CN105289657B - The preparation method of graphene antimony sulfide nano rod composite visible light catalyst - Google Patents
The preparation method of graphene antimony sulfide nano rod composite visible light catalyst Download PDFInfo
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Abstract
The invention provides a kind of preparation method of graphene antimony sulfide nano rod composite visible light catalyst.This method is first added graphene oxide into adjacent hydroxy diol, ultrasonic disperse, then adds SbCl3, after heating, stirring is allowed to dissolving, sulphur powder is added, continues to stir and evenly mix, added sodium borohydride, stirring, after backflow a period of time, naturally cool to room temperature, centrifuge, obtain black precipitate；Black precipitate is washed, after drying, obtain graphene antimony sulfide nano rod composite visible light catalyst.Photochemical catalyst composite effect produced by the present invention is good, visible light photocatalysis active is high, has the advantages of simple production process, production process safety, response parameter is easily controlled, implementation cost is low and is easily achieved industrialized production.It can be widely used for the preparation of graphene-based compound monodimension nanometer material.
Description
Technical field
The invention belongs to photocatalysis technology field, and in particular to one kind uses circumfluence method synthesizing graphite alkene-antimony sulfide nano
The method of rod composite visible light catalyst.
Background technology
Environmental pollution and two hang-ups that energy shortage is 21 century facing mankind.Heterogeneous Photocatalysis of Semiconductors due to
Can directly using the oxygen in sunshine and air come thoroughly degrade environmental contaminants and by the most attention of people.The technology
With cost is low, wide adaptation range, it is environment-friendly, easy to use, to organic matter of the pollutant mineralising completely and to difficult degradation
It is that a very promising Green-pollution administers new technology with series of advantages such as good oxygenolysis.Photocatalysis
The key of technology application is to develop suitable semiconductor light-catalyst.
At present, in the semiconductor catalyst that multiphase photocatalysis reacts applied, nano-TiO2With its nontoxic, catalytic activity
High, the advantages that stability is good and oxidation resistance is strong and enjoy the favor of people.But use TiO2Photocatalyst has two big
Defect, first, its greater band gap (Eg=3.2eV), only wavelength X ＜ 387nm ultraviolet light can just be allowed to excite, and sunshine
In ultraviolet luminous energy proportion less than 5%, thus the utilization rate of solar energy is low；Second, caused light induced electron and sky are excited by light
Cave is easily compound, so that photocatalysis efficiency is low.To overcome these shortcomings, people are using multiple means to TiO2It is modified, its
Include dye sensitization, semiconductors coupling, noble metal decorated, transition metal ions and nonmetal doping etc., to change
TiO2Energy gap, make the response spectrum of reaction to visible ray Directional Extension, and effectively suppress electronics, hole is to answering
Close, so as to improve its photocatalysis efficiency.Pass through these modifications, TiO2Though photocatalytic activity obtained a certain degree of raising,
But its efficiency is still relatively low.
Antimony trisulfide (Sb2S3) it is a kind of common(V represents the 5th main group, and VI represents the 6th main group, A As,
Sb,Bi；B is S, Se, Te) type direct band-gap semicondictor material, band gap is 1.5~2.2eV, and it covers sunshine power spectrum
Visible and near infrared region, there is very strong light absorpting ability, 10 are up in the absorption coefficient of light of visible region5cm-1, therefore,
It is a kind of very promising visible-light photocatalysis material.But in photocatalytic process, antimony trisulfide and many other photocatalysis
Agent is the same, there is photo-generate electron-hole to easily it is compound the defects of so that photo-quantum efficiency is very low, and this is largely
Reduce the utilization rate of solar energy and the efficiency of light-catalyzed reaction.Therefore, antimony trisulfide photoproduction during light-catalyzed reaction is reduced
The compound probability of electron-hole pair is the effective way for improving its photocatalysis efficiency.
Graphene (graphene) is the sp by individual layer2The cellular two dimensional crystal that the carbon atom close-packed arrays of hydridization are formed
Structure, monoatomic layer thickness are only 0.335nm, and big pi bond present in it enables pi-electron to move freely, and its valence band and are led
It is zero clearance semi-metallic with the overlapping of fraction, and the intermolecular forces of the carbon atom of graphene are extremely strong, electronics is transmitting
During resistance very little, be not susceptible to scatter, thus it has excellent electric conductivity, electron mobility can be up to
200000cm2/ (Vs), electrical conductivity 106S/m.Graphene also possesses huge specific surface area, and (its theoretical specific surface area is up to
2600m2/ g), the prominent capacity of heat transmission and mechanical property, half-integer quantum hall effect, unique quantum tunneling effect etc. one
Series Properties.It is well known that after conductor photocatalysis material absorbs the light of certain wavelength, the electrons of valence band are excited and jumped
Conduction band is adjourned, but with the hole left spontaneous recombination reaction occurs for the electrons excited, with electronics and compound, the light in hole
Catalytic process also just terminates.As can be seen here, it is to suppress to excite electron-hole pair to improve one of effective ways of photocatalysis efficiency
Recombination reaction.If graphene is compound with semi-conducting material, the high electron mobility of graphene can be just utilized, makes to swash electricity
Son is moved in graphene film Rotating fields rapidly, rather than is accumulated in catalysis material surface, and this reduces excite electronics and sky
The compound probability in cave, so as to improve the photocatalysis efficiency of semi-conducting material.In addition, the huge ratio table that graphene possesses
Area, it is also beneficial to improve the photocatalysis efficiency of semi-conducting material.
Currently, the preparation research about graphene-sulfur antimony composite photo-catalyst is few both at home and abroad, and its known document is also only
See first, i.e. " Tao W G, Chang J L, Wu D P, et al.Solvothermal synthesis of graphene-
Sb2S3composite and the degradation activity under visible light[J].Materials
Research Bulletin, 2013,48,538-543. ", it is with graphene oxide, SbCl3, thiocarbamide be raw material, ethylene glycol
For solvent, 12 hours are reacted to prepare graphene-sulfur antimony composite photo-catalyst at 100 DEG C by solvent-thermal method.This method is deposited
It is micron particles rather than antimony sulfide nano rod, preparation condition in the antimony trisulfide of poor product quality, appendix on graphene sheet layer
It is harsh and be difficult to control, the defects of production cost is high.The present invention is using graphene oxide, SbCl3, sulphur powder be raw material, hydroboration
Sodium is reducing agent and adjacent hydroxy diol is solvent, and being prepared for graphene-sulfur antimony nanometer rods composite visible light with circumfluence method urges
Agent.During the course of the reaction, sodium borohydride generates H with sulphur powder reaction2S, H2S again under reflux conditions with SbCl3Reaction generation
Antimony sulfide nano rod, meanwhile, graphene oxide (GO) by sodium borohydride reduction turn into graphene (or be redox graphene,
RGO), graphene with antimony sulfide nano rod is compound turns into graphene-sulfur antimony nanometer rod composite material.By to composite
Visible light photocatalysis performance is investigated, the results showed that, the visible light photocatalysis active of product is high, can make full use of sunshine to environment
Pollutant carries out photocatalytic degradation.The synthetic method has no document report both at home and abroad, has novelty and creativeness.
The content of the invention
It is an object of the invention to provide a kind of simple production process, production process safety, composite effect be good, visible light catalytic
The preparation method of the high graphene-sulfur antimony nanometer rods composite visible light catalyst of activity.
The purpose of the present invention is realized in the following way：
A kind of preparation method of graphene-sulfur antimony nanometer rods composite visible light catalyst, comprises the following steps：
(a) add graphene oxide into adjacent hydroxy diol, ultrasonic disperse 1~3 hour, be configured to 0.5~2mg/mL
The dispersion liquid of graphene oxide-adjacent hydroxy diol；
(b) SbCl is added in dispersion liquid3, heating stirring is allowed to dissolve, SbCl3With the thing of adjacent hydroxy diol in dispersion liquid
The ratio between amount of matter is 1:300~550；Then sulphur powder is added, the amount of the material of the sulphur powder is SbCl3The 2~4 of the amount of material
Times, continue to stir and evenly mix, obtain mixed liquor；
(c) sodium borohydride is added in mixed liquor, is stirred continuously simultaneously, the amount of the material of the sodium borohydride is sulphur powder thing
2~4 times of the amount of matter；Then, it is stirred at reflux at 160~200 DEG C 5~15 hours；
(d) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate；Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace supersound washing, and graphene-sulfur antimony nanometer rods composite visible light catalyst is obtained after drying.
Described adjacent hydroxy diol is ethylene glycol or 1,2- propane diols.
The beneficial effects of the present invention are：
(1) graphene oxide and SbCl that the present invention is prepared with improved Hummers methods3, sulphur powder be raw material, and with boron hydrogen
Change sodium is reducing agent and adjacent hydroxy diol is solvent, and it is compound visible to prepare graphene-sulfur antimony nanometer rods by circumfluence method
Photochemical catalyst, solve poor product quality, visible light photocatalysis active existing for existing preparation method are low, production cost is high, peace
The defects of full property difference, there is simple production process, production process safety, response parameter is easily controlled, implementation cost is low, it is real to be easy to
Existing large-scale industrial production, the advantages of photocatalysis efficiency is high.
(2) the graphene-sulfur antimony nanometer rods composite visible light catalyst category composite for preparing of the present invention, on the one hand its
There is very strong absorption to visible ray, electron mobility is high, conductive capability is strong, and photo-generate electron-hole is to can be easily separated；The opposing party
Its graphene sheet layer of face and antimony sulfide nano rod are respectively provided with very big specific surface area, therefore, add the work of its visible light photocatalysis
Property, sunshine can be made full use of to carry out photocatalytic degradation to environmental pollutants, reduce the cost of environmental improvement.The present invention
It can be widely used for the preparation of graphene-based compound monodimension nanometer material.
Brief description of the drawings
Fig. 1 is the X-ray diffraction of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 1
(XRD) figure.
Fig. 2 is the SEM of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 1
(SEM) figure.
Fig. 3 is the SEM of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 2
(SEM) figure.
Fig. 4 is the SEM of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 3
(SEM) figure.
Fig. 5 is the SEM of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 4
(SEM) figure.
Fig. 6 is SEM (SEM) figure of antimony sulfide nano rod prepared by comparative example.
Fig. 7 is antimony sulfide nano rod prepared by comparative example and graphene-sulfur antimony nanometer rods composite visible light catalyst
Photocatalysis effect figure.Wherein e is antimony sulfide nano rod, and a, b, c, d are respectively embodiment 1, embodiment 4, embodiment 3, embodiment 2
The graphene-sulfur antimony nanometer rods composite visible light catalyst of preparation, abscissa represent degradation time, and ordinate represents degraded
Rate.
Embodiment
With reference to specific embodiment, the present invention is further illustrated：
Embodiment 1
(1) graphene oxide for weighing 60mg is added in 60mL 1,2-PD, ultrasonic disperse 2 hours, is obtained
The dispersion liquid of 1mg/mL graphene oxide -1,2- propane diols.
(2) 0.46g SbCl are added in dispersion liquid3, slightly hot, stirring is allowed to dissolve (SbCl3With 1,2- third in dispersion liquid
The ratio of the amount of the material of glycol is 1:405) 0.18g sulphur powders, are then added, the amount for adding the material of sulphur powder is SbCl3Material
2.8 times of amount, continue to stir and evenly mix, obtain mixed liquor, mixed liquor is transferred in three-neck flask.
(3) 0.56g sodium borohydrides, while continuous magnetic agitation are slowly added into mixed liquor, the material of sodium borohydride
Measure the amount for sulphur powder material 2.6 times.Then, with oil bath heating, it is stirred at reflux at 160 DEG C 15 hours.
(4) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate.Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace each 3 times of supersound washing, and graphene-sulfur antimony nanometer is obtained after 60 DEG C of dryings in thermostatic drying chamber
Rod composite visible light catalyst product.
Embodiment 2
(1) graphene oxide for weighing 25mg is added in 50mL ethylene glycol, ultrasonic disperse 1 hour, obtains 0.5mg/
The dispersion liquid of mL graphene oxides-ethylene glycol.
(2) 0.37g SbCl are added in dispersion liquid3, slightly hot, stirring is allowed to dissolve (SbCl3With ethylene glycol in dispersion liquid
Material amount ratio be 1:550) 0.20g sulphur powders, are then added, the amount for adding the material of sulphur powder is SbCl3The amount of material
3.9 times, continue to stir and evenly mix, obtain mixed liquor, mixed liquor is transferred in three-neck flask.
(3) 0.48g sodium borohydrides, while continuous magnetic agitation are slowly added into mixed liquor, the material of sodium borohydride
Measure the amount for sulphur powder material 2.0 times.Then, with oil bath heating, it is stirred at reflux at 190 DEG C 5 hours.
(4) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate.Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace each 3 times of supersound washing, and graphene-sulfur antimony nanometer is obtained after 60 DEG C of dryings in thermostatic drying chamber
Rod composite visible light catalyst product.
Embodiment 3
(1) graphene oxide for weighing 90mg is added in 45mL 1,2-PD, ultrasonic disperse 3 hours, is obtained
The dispersion liquid of 2mg/mL graphene oxide -1,2- propane diols.
(2) 0.47g SbCl are added in dispersion liquid3, slightly hot, stirring is allowed to dissolve (SbCl3With 1,2- third in dispersion liquid
The ratio of the amount of the material of glycol is 1:300) 0.14g sulphur powders, are then added, the amount for adding the material of sulphur powder is SbCl3Material
2.2 times of amount, continue to stir and evenly mix, obtain mixed liquor, mixed liquor is transferred in three-neck flask.
(3) 0.68g sodium borohydrides, while continuous magnetic agitation are slowly added into mixed liquor, the material of sodium borohydride
Measure the amount for sulphur powder material 4.0 times.Then, with oil bath heating, it is stirred at reflux at 170 DEG C 10 hours.
(4) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate.Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace each 3 times of supersound washing, and graphene-sulfur antimony nanometer is obtained after 60 DEG C of dryings in thermostatic drying chamber
Rod composite visible light catalyst product.
Embodiment 4
(1) graphene oxide for weighing 78mg is added in 52mL ethylene glycol, ultrasonic disperse 2 hours, obtains 1.5mg/
The dispersion liquid of mL graphene oxides-ethylene glycol.
(2) 0.47g SbCl are added in dispersion liquid3, slightly hot, stirring is allowed to dissolve (SbCl3With ethylene glycol in dispersion liquid
Material amount ratio be 1:450) 0.20g sulphur powders, are then added, the amount for adding the material of sulphur powder is SbCl3The amount of material
3.0 times, continue to stir and evenly mix, obtain mixed liquor, mixed liquor is transferred in three-neck flask.
(3) 0.75g sodium borohydrides, while continuous magnetic agitation are slowly added into mixed liquor, the material of sodium borohydride
Measure the amount for sulphur powder material 3.2 times.Then, with oil bath heating, it is stirred at reflux at 180 DEG C 12 hours.
(4) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate.Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace each 3 times of supersound washing, and graphene-sulfur antimony nanometer is obtained after 60 DEG C of dryings in thermostatic drying chamber
Rod composite visible light catalyst product.
Comparative example
For the photocatalysis performance of graphene-sulfur antimony nanometer rod composite material and antimony sulfide nano rod is contrasted, use
Prepare composite identical method and prepare antimony sulfide nano rod, it is concretely comprised the following steps：
(1) 0.46g SbCl are added in 60mL 1,2- propane diols3, slightly hot, stirring is allowed to dissolve (SbCl3With 1,2-
The ratio of the amount of the material of propane diols is 1:405) 0.18g sulphur powders, are then added, the amount for adding the material of sulphur powder is SbCl3Thing
2.8 times of the amount of matter, continue to stir and evenly mix, obtain mixed liquor, mixed liquor is transferred in three-neck flask.
(2) 0.56g sodium borohydrides, while continuous magnetic agitation are slowly added into mixed liquor, the material of sodium borohydride
Measure the amount for sulphur powder material 2.6 times.Then, with oil bath heating, it is stirred at reflux at 160 DEG C 15 hours.
(3) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate.Black precipitate is spent respectively from
Sub- water and absolute ethyl alcohol replace each 3 times of supersound washing, and antimony sulfide nano rod product is obtained after 60 DEG C of dryings in thermostatic drying chamber.
Visible light photocatalysis performance is tested：
50mg photochemical catalyst is added in 100mL 10mg/L methylene blue (MB) solution, lucifuge ultrasonic disperse 5
Minute, then magnetic agitation 30 minutes in the dark, methylene blue is reached adsorption equilibrium in catalyst surface.5mL sample liquids are taken to centrifuge
It is separated off that catalyst powder is last, it is tested in the 664nm (maximum absorption waves of methylene blue with ultraviolet-visible spectrophotometer
It is long) absorbance at place and as the initial absorbance A for the liquid that is degraded0.Then, visible ray light is carried out as light source using 300W xenon lamps to urge
Change degradation experiment (top of xenon lamp is away from liquid level 15cm), while magnetic agitation, sample liquid 5mL every 10 minutes, centrifugation is gone
After falling catalyst solid, supernatant liquor is taken to determine its absorbance A at phase co-wavelengthx, and the drop of methylene blue is calculated accordingly
Solution rate.
X-ray diffraction (XRD) figure of graphene-sulfur antimony nanometer rods composite visible light catalyst prepared by embodiment 1 is such as
(embodiment 1 is basically identical to the x-ray diffraction pattern of the gained catalyst of embodiment 4) shown in Fig. 1.By Fig. 1 and Sb2S3Standard spectrum
Figure (JCPDS No.42-1393) control knows that its all diffraction maximum position is all consistent with standard spectrogram, and diffracted intensity is higher,
Illustrate that the antimony trisulfide for the orthorhombic crystal phase that product is well-crystallized is supported on graphene film, but can't see the diffraction maximum of graphene,
This antimony sulfide nano rod that has been due to the piece Intercalation reaction of graphene, so as to destroy piling up in order for graphene film.
Embodiment 1, embodiment 2, embodiment 3, the graphene-sulfur antimony nanometer rods composite visible light prepared by embodiment 4
SEM (SEM) photo of catalyst is respectively as shown in Fig. 2, Fig. 3, Fig. 4, Fig. 5.As seen from the figure, the sulphur in product
Change antimony nanometer rods except uniform load between graphene sheet layer in addition to graphene film layer surface, is also inserted (graphene film it is very thin and
Translucency is good, transparent shape, it may be clearly seen that the antimony sulfide nano rod of insertion piece interlayer), graphene film and antimony sulfide nano
The composite effect of rod is good.Antimony sulfide nano rod in embodiment 1, embodiment 2, embodiment 3, the composite prepared by embodiment 4
Length be respectively 0.2~1.2 μm (micron), 0.3~2.0 μm, 0.2~1.2 μm, 0.2~1.5 μm；Diameter is respectively 50~
100nm (nanometer), 35~200nm, 75~150nm, 50~150nm.
SEM (SEM) photo of antimony sulfide nano rod prepared by comparative example as shown in fig. 6, as seen from Figure 6,
Gained antimony sulfide nano rod grows 0.3~1.8 μm, a diameter of 60~130nm.
Antimony sulfide nano rod that comparative example is prepared with embodiment and graphene-sulfur antimony nanometer rod composite material is taken to enter respectively
Row photocatalysis performance is tested, as a result as shown in Figure 7.As seen from Figure 7, graphene-sulfur antimony nanometer rod composite material (sample a, b,
C, visible light photocatalysis active d) is apparently higher than antimony sulfide nano rod (sample e), composite wherein made from embodiment 1
(sample a) visible light photocatalysis active is highest.As can be seen here, antimony sulfide nano rod greatly improved in the compound of graphene
Visible light photocatalysis active.
Claims (2)
1. a kind of preparation method of graphene-sulfur antimony nanometer rods composite visible light catalyst, it is characterised in that including following step
Suddenly：
(a) add graphene oxide into adjacent hydroxy diol, ultrasonic disperse 1~3 hour, be configured to 0.5~2mg/mL oxidations
The dispersion liquid of graphene-adjacent hydroxy diol；
(b) SbCl is added in dispersion liquid3, heating stirring is allowed to dissolve, SbCl3With the material of adjacent hydroxy diol in dispersion liquid
The ratio between amount is 1:300~550；Then sulphur powder is added, the amount of the material of the sulphur powder is SbCl32~4 times of the amount of material, after
It is continuous to stir and evenly mix, obtain mixed liquor；
(c) sodium borohydride is added in mixed liquor, is stirred continuously simultaneously, the amount of the material of the sodium borohydride is sulphur powder material
2~4 times of amount；Then, it is stirred at reflux at 160~200 DEG C 5~15 hours；
(d) after the completion of reacting, room temperature is naturally cooled to, centrifuges, obtains black precipitate；Deionized water is used into black precipitate respectively
Replace supersound washing with absolute ethyl alcohol, graphene-sulfur antimony nanometer rods composite visible light catalyst is obtained after drying.
2. the preparation method of graphene-sulfur antimony nanometer rods composite visible light catalyst according to claim 1, its feature
It is：Described adjacent hydroxy diol is ethylene glycol or 1,2- propane diols.
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| CN106622294A (en) * | 2016-12-31 | 2017-05-10 | 湘潭大学 | Preparation method of graphene-based composite Sb2S3 photocatalyst |
| CN107819044B (en) * | 2017-10-24 | 2019-08-23 | 三峡大学 | A kind of preparation method of antimony trisulfide base photodetector |
| CN108579767A (en) * | 2018-05-04 | 2018-09-28 | 南开大学 | It is grown on the Sb of graphene surface2S3Nanometer sheet and its preparation method and application |
| CN110931731B (en) * | 2019-11-08 | 2020-10-23 | 上海应用技术大学 | Two-dimensional carbide crystal-based antimony sulfide negative electrode material and preparation method and application thereof |
| CN111933900B (en) * | 2020-06-23 | 2022-05-10 | 南京农业大学 | Antimony sulfide/graphene composite nano material and preparation method and application thereof |
| CN113436898B (en) * | 2021-07-08 | 2022-06-07 | 新余学院 | Thin film electrode material for dye-sensitized solar cell and preparation method thereof |
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