CN110723752A - Preparation method of special-shaped nano MoS2 material - Google Patents
Preparation method of special-shaped nano MoS2 material Download PDFInfo
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- CN110723752A CN110723752A CN201911080287.2A CN201911080287A CN110723752A CN 110723752 A CN110723752 A CN 110723752A CN 201911080287 A CN201911080287 A CN 201911080287A CN 110723752 A CN110723752 A CN 110723752A
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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
- C01G39/06—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- 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
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The invention relates to the technical field of MoS2 material preparation, and discloses a preparation method of a special-shaped nano-sized MoS2 material, which comprises the following steps of; s1, preparing materials, namely firstly preparing sodium sulfide, sodium molybdate, water and a reaction vessel; s2, adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, and stirring and mixing for 10-15 minutes by using stirring equipment; s3, adding a certain amount of sulfuric acid and a catalyst solution into the mixed solution of sodium sulfide and sodium molybdate in the reaction vessel, and finally reacting to generate brown molybdenum trisulfide paste-shaped precipitate at the bottom of the reaction vessel. The preparation method of the special-shaped nano-sized MoS2 material has the advantages of simple reaction process of the special-shaped nano-sized MoS2 material, convenience in operation and high yield of the special-shaped nano-sized MoS2 material, reduces the production cost of the special-shaped nano-sized MoS2 material, and facilitates large-scale industrial production of the special-shaped nano-sized MoS2 material.
Description
Technical Field
The invention relates to the technical field of preparation of MoS2 materials, in particular to a preparation method of a special-shaped nano-sized MoS2 material.
Background
As a common solid lubricant, on one hand, because the molybdenum disulfide has a layered structure, the bonding force of sulfur atoms between layers is weak, the molybdenum disulfide is easy to slide, so that a good antifriction effect is shown, on the other hand, the sulfur atoms exposed on the surface of a crystal generate a strong adhesion effect on the surface of metal, so that the formed firm film lubricating property is superior to that of graphite, and compared with the common molybdenum disulfide, the nano molybdenum disulfide has many excellent properties such as excellent friction property, large specific surface area, stronger adsorption capacity, high reaction activity, and the catalytic property, particularly the catalytic hydrodesulfurization property, is stronger, and can be used for preparing special catalytic materials and gas storage materials. The nano-intercalation composite material formed by inserting other groups between nano-molybdenum disulfide layers has a plurality of excellent physical properties, such as functions of light, electricity, magnetic catalysis, lubrication and the like, so that the preparation of the molybdenum disulfide nano-material becomes a hot point of research of people.
The existing preparation process of the special-shaped nano-sized MoS2 material is too complicated, and the time and labor of the rice and grass are consumed, so that the yield of the special-shaped nano-sized MoS2 material is low, the preparation cost is high, and the large-scale industrial production of the special-shaped nano-sized MoS2 material is inconvenient.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method of a special-shaped nano-sized MoS2 material, which has the advantages of simple reaction process, convenient operation and high yield of the special-shaped nano-sized MoS2 material, simultaneously reduces the production cost of the special-shaped nano-sized MoS2 material, facilitates large-scale industrial production of the special-shaped nano-sized MoS2 material and the like, and solves the problems that the preparation process of the special-shaped nano-sized MoS2 material is too complicated, and the time and labor are consumed by millet and grass, so that the yield of the special-shaped nano-sized MoS2 material is low, the preparation cost is high, and the large-scale industrial production of the special-shaped nano-sized MoS2 material is.
(II) technical scheme
In order to realize the advantages of simple reaction process, convenient operation and high yield of the special-shaped nano-grade MoS2 material, reduce the production cost of the special-shaped nano-grade MoS2 material and facilitate the large-scale industrial production of the special-shaped nano-grade MoS2 material, the invention provides the following technical scheme: a preparation method of a special-shaped nano-grade MoS2 material comprises the following steps;
s1, preparing materials, namely firstly preparing sodium sulfide, sodium molybdate, water and a reaction vessel;
s2, adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, and stirring and mixing for 10-15 minutes by using stirring equipment;
s3, adding a certain amount of sulfuric acid and a catalyst solution into the mixed solution of sodium sulfide and sodium molybdate in the reaction vessel, and finally reacting to generate brown molybdenum trisulfide paste precipitate at the bottom of the reaction vessel;
s4, taking out the pasty molybdenum trisulfide, and cleaning the pasty molybdenum trisulfide by distilled water to remove impurity ions in the molybdenum trisulfide;
s5, passing the cleaned pasty molybdenum trisulfide through a dryer, and drying for 25-30 minutes to ensure that the pasty molybdenum trisulfide can be fully dried;
s6, grinding the dried molybdenum trisulfide powder in a mortar for about 1 hour to ensure that the particle size of the molybdenum trisulfide powder is less than 256 nanometers;
and S7, feeding the molybdenum trisulfide powder into roasting equipment to roast for 30-40 minutes, and roasting and desulfurizing the molybdenum trisulfide powder in a hydrogen environment to obtain the special-shaped nano-grade molybdenum disulfide material.
Preferably, the temperature of the calcination in the step S7 is 650-750 ℃.
Preferably, in step S1, the sodium sulfide is prepared by mixing mirabilite and coal powder in a ratio of 100: the sodium molybdate is prepared by oxidizing and roasting molybdenum concentrate to generate molybdenum trioxide, leaching with alkali liquor to obtain a sodium molybdate solution, and then carrying out suction filtration, evaporative concentration, cooling crystallization and drying on a leachate to obtain the sodium molybdate solution.
Preferably, the reaction vessel in step S1 is generally a reaction kettle.
Preferably, the drying in step S5 is drying at an air temperature of 450-510 ℃ for 25-30 minutes.
Preferably, the sulfuric acid in step S3 is prepared by heating iron disulfide under oxygen atmosphere at high temperature to obtain sulfur dioxide, introducing the sulfur dioxide into water to easily obtain sulfurous acid, and oxidizing the sulfurous acid.
Preferably, the drying step in step S5 requires a mixer to mix and dry the mixture.
(III) advantageous effects
Compared with the prior art, the invention provides a preparation method of the special-shaped nano-grade MoS2 material, which has the following beneficial effects:
the preparation method of the special-shaped nano-sized MoS2 material comprises the steps of adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, adding a certain amount of sulfuric acid and a catalyst solution into the mixed solution of sodium sulfide and sodium molybdate in the reaction vessel, finally reacting to generate brown molybdenum trisulfide paste precipitate at the bottom of the reaction vessel, taking out the paste molybdenum trisulfide, cleaning the paste molybdenum trisulfide by distilled water, fully drying the cleaned paste molybdenum trisulfide by a dryer, grinding the dried molybdenum trisulfide powder in a mortar, sending the molybdenum trisulfide powder into a roasting device for roasting for 30-40 minutes, roasting and desulfurizing the molybdenum trisulfide powder in a hydrogen environment to obtain the special-shaped nano-sized molybdenum disulfide material, wherein the preparation method has the advantages of simple reaction process and convenient operation of the special-shaped nano-sized MoS2 material, the special-shaped nano-grade MoS2 material has the advantage of high yield, reduces the production cost of the special-shaped nano-grade MoS2 material, and is convenient for large-scale industrial production of the special-shaped nano-grade MoS2 material.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, 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 invention.
A preparation method of a special-shaped nano-grade MoS2 material comprises the following steps;
s1, preparing materials, namely firstly preparing sodium sulfide, sodium molybdate, water and a reaction vessel;
s2, adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, and stirring and mixing for 10-15 minutes by using stirring equipment, wherein the sodium sulfide and the sodium molybdate can be uniformly mixed in the water by using a stirrer;
s3, adding a certain amount of sulfuric acid and a catalyst solution into the mixed solution of sodium sulfide and sodium molybdate in the reaction vessel, and finally reacting to generate brown molybdenum trisulfide paste precipitate at the bottom of the reaction vessel;
s4, taking out the pasty molybdenum trisulfide, and cleaning the pasty molybdenum trisulfide by distilled water to remove impurity ions in the molybdenum trisulfide and ensure the quality of the special-shaped nano MoS2 material;
s5, passing the cleaned pasty molybdenum trisulfide through a dryer, and drying for 25-30 minutes to ensure that the pasty molybdenum trisulfide can be fully dried;
s6, grinding the dried molybdenum trisulfide powder in a mortar for about 1 hour to ensure that the particle size of the molybdenum trisulfide powder is less than 256 nanometers;
and S7, feeding the molybdenum trisulfide powder into roasting equipment to roast for 30-40 minutes, and roasting and desulfurizing the molybdenum trisulfide powder in a hydrogen environment to obtain the special-shaped nano-grade molybdenum disulfide material.
The roasting temperature in the step S7 is 650-750 ℃, the high temperature can ensure the roasting quality of the molybdenum disulfide, and the preparation method has the advantages of simple reaction process of the special-shaped nano-grade MoS2 material, convenient operation and high yield of the special-shaped nano-grade MoS2 material.
In the step S1, sodium sulfide is prepared by mixing mirabilite and coal powder according to the ratio of 100: the preparation method comprises the following steps of mixing the components in a proportion of 22 weight parts, calcining and reducing at a high temperature of 850-1050 ℃, cooling a product, dissolving the product into liquid by using dilute alkali liquor, standing and clarifying, carrying out evaporation concentration on upper concentrated alkali liquor, carrying out leaching on sodium molybdate by using alkali liquor to obtain a sodium molybdate solution, and carrying out suction filtration, evaporation concentration, cooling crystallization and drying on a leachate to obtain the sodium molybdate solution.
In the step S1, the reaction vessel is generally a reaction kettle, and the reaction kettle is suitable for synthesizing various materials under different reaction conditions, thereby ensuring the quality of material synthesis.
The drying in step S5 is drying at the drying temperature of 450-510 ℃ for 25-30 minutes in the air range.
Step S3 the sulfuric acid is prepared by heating iron disulfide at high temperature in oxygen environment to obtain sulfur dioxide, introducing sulfur dioxide into water to easily obtain sulfurous acid, and oxidizing sulfurous acid.
The drying process in the step S5 needs to be matched with a stirrer to stir and dry, the stirring and drying can increase the drying area of the paste molybdenum trisulfide, and meanwhile, the drying efficiency of the paste molybdenum trisulfide can be improved.
In conclusion, the preparation method of the special-shaped nano-sized MoS2 material comprises the steps of adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, stirring and mixing for 10-15 minutes by a stirring device, adding a certain amount of sulfuric acid and a catalyst solution into a mixed solution of the sodium sulfide and the sodium molybdate in the reaction vessel, finally reacting to generate brown molybdenum trisulfide paste precipitate at the bottom of the reaction vessel, taking out the paste molybdenum trisulfide for cleaning by distilled water, removing impurity ions in the molybdenum trisulfide, passing the cleaned paste molybdenum trisulfide through a dryer, drying for 25-30 minutes to ensure that the paste molybdenum trisulfide can be fully dried, then grinding the dried molybdenum trisulfide powder in a mortar for about 1 hour to ensure that the particles of the molybdenum trisulfide are less than 256 nanometers, then sending the molybdenum trisulfide powder into a roasting device for roasting for 30-40 minutes, meanwhile, the special-shaped nano-grade molybdenum disulfide material is obtained by roasting and desulfurizing the molybdenum trisulfide powder in a hydrogen environment, and the preparation method has the advantages of simple reaction process of the special-shaped nano-grade MoS2 material, convenience in operation and high yield of the special-shaped nano-grade MoS2 material, reduces the production cost of the special-shaped nano-grade MoS2 material, and facilitates large-scale industrial production of the special-shaped nano-grade MoS2 material.
It is to be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (7)
1. A preparation method of a special-shaped nano-grade MoS2 material is characterized by comprising the following steps: comprises the following steps;
s1, preparing materials, namely firstly preparing sodium sulfide, sodium molybdate, water and a reaction vessel;
s2, adding a certain amount of sodium sulfide and sodium molybdate into a reaction vessel, adding water into the reaction vessel for mixing, and stirring and mixing for 10-15 minutes by using stirring equipment;
s3, adding a certain amount of sulfuric acid and a catalyst solution into the mixed solution of sodium sulfide and sodium molybdate in the reaction vessel, and finally reacting to generate brown molybdenum trisulfide paste precipitate at the bottom of the reaction vessel;
s4, taking out the pasty molybdenum trisulfide, and cleaning the pasty molybdenum trisulfide by distilled water to remove impurity ions in the molybdenum trisulfide;
s5, passing the cleaned pasty molybdenum trisulfide through a dryer, and drying for 25-30 minutes to ensure that the pasty molybdenum trisulfide can be fully dried;
s6, grinding the dried molybdenum trisulfide powder in a mortar for about 1 hour to ensure that the particle size of the molybdenum trisulfide powder is less than 256 nanometers;
and S7, feeding the molybdenum trisulfide powder into roasting equipment to roast for 30-40 minutes, and roasting and desulfurizing the molybdenum trisulfide powder in a hydrogen environment to obtain the special-shaped nano-grade molybdenum disulfide material.
2. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: the temperature of the calcination in the step S7 is 650-750 ℃.
3. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: in the step S1, the sodium sulfide is prepared by mixing mirabilite and coal powder according to the weight ratio of 100: the sodium molybdate is prepared by oxidizing and roasting molybdenum concentrate to generate molybdenum trioxide, leaching with alkali liquor to obtain a sodium molybdate solution, and then carrying out suction filtration, evaporative concentration, cooling crystallization and drying on a leachate to obtain the sodium molybdate solution.
4. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: the reaction vessel in step S1 is typically a reaction kettle.
5. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: in step S5, the drying is carried out at an air temperature of 450-510 ℃ for 25-30 minutes.
6. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: the sulfuric acid in the step S3 is prepared by heating iron disulfide at high temperature in an oxygen environment to prepare sulfur dioxide, then introducing the sulfur dioxide into water to prepare sulfurous acid easily, and finally oxidizing the sulfurous acid.
7. The method for preparing the specially-shaped nano-sized MoS2 material according to claim 1, wherein the method comprises the following steps: in the step S5, the drying process needs to be performed by a stirrer.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114455635A (en) * | 2022-03-11 | 2022-05-10 | 合肥学院 | Method for reducing particle size of hollow spherical nano molybdenum disulfide and improving shape regularity |
| CN116462228A (en) * | 2023-05-05 | 2023-07-21 | 四川顺应动力电池材料有限公司 | Method for producing high-purity molybdenum trioxide by crude sodium molybdate solution in short process |
-
2019
- 2019-11-07 CN CN201911080287.2A patent/CN110723752A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114455635A (en) * | 2022-03-11 | 2022-05-10 | 合肥学院 | Method for reducing particle size of hollow spherical nano molybdenum disulfide and improving shape regularity |
| CN114455635B (en) * | 2022-03-11 | 2023-09-15 | 合肥学院 | Method for reducing particle size and improving morphology regularity of hollow spherical nano molybdenum disulfide |
| CN116462228A (en) * | 2023-05-05 | 2023-07-21 | 四川顺应动力电池材料有限公司 | Method for producing high-purity molybdenum trioxide by crude sodium molybdate solution in short process |
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