CN103833081B - The preparation method of the molybdenum disulfide nano sheet of reactive group is contained on a kind of surface - Google Patents
The preparation method of the molybdenum disulfide nano sheet of reactive group is contained on a kind of surface Download PDFInfo
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- CN103833081B CN103833081B CN201410059743.6A CN201410059743A CN103833081B CN 103833081 B CN103833081 B CN 103833081B CN 201410059743 A CN201410059743 A CN 201410059743A CN 103833081 B CN103833081 B CN 103833081B
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Abstract
The invention discloses the preparation method that the molybdenum disulfide nano sheet of reactive group is contained on a kind of surface.By the molybdenumdisulphide of 1 weight part, the n-Butyl Lithium of 2 ~ 5 weight parts and the normal hexane of 10 ~ 20 weight parts join in hydrothermal reaction kettle, heat 0.5 ~ 12 hour at 50 ~ 150 DEG C, be cooled to room temperature, through centrifugation and n-hexane 5 times, 50 DEG C of dryings 12 hours, the molybdenum disulfide powder of obtained lithium ion intercalation, by the molybdenum disulfide powder of 1 weight part lithium ion intercalation, the sulfhydryl reagent with reactive group of 0.05 ~ 10 weight part, the water of 100 ~ 1000 weight parts to add in beaker under 50 ~ 1000 watts ultrasonic 1 minute ~ 5 hours, the i.e. molybdenum disulfide nano sheet of obtained surface containing reactive group.The inventive method raw material is easy to get, reaction temperature and, simple to operate and environmental pollution is little; Prepared nanometer sheet can functionalization further, has and has good application prospect.
Description
Technical field
The invention belongs to technical field of nano material, particularly the preparation method of the molybdenum disulfide nano sheet of 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 the laminate structure of its uniqueness.In addition, compared to other stratified materials, there is regulatable band gap in molybdenumdisulphide, thus 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 obtain molybdenum disulfide nano sheet, the molybdenum disulfide nano sheet surface obtained does not have to proceed the reactive group (as hydroxyl, carboxyl or amino) of functionalization, greatly limit the range of application of molybdenum disulfide nano sheet.On the other hand, the molybdenum disulfide nano sheet of preparation surface containing reactive group, not only can improve the solvability of molybdenum disulfide nano sheet in different chemical solvent, improve its processing characteristics, and by reacting organic molecule and the polymkeric substance of grafting functional further, the molybdenum disulfide nano sheet with difference in functionality can be obtained.Therefore, realize the preparation of the molybdenum disulfide nano sheet of surface containing reactive group, 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 the preparation method of reactive group as 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 while adding sulfhydryl reagent, carries out ultrasonic stripping, the molybdenum disulfide nano sheet of obtained surface containing reactive group.
Concrete steps are:
(1) n-Butyl Lithium of the molybdenumdisulphide of 1 weight part, 2 ~ 5 weight parts is joined in hydrothermal reaction kettle together with the normal hexane of 10 ~ 20 weight parts, heat 0.5 ~ 12 hour at 50 ~ 150 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 1 weight part step (1), the sulfhydryl reagent with hydroxyl, carboxyl or amino of 0.05 ~ 10 weight part, the water of 100 ~ 1000 weight parts are added carry out in beaker ultrasonic, ultrasonic time is 1 minute ~ 5 hours, ultrasonic power is 50 ~ 1000 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing reactive group.
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-mercaptopropionyl)-glycine and captopril.
The described sulfhydryl reagent with amino is the one in mercaptoethylamine, halfcystine and 3-amino-1,2,4-triazole-5-mercaptan.
Described chemical reagent is chemical pure and above purity.
The molybdenum disulfide nano sheet that reactive group is contained on surface prepared by the inventive method measures organic composition kind and the content on its surface through infrared spectra and thermogravimetic analysis (TGA), result confirms that reactive group has been grafted to the surface of molybdenum disulfide nano sheet; Atomic force microscope and transmission electron microscope test its size, and finding 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 have that raw material is easy to get, reaction temperature with, simple to operate, be convenient to be separated, synthesize the advantages such as the high and environmental pollution of security is little; The molybdenum disulfide nano sheet that reactive group is contained on prepared surface can be stable dispersion in aqueous, and the reactive group on its surface can functionalization further, has good application prospect in lubricant, photoelectric material and catalytic material etc.
Accompanying drawing explanation
Fig. 1 is that the infrared spectrogram of the molybdenum disulfide nano sheet of hydroxyl is contained on surface prepared by the embodiment of the present invention 1.
Fig. 2 is that the infrared spectrogram of the molybdenum disulfide nano sheet of carboxyl is contained on surface prepared by the embodiment of the present invention 2.
Fig. 3 is that the thermogravimetric curve figure of the molybdenum disulfide nano sheet of hydroxyl is contained on surface prepared by the embodiment of the present invention 1.
Fig. 4 is that the thermogravimetric curve figure of the molybdenum disulfide nano sheet of carboxyl is contained on surface prepared by the embodiment of the present invention 2.
Fig. 5 is that the atomic force microscope figure of the molybdenum disulfide nano sheet of hydroxyl is contained on surface prepared by the embodiment of the present invention 1.
Fig. 6 is that the atomic force microscope figure of the molybdenum disulfide nano sheet of carboxyl is contained on surface prepared by the embodiment of the present invention 2.
Fig. 7 is that the transmission electron microscope figure of the molybdenum disulfide nano sheet of hydroxyl is contained on surface prepared by the embodiment of the present invention 1.
Fig. 8 is that the transmission electron microscope figure of the molybdenum disulfide nano sheet of carboxyl is contained on surface prepared by the embodiment of the present invention 2.
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, heat 2 hours at 100 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.4 gram of step (1), 1 gram of 1-thioglycerin, 400 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 1 hour, ultrasonic power is 300 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing hydroxyl.
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, heat 0.5 hour at 150 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.1 gram of step (1), 0.2 gram of 3-thiohydracrylic acid, 50 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 3 hours, ultrasonic power is 200 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing carboxyl.
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, heat 3 hours at 80 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.2 gram of step (1), 2 grams of halfcystines, 20 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 1 minute, ultrasonic power is 1000 watts, and namely obtained surface is containing 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, heat 3 hours at 90 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) by the molybdenum disulfide powder of lithium ion intercalation obtained for 0.5 gram of step (1), 0.025 gram 2,3-dimercapto-1-propyl alcohol, 250 grams of water add carry out in beaker ultrasonic, ultrasonic time is 5 hours, ultrasonic power is 50 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing hydroxyl.
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, heat 8 hours at 70 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) by the molybdenum disulfide powder of lithium ion intercalation obtained for 0.5 gram of step (1), 0.2 gram 2,3-dimercaptosuccinic acid, 150 grams of water add carry out in beaker ultrasonic, ultrasonic time is 1.5 hours, ultrasonic power is 700 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing carboxyl.
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, heat 4 hours at 140 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.5 gram of step (1), 1.3 grams of mercaptoethylamines, 500 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 2.5 hours, ultrasonic power is 100 watts, and namely obtained surface is containing 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, heat 9 hours at 90 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.5 gram of step (1), 3.5 grams of dithiothreitol (DTT), 300 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 0.5 hour, ultrasonic power is 400 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing hydroxyl.
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, heat 2 hours at 130 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation.
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 0.5 gram of step (1), 3 grams of Thiovanic acids, 400 grams of water are added carry out in beaker ultrasonic, ultrasonic time is 20 minutes, ultrasonic power is 600 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing carboxyl.
Claims (1)
1. a preparation method for the molybdenum disulfide nano sheet of reactive group is contained on surface, it is characterized in that concrete steps are:
(1) n-Butyl Lithium of the molybdenumdisulphide of 1 weight part, 2 ~ 5 weight parts is joined in hydrothermal reaction kettle together with the normal hexane of 10 ~ 20 weight parts, heat 0.5 ~ 12 hour at 50 ~ 150 DEG C, then room temperature is cooled to, after centrifugation and n-hexane 5 times, drying 12 hours at 50 DEG C, the molybdenum disulfide powder of obtained lithium ion intercalation;
(2) molybdenum disulfide powder of lithium ion intercalation obtained for 1 weight part step (1), the sulfhydryl reagent with hydroxyl, carboxyl or amino of 0.05 ~ 10 weight part, the water of 100 ~ 1000 weight parts are added carry out in beaker ultrasonic, ultrasonic time is 1 minute ~ 5 hours, ultrasonic power is 50 ~ 1000 watts, i.e. the molybdenum disulfide nano sheet of obtained surface containing reactive group;
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-mercaptopropionyl)-glycine and captopril;
The described sulfhydryl reagent with amino is the one in mercaptoethylamine, halfcystine and 3-amino-1,2,4-triazole-5-mercaptan;
Described chemical reagent is chemical pure and above purity.
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| US9409792B2 (en) * | 2014-10-29 | 2016-08-09 | Toyota Motor Engineering & Manufacturing North America, Inc. | Solventhermal synthesis of nanosized two dimensional materials |
| CN106277055B (en) * | 2016-07-18 | 2018-02-27 | 安徽师范大学 | A kind of one-dimensional molybdenum disulfide nano material of lamella accumulation and preparation method thereof |
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| 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 |
| CN108190960B (en) * | 2018-01-23 | 2020-05-08 | 福州大学 | Method for preparing monolayer molybdenum disulfide based on hot lithium insertion stripping of electrolyte solvent |
| CN109762369B (en) * | 2019-02-28 | 2021-02-26 | 中山大学惠州研究院 | Preparation method of water-based high-dispersity nano molybdenum disulfide |
| CN110078124A (en) * | 2019-04-18 | 2019-08-02 | 哈尔滨理工大学 | A kind of mercaptan modification molybdenum disulfide composite material and preparation method |
| CN110902722A (en) * | 2019-12-17 | 2020-03-24 | 西南大学 | Device and method for preparing molybdenum disulfide nanosheet by anhydrous oxygen-free one-pot method |
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| CN114106811B (en) * | 2021-11-10 | 2023-06-02 | 中国石油大学(华东) | Two-dimensional nanomaterial reinforced clean fracturing fluid and preparation method and application thereof |
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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 |
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