CN103934012B - SnS 2/ g-C 3n 4composite nano plate photochemical catalyst and preparation method - Google Patents
SnS 2/ g-C 3n 4composite nano plate photochemical catalyst and preparation method Download PDFInfo
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Abstract
A kind of SnS
2/ g-C
3n
4composite nano plate photochemical catalyst, it is by SnS
2nanometer sheet and g-C
3n
4the SnS that nanometer sheet two sheet layer materials are constructed
2/ g-C
3n
4composite nano plate.This SnS
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst is mainly: stannic chloride pentahydrate and thioacetyl amine aqueous solution are placed in reactor, again the reactor of sealing is placed in electric dry oven and carries out hydro-thermal reaction, take out obtained product centrifugation and obtain yellow mercury oxide, after washing, namely product drying is obtained SnS
2nanometer sheet material; Urea powder is loaded in crucible, put into Muffle furnace after adding a cover and heat, namely obtain yellow g-C
3n
4nanometer sheet material; By SnS obtained above
2nanometer sheet and g-C
3n
4nanometer sheet is placed in methanol solution, carries out magnetic agitation again after water bath sonicator process, and put into reactor after removing methyl alcohol, reactor is placed in electric dry oven again and heats.The present invention can efficiently administer organic dyestuff sewage and preparation method is simple, with low cost.
Description
Technical field:
The present invention relates to a kind of visible light catalyst and preparation method.
Background technology:
Along with the fast development of urban industry, to be discharged arbitrarily by industrial wastewater and the water pollution problems caused is increasingly sharpened, the serious living environment that threaten people and healthy.The appearing as of Photocatalitic Technique of Semiconductor solves water pollution problems and provides a green brand-new route.Utilize this natural energy source of sunshine, semiconductor light-catalyst can organic pollution effectively in mineralizing and degrading sewage, reduce heavy metal ions in sewage and the bacterium killed in sewage.But, for TiO
2, the semiconductor light-catalyst that ZnO etc. are traditional, its greater band gap and absorb threshold wave-length be less than ~ 390nm, the ultraviolet portion of in solar energy about 4% can only be utilized, strongly limit the photocatalysis efficiency of these photochemical catalysts.Therefore, in order to the more effective visible region utilized in solar energy, the narrow bandgap semiconductor material with photocatalysis performance causes the extensive concern of researcher.As a kind of semi-conducting material of not containing metal element, the nitrogen carbon compound (g-C of graphite-like structure
3n
4) nanometer sheet because having band gap width narrow (~ 2.7eV), chemical stability and heat endurance is high, with low cost, environmental friendliness and the feature such as preparation technology is simple, and become the new lover of current photocatalysis field research.But the photo-quantum efficiency of himself needs to improve further.
Summary of the invention:
The object of the present invention is to provide the narrow gap semiconductor SnS that a kind of photocatalysis efficiency is high
2/ g-C
3n
4composite nano plate photochemical catalyst and preparation method.
SnS of the present invention
2/ g-C
3n
4composite nano plate photochemical catalyst is by SnS
2nanometer sheet and g-C
3n
4the SnS that nanometer sheet two sheet layer materials are constructed
2/ g-C
3n
4composite nano plate, utilizes the light cooperative effect of composite nano plate hetero-junctions to reduce the recombination probability of photo-generated carrier, thus improves the performance of photocatalyst for degrading organic dyestuff.
Above-mentioned SnS
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst is as follows:
1) SnS
2the preparation of nanometer sheet:
Stannic chloride pentahydrate and thioacetamide are pressed 1:5 ~ 20 mol ratio, and soluble in water, the solution after dissolving is placed in reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 160 ~ 180 DEG C, and the time is 12 ~ 16 hours.Reaction terminates rear reactor and naturally cools to room temperature, drives still, takes out obtained product centrifugation and obtains yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 8 ~ 12 hours at 60 DEG C, namely obtains SnS
2nanometer sheet material.
2) g-C
3n
4the preparation of nanometer sheet:
Take appropriate urea powder, load in alumina crucible after grinding is mixed, after adding a cover, put into Muffle furnace, in air atmosphere, (oxygen in air preferably in a nitrogen atmosphere, can be reduced and, to the consumption of nitrogen, improve C
3n
4output) rise to 500 ~ 600 DEG C with the speed of 15 ~ 35 DEG C/min, and keep 1 ~ 3 hour, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material.
3) by SnS
2with g-C
3n
4nanometer sheet compound:
By SnS obtained in step 1)
2nanometer sheet and step 2) in obtained g-C
3n
4nanometer sheet takes by 0.1 ~ 10:100 mass ratio, is placed in methanol solution, and above-mentioned two kinds of nanometer sheet materials 100 milligrams are corresponding with 20-40ml methyl alcohol, and then water bath sonicator process 0.5 ~ 1 is little disperses completely up to nanometer sheet, best SnS
2evenly be laid in g-C nanometer sheet single dispersing
3n
4nanometer sheet surface, to reduce SnS
2the agglomeration of nanometer sheet, improves its exposed area.At room temperature magnetic agitation 24 ~ 36 hours again, puts into reactor after methyl alcohol volatilizees completely, then the reactor of sealing is placed in electric dry oven heats, heating-up temperature 130 ~ 150 DEG C, 4 ~ 6 hours time.Reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.
According to band theory, when forming hetero-junctions between the semi-conducting material that band structure is mated mutually, because the two fermi level position of energy band difference can cause generating built in field in its interface, photo-generate electron-hole shifted effectively and is separated, thus improving the photo-quantum efficiency of conductor photocatalysis material.G-C
3n
4nanometer sheet and SnS
2nanometer sheet is all a kind of narrow gap semiconductor catalysis material with practical application foreground, and, SnS
2with g-C
3n
4there is the band structure of coupling mutually.Therefore, the two compound can be become heterojunction photocatalysis material to improve its photocatalysis performance.Particularly by the nano-lamellar structure Material cladding of the two, the photo-generated carrier stalling characteristic of its heterojunction boundary can be utilized to greatest extent to improve the performance of catalysis material.
The present invention compared with prior art tool has the following advantages:
1) SnS
2with g-C
3n
4double nano lamellar structure compound improves effective contact area in hetero-junctions region, inhibits the recombination probability of photo-generated carrier, obviously strengthens than the photochemical catalyst of one-component the degradation efficiency of organic dye pollutant.Therefore SnS of the present invention
2/ g-C
3n
4composite nano plate photochemical catalyst has efficient improvement organic dyestuff sewage ability.
2) SnS
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst is simple, easily manipulation, with low cost, pollute low, be applicable to large-scale industrial production.
Accompanying drawing explanation
The SnS of Fig. 1 prepared by the embodiment of the present invention 1
2the transmission electron microscope photo figure of nanometer sheet.
The g-C of Fig. 2 prepared by the embodiment of the present invention 1
3n
4the transmission electron microscope photo figure of nanometer sheet.
The SnS of Fig. 3 prepared by the embodiment of the present invention 1
2/ g-C
3n
4the transmission electron microscope photo figure of composite nano plate.
The SnS of Fig. 4 prepared by the embodiment of the present invention 1
2nanometer sheet, g-C
3n
4nanometer sheet and SnS
2/ g-C
3n
4the X-ray diffraction spectrogram of composite nano plate.
The SnS of Fig. 5 prepared by the embodiment of the present invention 1
2nanometer sheet, g-C
3n
4nanometer sheet and SnS
2/ g-C
3n
4the UV-Vis abosrption spectrogram of composite nano plate.
The SnS of Fig. 6 prepared by embodiment in the present invention 1 ~ 4
2/ g-C
3n
4composite nano plate and the SnS prepared by embodiment 1
2nanometer sheet, g-C
3n
4the curve map of nanometer sheet degradating organic dye rhodamine B,
Wherein a ~ d is respectively the SnS prepared by embodiment 1 ~ 4
2/ g-C
3n
4composite nano plate; The SnS of e prepared by embodiment 1
2nanometer sheet; The g-C of f prepared by embodiment 1
3n
4nanometer sheet.
The SnS of Fig. 7 prepared by embodiment 1
2nanometer sheet, g-C
3n
4nanometer sheet and SnS
2/ g-C
3n
4the curve map of composite nano plate degradating organic dye methyl orange.
Detailed description of the invention
In the mode of specific embodiment, the invention will be further described below:
Embodiment 1:
0.125mmol stannic chloride pentahydrate and 1mmol thioacetamide are dissolved in the 20ml aqueous solution, stir 30 minutes.Solution after dissolving is placed in 25ml reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 160 DEG C, and the time is 12 hours.Reaction terminates rear reactor and naturally cools to room temperature, drives still, takes out obtained product centrifugation and obtains yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 8 hours at 60 DEG C, namely obtains SnS
2nanometer sheet material.Obtained SnS
2the transmission electron microscope photo of nanometer sheet as shown in Figure 1.High-visible obtained SnS from figure
2nanometer sheet is of a size of 40 ~ 80nm, and thickness is 8 ~ 15nm.
Take 10g urea powder after grinding is mixed, load in alumina crucible, put into Muffle furnace after adding a cover, rise to 550 DEG C with the speed of 20 DEG C/min in a nitrogen atmosphere, and keep 2 hours, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material.Obtained g-C
3n
4the transmission electron microscope photo of nanometer sheet as shown in Figure 2.High-visible obtained g-C from figure
3n
4it is curling nanometer sheet.
By 5mgSnS obtained above
2nanometer sheet and 100mg g-C obtained above
3n
4nanometer sheet is placed in that the methanol solution water bath sonicator process 1 of 30ml is little to be disperseed completely up to nanometer sheet, then proceed to room temperature lower magnetic force in uncovered beaker and stir 24 hours, 25ml reactor is put into after methyl alcohol volatilizees completely, again the reactor of sealing is placed in electric dry oven to heat, heating-up temperature 140 DEG C, 4 hours time, reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.Obtained SnS
2/ g-C
3n
4the transmission electron microscope photo of composite nano plate as shown in Figure 3.Find out monodispersed SnS as seen from the figure
2nanometer sheet is evenly laid in g-C
3n
4nanometer sheet surface.Fig. 4 is prepared SnS
2nanometer sheet, g-C
3n
4nanometer sheet and SnS
2/ g-C
3n
4the X-ray diffraction spectrogram of composite nano plate, can find out SnS
2/ g-C
3n
4except SnS in the diffraction maximum of composite nano plate
2outside diffraction maximum, also there is other new diffraction maximum, they and graphite-like structure C
3n
4diffraction maximum consistent, and there is no other impurity diffraction maximum.This shows to have prepared SnS further
2/ g-C
3n
4composite nano-grade sheet material.From the SnS that Fig. 5 is prepared
2nanometer sheet, g-C
3n
4nanometer sheet and SnS
2/ g-C
3n
4can find out that above-mentioned material all has stronger visible light absorption in the UV-Vis abosrption spectrogram of composite nano plate.
Example 2
0.125mmol stannic chloride pentahydrate and 2mmol thioacetamide are dissolved in the 20ml aqueous solution, stir 30 minutes.Solution after dissolving is placed in 25ml reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 170 DEG C, and the time is 10 hours.Reaction terminates rear reactor and naturally cools to room temperature, drives still, takes out obtained product centrifugation and obtains yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 12 hours at 60 DEG C, namely obtains SnS2 nanometer sheet material.
Take 10g urea powder after grinding is mixed, load in alumina crucible, put into Muffle furnace after adding a cover, rise to 580 DEG C with the speed of 30 DEG C/min in air atmosphere, and keep 2.5 hours, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material.
By 1mgSnS obtained above
2nanometer sheet and 100mg g-C obtained above
3n
4nanometer sheet is placed in that the methanol solution water bath sonicator process 1 of 35ml is little to be disperseed completely up to nanometer sheet, then proceed to room temperature lower magnetic force in uncovered beaker and stir 30 hours, 25ml reactor is put into after methyl alcohol volatilizees completely, again the reactor of sealing is placed in electric dry oven to heat, heating-up temperature 145 DEG C, 5 hours time, reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.
Example 3
0.125mmol stannic chloride pentahydrate and 0.625mmol thioacetamide are dissolved in the 20ml aqueous solution, stir 30 minutes.Solution after dissolving is placed in 25ml reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 180 DEG C, and the time is 16 hours.Reaction terminates rear reactor and naturally cools to room temperature, drives still, takes out obtained product centrifugation and obtains yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 9 hours at 60 DEG C, namely obtains SnS
2nanometer sheet material.
Take 10g urea powder after grinding is mixed, load in alumina crucible, put into Muffle furnace after adding a cover, rise to 500 DEG C with the speed of 15 DEG C/min in a nitrogen atmosphere, and keep 3 hours, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material.
By 0.5mgSnS obtained above
2nanometer sheet and 100mg g-C obtained above
3n
4nanometer sheet is placed in that the methanol solution water bath sonicator process 0.5 of 20ml is little to be disperseed completely up to nanometer sheet, then proceed to room temperature lower magnetic force in uncovered beaker and stir 24 hours, 25ml reactor is put into after methyl alcohol volatilizees completely, again the reactor of sealing is placed in electric dry oven to heat, heating-up temperature 140 DEG C, 6 hours time, reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.
Example 4
0.125mmol stannic chloride pentahydrate and 2.5mmol thioacetamide are dissolved in the 20ml aqueous solution, stir 30 minutes.Solution after dissolving is placed in 25ml reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 160 DEG C, and the time is 13 hours.Reaction terminates rear reactor and naturally cools to room temperature, drives still, takes out obtained product centrifugation and obtains yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 12 hours at 60 DEG C, namely obtains SnS
2nanometer sheet material.
Take 10g urea powder after grinding is mixed, load in alumina crucible, put into Muffle furnace after adding a cover, rise to 600 DEG C with the speed of 35 DEG C/min in a nitrogen atmosphere, and keep 1 hour, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material.
By 10mgSnS obtained above
2nanometer sheet and 100mg g-C obtained above
3n
4nanometer sheet is placed in that the methanol solution water bath sonicator process 1 of 40ml is little to be disperseed completely up to nanometer sheet, then proceed to room temperature lower magnetic force in uncovered beaker and stir 36 hours, 25ml reactor is put into after methyl alcohol volatilizees completely, again the reactor of sealing is placed in electric dry oven to heat, heating-up temperature 150 DEG C, 5 hours time, reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.
Embodiment 5:
SnS
2/ g-C
3n
4the application of composite nano plate photochemical catalyst in degradating organic dye sewage, this photochemical catalyst of high spot reviews is to the visible light photocatalytic degradation ability of organic dyestuff rhodamine B sewage.The concrete practice is as follows: in photo catalysis reactor, add the rhodamine B aqueous solution that 100ml concentration is 10mg/L, then put into the SnS of 10mg
2/ g-C
3n
4composite nano plate photochemical catalyst, in darkroom magnetic agitation 30 minutes to adsorption equilibrium under room temperature.Then open the 300W xenon lamp that 400nm< λ <780nm optical filter is housed to irradiate, carry out photocatalytic degradation reaction.With the change with light application time of the trap of measurement of ultraviolet-visible spectrophotometer dye, rhodamine B, and calculate the degradation rate of dye, rhodamine B, the results are shown in Figure 6.SnS as can be known from Fig. 6 prepared by the present invention
2/ g-C
3n
4composite nano plate photochemical catalyst has efficient degradation capability to dye, rhodamine B, the SnS obtained by embodiment 1 ~ 4
2/ g-C
3n
4composite nano plate photochemical catalyst all reached the degradation rate of more than 90% in 60 minutes, and wherein obtained in embodiment 1 photochemical catalyst reached the degradation rate of 99.6% especially at 20 minutes; And one pack system SnS
2only degrade more than 20%, one pack system g-C
3n
4only degrade more than 50%.
Embodiment 6:
SnS
2/ g-C
3n
4the application of composite nano plate photochemical catalyst in degradating organic dye sewage, this photochemical catalyst of high spot reviews is to the visible light photocatalytic degradation ability of organic dyestuff methyl orange sewage.Detailed process is as follows: in photo catalysis reactor, add the methyl orange aqueous solution that 100ml concentration is 10mg/L, then put into the SnS of 10mg
2/ g-C
3n
4composite nano plate photochemical catalyst, in darkroom magnetic agitation 30 minutes to adsorption equilibrium under room temperature.Then open the 300W xenon lamp that 400nm< λ <780nm optical filter is housed to irradiate, carry out photocatalytic degradation reaction.With the change with light application time of the trap of measurement of ultraviolet-visible spectrophotometer methyl orange, and calculate the degradation rate of methyl orange, the results are shown in Figure 7.SnS as can be known from Fig. 7 prepared by the present invention
2/ g-C
3n
4composite nano plate photochemical catalyst has efficient degradation capability to methyl orange, the SnS obtained by embodiment 1
2/ g-C
3n
4composite nano plate photochemical catalyst reached the degradation rate of 99.2% in 40 minutes; And one pack system SnS
2only degrade more than 20%, one pack system g-C
3n
4only degrade more than 30%.
Claims (4)
1. a SnS
2/ g-C
3n
4composite nano plate photochemical catalyst, is characterized in that: it is by SnS
2nanometer sheet and g-C
3n
4the SnS that nanometer sheet two sheet layer materials are constructed
2/ g-C
3n
4composite nano plate.
2. the SnS of claim 1
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst, is characterized in that:
1) SnS
2the preparation of nanometer sheet:
Stannic chloride pentahydrate and thioacetamide are pressed 1:5 ~ 20 mol ratio, soluble in water, the solution after dissolving is placed in reactor, then the reactor of sealing is placed in electric dry oven carries out hydro-thermal reaction, hydrothermal temperature is 160 ~ 180 DEG C, time is 12 ~ 16 hours, and reaction terminates rear reactor and naturally cools to room temperature, drives still, take out obtained product centrifugation and obtain yellow mercury oxide, respectively with deionized water and ethanol washing, then by product vacuum drying 8 ~ 12 hours at 60 DEG C, namely obtain SnS
2nanometer sheet material;
2) g-C
3n
4the preparation of nanometer sheet:
Take appropriate urea powder, load in alumina crucible after grinding is mixed, after adding a cover, put into Muffle furnace, in air atmosphere, rise to 500 ~ 600 DEG C with the speed of 15 ~ 35 DEG C/min, and keep 1 ~ 3 hour, after naturally cooling to room temperature, take out porphyrize, namely obtain yellow g-C
3n
4nanometer sheet material;
3) by SnS
2with g-C
3n
4nanometer sheet compound:
By SnS obtained in step 1)
2nanometer sheet and step 2) in obtained g-C
3n
4nanometer sheet takes by 0.1 ~ 10:100 mass ratio, be placed in methanol solution, above-mentioned two kinds of nanometer sheet materials 100 milligrams are corresponding with 20-40ml methyl alcohol, then water bath sonicator process 0.5 ~ 1 is little disperses completely up to nanometer sheet, at room temperature magnetic agitation 24 ~ 36 hours again, reactor is put into after methyl alcohol volatilizees completely, again the reactor of sealing is placed in electric dry oven to heat, heating-up temperature 130 ~ 150 DEG C, 4 ~ 6 hours time, reaction terminates to take out after rear reactor naturally cools to room temperature, obtains final goal product S nS
2/ g-C
3n
4composite nano plate photochemical catalyst.
3. SnS according to claim 2
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst, is characterized in that: urea loads crucible, puts into Muffle furnace, heat in a nitrogen atmosphere after adding a cover.
4. SnS according to claim 2
2/ g-C
3n
4the preparation method of composite nano plate photochemical catalyst, is characterized in that: SnS
2evenly be laid in g-C nanometer sheet single dispersing
3n
4nanometer sheet surface.
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| CN104174423A (en) * | 2014-08-19 | 2014-12-03 | 河北科技大学 | Al2O3/g-C3N4 heterojunction photocatalyst and preparation method thereof |
| CN105195190A (en) * | 2015-07-06 | 2015-12-30 | 阜阳师范学院 | Heterojunction photocatalyst SnS2/g-C3N4 as well as preparation method and application thereof |
| CN106732719B (en) * | 2016-12-05 | 2019-04-16 | 厦门大学 | A kind of preparation method of carbonitride/stannic disulfide quantum dot composite photo-catalyst |
| CN107045010B (en) * | 2017-01-19 | 2019-03-15 | 济南大学 | The preparation method of optical electro-chemistry sensor based on the mesoporous carbonitride of stannic disulfide- |
| CN106964388B (en) * | 2017-03-06 | 2019-11-12 | 常州大学 | A kind of wolframic acid stannous adulterates the preparation method of two-dimentional graphite phase carbon nitride composite photo-catalyst |
| CN107149939B (en) * | 2017-04-26 | 2019-11-19 | 河北科技大学 | A kind of g-C3N4/Al2O3/ZnO hetero-junctions of visible light catalysis activity and preparation method thereof |
| CN107233910B (en) * | 2017-07-25 | 2019-11-19 | 洛阳理工学院 | One type graphitic nitralloy carbon/stannous sulfide nano heterojunction synthetic method |
| CN109701584A (en) * | 2019-03-01 | 2019-05-03 | 华东交通大学 | A kind of Z-type light-catalyst ZnO/Fe2O3/g-C3N4Preparation method and application |
| CN109939698B (en) * | 2019-03-28 | 2023-03-31 | 南京工业大学 | Preparation method of copper-tin-sulfur-carbon nanotube composite photocatalyst |
| CN109999841B (en) * | 2019-04-29 | 2022-05-17 | 陕西科技大学 | SnS2/1T-MoS2QDS composite photocatalyst, preparation method and application |
| CN110180579B (en) * | 2019-07-03 | 2022-04-01 | 河北工业大学 | Multi-stage SnS2Nanoflower and C3N4Quantum dot composite material and preparation method and application thereof |
| CN113024128B (en) * | 2021-03-31 | 2023-04-07 | 桂林理工大学 | Tin disulfide-C 3 N 4 Nanosheet array photoanode and preparation method thereof |
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