CN108483502B - Preparation method and application of rhenium disulfide nanosheet - Google Patents
Preparation method and application of rhenium disulfide nanosheet Download PDFInfo
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Abstract
The invention discloses a preparation method of a rhenium disulfide nanosheet, which comprises the steps of mixing a rhenium source and xanthate, and carrying out hydrothermal reaction to obtain a single-layer and/or few-layer rhenium disulfide nanosheet. The method selects xanthate produced commercially in large scale as a sulfur source, has good repeatability and low cost, and can prepare single-layer and/or few-layer rhenium disulfide nanosheets. The nano sheet can be applied to the fields of adsorption, photocatalysis, photodegradation, lubrication, photoelectric devices and the like.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method of a single-layer and/or few-layer rhenium disulfide nanosheet.
Background
The nano material has excellent performance and is widely applied to the fields of scientific research and engineering. Rhenium disulfide (ReS)2) The interlayer effect in the structure of the nano material is weak, and the single layer or few layers of rhenium disulfide have the characteristics of large specific surface area, strong adsorption capacity, high reaction activity and the like, so that the nano material is applied to the fields of adsorption, photocatalysis, electronic devices, energy storage materials and the like. Currently, methods for preparing rhenium disulfide materials include chemical vapor deposition, chemical liquid phase stripping, and hydrothermal methods.
The common rhenium sources such as elemental rhenium, rhenium chloride and the like for chemical vapor deposition have harsh preparation conditions, high reaction temperature and high preparation cost.
Kim et al S Kim, H K Yu, S Yoon, N S Lee, MH Kim growth of two-dimensional rhodium complex (ReS)2) The nanosheets with a new layers at low temperature CrystEngComm,2017 and 19,5341 adopt a chemical vapor deposition method, and rhenium trichloride is taken as a rhenium source, and rhenium disulfide is prepared at the reaction temperature of 450 ℃ in a helium atmosphere under normal pressure.
Chemical liquid phase stripping generally requires that rhenium disulfide powder and a lithium-containing intercalation agent are fully mixed in an inert gas environment, then heating is carried out for a long time at a high temperature, and separation is carried out after the reaction is finished to obtain a rhenium disulfide nanosheet in a certain size range.
Fujita et al, Fujita, T.Ito, Y.A., Tan, Y.A., Yamaguchi, H.A., Hojo, D.A., Hirata, A.A., Voiry, D.A., Chowalla, M.A., Chen, M.A. chemical ex-oriented ReS2nanoscales, 2014,6(21):12458-12462 using rhenium disulfide powder as the rhenium source with lithium borohydride (LiBH)4) The intercalation agent is uniformly mixed in an argon atmosphere, then the mixture is heated to 350 ℃ and is kept warm for 3 days, the product is dissolved in argon bubbling water for ultrasonic treatment for 1 hour, and centrifugal separation is carried out to obtain the rhenium disulfide nanosheet with the particle size of about 50-100 nm.
The hydrothermal method is a method for synthesizing the micro-nano material, and the micro-nano material can be obtained by placing a certain proportion of precursor solution in a high-pressure reaction kettle, sealing, keeping the temperature for a period of time at a certain temperature, separating and washing.
Patent No. 201610580163.0 (chenyu, chiffon, zhengbin, li nun jian, zhou jinhao, wangxinqiang, zhanwanli. a method for preparing rhenium disulfide nanosheets, 201610580163.0,2016-07-22) discloses a method for preparing rhenium disulfide nanosheets. The method comprises the steps of respectively dissolving ammonium perrhenate, hydroxylamine hydrochloride and thiourea in water, uniformly mixing, transferring into a high-pressure reaction, sealing, and keeping the temperature at 160-260 ℃ for 6-48 hours to obtain the rhenium disulfide nanosheet.
The hydrothermal synthesis method has the characteristics of mild reaction conditions, simple process, low cost, easy industrial production and the like. However, the existing hydrothermal method does not prepare a single-layer or few-layer rhenium disulfide nanosheet. In the prior art, if a single-layer or few-layer rhenium disulfide nanosheet with high specific surface area, strong adsorption capacity and high reaction activity is to be obtained, multiple layers of rhenium disulfide are required to be stripped from one another through chemical vapor deposition or chemical liquid phase stripping, the reaction conditions are harsh, and the cost is high.
Disclosure of Invention
The first purpose of the invention is to provide a hydrothermal synthesis method of rhenium disulfide nanosheets, which has the advantages of low cost, mild reaction conditions, good repeatability, effective and controllable single-layer and/or few-layer. The method of the invention is suitable for large-scale industrial preparation.
The second purpose of the invention is to provide an application of single-layer and/or few-layer molybdenum disulfide nanosheets for adsorbing and degrading xanthic acid.
The invention relates to a preparation method of rhenium disulfide, which is characterized in that a rhenium source and xanthate are mixed, and a single-layer or few-layer rhenium disulfide nanosheet is prepared through hydrothermal reaction.
Different from the existing hydrothermal synthesis technology in which thiourea, thioacetamide and the like are selected as sulfur sources to prepare the rhenium disulfide nano material, xanthate is selected as the sulfur source, and is easy to obtain as an industrial product, the cost is low, and the inventor finds that single-layer and/or few-layer rhenium disulfide nano sheets can be conveniently prepared by using the xanthate as the sulfur source through research. The method has low cost and good repeatability, and is suitable for large-scale industrial preparation.
The number of the single-layer and/or few-layer rhenium disulfide nanosheets is not more than 5.
The thickness of the single-layer and/or few-layer rhenium disulfide nanosheet is 0.5-4.0 nm.
The single layer and/or few layers of rhenium disulfide have the characteristics of large specific surface area, strong adsorption capacity, high reaction activity and the like.
The amount ratio of the xanthate to the sulfur and rhenium in the rhenium source is 2-12: 1.
the pH value of the rhenium source solution is 5-12.
The temperature of the hydrothermal reaction is 140-240 ℃.
Rhenium disulfide can be collected by standing or high speed centrifugation. The solvent selected for washing and impurity removal of rhenium disulfide comprises one or more of deionized water and absolute ethyl alcohol. The drying of the rhenium disulfide can be one or more of air drying, vacuum heating drying and vacuum freeze drying.
The xanthate has the following structural formula:
in the formula I, R is C1～C20Aliphatic hydrocarbon radical of (C)6～C20One of aryl groups of (1).
The xanthate is sodium xanthate or potassium xanthate.
The aliphatic hydrocarbon group is C1-C8Straight or branched chain alkyl groups.
The xanthate is one or more of methyl xanthate, ethyl xanthate, n-propyl xanthate, isopropyl xanthate, n-butyl xanthate, isobutyl xanthate, amyl xanthate or hexyl xanthate.
The rhenium source is one or more of ammonium rhenate or ammonium perrhenate.
The pH value of the rhenium source solution can be adjusted by alkaline solution, and the pH value of the rhenium source solution can be adjusted by one or more of sodium hydroxide solution, potassium hydroxide solution, sodium carbonate solution, sodium bicarbonate solution, sodium acetate solution, potassium carbonate solution, potassium bicarbonate solution, potassium acetate solution, sodium citrate, potassium citrate and concentrated ammonia water.
The inventors have found through research that the rhenium source is almost quantitatively converted to rhenium disulfide in this preparation process.
The rhenium disulfide prepared by the preparation method is provided by the invention.
The rhenium disulfide provided by the invention is applied to adsorbing and/or degrading xanthic acid.
The single-layer or few-layer rhenium disulfide nanosheet is treated by a potassium hexyl xanthate solution at 25 ℃ for 12 hours, and the degradation/adsorption rate can reach 1346mg (potassium hexyl xanthate)/g (rhenium disulfide).
The invention has the beneficial effects that:
compared with the existing hydrothermal method for preparing the rhenium disulfide micro-nano material by using thiourea or thioacetamide as a sulfur source, the method disclosed by the invention can be used for preparing the single-layer and/or few-layer molybdenum disulfide nanosheets with large specific surface area, strong adsorption capacity and high reaction activity in one step by using the surfactant xanthate as the sulfur source, and does not need any subsequent dispersion and stripping treatment, so that the preparation cost and the process complexity are greatly reduced, and a reliable, economic and efficient preparation method is provided for the rhenium disulfide micro-nano material.
In the application aspect, the adsorption/degradation efficiency of the rhenium disulfide nanosheet material prepared by the method can reach 1346mg/g, and the effect is very obvious.
Drawings
Fig. 1 is a field emission electron scanning microscopy (FESEM) photograph of rhenium disulfide nanosheets prepared in example 1 of the present invention;
FIG. 2 is an electron microscopy energy spectrum (EDS) of a rhenium disulfide nanosheet prepared in example 1 of the present invention;
fig. 3 is a Raman spectrum (Raman spectra) of a rhenium disulfide nanosheet prepared in example 1 of the present invention;
FIG. 4 is an X-ray diffraction pattern (XRD) of rhenium disulfide nanoplates prepared according to example 1 of the present invention;
fig. 5 is an Atomic Force (AFM) plot of rhenium disulfide nanoplates prepared in example 1 of the present invention;
figure 6 is a Transmission Electron Microscope (TEM) image of rhenium disulfide nanoplates prepared in example 1 of the method of the present invention;
FIG. 7 shows that rhenium disulfide nanosheets prepared in example 1 of the method of the present invention were treated at 1X 10 at 25 deg.C-4And a small degradation/adsorption rate graph of 12 mol/L potassium hexyl xanthate.
DETAILED DESCRIPTION OF EMBODIMENT (S) OF INVENTION
The invention is further illustrated by the following examples, without restricting its scope.
All parts and percentages in the examples are by mass unless otherwise specified.
Example 1
0.5000g of ammonium rhenate ((NH)4)2ReO4) And 0.5400g of sodium ethylxanthate (C)3H5OS2Na) are respectively dissolved in 30mL deionized water, and after the Na is completely dissolved, (NH) is dissolved by strong ammonia water4)2ReO4The pH of the solution was adjusted to 7.00, after which C was added3H5OS2Na solution is added to the mixture to mix it evenly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the heat at 200 ℃ for 8h, and naturally cooling to room temperature. And separating the reaction product, washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, collecting the reaction product, and carrying out vacuum freeze drying to obtain a black powder product, namely the rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Figure 1 is a field emission electron scanning microscopy (FESEM) image of the rhenium disulfide material prepared in this example,as can be seen from FIG. 1, the nano-particles are composed of a plurality of fine nano-particles, and the whole nano-particles are sponge-shaped. FIG. 2 is an electron micrograph (EDS) of the region corresponding to FIG. 1, showing the presence of rhenium atoms and sulfur atoms only, indicating that the product is rhenium disulfide. Fig. 3 is a Raman spectrum of rhenium disulfide prepared in this example, which is a rhenium disulfide material with a few-layer structure. FIG. 4 is an XRD pattern of rhenium disulfide prepared in this example as an amorphous product, and is inferred to be a rhenium disulfide nanomaterial. FIG. 5 is an Atomic Force Microscope (AFM) picture of the rhenium disulfide product prepared in this example, showing that the rhenium disulfide nanosheets are mostly 1.8-2.1nm thick, secondly 1.1-1.4nm thick, and a few are 0.5-0.7nm thick, which indicates that they are mostly three-layered, and further include bilayer and monolayer nanosheets. Fig. 6 is a Transmission Electron Microscope (TEM) image of rhenium disulfide nanoplates prepared in this example, again identified as single and few layer nanostructures. FIG. 7 shows rhenium disulfide prepared in this example treated at 25 ℃ at 1X 10-4And a small degradation/adsorption rate graph of 12 mol/L potassium hexyl xanthate. As can be seen from FIG. 7, the prepared single-layer and few-layer rhenium disulfide nanosheets have very good removal effect on low-concentration potassium hexyl xanthate (xanthate is one of main pollutants in mine beneficiation wastewater), and the degradation/adsorption rate reaches 1346mg (potassium hexyl xanthate)/g (rhenium disulfide).
Example 2
0.5000g of ammonium rhenate ((NH)4)2ReO4) And 0.5400g of sodium ethylxanthate (C)3H5OS2Na) are respectively dissolved in 30mL of deionized water, and C is dissolved after complete dissolution3H5OS2Na solution is added (NH)4)2ReO4In the solution, the two are mixed uniformly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the temperature at 200 ℃ for 10h, and naturally cooling to room temperature. And separating the reaction product, washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, collecting the reaction product, and carrying out vacuum freeze drying to obtain a black powder product, namely the rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Example 3
0.5000g of ammonium rhenate ((NH)4)2ReO4) And 0.5400g sodium Ethyl xanthate (C)3H5OS2Na) are respectively dissolved in water, and after complete dissolution, (NH) is dissolved by strong ammonia water4)2ReO4The pH of the solution was adjusted to 9.00, after which C was added3H5OS2Na solution is added to the mixture to mix it evenly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the temperature at 190 ℃ for 12h, and naturally cooling to room temperature. And separating the reaction product, washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, collecting the reaction product, and carrying out vacuum freeze drying to obtain a black powder product, namely the rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Example 4
0.5000g of ammonium rhenate ((NH)4)2ReO4) And 0.6500g of sodium isobutyl xanthate (C)5H9OS2Na) are respectively dissolved in water, and after complete dissolution, (NH) is dissolved by strong ammonia water4)2ReO4The pH of the solution was adjusted to 7.00, after which C was added5H9OS2Na solution is added, and the mixture is stirred for 20min by magnetic force to be mixed evenly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the heat at 200 ℃ for 8h, and naturally cooling to room temperature. And separating the reaction product, washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, collecting the reaction product, and carrying out vacuum freeze drying to obtain a black powder product, namely the rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Example 5
0.7000g of ammonium rhenate ((NH)4)2ReO4) And 0.8500g of sodium isobutyl xanthate (C)5H9OS2Na) are respectively dissolved in 30mL of deionized water, and C is dissolved after complete dissolution5H9OS2Na solution is added (NH)4)2ReO4In the solution, the two are mixed uniformly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the heat at 220 ℃ for 6h, and naturally cooling to room temperature. Separating the reaction product, washing with deionized water and anhydrous ethanol for multiple times, collecting, and vacuum freeze drying to obtain black powder productA rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Example 6
1.000g of ammonium rhenate ((NH)4)2ReO4) And 1.8000g of sodium isobutyl xanthate (C)5H9OS2Na) are respectively dissolved in 30mL deionized water, and after the Na is completely dissolved, (NH) is dissolved by strong ammonia water4)2ReO4The pH of the solution was adjusted to 8.50, after which C was added5H9OS2Na solution is added to the mixture to mix it evenly. Transferring the mixed solution into a 100mL high-pressure reaction kettle, sealing, placing in an oven, preserving the temperature at 190 ℃ for 12h, and naturally cooling to room temperature. And separating the reaction product, washing the reaction product for multiple times by using deionized water and absolute ethyl alcohol, collecting the reaction product, and carrying out vacuum freeze drying to obtain a black powder product, namely the rhenium disulfide material. Where the ammonium rhenate is almost quantitatively converted to rhenium disulfide.
Claims (8)
1. A preparation method of a rhenium disulfide nanosheet is characterized in that a rhenium source and xanthate are mixed and subjected to hydrothermal reaction to prepare a single-layer and/or few-layer rhenium disulfide nanosheet; the amount ratio of the xanthate to the sulfur and rhenium in the rhenium source is 2-12: 1; the pH value of the rhenium source solution is 5-12; the temperature of the hydrothermal reaction is 140-240 ℃.
2. A method of preparing rhenium disulfide nanoplates as in claim 1, wherein: the number of the single-layer and/or few-layer rhenium disulfide nanosheets is not more than 5.
3. A method of preparing rhenium disulfide nanoplates as in claim 1, wherein: the thickness of the single-layer and/or few-layer rhenium disulfide nanosheet is 0.5-4.0 nm.
4. A method of preparing rhenium disulfide nanoplates as in claim 1, wherein: the xanthate has the following structural formula:
in the formula I, R is C1～C20Aliphatic hydrocarbon radical of (C)6～C20One of aryl groups of (1).
5. A method of preparing rhenium disulfide nanoplates as in claim 4, wherein: the aliphatic hydrocarbon group is C1-C8Straight or branched chain alkyl groups.
6. A method of preparing rhenium disulfide nanoplates as in claim 5, wherein: the xanthate is one or more of methyl xanthate, ethyl xanthate, n-propyl xanthate, isopropyl xanthate, n-butyl xanthate, isobutyl xanthate, amyl xanthate or hexyl xanthate.
7. A method of making rhenium disulfide nanoplates as in claim 1 wherein the rhenium source is one or both of ammonium rhenate or ammonium perrhenate.
8. Use of rhenium disulphide nanosheets, prepared according to the process of any one of claims 1 to 7, wherein: for adsorbing and/or degrading xanthic acid.
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| WO2018085413A1 (en) * | 2016-11-01 | 2018-05-11 | Northwestern University | Layer-by-layer sorting of rhenium disulfide via high-density isopycnic density gradient ultracentrufugation |
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