CN106944101A - The method that one-step method prepares N doping molybdenum disulfide nano sheet - Google Patents
The method that one-step method prepares N doping molybdenum disulfide nano sheet Download PDFInfo
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- CN106944101A CN106944101A CN201710304962.XA CN201710304962A CN106944101A CN 106944101 A CN106944101 A CN 106944101A CN 201710304962 A CN201710304962 A CN 201710304962A CN 106944101 A CN106944101 A CN 106944101A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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Abstract
The invention discloses the method that one-step method prepares N doping molybdenum disulfide nano sheet, step is as follows：First, a certain amount of Ammonium Molybdate Tetrahydrate, thiocarbamide and methenamine are weighed, and they are dispersed in the container equipped with deionized water, fully dissolving is scattered in the presence of ultrasound and magnetic agitation；2nd, the solution obtained by step one is transferred in the reactor of polytetrafluoroethyllining lining, is placed in heating in air dry oven and is chemically reacted, question response for a period of time after, stop heating, allow reactor to naturally cool to room temperature；3rd, it is cooled to after room temperature, by reacted solution centrifugal, collects the atrament of synthesis, washed with the mixed solutions for many times of deionized water and absolute ethyl alcohol；4th, the powder obtained after step 3 is washed is positioned over vacuum drying to constant weight in vacuum drying chamber and produced.The present invention is using cheap methenamine as nitrogen source, and reaction temperature is low, simple to operate, and the method for breaching traditional complexity, yield is big, and catalytic activity is good, and performance is stable.
Description
Technical field
The present invention relates to a kind of method that one-step method prepares N doping molybdenum disulfide nano sheet, belong to novel energy resource material technology
Field.
Background technology
Water electrolysis hydrogen production is one of current heat subject studied for reply energy crisis.The stable catalysis of Cheap highly effective
Agent is always the target that people pursue, in these catalyst, because molybdenum disulfide is cheap, structure is novel, excellent performance,
Good stability, is always emphasis material of concern.Related technology of preparing report is a lot, but is due to that molybdenum disulfide is also deposited
Poorly conductive, active site is limited the shortcomings of, limit it and use, prior art not can solve this and ask
Topic.
Such as application number：201610021038.6, a kind of nitrating molybdenum disulfide loaded platinum photo catalyst and preparation method thereof.The party
Method selects sodium molybdate and thioacetamide as raw material first, and molybdenum disulfide nano sheet is prepared using hydro-thermal method；Then by two sulphur
Change molybdenum nanometer sheet to be heat-treated under ammonia atmosphere, nitrating molybdenum disulfide nano sheet is obtained, finally by nitrating molybdenum disulfide nano sheet
With photoreduction met hod carried noble metal platinum, nitrating molybdenum disulfide loaded platinum photo catalyst is obtained.The invention complex operation is, it is necessary to first prepare two
Molybdenum sulfide nitrogen treatment again, finally Supported Pt Nanoparticles again.1~1 .5h heat is carried out under ammonia atmosphere and at a temperature of 400~700 DEG C
Processing.Two-step method process is complicated, and heat treatment temperature used is high, ammonia price, and the nitrogen quantity of doping is difficult to control.
In addition to disclosed in above-mentioned patent, noble metal platinum is to generally acknowledge best catalyst, but the high reserves of its price are few, limit
Its large-scale use.As typical two-dimensional material, molybdenum disulfide is closed because of its unique structure and cheap price by people
Note, shows good in the application of electro-catalysis hydrogen manufacturing, but its active sites is mainly distributed on edge and poorly conductive, limitation
Its performance.Its electric conductivity can be not only improved by mixing nitrogen, while active sites can be increased, carrying for its performance is brought
Height, usual people are doped using ammonia as nitrogen source by high-temperature heat treatment, and this method not only high cost, process is complicated, and
And pyroprocess easily makes nanometer sheet aggregate stack, its specific surface area is reduced, accordingly, it would be desirable to new method.
The content of the invention
The present invention is in order to solve the above technical problems, provide the side that a kind of one-step method prepares N doping molybdenum disulfide nano sheet
Method.
To reach above-mentioned purpose, the technology used in the present invention means are：One-step method prepares N doping molybdenum disulfide nano
The method of piece, step is as follows：
First, a certain amount of Ammonium Molybdate Tetrahydrate, thiocarbamide and methenamine are weighed, and they are dispersed in the appearance equipped with deionized water
In device, fully dissolving is scattered in the presence of ultrasound and magnetic agitation；
2nd, solution resulting in step one is transferred in the reactor of polytetrafluoroethyllining lining, be placed in air dry oven
Heating chemically reacted, question response for a period of time after, stop heating, allow reactor to naturally cool to room temperature；
3rd, it is cooled to after room temperature, by reacted solution centrifugal, collects the atrament of synthesis, with deionized water and anhydrous
The mixed solutions for many times washing of ethanol；
4th, the powder obtained after step 3 is washed is positioned over vacuum drying to constant weight in vacuum drying chamber and produced.
Further, the mass ratio of ammonium molybdate, thiocarbamide and methenamine is 1 in the raw material:1.5~2:0.6~0.8.
Further, in the step 2, heating and temperature control is at 180~230 DEG C.
Further, in the step 2, the reaction time is 20~25h.
Further, described vacuum drying the temperature inside the box sets 60 DEG C.
The beneficial effects of the present invention are：Noble metal is not used, nitrogen source, reaction temperature are used as using cheap methenamine
Degree is low so that whole operation was both simple, and inexpensive；In addition, one step hydro thermal method is the N doping curing for obtaining two-dimensional structure
Molybdenum nanometer sheet, the method for breaching traditional complexity is simple and quick, and obtained product yield is big, and catalytic activity is good, and performance is steady
It is fixed.
Brief description of the drawings
The present invention is further elaborated with reference to the accompanying drawings and examples.
Fig. 1 is the electron scanning micrograph of finished product prepared by the embodiment of the present invention 1；
Fig. 2 is the transmission electron microscope photo of finished product prepared by the embodiment of the present invention 1；
Fig. 3 is the XRD test result figures of finished product prepared by the embodiment of the present invention 1；
Fig. 4 is the XPS test result figures of finished product prepared by the embodiment of the present invention 1；
Fig. 5 LSV of product prepared by present invention checking example electrocatalysis characteristic test chart.
Specific embodiment
Embodiment 1
The method that one-step method prepares N doping molybdenum disulfide nano sheet, comprises the following steps：
(1) 1.236 grams of Ammonium Molybdate Tetrahydrate, 2.284 grams of thiocarbamide and 0.843 gram of methenamine is weighed, they are dispersed in
In 40 milliliters of deionized water, in the presence of ultrasound and magnetic agitation, make its fully dispersed dissolving.
(2) the above-mentioned sample prepared is transferred in the reactor of 50 milliliters of volume, tightens reactor, it is placed in
Heating 24 hours is carried out in air dry oven at 220 DEG C, after question response terminates, room temperature is naturally cooled to.
(3) the black precipitate product generated after reaction is taken out, is cleaned multiple times, must centrifuge through deionized water and absolute ethyl alcohol
Sample is collected, solid powder is obtained.
(4) by above-mentioned black solid powder, 60 DEG C of drying are standby to constant weight in vacuum drying chamber.The pattern and thing of product
Mutually characterize as Figure 1-4.
Verify example
Performance test to gained catalyst N doping molybdenum disulfide nano sheet in embodiment 1, carries out electro-catalysis experiment：
(1) the two-dimentional N doping molybdenum disulfide nano sheet that precise 20mg is prepared, is dispersed in 6 milliliters of isopropanols and 4 millis
In the mixed solution for rising deionized water, 10 microlitres of 5% naphthols aqueous isopropanol is added, ultrasound causes uniform point for 30 minutes
Dissipate.
Take 5ul above-mentioned dispersant liquid drop to be added on glassy carbon electrode, electro-chemical test is carried out after being completely dried, is obtained
LSV curves（Fig. 5）, it is observed that after nitrating, the initial action current potential of sample is significantly improved, and in same current potential bar
Compared to the sample without nitrating under part, its reduction current substantially becomes big.
As can be seen that not using noble metal from embodiment 1, but cheap methenamine is used as nitrogen source, instead
Answer temperature low so that whole operation was both simple, and inexpensive；One step hydro thermal method is the N doping molybdenum disulfide for obtaining two-dimensional structure
Nanometer sheet, the method for breaching traditional complexity is simple and quick, and obtained product yield is big, and catalytic activity is good, and performance is steady
It is fixed.
Embodiment 2
The method that one-step method prepares N doping molybdenum disulfide nano sheet, step is as follows：
First, a certain amount of Ammonium Molybdate Tetrahydrate, thiocarbamide and methenamine are weighed, and they are dispersed in the appearance equipped with deionized water
In device, fully dissolving is scattered in the presence of ultrasound and magnetic agitation；
2nd, solution resulting in step one is transferred in the reactor of polytetrafluoroethyllining lining, be placed in air dry oven
Heating chemically reacted, question response for a period of time after, stop heating, allow reactor to naturally cool to room temperature；
3rd, it is cooled to after room temperature, by reacted solution centrifugal, collects the atrament of synthesis, with deionized water and anhydrous
The mixed solutions for many times washing of ethanol；
4th, the powder obtained after step 3 is washed is positioned over vacuum drying to constant weight in vacuum drying chamber and produced.
The mass ratio of ammonium molybdate, thiocarbamide and methenamine is 1 in the raw material:1.5~2:0.6~0.8；
In the step 2, heating and temperature control is at 180~230 DEG C.
In the step 2, the reaction time is 20~25h.In above-mentioned temperature and the equal energy of the product produced in the reaction time
The parameter provided in the technique effect to be reached, embodiment 1 is one of example.
Described vacuum drying the temperature inside the box sets 60 DEG C.
Above is embodiments of the invention, but the present invention is not limited in the above embodiments, is familiar with the section of this area
Skill personnel can also make a variety of equivalent deformations or replacement, these etc. under the precondition without prejudice to spirit of the present invention
Same deformation or replacement is all contained in the protection domain that the present invention is limited.
Claims (5)
1. the method that one-step method prepares N doping molybdenum disulfide nano sheet, step is as follows：
First, a certain amount of Ammonium Molybdate Tetrahydrate, thiocarbamide and methenamine are weighed, and they are dispersed in the appearance equipped with deionized water
In device, fully dissolving is scattered in the presence of ultrasound and magnetic agitation；
2nd, solution resulting in step one is transferred in the reactor of polytetrafluoroethyllining lining, be placed in air dry oven
Heating chemically reacted, question response for a period of time after, stop heating, allow reactor to naturally cool to room temperature；
3rd, it is cooled to after room temperature, by reacted solution centrifugal, collects the atrament of synthesis, with deionized water and anhydrous
The mixed solutions for many times washing of ethanol；
4th, the powder obtained after step 3 is washed is positioned over vacuum drying to constant weight in vacuum drying chamber and produced.
2. it is according to claim 1, it is characterised in that：The mass ratio of ammonium molybdate, thiocarbamide and methenamine in the raw material
For 1:1.5~2:0.6~0.8.
3. the method that one-step method according to claim 1 prepares N doping molybdenum disulfide nano sheet, it is characterised in that：It is described
In step 2, heating and temperature control is at 180~230 DEG C.
4. the method that one-step method according to claim 1 prepares N doping molybdenum disulfide nano sheet, it is characterised in that：It is described
In step 2, the reaction time is 20~25h.
5. the method that one-step method according to claim 4 prepares N doping molybdenum disulfide nano sheet, it is characterised in that：It is described
It is dried in vacuo the temperature inside the box and sets 60 DEG C.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107552081A (en) * | 2017-09-11 | 2018-01-09 | 常州大学 | A kind of preparation method of N doping manganese molybdate photochemical catalyst |
| CN109574077A (en) * | 2019-01-29 | 2019-04-05 | 中国科学院高能物理研究所 | A kind of laminar nano sulfide and its preparation method and application |
| CN111111729A (en) * | 2019-12-18 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111286752A (en) * | 2018-12-10 | 2020-06-16 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof |
| CN111647852A (en) * | 2020-06-30 | 2020-09-11 | 南方科技大学 | Solid lubricating film and preparation method and application thereof |
| CN111755696A (en) * | 2020-06-30 | 2020-10-09 | 贝特瑞(江苏)新能源材料有限公司 | Composite negative electrode material, preparation method and application thereof |
| CN113461046A (en) * | 2021-07-28 | 2021-10-01 | 四川恒瑞天成科技有限公司 | Comb-shaped nitrogen-doped indium sulfide gas-sensitive material, preparation method and application |
| CN114602510A (en) * | 2020-12-04 | 2022-06-10 | 中国科学院大连化学物理研究所 | Nitrogen-doped transition metal sulfide catalyst, preparation and application thereof |
| CN116640509A (en) * | 2023-06-25 | 2023-08-25 | 佛山市南伽科技有限公司 | High-temperature-resistant organosilicon paint |
-
2017
- 2017-05-03 CN CN201710304962.XA patent/CN106944101B/en not_active Expired - Fee Related
Non-Patent Citations (3)
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| RUCHUN LI ET.AL: ""Nitrogen doped MoS2 nanosheets synthesized via a low-temperature process as electrocatalysts with enhanced activity for hydrogen evolution reaction"", 《JOURNAL OF POWER SOURCES》 * |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107552081A (en) * | 2017-09-11 | 2018-01-09 | 常州大学 | A kind of preparation method of N doping manganese molybdate photochemical catalyst |
| CN111286752B (en) * | 2018-12-10 | 2021-11-09 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof |
| CN111286752A (en) * | 2018-12-10 | 2020-06-16 | 南京理工大学 | Nitrogen-doped graphite phase carbon nitride nanosheet/molybdenum disulfide composite material and preparation method thereof |
| CN109574077A (en) * | 2019-01-29 | 2019-04-05 | 中国科学院高能物理研究所 | A kind of laminar nano sulfide and its preparation method and application |
| CN109574077B (en) * | 2019-01-29 | 2020-03-17 | 中国科学院高能物理研究所 | Layered nano sulfide and preparation method and application thereof |
| CN111111729A (en) * | 2019-12-18 | 2020-05-08 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111111729B (en) * | 2019-12-18 | 2021-08-13 | 西安交通大学 | Molybdenum disulfide-based nanocomposite material with hollow sandwich laminated structure and preparation method thereof |
| CN111755696A (en) * | 2020-06-30 | 2020-10-09 | 贝特瑞(江苏)新能源材料有限公司 | Composite negative electrode material, preparation method and application thereof |
| CN111647852A (en) * | 2020-06-30 | 2020-09-11 | 南方科技大学 | Solid lubricating film and preparation method and application thereof |
| CN111755696B (en) * | 2020-06-30 | 2022-07-01 | 贝特瑞(江苏)新能源材料有限公司 | Composite negative electrode material, preparation method and application thereof |
| CN114602510A (en) * | 2020-12-04 | 2022-06-10 | 中国科学院大连化学物理研究所 | Nitrogen-doped transition metal sulfide catalyst, preparation and application thereof |
| CN113461046A (en) * | 2021-07-28 | 2021-10-01 | 四川恒瑞天成科技有限公司 | Comb-shaped nitrogen-doped indium sulfide gas-sensitive material, preparation method and application |
| CN116640509A (en) * | 2023-06-25 | 2023-08-25 | 佛山市南伽科技有限公司 | High-temperature-resistant organosilicon paint |
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