CN108483502A - A kind of preparation method and application of rhenium disulfide nanometer sheet - Google Patents
A kind of preparation method and application of rhenium disulfide nanometer sheet Download PDFInfo
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- CN108483502A CN108483502A CN201810568244.8A CN201810568244A CN108483502A CN 108483502 A CN108483502 A CN 108483502A CN 201810568244 A CN201810568244 A CN 201810568244A CN 108483502 A CN108483502 A CN 108483502A
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- C02F2101/40—Organic compounds containing sulfur
Abstract
The invention discloses a kind of preparation methods of rhenium disulfide nanometer sheet, and rhenium source and xanthate are mixed, and through hydro-thermal reaction, single layer and/or few layer rhenium disulfide nanometer sheet is made.It is sulphur source that this method, which selects the xanthates of large-scale commercial production, reproducible, at low cost, and can prepare single layer and/or few layer rhenium disulfide nanometer sheet.The nanometer sheet can be applied to the fields such as absorption, photocatalysis, light degradation, lubrication, photoelectric device.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, and in particular to a kind of single layer and/or few layer rhenium disulfide nanometer
The preparation method of piece.
Background technology
Nano material has excellent performance, is widely used in scientific research and engineering field.Rhenium disulfide (ReS2) receive
Interlaminar action is faint in rice material structure, and single layer or few layer rhenium disulfide have that large specific surface area, adsorption capacity be strong, reactivity
The features such as high, makes it be applied in the fields such as absorption, photocatalysis, electronic device, energy storage material.Currently, rhenium disulfide material
The preparation method of material includes chemical vapor deposition, chemical liquid phase stripping and hydro-thermal method.
Chemical vapor deposition often uses the rheniums sources such as simple substance rhenium, chlorination rhenium, and preparation condition is harsh, and reaction temperature is high, manufacturing cost
It is high.
Kim etc.《S Kim,H K Yu,S Yoon,N S Lee,MH Kim.Growth of two-dimensional
rhenium disulfide(ReS2)nanosheets with a few layers at low
temperature.CrystEngComm,2017,19,5341》Using the method for chemical vapor deposition, using rhenium trichloride as rhenium
Source, under normal pressure in helium atmosphere, reaction temperature prepares rhenium disulfide when being 450 DEG C.
Chemical liquid phase stripping usually requires in an inert atmosphere, and rhenium disulfide powder and intercalator containing lithium is fully mixed
It closes, heats at high temperature later the long period, after reaction the rhenium disulfide nanometer sheet of isolated certain size range.
Fujita etc.《Fujita,T.,Ito,Y.,Tan,Y.,Yamaguchi,H.,Hojo,D.,Hirata,A.,
Voiry,D.,Chhowalla,M.,Chen,M..Chemically exfoliated ReS2nanosheets.Nanoscale,
2014,6(21):12458-12462》The use of rhenium disulfide powder is rhenium source, with lithium borohydride (LiBH4) intercalator is in argon atmospher
It is uniformly mixed in enclosing, is then heated to 350 DEG C and keeps the temperature 3 days, product is dissolved in ultrasound 1h in bubbling argon water, is centrifugally separating to obtain
The rhenium disulfide nanometer sheet of grain size about 50~100nm, the preparation process reaction time is longer, and reaction temperature is higher, experimental facilities
It is required that high, complex process is expensive.
Hydro-thermal method is a kind of method of synthetizing micro-nano material, and a certain proportion of precursor solution is placed in autoclave
In, sealing keeps the temperature a period of time under certain temperature, detaches and washs and can be obtained micro Nano material.
Application No. is 201610580163.0 patent (Chen Yuanfu, Qi Fei, Zheng Binjie, Li Pingjian, Zhou Jinhao, Wang Xinqiang,
A kind of methods preparing rhenium disulfide nanometer sheet of Zhang Wanli, 201610580163.0,2016-07-22) disclose a kind of prepare
The method of rhenium disulfide nanometer sheet.This method be by ammonium perrhenate, hydroxylamine hydrochloride and thiocarbamide distinguish it is soluble in water, after mixing
It moves into reaction under high pressure, sealing, rhenium disulfide nanometer sheet is made in 160~260 DEG C of 6~48h of heat preservation.
Hydrothermal synthesis method has reaction condition mild, simple process and low cost, the features such as being easy to industrialized production.But it is existing
Some hydro-thermal methods do not prepare single layer or few layer rhenium disulfide nanometer sheet.If the prior art to obtain high-specific surface area,
Strong adsorption capacity, the single layer of high reaction activity or few layer rhenium disulfide nanometer sheet also need to pass through chemical gas to multilayer rhenium disulfide
Mutually deposition or chemical liquid phase stripping make it remove between layers, and severe reaction conditions are of high cost.
Invention content
The first purpose of the invention is to provide it is a kind of it is at low cost, reaction condition is mild, reproducible, and can effectively and can
Control single layer and/or the hydrothermal synthesis method of few layer rhenium disulfide nanometer sheet.The method of the present invention is prepared suitable for large-scale industry.
Second object of the present invention is to provide a kind of single layer and/or few layer molybdenum disulfide nano sheet absorption degradation xanthic acid
Application.
A kind of preparation method of rhenium disulfide of the present invention, rhenium source is mixed with xanthates, and through hydro-thermal reaction, single layer is made
Or few layer rhenium disulfide nanometer sheet.
Different from selecting thiocarbamide, thioacetamide etc. to prepare rhenium disulfide nanometer material for sulphur source in existing hydrothermal synthesis technology
Material, the present invention select xanthates to be sulphur source, are easily obtained as industrial products, and price is low, and inventor, which passes through to study, to be sent out
Sulphur source is now done using the xanthates in the present invention, can facilitate and prepare single layer and/or few layer rhenium disulfide nanometer sheet.The present invention
Method it is at low cost, reproducible, suitable for large-scale industry prepare.
The single layer and/or few layer rhenium disulfide nanometer sheet number of plies are not higher than 5 layers.
The single layer and/or few layer rhenium disulfide nanometer sheet, thickness are 0.5~4.0nm.
Single layer and/or few layer rhenium disulfide have the characteristics that large specific surface area, adsorption capacity are strong, reactivity is high.
The ratio between amount of substance of sulphur, rhenium is 2~12 in xanthates and rhenium source：1.
The pH value of rhenium source solution is 5~12.
The temperature of the hydro-thermal reaction is 140~240 DEG C.
Rhenium disulfide can be collected by standing or high speed centrifugation.The solvent that the washing impurity-removing of rhenium disulfide is selected include go from
One or more of sub- water, absolute ethyl alcohol.The drying of rhenium disulfide can be cold by forced air drying, vacuum and heating drying, vacuum
It is lyophilized one or more of dry.
The structural formula of the xanthates is as follows：
In formula I, the R is C1~C20Aliphatic group or C6~C20Aryl in one kind.
The xanthates is sodium xanthogenate or potassium xanthate.
The aliphatic group is C1-C8Straight chain or branched alkyl.
Xanthates is methyl xanthates, ethyl xanthate, n-propyl xanthates, isopropyl xanthan hydrochlorate, just
One or more of butyl xanthate, isobutyl group xanthates, amyl xanthate or hexyl xanthates.
The rhenium source is one or more of rehenic acid ammonium or perrhenate ammonium.
The pH value of rhenium source solution can be adjusted with alkaline solution, including sodium hydroxide solution, potassium hydroxide solution, sodium carbonate are molten
Liquid, sodium bicarbonate solution, sodium acetate solution, solution of potassium carbonate, potassium bicarbonate solution, potassium acetate solution, sodium citrate, citric acid
One or more of potassium, concentrated ammonia liquor.
Inventors discovered through research that almost Quantitative yield is rhenium disulfide in rhenium source in the preparation method.
The rhenium disulfide that preparation method of the present invention is prepared.
Rhenium disulfide of the present invention is applied to adsorb and/or degrade xanthic acid.
The single layer or few layer rhenium disulfide nanometer sheet, handle hexyl potassium xanthate solution 12 hours at 25 DEG C, and degradation/
Adsorption rate can reach 1346mg (hexyl potassium xanthate)/g (rhenium disulfide).
Beneficial effects of the present invention are：
Compared with existing hydro-thermal method uses thiocarbamide or thioacetamide to prepare rhenium disulfide micro-nano material for sulphur source, this hair
It is bright, using surfactant xanthates as sulphur source, can a step prepare that large specific surface area, adsorption capacity are strong, reactivity is high
Single layer and/or few layer molybdenum disulfide nano sheet, and be not necessarily to any follow-up dispersion and lift-off processing, greatly reduce manufacturing cost and
Process complexity provides reliable, economic, efficient preparation method for rhenium disulfide micro-nano material.
In application aspect, rhenium disulfide nanometer sheet material prepared by the present invention, absorption/degradation to hexyl potassium xanthate
Efficiency is up to 1346mg/g, effect highly significant.
Description of the drawings
Fig. 1 is that the field emission electron of the rhenium disulfide nanometer sheet prepared by the embodiment of the present invention 1 scans micro- Electronic Speculum
(FESEM) photo；
Fig. 2 is the electro microscope energy spectrum figure (EDS) of the rhenium disulfide nanometer sheet prepared by the embodiment of the present invention 1；
Fig. 3 is the Raman spectrum (Raman spectra) of the rhenium disulfide nanometer sheet prepared by the embodiment of the present invention 1；
Fig. 4 is the x-ray diffraction pattern (XRD) of the rhenium disulfide nanometer sheet prepared by the embodiment of the present invention 1；
Fig. 5 is atomic force (AFM) figure of the rhenium disulfide nanometer sheet prepared by the embodiment of the present invention 1；
Fig. 6 is the transmission electron microscope (TEM) of the rhenium disulfide nanometer sheet prepared by embodiment 1 in the method for the present invention
Figure；
Fig. 7 is that the rhenium disulfide nanometer sheet in the method for the present invention prepared by embodiment 1 handles 1 × 10 at 25 DEG C-4mol/L
The small degradation of hexyl potassium xanthate 12/adsorption rate figure.
Specific embodiment
The content of present invention is further illustrated by the following example, but protection scope of the present invention is not limited by these embodiments
System.
In embodiment unless otherwise specified all parts and percentages refer both to quality.
Embodiment 1
By 0.5000g rehenic acid ammoniums ((NH4)2ReO4) and 0.5400g sodium ethylxanthates (C3H5OS2Na it) is dissolved in 30mL respectively
In deionized water, until completely dissolved, with concentrated ammonia liquor by (NH4)2ReO4The pH value of solution is adjusted to 7.00, later by C3H5OS2Na
Solution is added thereto, it is made to be uniformly mixed.Mixed liquor is transferred in 100mL autoclaves, seal, be placed in baking oven in
200 DEG C of heat preservation 8h, cooled to room temperature.Reaction product is repeatedly washed after separation with deionized water and absolute ethyl alcohol, is collected
And black powder product is obtained after vacuum freeze drying, as rhenium disulfide material.Wherein almost Quantitative yield is two to rehenic acid ammonium
Sulfuration rhenium.
Fig. 1 is that the field emission electron of the rhenium disulfide material prepared by the present embodiment scans micro- Electronic Speculum (FESEM) picture,
It is made of as can be seen from Figure 1 numerous tiny nanometer sheets, it is whole in spongy.Fig. 2 is the electro microscope energy spectrum in 1 region of corresponding diagram
Scheme (EDS), only exist rhenium atom and sulphur atom, illustrates that product is rhenium disulfide.Fig. 3 is rhenium disulfide prepared by the present embodiment
Raman collection of illustrative plates belongs to few layer of structure rhenium disulfide material.Fig. 4 is the XRD spectrum of rhenium disulfide prepared by the present embodiment, is
The unformed class product of amorphous phase, is inferred as rhenium disulfide nano material.Fig. 5 is the rhenium disulfide product prepared by the embodiment
Atomic force microscope (AFM) picture shows that the rhenium disulfide nanometer sheet thickness is mostly 1.8-2.1nm, is secondly 1.1-1.4nm,
Minority is 0.5-0.7nm, illustrates that it is mostly three layers, further includes double-deck and individual layer nanometer sheet.Fig. 6 is prepared by the embodiment
Transmission electron microscope (TEM) figure of rhenium disulfide nanometer sheet is determined as single layer and few layer nanostructure again.Fig. 7 is this reality
It applies rhenium disulfide prepared by example and handles 1 × 10 at 25 DEG C-4The small degradation of mol/L hexyls potassium xanthate 12/adsorption rate figure.From figure
7 it is found that prepared single layer and few layer rhenium disulfide nanometer sheet to low concentration hexyl potassium xanthate, (xanthates is mine ore dressing
One of major pollutants of waste water) removal effect it is very good, degradation/adsorption rate reaches 1346mg (hexyl potassium xanthate)/g
(rhenium disulfide).
Embodiment 2
By 0.5000g rehenic acid ammoniums ((NH4)2ReO4) and 0.5400g sodium ethylxanthates (C3H5OS2Na it) is dissolved in 30mL respectively
In deionized water, until completely dissolved by C3H5OS2(NH is added in Na solution4)2ReO4In solution, the two is made to be uniformly mixed.It will mix
It closes liquid to be transferred in 100mL autoclaves, seal, be placed in baking oven and keep the temperature 10h, cooled to room temperature in 200 DEG C.Reaction
Product is repeatedly washed after separation with deionized water and absolute ethyl alcohol, is collected and is obtained black powder production after vacuum freeze drying
Object, as rhenium disulfide material.Wherein almost Quantitative yield is rhenium disulfide to rehenic acid ammonium.
Embodiment 3
By 0.5000g rehenic acid ammoniums ((NH4)2ReO4) and 0.5400g sodium ethylxanthates (C3H5OS2Na it) is dissolved in water respectively
In, until completely dissolved, with concentrated ammonia liquor by (NH4)2ReO4The pH value of solution is adjusted to 9.00, later by C3H5OS2Na solution is added
Wherein, it is made to be uniformly mixed.Mixed liquor is transferred in 100mL autoclaves, is sealed, is placed in baking oven in 190 DEG C of heat preservations
12h, cooled to room temperature.Reaction product is repeatedly washed after separation with deionized water and absolute ethyl alcohol, collects and vacuum is cold
Be lyophilized it is dry after obtain black powder product, as rhenium disulfide material.Wherein almost Quantitative yield is rhenium disulfide to rehenic acid ammonium.
Embodiment 4
By 0.5000g rehenic acid ammoniums ((NH4)2ReO4) and 0.6500g sodium isobutyl xanthans (C5H9OS2Na it) is dissolved in water respectively
In, until completely dissolved, with concentrated ammonia liquor by (NH4)2ReO4The pH value of solution is adjusted to 7.00, later by C5H9OS2Na solution is added
Wherein, magnetic agitation 20min makes it be uniformly mixed.Mixed liquor is transferred in 100mL autoclaves, seals, is placed in baking oven
In in 200 DEG C keep the temperature 8h, cooled to room temperature.Reaction product is repeatedly washed after separation with deionized water and absolute ethyl alcohol,
It collects and obtains black powder product, as rhenium disulfide material after vacuum freeze drying.Wherein rehenic acid ammonium almost Quantitative yield
For rhenium disulfide.
Embodiment 5
By 0.7000g rehenic acid ammoniums ((NH4)2ReO4) and 0.8500g sodium isobutyl xanthans (C5H9OS2Na it) is dissolved in respectively
In 30mL deionized waters, until completely dissolved by C5H9OS2(NH is added in Na solution4)2ReO4In solution, the two is made to be uniformly mixed.
Mixed liquor is transferred in 100mL autoclaves, is sealed, is placed in baking oven and keeps the temperature 6h, cooled to room temperature in 220 DEG C.
Reaction product is repeatedly washed after separation with deionized water and absolute ethyl alcohol, is collected and is obtained black powder after vacuum freeze drying
Last product, as rhenium disulfide material.Wherein almost Quantitative yield is rhenium disulfide to rehenic acid ammonium.
Embodiment 6
By 1.000g rehenic acid ammoniums ((NH4)2ReO4) and 1.8000g sodium isobutyl xanthans (C5H9OS2Na it) is dissolved in respectively
In 30mL deionized waters, until completely dissolved, with concentrated ammonia liquor by (NH4)2ReO4The pH value of solution is adjusted to 8.50, later will
C5H9OS2Na solution is added thereto, it is made to be uniformly mixed.Mixed liquor is transferred in 100mL autoclaves, seals, is placed in baking
In case 12h, cooled to room temperature are kept the temperature in 190 DEG C.Reaction product is repeatedly washed after separation with deionized water and absolute ethyl alcohol
It washs, collect and obtains black powder product, as rhenium disulfide material after vacuum freeze drying.Wherein rehenic acid ammonium almost quantitatively turns
Turn to rhenium disulfide.
Claims (10)
1. a kind of preparation method of rhenium disulfide nanometer sheet, which is characterized in that rhenium source is mixed with xanthates, it is anti-through hydro-thermal
It answers, single layer and/or few layer rhenium disulfide nanometer sheet is made.
2. the preparation method of rhenium disulfide nanometer sheet as described in claim 1, it is characterised in that：The single layer and/or few layer
The rhenium disulfide nanometer sheet number of plies is not higher than 5 layers.
3. the preparation method of rhenium disulfide nanometer sheet as described in claim 1, it is characterised in that：The single layer and/or few layer
The thickness of rhenium disulfide nanometer sheet is 0.5-4.0nm.
4. the preparation method of rhenium disulfide nanometer sheet as described in claim 1, it is characterised in that：Sulphur in xanthates and rhenium source,
The ratio between amount of substance of rhenium is 2~12：1.
5. the preparation method of rhenium disulfide nanometer sheet as described in claim 1, it is characterised in that：The pH value of rhenium source solution is 5
~12；The temperature of the hydro-thermal reaction is 140~240 DEG C.
6. the preparation method of rhenium disulfide nanometer sheet as claimed in any one of claims 1 to 6, it is characterised in that：The xanthan
The structural formula of hydrochlorate is as follows：
In formula I, the R is C1~C20Aliphatic group or C6~C20Aryl in one kind.
7. the preparation method of rhenium disulfide nanometer sheet as claimed in claim 6, it is characterised in that：The aliphatic group is C1-
C8Straight chain or branched alkyl.
8. the preparation method of rhenium disulfide nanometer sheet as claimed in claim 7, it is characterised in that：Xanthates is methyl xanthan
Hydrochlorate, ethyl xanthate, n-propyl xanthates, isopropyl xanthan hydrochlorate, normal-butyl xanthates, isobutyl group xanthic acid
One or more of salt, amyl xanthate or hexyl xanthates.
9. the preparation method of rhenium disulfide nanometer sheet as described in claim 1, which is characterized in that the rhenium source is rehenic acid ammonium
Or one or more of ammonium perrhenate.
10. a kind of application for the rhenium disulfide nanometer sheet being prepared based on claim 1-9 any one of them methods, special
Sign is：For the xanthic acid that adsorbs and/or degrade.
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Cited By (7)
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| CN109160542A (en) * | 2018-09-28 | 2019-01-08 | 航天材料及工艺研究所 | A method of preparing rhenium pentachloride |
| CN109954502A (en) * | 2019-04-02 | 2019-07-02 | 浙江大学 | A kind of few layer ReS2Nanometer sheet@MoS2Quantum dot composite photo-catalyst and preparation method thereof |
| CN110061204A (en) * | 2019-03-21 | 2019-07-26 | 天津大学 | Two-dimensional honeycomb carbon nanosheet coated 1T' -ReS2Preparation method of sodium ion battery cathode material |
| CN110357147A (en) * | 2019-07-23 | 2019-10-22 | 中国科学技术大学 | The heterogeneous nano material of rhenium disulfide-stannic disulfide, preparation method and application |
| CN110508292A (en) * | 2019-07-15 | 2019-11-29 | 天津大学 | The preparation method of metal-doped rhenium disulfide nano-chip arrays for electro-catalysis complete solution water |
| CN111060568A (en) * | 2019-12-18 | 2020-04-24 | 温州医科大学 | Method for constructing collagen type III photoelectrochemical sensor based on rhenium disulfide nanosheet and application |
| CN111072069A (en) * | 2019-09-25 | 2020-04-28 | 江南大学 | Method for preparing visible light response 2D rhenium disulfide and application |
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