CN106745271A - A kind of sodium taurocholate for preparing tungsten disulfide nano slices improves hydro-thermal method - Google Patents
A kind of sodium taurocholate for preparing tungsten disulfide nano slices improves hydro-thermal method Download PDFInfo
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- CN106745271A CN106745271A CN201710068917.9A CN201710068917A CN106745271A CN 106745271 A CN106745271 A CN 106745271A CN 201710068917 A CN201710068917 A CN 201710068917A CN 106745271 A CN106745271 A CN 106745271A
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- tungsten disulfide
- disulfide nano
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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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
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
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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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Abstract
Hydro-thermal method is improved the invention discloses a kind of sodium taurocholate for preparing tungsten disulfide nano slices.The method is dissolved in deionized water and obtains yellow solution according to a certain percentage using wolframic acid and thiocarbamide as raw material, adjusts solution PH=6.To adding 34 51 mg sodium taurocholates as surfactant in solution, 30 min are stirred.Mixed solution is transferred in hydrothermal reaction kettle the h of stirring reaction 8 12 under the conditions of 180 DEG C, is cooled to room temperature.Filter the water-filling of going forward side by side of reacted mixed liquor to wash and washed with alcohol, collect filter cake.The filter cake of collection is vacuum dried 12 h under the conditions of 60 DEG C, black solid is obtained for tungsten disulfide nano slices.This method overcomes that stripping method is cumbersome, yield is extremely low, product form is uneven first-class not enough, tungsten disulfide nano slices " from the bottom to top " are simplified to prepare and separating technology, product form is homogeneous, product yield high, is that the magnanimity of nanostructured tungsten disulfide is prepared, performance study and opened up new technological approaches in the field such as catalyzing manufacturing of hydrogen, semi-conductor electronic device, energy storage industrial applications.
Description
Technical field
The few layer of sodium taurocholate improvement hydro-thermal method of tungsten disulfide nano slices is prepared the present invention relates to a kind of.
Background technology
Tungsten disulfide（WS2）A kind of typical transition-metal sulphides (TMD), with stratiform knot as graphite-phase
Structure, belongs to hexagonal crystal system.The elementary layer of tungsten disulfide crystal is made up of tri- plane layers of S-W-S, inside elementary layer, three
The sulphur atom of prismatic distribution surrounds tungsten atom, is linked together with very strong covalent bond between sulphur atom and tungsten atom, and
Adhesion between layers is Van der Waals force, and bonding force is weak.The polymorphism of crystal is one of key property of tungsten disulfide, body
Phase structure tungsten disulfide is the 2H- semiconductor phase structures of stabilization, and two-dimensional sheet nanostructured tungsten disulfide is then 1T- metal phases
Structure.Due to reasons such as skin effect and dielectric effects, tungsten disulfide nano slices possess many new compared with body phase tungsten disulfide
Characteristic, possess potential application value in fields such as catalyzing manufacturing of hydrogen, energy storage, microelectronic components.
In recent years, the preparation method both at home and abroad to tungsten disulfide nano slices has carried out numerous studies, is broadly divided into " by up to
Under " prepare and two class methods of " from the bottom to top " preparation.It is the preparation method of " from top to bottom " to study at present more, and Late is used
Mechanical stripping method, few layer of tungsten disulfide nano slices are obtained by the folding one piece adhesive tape with tungsten disulfide powder.
Be immersed in tungsten disulfide powder in the hexane solution containing n-BuLi and heating is carried out and ultrasonically treated by Yang et al., obtains
Obtained ultra-thin sheet tungsten disulfide.Hibernian ColemanJ.N et al. proposes water mutually ultrasonic stripping method, by tungsten disulfide
Powder is immersed in the aqueous solution containing isopropanol or sodium taurocholate, it is carried out ultrasonically treated, and individual layer two is separated from powder surface
Tungsten sulfide nanometer sheet.Methods described above has the Wolfram disulfide nano that preparation efficiency is low, preparation technology is cumbersome, prepare
The problems such as piece uneven thickness, it is difficult to large-scale popularization and application.Patent of the present invention provides a kind of synthesis tungsten disulfide nano slices
Improvement hydro-thermal method, using wolframic acid and thiocarbamide as raw material, sodium taurocholate as the surfactant in liquid-phase system, suitable
At a temperature of carry out a step hydro-thermal reaction and directly prepare tungsten disulfide nano slices.
This method overcomes that stripping method is cumbersome, yield is extremely low, product form is uneven first-class not enough, simplifies two sulphur
Change tungsten nanometer sheet " from the bottom to top " to prepare and separating technology, product form is homogeneous, and product yield high is nanostructured tungsten disulfide
Magnanimity prepare, performance study and industrial applications have opened up new technological approaches.
The content of the invention
Tungsten disulfide nano slices are prepared it is an object of the invention to provide one kind simply improve hydro-thermal method.In the hydrothermal system
In, wolframic acid and thiocarbamide respectively as tungsten source and sulphur source, sodium taurocholate as surfactant, by controlling Hydrothermal Synthesiss during
Temperature make surfactant formed lameller micelles, wolframic acid and thiocarbamide reacted in the liquid phase and using lameller micelles as template into
Core and growth, so as to form two-dimensional nano sheet tungsten disulfide.Reaction equation is as follows：
A kind of sodium taurocholate for preparing tungsten disulfide nano slices of the invention improves hydro-thermal method, it is characterised in that：
200 mg wolframic acids and 228 mg thiocarbamides are weighed first（The mol ratio of wolframic acid and thiocarbamide is 1:4）It is added to 60 ml deionizations
In water, stirring obtains yellow solution until solid is completely dissolved；To adding a certain amount of sodium taurocholate (34-51 in above-mentioned solution
Mg) and after continuing 30 min of stirring, the pH value for adjusting solution using hydrochloric acid and ammoniacal liquor is 6；Mixed solution is transferred to one 100
In the hydrothermal reaction kettle of ml, design temperature is cooled to room temperature for 180 DEG C and persistently after stirring reaction 8-12 h, obtains black liquid
Body；The alcohol that product is carried out repeatedly is simultaneously washed and washed by filtering black liquor, collects filter cake；The filter cake that will be obtained is in 60 DEG C of vacuum bars
12 h are dried under part and is collected into black solid for tungsten disulfide nano slices.The advantage of the method there are provided a kind of simple one
One-step hydrothermal hair has prepared the preferable tungsten disulfide nano slices of pattern, the hydro-thermal compared with traditional " from top to bottom " preparation method
The process is simple of method and product amount is more, facilitates follow-up correlated performance to study and industrialization promotion.
The present invention devises following technical scheme for achieving the above object：
（1）Weigh 200 mg wolframic acids and 228 mg thiocarbamides are added in 100 ml beakers, be added thereto to 60 ml deionized waters simultaneously
Stirring obtains uniform yellow solution；
（2）To adding 34 mg sodium taurocholates to continue to stir 30 min in yellow solution, the PH of solution is adjusted using hydrochloric acid and ammoniacal liquor
Be worth is 6；
（3）Above-mentioned solution is transferred in the hydrothermal reaction kettle of 100 ml, after 180 DEG C of design temperature and the persistently h of stirring reaction 8
It is cooled to room temperature and obtains black liquor；
（4）Filtering black liquor, and the filter cake after the alcohol for carrying out repeatedly is washed and wash on collection filter membrane.
（5）The filter cake of collection is vacuum dried 12 h at 60 DEG C, 180 mg black solids is obtained for Wolfram disulfide nano
Piece, a diameter of 400-800 nm of nanometer sheet, thickness is about 1-10 nm.
The beneficial effects of the invention are as follows：Surfactant is added in hydro-thermal reaction, the table of system is significantly reduced
Face tension force, for two-dimensional nano chip architecture, stable existence provides specific microenvironment in the liquid phase；Selection sodium taurocholate is used as surface
Activating agent, the micellar concentration of sodium taurocholate can change with temperature, therefore can be by adjusting the temperature control courage of hydro-thermal reaction
Sour sodium forms lameller micelles, and tungsten disulfide is with this lameller micelles as template and then nucleating growth is two-dimensional sheet structure；Hydro-thermal method
The efficiency high of tungsten disulfide nano slices is prepared, yield is big, and requirement of the hydro-thermal method to environment and equipment is relatively low, than other
Method is more suitable for promoting useful industrially, is the performance study of tungsten disulfide nano slices and its is opened up in the application of various fields
Road.
Specific embodiment
Embodiment 1：
（1）Weigh 200 mg wolframic acids and 228 mg thiocarbamides are added in 100 ml beakers, be added thereto to 60 ml deionized waters simultaneously
Stirring obtains uniform yellow solution；
（2）To adding 34 mg sodium taurocholates to continue to stir 30 min in yellow solution, the PH of solution is adjusted using hydrochloric acid and ammoniacal liquor
Be worth is 6；
（3）Above-mentioned solution is transferred in the hydrothermal reaction kettle of 100 ml, after 180 DEG C of design temperature and the persistently h of stirring reaction 8
It is cooled to room temperature and obtains black liquor；
（4）Filtering black liquor, and the filter cake after the alcohol for carrying out repeatedly is washed and wash on collection filter membrane.
（5）The filter cake of collection is vacuum dried 12 h at 60 DEG C, 180 mg black solids is obtained for Wolfram disulfide nano
Piece, a diameter of 400-800 nm of nanometer sheet, thickness is about 5 nm.
Embodiment 2：
（1）Weigh 200 mg wolframic acids and 228 mg thiocarbamides are added in 100 ml beakers, be added thereto to 60 ml deionized waters simultaneously
Stirring obtains uniform yellow solution；
（2）To adding 51 mg sodium taurocholates to continue to stir 30 min in yellow solution, the PH of solution is adjusted using hydrochloric acid and ammoniacal liquor
Be worth is 6；
（3）Above-mentioned solution is transferred in the hydrothermal reaction kettle of 100 ml, after 180 DEG C of design temperature and the persistently h of stirring reaction 8
It is cooled to room temperature and obtains black liquor；
（4）Filtering black liquor, and the filter cake after the alcohol for carrying out repeatedly is washed and wash on collection filter membrane.
（5）The filter cake of collection is vacuum dried 12 h at 60 DEG C, 180 mg black solids is obtained for Wolfram disulfide nano
Piece, a diameter of 50-200 nm of nanometer sheet, thickness is about 1-10 nm.
Embodiment 3：
（1）Weigh 200 mg wolframic acids and 228 mg thiocarbamides are added in 100 ml beakers, be added thereto to 60 ml deionized waters simultaneously
Stirring obtains uniform yellow solution；
（2）To adding 34 mg sodium taurocholates to continue to stir 30 min in yellow solution, the PH of solution is adjusted using hydrochloric acid and ammoniacal liquor
Be worth is 6；
（3）Above-mentioned solution is transferred in the hydrothermal reaction kettle of 100 ml, 180 DEG C of design temperature and the persistently h of stirring reaction 12
After be cooled to room temperature and obtain black liquor；
（4）Filtering black liquor, and the filter cake after the alcohol for carrying out repeatedly is washed and wash on collection filter membrane.
（5）The filter cake of collection is vacuum dried 12 h at 60 DEG C, 180 mg black solids is obtained for Wolfram disulfide nano
Piece, a diameter of 500-1000 nm of nanometer sheet, thickness is 10-30 nm.
Claims (1)
1. a kind of sodium taurocholate improves the method that hydro-thermal method prepares tungsten disulfide nano slices, it is characterised in that：
（1）Weigh 200 mg wolframic acids and 228 mg thiocarbamides（The mol ratio of wolframic acid and thiocarbamide is 1:4）It is added to 60 ml deionized waters
In, stirring obtains yellow solution until solid is completely dissolved；
（2）To after adding a certain amount of sodium taurocholate (34-51 mg) in above-mentioned solution and continuing 30 min of stirring, using hydrochloric acid and
The pH value of ammoniacal liquor regulation solution is 6；
（3）Mixed solution is transferred in a hydrothermal reaction kettle of 100 ml, design temperature is 180 DEG C and continues stirring instead
Room temperature is cooled to after answering 8-12 h, black liquor is obtained；
（4）The alcohol that product is carried out repeatedly is simultaneously washed and washed by filtering black liquor, collects filter cake；
（5）The filter cake that will be obtained dries 12 h under 60 DEG C of vacuum conditions and is collected into black solid for tungsten disulfide nano slices.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110935443A (en) * | 2019-12-18 | 2020-03-31 | 福建师范大学泉港石化研究院 | Palladium-based alumina catalyst with Br phi nsted acid site and strong palladium anchoring effect and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
Citations (4)
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| CN104593131A (en) * | 2014-12-29 | 2015-05-06 | 北京航空航天大学 | Method for preparing tungsten disulfide nanosheet water-based lubricating agent in situ |
| WO2016042305A1 (en) * | 2014-09-16 | 2016-03-24 | Thomas Swan & Co. Ltd | Two-dimensional materials |
| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
| CN106075439A (en) * | 2016-06-17 | 2016-11-09 | 上海理工大学 | A kind of WS2pVP nanometer sheet and its preparation method and application |
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- 2017-02-08 CN CN201710068917.9A patent/CN106745271B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016042305A1 (en) * | 2014-09-16 | 2016-03-24 | Thomas Swan & Co. Ltd | Two-dimensional materials |
| CN104593131A (en) * | 2014-12-29 | 2015-05-06 | 北京航空航天大学 | Method for preparing tungsten disulfide nanosheet water-based lubricating agent in situ |
| CN105858646A (en) * | 2016-04-19 | 2016-08-17 | 北京航空航天大学 | Preparation method of transparent thin film |
| CN106075439A (en) * | 2016-06-17 | 2016-11-09 | 上海理工大学 | A kind of WS2pVP nanometer sheet and its preparation method and application |
Non-Patent Citations (2)
| Title |
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| S.V. PRABHAKAR VATTIKUTI等: "Selective hydrothermally synthesis of hexagonal WS2 platelets and their photocatalytic performance under visible light irradiation", 《SUPERLATTICES AND MICROSTRUCTURES》 * |
| SHIXIU CAO等: "Hydrothermal synthesis of variety low dimensional WS2 nanostructures", 《MATERIALS LETTERS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110935443A (en) * | 2019-12-18 | 2020-03-31 | 福建师范大学泉港石化研究院 | Palladium-based alumina catalyst with Br phi nsted acid site and strong palladium anchoring effect and preparation method thereof |
| CN110935443B (en) * | 2019-12-18 | 2023-04-28 | 福建师范大学泉港石化研究院 | Palladium-based aluminum oxide catalyst with BrPhinsted acid site and strong palladium anchoring function and preparation method thereof |
| CN113023780A (en) * | 2021-03-17 | 2021-06-25 | 李伟强 | Nanoscale tungsten disulfide material, preparation method and preparation device thereof |
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