a reacted suspension; the electrodes include graphite foil electrodes or metal foil electrodes.

It should be noted that the "putting double electrodes in the electrolyte" refers to putting two electrodes, a positive electrode and a negative electrode, in the electrolyte. Both the positive and negative electrodes may include graphene electrodes or metal foil electrodes. However, it should be noted that the material of the positive electrode and the material of the negative electrode need to be the same.

As an example, the length, width and thickness of the electrodes can be designed according to actual needs; in this embodiment, the length of the electrodes can be but not limited to 3-8 cm, and the width of the electrodes can be but not limited to 3 cm ~10cm, the thickness of the electrode may be less than or equal to 0.3mm.

Specifically, the length of the electrode can be 3cm, 5cm, 7cm or 8cm, etc., the width of the electrode can be 3cm, 5cm, 7cm, 9cm, or 10cm, etc., and the thickness of the electrode can be 0.1mm, 0.2mm or 0.3mm and so on.

As an example, the power supply may include a square wave stabilized power supply, the voltage of the power supply is 6-20V, and the voltage conversion time of the power supply is 10-60s.

Specifically, the voltage of the power supply may be 6V, 10V, 15V or 20V and so on, and the voltage conversion time of the power supply may be 10s, 20s, 30s, 50s or 60s and so on.

As an example, neither the positive electrode nor the negative electrode participates in the reaction in this step, and both serve as electrodes only.

As an example, when the electrode is a metal foil electrode, the material of the metal foil electrode includes at least one of iron, aluminum, nickel, copper, zinc and titanium. Specifically, the material of the metal foil electrode can be any one of iron, aluminum, nickel, copper, zinc or titanium, or two or more of iron, aluminum, nickel, copper, zinc and titanium alloy.

In step S4, the suspension is suction-filtered to obtain a solid reactant.

Specifically, any existing suction filtration method can be used to perform suction filtration on the suspension to obtain the solid reactant.

In step S5, the solid reactant is washed to obtain molybdenum oxide nanomaterials.

As an example, the solid reactant may be repeatedly washed with absolute ethanol and deionized water. Specifically, the solid reactant may be alternately and repeatedly washed with the absolute ethanol and the deionized water for multiple times.

As an example, after washing the solid reactant and before obtaining the molybdenum oxide nanomaterial, the method further includes: drying the washed solid reactant.

As an example, the washed solid reactant may be placed in a vacuum drying oven for drying.

Specifically, the drying temperature for drying the solid reactant may be, but not limited to, 40-70°C.

Specifically, the drying temperature for placing the washed solid reactant in a vacuum drying oven may be 40°C, 50°C, 60°C or 70°C, etc.

When described molybdate selects ammonium molybdate for use, the XRD figure of the molybdenum oxide nanomaterial that finally obtains is as shown in Figure 2, and when described molybdate selects sodium molybdate, the XRD figure of the molybdenum oxide nanomaterial that finally obtains is shown in Figure 2 3. As shown in Fig. 2 and Fig. 3, no matter select ammonium molybdate or select sodium molybdate as described molybdate, can obtain molybdenum oxide nanomaterial, and select sodium molybdate as the XRD of the molybdenum oxide nanomaterial that molybdate obtains There are no miscellaneous peaks in the figure, the purity is high, and the crystallinity is good.

The invention provides a method for preparing a molybdenum oxide nanometer material. Since graphite foil or metal foil is used as positive and negative electrodes respectively, the use of noble metal foil electrodes is reduced and the cost is effectively reduced. The inventive device can be implemented simply in a general beaker or glass vessel, and the selected molybdate as a raw material is relatively common in industry and low in price. The molybdenum oxide nanomaterial of the present invention can be prepared by a one-step method, and the electrochemical operation reaction time is short, the process is simple, the operation is convenient, the conversion rate is high, no by-products are produced, no toxic and harmful gases are produced, and the method is environmentally friendly.

It will be apparent to those skilled in the art that the invention is not limited to the details of the above-described exemplary embodiments, but that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Accordingly, the embodiments should be regarded in all points of view as exemplary and not restrictive, the scope of the invention being defined by the appended claims rather than the foregoing description, and it is therefore intended that the scope of the invention be defined by the appended claims rather than by the foregoing description. All changes within the meaning and range of equivalents of the elements are embraced in the present invention. Any reference sign in a claim should not be construed as limiting the claim concerned.

In addition, it should be understood that although this specification is described according to implementation modes, not each implementation mode only contains an independent technical solution, and this description in the specification is only for clarity, and those skilled in the art should take the specification as a whole , the technical solutions in the various embodiments can also be properly combined to form other implementations that can be understood by those skilled in the art.

Claims (10)

1. A preparation method for molybdenum oxide nanomaterials, characterized in that, comprising: Provide molybdate; Dissolving the molybdate in deionized water to form an electrolyte; Putting double electrodes into the electrolyte, and connecting the electrodes to a power source, so that the electrolyte reacts to obtain a reacted suspension; the electrodes include graphite foil electrodes or metal foil electrodes; The suspension is suction filtered to obtain a solid reactant; The solid reactant is cleaned to obtain molybdenum oxide nanometer material. 2. The method for preparing molybdenum oxide nanomaterials according to claim 1, characterized in that, in the electrolyte, the molar concentration of the molybdate is greater than or equal to 0.05mol/L. 3. the preparation method of molybdenum oxide nano material according to claim 1 is characterized in that, described molybdate comprises ammonium molybdate, sodium molybdate, magnesium molybdate, zinc molybdate, lithium molybdate and manganese molybdate at least one of the 4 . The method for preparing molybdenum oxide nanomaterials according to claim 1 , wherein the molybdate is dissolved in 50-500 mL of deionized water to form the electrolyte. 5. The preparation method of molybdenum oxide nanomaterial according to claim 1, characterized in that, the length of the electrode is 3-8 cm, the width of the electrode is 3-10 cm, and the thickness of the electrode is less than or equal to 0.3 mm . 6. the preparation method of molybdenum oxide nanomaterial according to claim 1 is characterized in that, when described electrode is metal foil electrode, the material of described metal foil electrode comprises iron, aluminum, nickel, copper, zinc and titanium at least one of . 7. the preparation method of molybdenum oxide nanomaterial according to claim 1 is characterized in that, described power supply comprises square-wave stabilized voltage supply, and the voltage of described power supply is 6～20V, and the voltage conversion time of described power supply is 10-60s. 8. The preparation method of molybdenum oxide nanomaterial according to claim 1, characterized in that, the solid reactant is repeatedly cleaned by using absolute ethanol and deionized water. 9. the preparation method of molybdenum oxide nanomaterial according to claim 1, is characterized in that, after described solid reactant is cleaned, before obtaining molybdenum oxide nanomaterial, also comprises: described solid reactant after cleaning to dry. 10 . The method for preparing molybdenum oxide nanomaterials according to claim 9 , characterized in that, the cleaned solid reactants are dried in a vacuum oven at a drying temperature of 40-70° C. 11 .

Images