CN103613137A - Hydrothermal synthesis method of molybdenum disulfide nano flowers - Google Patents
Hydrothermal synthesis method of molybdenum disulfide nano flowers Download PDFInfo
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- CN103613137A CN103613137A CN201310547151.4A CN201310547151A CN103613137A CN 103613137 A CN103613137 A CN 103613137A CN 201310547151 A CN201310547151 A CN 201310547151A CN 103613137 A CN103613137 A CN 103613137A
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Abstract
The invention discloses a hydrothermal synthesis method of molybdenum disulfide nano flowers. The hydrothermal synthesis method mainly comprises the following steps: adding an inorganic molybdenum source, an organic sulfur source and a proper amount of reducing agent into deionized water, uniformly mixing the ingredients, transferring the mixture into a high pressure reaction kettle, and then heating the mixture at a high temperature for 24 hours; washing and centrifugally separating the obtained solution for multiple times, and finally drying the solution to obtain black solid powder, namely, the molybdenum disulfide nano flowers. The hydrothermal synthesis method disclosed by the invention has the beneficial effects that the whole reaction and drying process is carried out in a sealed environment to avoid direct air exposure so as to ensure the product purity; since the reducing agent adopted by the hydrothermal synthesis method disclosed by the invention can be both used as the sulfur source and as a catalyst, no impurity is generated, and thus, the product purity is further improved.
Description
Technical field
The present invention relates to a kind of synthetic method of nano flower, particularly relate to a kind of hydrothermal synthesis method of molybdenum disulfide nano flower.
Background technology
Nano material refers in three-dimensional space, to have one dimension at least in nanoscale scope or the material that consists of as elementary cell them.Nano material, due to its small size, can produce significant variation in physics and chemistry properties conventionally.These change, and the applied research of nano material is developed rapidly, and is widely used in industries such as traditional material, medical device, electronics, coating.
Molybdenumdisulphide has hexagonal layered structure, is fixed between layers by Van der Waals force.The characteristic of this structure, is widely used in solid lubricant, Hydrobon catalyst, semiconductor material, intercalation material and lithium cell, at aerospace field, also has very large purposes.The molybdenumdisulphide specific surface area of nanostructure is large, and surfactivity is high, is also having very wide application prospect aspect catalyzer.
The performance of nano material and its preparation method have closely and contact.Nano molybdenum disulfide preparation generally can be divided into chemical method and Physical.Physical method is prepared molybdenumdisulphide as mechanical ball milling method, sublimation recrystallization method etc., although less to the destruction of lattice, the pattern of product is comparatively single, and fineness is limited.And chemical process helps method etc. to make product purity as sluggish precipitation, hydrothermal method, solvent-thermal method, tensio-active agent are short is higher, pattern is controlled, and fineness approaches nano level.Nanometer flower-shaped structure has high surface area, high reaction activity etc. and is better than the character of the nano material of other shapes, as has very high catalytic activity, and nano flower film has super-hydrophobicity, is applied to the electrochemical activity that electrode can improve electrode.
Existing employing hydrothermal method is produced the technique of molybdenum disulfide nano flower, and when reactions steps, reaction environment can not get paying attention to always, causes whole reactions steps, is all exposed in air, thereby makes the product purity that obtains low.The present invention adopts high temperature in sealed environment to synthesize, and uses the method for reductive agent accelerated reaction process, and the molybdenum disulfide nano flower specific surface area of preparation is large, and purity is high.
Summary of the invention
The object of the invention is to overcome the shortcoming and defect of above-mentioned prior art, a kind of hydrothermal synthesis method of molybdenum disulfide nano flower is provided, solve existing Hydrothermal Synthesis and obtain the general not high defect of molybdenum disulfide nano flower purity.
Object of the present invention is achieved through the following technical solutions: a kind of hydrothermal synthesis method of molybdenum disulfide nano flower, comprises the following steps:
(1) prepare inorganic molybdenum source, organosulfur source and reductive agent, wherein inorganic molybdenum source accounts for the 40-50% of charging capacity, and organosulfur source accounts for the 40-50% of charging capacity, and reductive agent accounts for the 1-5% of charging capacity.
(2) material of preparing in step (1) is all mixed in deionized water, and stirs and make even mixing;
(3) mixed solution step (2) being obtained is put into reaction autoclave and is carried out reacting by heating, and temperature is 180 ℃～240 ℃, and be 20～28h heat-up time;
(4) solution obtaining in waiting step (3) is cooling, and the washing then this solution being circulated and centrifugation after circulation 3-5 time, then are dried the throw out obtaining, and obtains molybdenum disulfide nano flower.
In the present invention, mixed solution is put into reaction autoclave sealing and carry out pyroreaction, a good reaction environment is provided, can not contact with air, can not react with air, reduce impurity, and the present invention is washing and the centrifugation circulating, further reduced impurity.
Inorganic molybdenum source described in step (1) is molybdenum salt or molybdate, is preferably Sodium orthomolybdate.
Organosulfur source described in step (1) is the organic compound of sulfur-bearing, is preferably thiocarbamide.
Reductive agent described in step (1) is hydrazine or thiocyanide or thiocarbamide or thioacetamide, these compounds can not introduced new impurity as reductive agent, in the present invention, reductive agent adopts thiocarbamide, thiocarbamide has dual-use function in reaction, not only can be used as sulphur source but also as reductive agent, do not have impurity and produce, guaranteed the purity of product.
Mixed solution described in step (3) should first be put into a lining container, after sealing is good, put into again reaction autoclave and carry out pyroreaction, in the present invention, lining container adopts tetrafluoroethylene, and while avoiding reacting, in autoclave body, metal ion participates in reaction and produces pollution.
Washing described in step (4) refers to and adopts the alternately washing of inorganic solvent and organic solvent, removes organic and inorganic raw material remaining in product.
Described inorganic solvent adopts ionized water or clear water, and organic solvent adopts alcohol.
Dry described in step (4) refer to throw out be placed under the vacuum of 55 ℃-65 ℃ and be dried, dry in vacuum, further guaranteed the purity of product.
The invention has the beneficial effects as follows:
(1) in whole reaction of the present invention, dry process, be all to carry out in sealed environment, avoided direct exposed to air, guaranteed the purity of product;
(2) the present invention adopts reductive agent to can be used as sulphur source, also can be used as catalyzer, does not have impurity and produces, and has further promoted the purity of product.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 1;
Fig. 2 is the X ray diffracting spectrum of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 1;
Fig. 3 is the super-resolution transmission electron microscope picture of Hydrothermal Synthesis molybdenum disulfide nano flower in embodiment 2.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail:
[embodiment 1]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.72g Sodium orthomolybdate and 1g thioacetamide, wherein thioacetamide as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in 30mL deionized water, and stirs and make even mixing;
(3) mixed solution step (2) being obtained is put into reaction autoclave and is heated, and material in mixed solution is reacted, and in reaction, temperature is 180 ℃, and be 28h heat-up time;
(4) the solution naturally cooling obtaining in waiting step (3), the washing then this solution being circulated and centrifugation, circulate after 3 times, then the throw out obtaining is dried under the vacuum of 65 ℃, obtains molybdenum disulfide nano flower.
The colored scanning electron microscope (SEM) photograph of Hydrothermal Synthesis molybdenum disulfide nano if Fig. 1 is the present embodiment, as can be seen from the figure, adopts we to prepare molybdenum disulfide nano flower and presents homogeneous laminate structure, and specific surface area is large, is conducive to the application as catalyzer; Fig. 2 is the X ray diffracting spectrum of the Hydrothermal Synthesis molybdenum disulfide nano flower of the present embodiment, as can be seen from the figure, adopts in the synthetic product of present method the diffraction peak without other impurity.
[embodiment 2]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.72g Sodium orthomolybdate and 1.14g thiocarbamide, wherein thiocarbamide both as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in deionized water, and stirs and make even mixing;
(3) mixed solution step (2) being obtained is put into polytetrafluoroethyllining lining container, then this container is put into reaction autoclave and heats, and material in mixed solution is reacted, and in reaction, temperature is 240 ℃, and be 20h heat-up time;
(4) the solution naturally cooling obtaining in waiting step (3), the washing then this solution being circulated and centrifugation, circulate after 5 times, then the throw out obtaining is dried under the vacuum of 55 ℃, obtains molybdenum disulfide nano flower.
As the super-resolution transmission electron microscope picture of Fig. 3 Hydrothermal Synthesis molybdenum disulfide nano flower that is the present embodiment.
[embodiment 3]
A hydrothermal synthesis method for molybdenum disulfide nano flower, comprises the following steps:
(1) prepare 0.84g Sodium orthomolybdate and 1.20g thiocarbamide, wherein thiocarbamide both as sulphur source also as reductive agent;
(2) material of above-mentioned preparation is all mixed in deionized water, and stirs and make even mixing;
(3) mixed solution step (2) being obtained is put into polytetrafluoroethyllining lining container, then this container is put into reaction autoclave and heats, and material in mixed solution is reacted, and in reaction, temperature is 200 ℃, and be 24h heat-up time;
(4) the solution naturally cooling obtaining in waiting step (3), the washing then this solution being circulated and centrifugation, circulate after 4 times, then the throw out obtaining is dried under the vacuum of 60 ℃, obtains molybdenum disulfide nano flower.
Claims (9)
1. the hydrothermal synthesis method that molybdenum disulfide nano is spent, is characterized in that: comprise the following steps:
(1) prepare inorganic molybdenum source, organosulfur source and reductive agent, wherein inorganic molybdenum source accounts for the 40-50% of charging capacity, and organosulfur source accounts for the 40-50% of charging capacity, and reductive agent accounts for the 1-5% of charging capacity;
(2) material of preparing in step (1) is all mixed in deionized water, and stirs and make even mixing;
(3) mixed solution step (2) being obtained is put into reaction autoclave and is carried out reacting by heating, and temperature is 180 ℃～240 ℃, and be 20～28h heat-up time;
(4) solution obtaining in waiting step (3) is cooling, and the washing then this solution being circulated and centrifugation after circulation 3-5 time, then are dried the throw out obtaining, and obtains molybdenum disulfide nano flower.
2. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, the inorganic molybdenum source described in step (1) is molybdenum salt or molybdate.
3. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, the organosulfur source described in step (1) is the organic compound of sulfur-bearing.
4. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, the reductive agent described in step (1) is hydrazine or thiocyanide or thiocarbamide or thioacetamide.
5. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 4, is characterized in that, described reductive agent is thiocarbamide.
6. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, the mixed solution described in step (3) should first be put into a lining container, puts into reaction autoclave again and carry out pyroreaction after sealing is good.
7. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, the washing described in step (4) refers to and adopts the alternately washing of inorganic solvent and organic solvent.
8. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 7, is characterized in that, described inorganic solvent adopts ionized water or clear water, and organic solvent adopts alcohol.
9. the hydrothermal synthesis method of a kind of molybdenum disulfide nano flower according to claim 1, is characterized in that, dry described in step (4) refers to throw out is placed under the vacuum of 55 ℃-65 ℃ and is dried.
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