CN112374538A - Molybdenum trioxide micron rod with adjustable size and preparation method thereof - Google Patents

Molybdenum trioxide micron rod with adjustable size and preparation method thereof Download PDF

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Publication number
CN112374538A
CN112374538A CN201910923689.8A CN201910923689A CN112374538A CN 112374538 A CN112374538 A CN 112374538A CN 201910923689 A CN201910923689 A CN 201910923689A CN 112374538 A CN112374538 A CN 112374538A
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China
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molybdenum trioxide
preparation
adjustable size
molybdate
micrometer rod
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CN201910923689.8A
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孙建之
董岩
王新芳
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Dezhou University
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Dezhou University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G39/00—Compounds of molybdenum
    • C01G39/02—Oxides; Hydroxides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The application belongs to the technical field of electrochemistry, and particularly relates to a method for preparing a molybdenum trioxide micron rod with adjustable size. The invention discloses a preparation method of a molybdenum trioxide micron rod with adjustable size, which comprises the following steps: step 1, pretreating a biological template; step 2, mixing the biological template obtained in the step 1 with molybdate, and then washing and drying the mixture; and 3, putting the biological template obtained in the step 2 into an atmosphere furnace for roasting. Obtaining the molybdenum trioxide micron rod with adjustable size. The application provides a size adjustable molybdenum trioxide micron stick can solve traditional MoO3The material is easy to agglomerate, has different shapes and is used as a secondary battery material with low electrochemical capacity. The application also discloses a molybdenum trioxide micron rod with adjustable size, which can fill the gap of the existing preparation method of the molybdenum trioxide micron rod。

Description

Molybdenum trioxide micron rod with adjustable size and preparation method thereof
Technical Field
The application belongs to the technical field of electrochemistry, and particularly relates to a method for preparing a molybdenum trioxide micron rod with adjustable size.
Background
The large-scale energy storage needs batteries with low price, high safety, long cycle life and no pollution, and the search for a new battery system is urgent. The aluminum ion battery has lower cost compared with other batteries and has outstanding cost advantage.
Due to the unique structure and excellent electrochemical performance, the molybdenum trioxide has wide application in the fields of sensors, photoelectric materials, energy storage materials and the like. Molybdenum trioxide (MoO)3) Is a very worthy of research aluminum ion battery cathode material, and the molybdenum trioxide has unique layered structure and ion-extracting performanceBut is of great interest. Currently, the common methods for molybdenum trioxide include a thermal decomposition method, a sol-gel method, a hydrothermal method, a solvothermal method, and the like. But the production cost is high, the materials are easy to agglomerate, and the electrochemical performance is limited. In conclusion, the development of a preparation method of high-dispersion molybdenum trioxide, which is simple and low in cost, is an urgent technical problem to be solved by those skilled in the art.
The method has less synthesis reports about the high-dispersion molybdenum trioxide micron rods, the experimental process is simple, the operation is easy, and the synthesized rod-shaped MoO is3Good dispersibility, high uniformity and potential application prospect in the field of electrochemistry.
Disclosure of Invention
In view of the above, the first objective of the present application is to provide a molybdenum trioxide micron rod with adjustable size, which can solve the problem of the traditional MoO3Uneven powder size, easy agglomeration and adjustable non-size.
The second purpose of the application is to disclose a preparation method of the molybdenum trioxide nanorod with adjustable size, which can fill the gap of the existing preparation method of molybdenum trioxide.
The invention discloses a molybdenum trioxide micron rod with adjustable size and a preparation method thereof, wherein the preparation method comprises the following steps:
step 1, pretreating a biological template.
And 2, mixing the biological template obtained in the step 1 with molybdate, and then washing and drying.
And 3, putting the biological template obtained in the step 2 into an atmosphere furnace for roasting. Obtaining the high-dispersion molybdenum trioxide micron rods.
Preferably, in step 1, the biological template can be one or more of corn stalk, peanut shell, sodium alginate, starch and yeast.
Preferably, in the step 1, when the biological template is corn stalks or peanut shells, the corn stalks are sliced or crushed, soaked in alkali liquor for a period of time, then washed and dried.
Preferably, in the step 1, when the biological template is corn stalks or peanut shells, the corn stalks can be slices with the thickness of 50-500 μm or powder particles with the particle size of 10-200 μm.
Preferably, in the step 1, when the biological template is corn stalks or peanut shells, the alkali solution may be one or more of a sodium hydroxide solution, a potassium hydroxide solution, a lithium hydroxide solution and ammonia water, and the concentration is 1-30%.
Preferably, in the step 1, when the biological template is corn straw or peanut shell, the soaking time is 2-20 hours, and the ultrasonic dispersion is performed for 1-2 hours during the soaking.
More preferably, in the step 1, when the biological template is corn straws or peanut shells, the effect of ultrasonic dispersion is better for 1-2 hours when the biological template is soaked.
Preferably, in the step 1, when the biological template is corn stalks or peanut shells, the mass ratio of the corn stalks or the peanut shells to the alkali liquor is 1: (10-30).
Preferably, in the step 1, when the biological template is selected from sodium alginate, starch and yeast, the biological template is directly dissolved in water.
Preferably, in the step 2, when the biological template is corn stalks or peanut shells, the corn stalks or peanut shells pretreated in the step 1 are soaked in a molybdate solution for a period of time, and then the steps of washing, drying and repeated soaking-drying are carried out for a plurality of times.
Preferably, in step 2, the molybdate may be one or more of ammonium molybdate, sodium molybdate, potassium molybdate, cobalt molybdate, manganese molybdate and nickel molybdate.
Preferably, in the step 2, the concentration of the molybdate is 0.1-2 mol/L, the soaking time is 12-36 hours each time, and the soaking-drying step is repeated for 2-10 times.
Preferably, in the step 2, the mass ratio of the biological template to the molybdate is 1: (5-10).
Preferably, in step 3, the gas introduced into the atmosphere furnace during the calcination may be one or more of air, nitrogen, argon and hydrogen.
Preferably, in the step 3, the roasting temperature is 300-600 ℃, the temperature rising speed is 0.5-5 ℃/min, and the roasting time is 2-10 hours.
The invention also provides a molybdenum trioxide micron rod with adjustable size, which is prepared by the preparation method.
Preferably, the length range of the molybdenum trioxide micrometer rod with adjustable size is as follows: 2-100 μm, and the diameter of the cross section is 1-15 μm.
The invention discovers that the high-dispersion molybdenum trioxide nanorods are beneficial to the embedding and the separation of ions, and can improve the electronic conductivity and the ionic conductivity of the material, thereby improving the electrochemical capacity of the material. Therefore, the invention creatively provides the molybdenum trioxide micron rod with adjustable size. Meanwhile, the preparation method of the molybdenum trioxide micrometer rod with adjustable size provided by the invention is very simple, firstly a biological template is pretreated, then a molybdate solution is adsorbed by the template, and the molybdenum trioxide micrometer rod with high dispersion and adjustable size is prepared by utilizing a thermal decomposition reaction, wherein the biological template method is also the invention point of the invention. The preparation method of the biological template method and the molybdenum trioxide micrometer rod with adjustable size is simple, does not need expensive instruments, and has high yield and low cost. The prepared molybdenum trioxide micron rod is free from agglomeration and high in dispersibility.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 shows an SEM image of molybdenum trioxide nanorods prepared in example 1 provided herein;
FIG. 2 shows an SEM image of molybdenum trioxide nanorods prepared in example 2 provided herein;
Detailed Description
The application provides a molybdenum trioxide micron rod with adjustable size and a preparation method thereof, which are used for solving the problems that the traditional MoO3 is irregular in shape and MoO3The technical defect that the powder is easy to agglomerate can be overcome, and the gap of the preparation method of the molybdenum trioxide micron rod with adjustable size at present can be filled.
The technical solutions in the embodiments of the present application will be described clearly and completely below, and it should be understood that the described embodiments are only a part of the embodiments of the present application, and not all 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 application.
The raw materials used in the following examples are all commercially available or self-made.
Example 1
The embodiment provides a specific implementation manner of a preparation method of a molybdenum trioxide micron rod with adjustable size, which comprises the following steps:
1. removing the outer skin of the corn straw, and cutting into slices with the thickness of 0.1 mm;
2. weighing 0.3g of slice, and soaking in 100mL of 5% ammonia water solution for 10 hours; washing with distilled water for 3 times;
3. washing with distilled water for 3 times, and washing off ammonia water and soluble substances in the pore canal of the corn stalk;
4. placing the washed slices in an oven, and drying at 60 ℃ for 3h for later use;
5. soaking the corn straw slices treated in the step at room temperature in 100mL of 0.5 mol/L ammonium molybdate solution for 24 hours;
6. washing the soaked corn stalk slices with distilled water for 3 times, drying in a 60 ℃ oven, and repeating the soaking-drying operation for 3 times.
7. And putting the dried sample into a muffle furnace for roasting. The temperature rise speed is 2 ℃/min, the temperature is firstly preserved for 1 hour at 300 ℃, then the temperature is raised to 550 ℃, and the temperature is preserved for 3 hours, and finally the white molybdenum trioxide sample is prepared.
8. SEM detection and particle size measurement were performed on the molybdenum trioxide nanorods prepared in this example, and the length of the molybdenum trioxide nanorods in this example was: 2-20 μm and a cross-sectional diameter of about 1-2 μm.
Example 2
1. 2g of ammonium molybdate was dissolved in 10mL of water to prepare an ammonium molybdate solution;
2. dissolving 0.2g of sodium alginate in 20mL of water to prepare a sodium alginate solution;
3. slowly dripping ammonium molybdate solution into the sodium alginate solution, firstly stirring for 1 hour, and then placing the solution on a speed-regulating multipurpose oscillator for oscillation for 4 hours to enable the solution to be gelatinous;
4. drying the gel-like substance in a vacuum drying oven at 35 deg.C for 5 hr, and drying in an oven at 60 deg.C for 24 hr to obtain transparent film-like substance;
5. and (3) treating the transparent film-shaped substance in a high-temperature furnace at the temperature of 300 ℃ for 3 hours to finally prepare a white molybdenum trioxide sample.
6. SEM detection and particle size measurement were performed on the molybdenum trioxide nanorods prepared in this example, and the length of the molybdenum trioxide nanorods in this example was: 30-100 μm and a cross-sectional diameter of about 5-15 μm.

Claims (10)

1. A molybdenum trioxide micron rod with adjustable size and a preparation method thereof are characterized in that: the length range of the molybdenum trioxide micrometer rod is as follows: 2-100 μm, and the diameter of the cross section is 1-15 μm.
2. A molybdenum trioxide micron rod with adjustable size and a preparation method thereof are characterized in that: the method comprises the following steps:
step 1, pretreating a biological template;
step 2, mixing the biological template obtained in the step 1 with molybdate, and then washing and drying the mixture;
and 3, putting the biological template obtained in the step 2 into an atmosphere furnace for roasting to obtain the high-dispersion molybdenum trioxide nanorods.
3. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 1, the biological template can be one or more of corn straw, peanut shell, sodium alginate, starch and yeast, and the corn straw and the peanut shell can be in a sheet shape or a powder shape.
4. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 1, when the biological template is pretreated, the alkali liquor is selected from one or more of sodium hydroxide, potassium hydroxide, lithium hydroxide and ammonia water, and the concentration is 1-30%.
5. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 1, the mass ratio of the biological template to the alkali liquor is 1: (10-30).
6. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in step 2, the molybdate may be one or more of ammonium molybdate, sodium molybdate, potassium molybdate, cobalt molybdate, manganese molybdate, iron molybdate, and nickel molybdate.
7. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 2, the concentration of the molybdate is 0.1-2 mol/L, and the mixing time is 12-36 hours each time.
8. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 2, the mass ratio of the biological template to the molybdate is 1: (5-10).
9. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in step 3, the gas introduced into the atmosphere furnace during the calcination may be one or more of air, nitrogen, argon and hydrogen.
10. The molybdenum trioxide micrometer rod with adjustable size and the preparation method thereof as claimed in claim 2, wherein the molybdenum trioxide micrometer rod comprises the following components: in the step 3, the roasting temperature is 300-600 ℃, the temperature rising speed is 0.5-5 ℃/min, and the roasting time is 2-10 hours.
CN201910923689.8A 2019-09-27 2019-09-27 Molybdenum trioxide micron rod with adjustable size and preparation method thereof Pending CN112374538A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1762831A (en) * 2005-09-01 2006-04-26 武汉理工大学 Molybdenum trioxide laminated nanometer bar and preparation method
CN101125683A (en) * 2007-07-14 2008-02-20 安徽大学 Preparation method for photocatalysis water-purifying material MoO3 and application thereof
CN101412541A (en) * 2007-10-19 2009-04-22 中国科学院大连化学物理研究所 Method for synthesizing rod-like and echinoid molybdena-based nano-material

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1762831A (en) * 2005-09-01 2006-04-26 武汉理工大学 Molybdenum trioxide laminated nanometer bar and preparation method
CN101125683A (en) * 2007-07-14 2008-02-20 安徽大学 Preparation method for photocatalysis water-purifying material MoO3 and application thereof
CN101412541A (en) * 2007-10-19 2009-04-22 中国科学院大连化学物理研究所 Method for synthesizing rod-like and echinoid molybdena-based nano-material

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
DONGLIANG YAN: "Single-crystalline a-MoO3 microbelts derived from a bio-templating", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *
JIA LI: "Synthesis of a BiomorphicMolybdenum Trioxide Templated from Paper", 《JOURNAL OF THE AMERICAN CERAMIC SOCIETY》 *

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