CN111807415B - Fe 2 Mo 3 O 8 Micron-sized hollow sphere and preparation method thereof - Google Patents
Fe 2 Mo 3 O 8 Micron-sized hollow sphere and preparation method thereof Download PDFInfo
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- CN111807415B CN111807415B CN202010718002.XA CN202010718002A CN111807415B CN 111807415 B CN111807415 B CN 111807415B CN 202010718002 A CN202010718002 A CN 202010718002A CN 111807415 B CN111807415 B CN 111807415B
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Abstract
The invention discloses Fe 2 Mo 3 O 8 Micron hollow ball and its preparation process, and belongs to the field of nanometer material synthesis. Fe of the invention 2 Mo 3 O 8 Method for preparing micron hollow ball from ironSalt and molybdate are used as raw materials, and Fe is synthesized by combining a hydrothermal method with a calcination method 2 Mo 3 O 8 The micron hollow spheres have short reaction time, mild reaction conditions, easy repetition and suitability for low-cost mass production. The preparation method of the invention can be used for treating Fe by changing reaction parameters 2 Mo 3 O 8 The size of the micron hollow sphere is regulated and controlled to prepare Fe 2 Mo 3 O 8 The micron hollow sphere has stable shape, no agglomeration, high purity and high crystallinity.
Description
Technical Field
The invention belongs to the field of synthesis of nano materials, and particularly relates to Fe 2 Mo 3 O 8 Micron-sized hollow spheres and a preparation method thereof.
Background
Fe 2 Mo 3 O 8 The micro-nano material is an important inorganic functional material and has wide application in the fields of catalysis, adsorption, electromagnetism, sensors, energy storage and the like. In iron molybdate micro-nano materials, transition metals of iron and molybdenum have special crystal structures and performances of electrochemistry, catalysis and the like due to the existence of empty orbits, and are paid more and more attention.
For example, chinese patent CN201811410837.8 carries out synthetic reaction of molybdenum source and iron source in ionic liquid to obtain the product with specific surface area of 50-200 m 2 The iron molybdate material per gram shows better catalytic activity in the catalytic oxidation reaction. Chinese patent CN201710315937.1 prepares a monoclinic-crystal-form iron molybdate nanosheet with high activity and exposed crystal face by adding a crystal face control agent sodium nitrate or sodium fluoride, and has high catalytic activity in the reaction of catalyzing methanol to be converted into formaldehyde. Chinese patents CN201110347429.4 and CN201110347463.1 disclose that microwave reaction is used to prepare iron molybdate nanocones and iron molybdate nanosheets, and the method has short reaction time, but uses a microwave reactor, which is not beneficial to industrial low-cost mass production of products. The preparation method disclosed above still has certain technical improvement space in the aspects of product size control, low-cost preparation and the like. Fe 2 Mo 3 O 8 As one kind of inorganic molybdate micro-nano material, at present, the preparation method thereof has no large rangeReporting. Fe relative to other iron-based molybdates 2 Mo 3 O 8 The shape of the Fe alloy is relatively single, mainly in the shape of particles and sheets, for example, chinese patent CN201610211193.4 discloses a two-dimensional Fe with adjustable oxygen vacancy 2 Mo 3 O 8 Nano-oxide and preparation method thereof, but Fe prepared by nano-oxide 2 Mo 3 O 8 The nano-sheet has certain product agglomeration phenomenon, which is not beneficial to the aspects of energy storage, catalysis and the like of the product.
Disclosure of Invention
The object of the present invention is to overcome the disadvantages of the prior art mentioned above and to provide a Fe alloy 2 Mo 3 O 8 Micron-sized hollow spheres and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
fe 2 Mo 3 O 8 The preparation method of the micron-sized hollow sphere comprises the following steps:
1) Adding iron acetate into a mixed solution of deionized water and ethylene glycol, and uniformly stirring to obtain a mixed solution A;
adding sodium molybdate into a mixed solution of deionized water and ethylene glycol, and uniformly stirring to obtain a mixed solution B;
2) Dropwise adding the mixed solution A into the mixed solution B to obtain a precursor;
3) Transferring the precursor into a reaction kettle for hydrothermal reaction;
the hydrothermal reaction conditions are as follows: the temperature is 150 ℃, and the time is 5h;
4) After the hydrothermal reaction is finished, centrifugally washing a reaction product, then calcining under argon, and obtaining Fe after calcining is finished 2 Mo 3 O 8 Micron-sized hollow spheres.
Further, in step 1), the volume ratio of the deionized water to the ethylene glycol in the mixed solution a is 1.
Further, in the step 1), the volume ratio of the deionized water to the ethylene glycol in the mixed solution B is 1.
Further, in the step 2), the dropping rate is 2mL/min or less.
Further, in the step 4), the reaction product is centrifugally washed for more than 5 times to remove impurities.
Further, in the step 4), the calcining temperature is 400-600 ℃.
Further, in the step 4), the calcination time is 1-3h.
Fe of the present invention 2 Mo 3 O 8 Micron-sized hollow spheres of Fe 2 Mo 3 O 8 The micron hollow sphere has an outer diameter of 0.7-1.2 μm and a sphere wall thickness of 110-130nm.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides Fe 2 Mo 3 O 8 The preparation method of the micron-sized hollow sphere takes iron salt and molybdate as raw materials, and Fe is firstly synthesized by combining a hydrothermal method with a calcination method 2 Mo 3 O 8 The micron hollow spheres have short reaction time, mild reaction conditions, easy repetition and suitability for low-cost mass production. The preparation method of the invention can be used for treating Fe by changing reaction parameters 2 Mo 3 O 8 The size of the micron hollow sphere is regulated and controlled to prepare Fe 2 Mo 3 O 8 The micron hollow sphere has stable shape, no agglomeration, high purity and high crystallinity.
Fe of the invention 2 Mo 3 O 8 The micron hollow sphere and hollow sphere structure is beneficial to full contact between electrolyte and active substances, and the unique structure of the micron hollow sphere and hollow sphere structure provides theoretical basis and practical experience for wide application of iron molybdate micro-nano materials in the fields of energy storage, catalysis and the like.
Drawings
FIG. 1 is Fe of example 1 2 Mo 3 O 8 A transmission electron microscope image of the micron-sized hollow sphere;
FIG. 2 shows Fe in example 1 2 Mo 3 O 8 XRD pattern of micron-sized hollow sphere;
FIG. 3 is Fe of example 1 2 Mo 3 O 8 Micron-sized hollow sphere charge-discharge diagram.
Detailed Description
In order to make the technical solutions of the present invention better understood, 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.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
Example 1
Preparing a mixed solution of deionized water and ethylene glycol, wherein the volume ratio of the deionized water to the ethylene glycol is 1;
under electromagnetic stirring, 100mg of iron acetate is added into 100ml of mixed solution, and stirring is carried out for 10min;
then adding 100mg of sodium molybdate into another 100ml of mixed solution, and stirring for 10min;
then dropwise adding the iron acetate solution into the sodium molybdate solution, and controlling the dropwise adding speed to be 2mL/min to obtain a precursor;
and transferring the precursor into a reaction kettle, and carrying out hydrothermal heat preservation for 5 hours at the temperature of 150 ℃. After the reaction is finished, naturally cooling to room temperature;
the reaction product was washed 5 times by centrifugation with deionized water and ethanol (volume ratio 1. After removal of impurities, calcination was carried out at 400 ℃ for 1h under argon to obtain the final product.
Referring to FIG. 1, FIG. 1 shows Fe prepared by the present invention 2 Mo 3 O 8 TEM image of micron-sized hollow spheres, fe prepared therein 2 Mo 3 O8 had a diameter of 1.2 μm and a thickness of 130nm.
Referring to FIG. 2, FIG. 2 is an XRD pattern of the product of example 1, from which the composition of the phase can be determined as Fe 2 Mo 3 O 8 。
Referring to FIG. 3, FIG. 3 shows Fe 2 Mo 3 O 8 And the micron-sized hollow spheres are used as a charge-discharge diagram of the lithium ion battery cathode material, wherein the discharge specific capacity and the charge specific capacity are 1189mAh/g and 997mAh/g respectively under the condition that the current density is 100 mA/g.
The invention completes Fe by utilizing cheap and easily obtained raw materials and simple, convenient and efficient preparation conditions 2 Mo 3 O 8 And obtaining the shape of the micron-sized hollow sphere. Provides good theoretical basis and practical experience for the design and synthesis of the iron-based molybdate micro-nano material.
Example 2
Preparing a mixed solution of deionized water and ethylene glycol, wherein the volume ratio of the deionized water to the ethylene glycol is 1;
under electromagnetic stirring, adding 100mg of iron acetate into 50ml of the mixed solution, and stirring for 5min;
then adding 100mg of sodium molybdate into another 50ml of mixed solution, and stirring for 6min;
then dropwise adding the iron acetate solution into the sodium molybdate solution, and controlling the dropwise adding speed to be 1mL/min to obtain a precursor;
and transferring the precursor into a reaction kettle, and carrying out hydrothermal heat preservation for 5 hours at the temperature of 150 ℃. After the reaction is finished, naturally cooling to room temperature;
the reaction product was washed 6 times by centrifugation with deionized water and ethanol (volume ratio 1. After removal of impurities, calcination was carried out at 600 ℃ for 1h under argon to give the final product.
Example 3
Preparing a mixed solution of deionized water and ethylene glycol, wherein the volume ratio of the deionized water to the ethylene glycol is 1;
under electromagnetic stirring, adding 100mg of iron acetate into 60ml of the mixed solution, and stirring for 8min;
then adding 100mg of sodium molybdate into another 60ml of mixed solution, and stirring for 10min;
then dropwise adding the iron acetate solution into the sodium molybdate solution, and controlling the dropwise adding speed to be 2mL/min to obtain a precursor;
and transferring the precursor into a reaction kettle, and carrying out hydrothermal heat preservation for 5 hours at the temperature of 150 ℃. After the reaction is finished, naturally cooling to room temperature;
the reaction product was washed 5 times by centrifugation with deionized water and ethanol (volume ratio 1. After removal of impurities, calcination was carried out at 500 ℃ for 3h under argon to obtain the final product.
Example 4
Preparing a mixed solution of deionized water and ethylene glycol, wherein the volume ratio of the deionized water to the ethylene glycol is 1;
under electromagnetic stirring, adding 100mg of iron acetate into 30ml of the mixed solution, and stirring for 10min;
then adding 100mg of sodium molybdate into another 30ml of mixed solution, and stirring for 10min;
then dropwise adding the iron acetate solution into the sodium molybdate solution, and controlling the dropwise adding speed to be 2mL/min to obtain a precursor;
and transferring the precursor into a reaction kettle, and carrying out hydrothermal heat preservation for 5 hours at the temperature of 150 ℃. After the reaction is finished, naturally cooling to room temperature;
the reaction product was washed 5 times by centrifugation with deionized water and ethanol (volume ratio 1. After removal of impurities, calcination was carried out at 550 ℃ for 2h under argon to give the final product.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (6)
1. Fe 2 Mo 3 O 8 The preparation method of the micron-sized hollow sphere is characterized by comprising the following steps of:
1) Adding iron acetate into a mixed solution of deionized water and ethylene glycol, and uniformly stirring to obtain a mixed solution A;
adding sodium molybdate into a mixed solution of deionized water and ethylene glycol, and uniformly stirring to obtain a mixed solution B;
2) Dropwise adding the mixed solution A into the mixed solution B to obtain a precursor;
3) Transferring the precursor into a reaction kettle for hydrothermal reaction;
the hydrothermal reaction conditions are as follows: the temperature is 150 ℃, and the time is 5h;
4) After the hydrothermal reaction is finished, centrifugally washing a reaction product, then calcining under argon, and obtaining Fe after calcining is finished 2 Mo 3 O 8 Micron-sized hollow spheres;
the calcining temperature is 400-600 ℃, and the calcining time is 1-3h.
2. Fe of claim 1 2 Mo 3 O 8 The preparation method of the micron-sized hollow spheres is characterized in that in the step 1), the volume ratio of deionized water to ethylene glycol in the mixed solution A is 1.
3. Fe of claim 1 2 Mo 3 O 8 The preparation method of the micron hollow sphere is characterized in that in the step 1), the volume ratio of deionized water to ethylene glycol in the mixed solution B is 1.
4. Fe of claim 1 2 Mo 3 O 8 The preparation method of the micron hollow sphere is characterized in that in the step 2), the dropping speed is below 2 mL/min.
5. Fe of claim 1 2 Mo 3 O 8 The preparation method of the micron hollow sphere is characterized in thatIn the step 4), the reaction product is centrifugally washed for 5 times or more to remove impurities.
6. Fe prepared by the method of any one of claims 1 to 5 2 Mo 3 O 8 The micron hollow ball is characterized in that Fe 2 Mo 3 O 8 The micron hollow sphere has an outer diameter of 0.7-1.2 μm and a sphere wall thickness of 110-130nm.
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| CN115536079B (en) * | 2022-11-21 | 2023-08-11 | 齐鲁工业大学 | Self-template method for synthesizing hollow spherical molybdate micro-nano material with multilevel structure and preparation method thereof |
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| CN105712406B (en) * | 2016-04-07 | 2017-03-29 | 安徽工程大学 | A kind of two-dimentional Fe2Mo3O8Nano-oxide and preparation method thereof |
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