CN103833081A - Preparation method for molybdenum disulfide nanosheet with reactive group-containing surface - Google Patents
Preparation method for molybdenum disulfide nanosheet with reactive group-containing surface Download PDFInfo
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Abstract
The invention discloses a preparation method for a molybdenum disulfide nanosheet with a reactive group-containing surface. The preparation method comprises the following steps: adding one part by weight of molybdenum disulfide, 2-5 parts by weight of n-butyllithium and 10-20 parts by weight of n-hexane into a hydrothermal reaction kettle, heating at 50-150DEG C for 0.5-12 hours, cooling to room temperature, performing centrifugal separation and n-hexane washing for five times, drying at 50DEG C for 12 hours so as to obtain molybdenum disulfide powder with lithium ion intercalation, adding 1 part by weight of molybdenum disulfide powder with lithium ion intercalation, 0.05-10 parts by weight of sulihydryl reagents with reactive groups, and 100-1000 parts by weight of water into a flask for performing ultrasonic treatment for one minute to five hours under 50-100 watt, to obtain molybdenum disulfide nanosheet with the reactive group-containing surface. The method is easily available, mild to react, simple to operate, and small in environmental pollution; the prepared nanosheet can be further functionalized, thus having good application prospects.
Description
Technical field
The invention belongs to technical field of nano material, the preparation method of the molybdenum disulfide nano sheet that particularly reactive group is contained on a kind of surface.
Background technology
As a kind of important stratified nano materials, molybdenumdisulphide is widely applied in various fields such as lubricant, catalysis, energy storage, matrix materials with its unique laminate structure.In addition, than other stratified materials, there is regulatable band gap in molybdenumdisulphide, thereby have bright application prospect at field of photoelectric devices.General chemistry and physical method are difficult to prepare the molybdenumdisulphide with laminate structure, and current adoptable method mainly contains: mechanical force stripping method, liquid phase ultrasonic method and lithium ion graft process etc.Although these methods can make molybdenum disulfide nano sheet, the molybdenum disulfide nano sheet surface obtaining does not have to proceed the reactive group (as hydroxyl, carboxyl or amino) of functionalization, has greatly limited the range of application of molybdenum disulfide nano sheet.On the other hand, the molybdenum disulfide nano sheet that reactive group is contained on preparation surface, not only can improve the solvability of molybdenum disulfide nano sheet in different chemical solvent, improve its processing characteristics, and can come by further reaction organic molecule and the polymkeric substance of grafting functional, obtain the molybdenum disulfide nano sheet with difference in functionality.Therefore, realize the preparation of the molybdenum disulfide nano sheet that contains reactive group in surface, have far-reaching theory significance and application prospect.
Summary of the invention
The object of this invention is to provide a kind of surface and contain reactive group as the preparation method of the molybdenum disulfide nano sheet of hydroxyl, carboxyl or amino.
The thinking of the inventive method: the inventive method utilizes molybdenumdisulphide for raw material, first carries out lithium ion intercalation at a certain temperature, then in adding sulfhydryl reagent, carries out ultrasonic peeling off, and makes the molybdenum disulfide nano sheet that reactive group is contained on surface.
Concrete steps are:
(1) together with the normal hexane of the n-Butyl Lithium of the molybdenumdisulphide of 1 weight part, 2 ~ 5 weight parts and 10 ~ 20 weight parts, join in hydrothermal reaction kettle, at 50 ~ 150 DEG C, heat 0.5 ~ 12 hour, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) water with hydroxyl, carboxyl or amino sulfhydryl reagent, 100 ~ 1000 weight parts of the molybdenum disulfide powder of the lithium ion intercalation 1 weight part step (1) being made, 0.05 ~ 10 weight part add in beaker, carry out ultrasonic, ultrasonic time is 1 minute ~ 5 hours, ultrasonic power is 50 ~ 1000 watts, makes the molybdenum disulfide nano sheet that reactive group is contained on surface.
The described sulfhydryl reagent with hydroxyl is the one in 1-sulfydryl-2-propyl alcohol, 3-sulfydryl-1-propyl alcohol, dithiothreitol (DTT), 1-thioglycerin and 2,3-dimercapto-1-propyl alcohol.
The described sulfhydryl reagent with carboxyl is the one in Thiovanic acid, 3-thiohydracrylic acid, 2 mercaptopropionic acid, dimercaptosuccinic acid, DMSA, N-(2-sulfydryl propionyl)-glycine and captopril.
Described is the one in mercaptoethylamine, halfcystine and 3-amino-1,2,4-triazole-5-mercaptan with amino sulfhydryl reagent.
Described chemical reagent is chemical pure and above purity.
The molybdenum disulfide nano sheet that reactive group is contained on the prepared surface of the inventive method is measured its surperficial organic composition kind and content through infrared spectra and thermogravimetic analysis (TGA), and result has confirmed that reactive group has been grafted to the surface of molybdenum disulfide nano sheet; Atomic force microscope and transmission electron microscope have been tested its size, find that it is rendered as thickness is 0.6 ~ 3 nanometer, are of a size of the laminar nano sheet of 50 nanometer ~ 2 micron.In addition, preparation method of the present invention has that raw material is easy to get, reaction temperature with, simple to operate, be convenient to separate, the advantage such as synthetic safe and environmental pollution is little; The molybdenum disulfide nano sheet that reactive group is contained on prepared surface can be stable be dispersed in the aqueous solution, and further functionalization of its surperficial reactive group, has good application prospect at aspects such as lubricant, photoelectric material and catalytic materials.
Brief description of the drawings
Fig. 1 is the infrared spectrogram of surface prepared by the embodiment of the present invention 1 molybdenum disulfide nano sheet that contains hydroxyl.
Fig. 2 is the infrared spectrogram of surface prepared by the embodiment of the present invention 2 molybdenum disulfide nano sheet that contains carboxyl.
Fig. 3 is the thermogravimetric curve figure of surface prepared by the embodiment of the present invention 1 molybdenum disulfide nano sheet that contains hydroxyl.
Fig. 4 is the thermogravimetric curve figure of surface prepared by the embodiment of the present invention 2 molybdenum disulfide nano sheet that contains carboxyl.
Fig. 5 is the atomic force microscope figure of surface prepared by the embodiment of the present invention 1 molybdenum disulfide nano sheet that contains hydroxyl.
Fig. 6 is the atomic force microscope figure of surface prepared by the embodiment of the present invention 2 molybdenum disulfide nano sheet that contains carboxyl.
Fig. 7 is the transmission electron microscope figure of surface prepared by the embodiment of the present invention 1 molybdenum disulfide nano sheet that contains hydroxyl.
Fig. 8 is the transmission electron microscope figure of surface prepared by the embodiment of the present invention 2 molybdenum disulfide nano sheet that contains carboxyl.
Embodiment
embodiment 1:
(1) molybdenumdisulphide of 0.4 gram, 1.2 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 6.8 grams of normal hexanes, at 100 DEG C, heat 2 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.4 gram of step (1) being made, 1 gram of 1-thioglycerin, 400 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 1 hour, ultrasonic power is 300 watts, makes the molybdenum disulfide nano sheet that hydroxyl is contained on surface.
embodiment 2:
(1) 0.1 gram of molybdenumdisulphide, 0.5 gram of n-Butyl Lithium are joined in hydrothermal reaction kettle together with 2 grams of normal hexanes, at 150 DEG C, heat 0.5 hour, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.1 gram of step (1) being made, 0.2 gram of 3-thiohydracrylic acid, 50 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 3 hours, ultrasonic power is 200 watts, makes the molybdenum disulfide nano sheet that carboxyl is contained on surface.
embodiment 3:
(1) 0.25 gram of molybdenumdisulphide, 0.5 gram of n-Butyl Lithium are joined in hydrothermal reaction kettle together with 2.5 grams of normal hexanes, at 80 DEG C, heat 3 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.2 gram of step (1) being made, 2 grams of halfcystines, 20 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 1 minute, ultrasonic power is 1000 watts, makes surface and contains amino molybdenum disulfide nano sheet.
embodiment 4:
(1) molybdenumdisulphide of 0.8 gram, 2.6 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 16 grams of normal hexanes, at 90 DEG C, heat 3 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.5 gram of step (1) being made, 0.025 gram 2,3-dimercapto-1-propyl alcohol, 250 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 5 hours, ultrasonic power is 50 watts, makes the molybdenum disulfide nano sheet that hydroxyl is contained on surface.
embodiment 5:
(1) molybdenumdisulphide of 0.8 gram, 3.5 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 15 grams of normal hexanes, at 70 DEG C, heat 8 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.5 gram of step (1) being made, 0.2 gram 2,3-dimercaptosuccinic acid, 150 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 1.5 hours, ultrasonic power is 700 watts, makes the molybdenum disulfide nano sheet that carboxyl is contained on surface.
embodiment 6:
(1) molybdenumdisulphide of 0.8 gram, 3.6 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 13 grams of normal hexanes, at 140 DEG C, heat 4 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.5 gram of step (1) being made, 1.3 grams of mercaptoethylamines, 500 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 2.5 hours, ultrasonic power is 100 watts, makes surface and contains amino molybdenum disulfide nano sheet.
embodiment 7:
(1) molybdenumdisulphide of 0.8 gram, 2 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 12 grams of normal hexanes, at 90 DEG C, heat 9 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.5 gram of step (1) being made, 3.5 grams of dithiothreitol (DTT), 300 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 0.5 hour, ultrasonic power is 400 watts, makes the molybdenum disulfide nano sheet that hydroxyl is contained on surface.
embodiment 8:
(1) molybdenumdisulphide of 0.8 gram, 2.8 grams of n-Butyl Lithiums are joined in hydrothermal reaction kettle together with 8 grams of normal hexanes, at 130 DEG C, heat 2 hours, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation.
(2) molybdenum disulfide powder of the lithium ion intercalation 0.5 gram of step (1) being made, 3 grams of Thiovanic acids, 400 grams of water add in beaker, carry out ultrasonic, ultrasonic time is 20 minutes, ultrasonic power is 600 watts, makes the molybdenum disulfide nano sheet that carboxyl is contained on surface.
Claims (1)
1. a preparation method for the molybdenum disulfide nano sheet that reactive group is contained on surface, is characterized in that concrete steps are:
(1) together with the normal hexane of the n-Butyl Lithium of the molybdenumdisulphide of 1 weight part, 2 ~ 5 weight parts and 10 ~ 20 weight parts, join in hydrothermal reaction kettle, at 50 ~ 150 DEG C, heat 0.5 ~ 12 hour, then be cooled to room temperature, wash after 5 times through centrifugation and normal hexane, at 50 DEG C, be dried 12 hours, make the molybdenum disulfide powder of lithium ion intercalation;
(2) water with hydroxyl, carboxyl or amino sulfhydryl reagent, 100 ~ 1000 weight parts of the molybdenum disulfide powder of the lithium ion intercalation 1 weight part step (1) being made, 0.05 ~ 10 weight part add in beaker, carry out ultrasonic, ultrasonic time is 1 minute ~ 5 hours, ultrasonic power is 50 ~ 1000 watts, makes the molybdenum disulfide nano sheet that reactive group is contained on surface;
The described sulfhydryl reagent with hydroxyl is the one in 1-sulfydryl-2-propyl alcohol, 3-sulfydryl-1-propyl alcohol, dithiothreitol (DTT), 1-thioglycerin and 2,3-dimercapto-1-propyl alcohol;
The described sulfhydryl reagent with carboxyl is the one in Thiovanic acid, 3-thiohydracrylic acid, 2 mercaptopropionic acid, dimercaptosuccinic acid, DMSA, N-(2-sulfydryl propionyl)-glycine and captopril;
Described is the one in mercaptoethylamine, halfcystine and 3-amino-1,2,4-triazole-5-mercaptan with amino sulfhydryl reagent;
Described chemical reagent is chemical pure and above purity.
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| CN105565383A (en) * | 2014-10-29 | 2016-05-11 | 丰田自动车工程及制造北美公司 | Solventhermal synthesis of nanosized two dimensional materials |
| CN106277055A (en) * | 2016-07-18 | 2017-01-04 | 安徽师范大学 | One-dimensional molybdenum disulfide nano material that a kind of lamella is piled up and preparation method thereof |
| CN106568936A (en) * | 2016-10-12 | 2017-04-19 | 宁波大学 | Preparation method and applications of miRNA-21 electroluminescent immunosensor based on multi-functionalized molybdenum disulfide |
| CN106698518A (en) * | 2017-01-18 | 2017-05-24 | 四川大学 | Hydrothermal method for preparing thiol-modified layered molybdenum disulfide |
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| CN105565383A (en) * | 2014-10-29 | 2016-05-11 | 丰田自动车工程及制造北美公司 | Solventhermal synthesis of nanosized two dimensional materials |
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| CN106568936B (en) * | 2016-10-12 | 2018-04-24 | 宁波大学 | The preparation method and applications of miRNA-21 electrochemical luminescence immunosensors based on multifunction molybdenum disulfide |
| CN106568936A (en) * | 2016-10-12 | 2017-04-19 | 宁波大学 | Preparation method and applications of miRNA-21 electroluminescent immunosensor based on multi-functionalized molybdenum disulfide |
| CN106833810A (en) * | 2016-12-27 | 2017-06-13 | 唐林元 | A kind of preparation method of stable type Composite nanometer antiwear agent |
| CN106698518A (en) * | 2017-01-18 | 2017-05-24 | 四川大学 | Hydrothermal method for preparing thiol-modified layered molybdenum disulfide |
| CN106995694B (en) * | 2017-05-04 | 2019-08-13 | 安徽师范大学 | The detection method of mercapto-modified molybdenum sulfide quantum dot and preparation method thereof and 2,4,6- trinitrotoluene |
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Application publication date: 20140604 Assignee: Kunshan Xuchang Polymer Materials Co.,Ltd. Assignor: GUILIN University OF TECHNOLOGY Contract record no.: X2022450000455 Denomination of invention: A Preparation Method of Molybdenum Disulfide Nanosheets Containing Reactive Groups on the Surface Granted publication date: 20160406 License type: Common License Record date: 20221228 |