CN105148949A - Bismuth oxyiodide-bismuth vanadium oxide heterojunction photocatalyst and preparation method thereof - Google Patents

Bismuth oxyiodide-bismuth vanadium oxide heterojunction photocatalyst and preparation method thereof Download PDF

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CN105148949A
CN105148949A CN201510459089.2A CN201510459089A CN105148949A CN 105148949 A CN105148949 A CN 105148949A CN 201510459089 A CN201510459089 A CN 201510459089A CN 105148949 A CN105148949 A CN 105148949A
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solution
pucherite
bismuth
bismuth oxyiodide
heterojunction photocatalyst
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CN105148949B (en
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王永强
刘思瑶
刘芳
赵朝成
赵东风
李石
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China University of Petroleum East China
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Abstract

The invention belongs to the technical field of semiconductor photocatalysis, and discloses a bismuth oxyiodide-bismuth vanadium oxide heterojunction photocatalyst and a preparation method thereof. The photocatalyst is a heterostructure formed by combination of bismuth oxyiodide ad bismuth vanadium oxide, and bismuth vanadium oxide nanoparticles are uniformly dispersed on bismuth oxyiodide nanoparticle surfaces. The preparation method comprises firstly dissolving bismuth nitrate pentahydrate and citric acid in diluted nitric acid and adjusting pH value, dissolving ammonium metavanadate and citric acid in distilled water and heating, and mixing the two solutions; and dissolving bismuth nitrate pentahydrate in glycol, dissolving potassium iodide KI in distilled water, mixing the two solutions and putting into the above mixed solutions, stirring, ageing, drying, calcining and grinding, so as to obtain the heterojunction photocatalyst. The synthesized photocatalyst possesses the typical heterostructure, possesses the characteristics of inhibiting electron-cavity recombination and effectively promoting carrier separation, and compared with a monomer bismuth vanadium oxide, the synthesized photocatalyst is relatively wide in photoresponse scope and relatively good in catalytic activity and stability.

Description

A kind of bismuth oxyiodide-pucherite heterojunction photocatalyst and preparation method thereof
Technical field
The invention belongs to Photocatalitic Technique of Semiconductor field, specifically, particularly a kind of heterojunction photocatalyst and preparation method thereof.
Background technology
Along with environmental pollution and energy shortage problem are more serious, photocatalysis technology due to the features such as its economy, environmental protection, degraded be thorough in purification of air, dispose of sewage, sterilization, the field such as hydrogen manufacturing receive much concern.With TiO 2for representative traditional catalysis material because stable, cheap, nontoxic, catalytic activity is good and be subject to extensive research, but, broad-band gap due to photochemical catalyst can make it can only have the shortcoming of catalytic activity at ultraviolet region, greatly limit the application in every field.
The non-titania-based visible-light photocatalysis material of pucherite to be energy gap be 2.2-2.4eV, mainly contains three kinds of crystal structures, is respectively monocline scheelite, cubic scheelite and cubic Zircon cut.Wherein, the photocatalytic activity of monoclinic phase scheelite type is best, but causes because adsorptivity is poor at the bottom of the separative efficiency of its photo-generated carrier.
At present, Co 3o 4/ BiVO 4, TiO 2/ BiVO 4, BiVO 4/ Bi 2o 3, BiOCl/BiVO 4, BiOBr/BiVO 4photochemical catalyst Deng heterojunction structure is successfully synthesized.Research shows, the catalyst after compound effectively can suppress the compound again of electron-hole, greatly improves photocatalytic activity.
BiOX (BiOX, X=Cl, Br, I) has the high anisotropy layer structure of PbFCl type, has good adsorptivity, and the energy gap of BiOI is only 1.76-1.85eV simultaneously.
By means such as element doping, semiconductors coupling, photoactivates to only carrying out modification in the luminescent material of ultraviolet region response, develop the catalysis material of high activity, wide spectral response, the visible ray utilization rate improving catalyst becomes current study hotspot.Therefore, based on catalysis material theory analysis, BiOX and BiVO 4compound has the feature of strengths and weaknesses complementation, from being with coupling angle, easily forms heterojunction photocatalysis material.
Summary of the invention
The present invention is to solve with TiO 2traditional photochemical catalyst for representative only can absorb ultraviolet light and cause the technical problem of Solar use rate variance, provide a kind of bismuth oxyiodide-pucherite heterojunction photocatalyst and preparation method thereof, this heterojunction photocatalyst light abstraction width is wide, visible ray utilization rate is high, have and promote that photo-generated carrier is separated, effective feature improving electron transfer rate, its photocatalytic activity and stability better, can rapid rhodamine B degradation dyestuff in short time, preparation method's simple, safety, economy, environmental protection simultaneously.
In order to solve the problems of the technologies described above, the present invention is achieved by following technical scheme:
A kind of bismuth oxyiodide-pucherite heterojunction photocatalyst, be that the bismuth oxyiodide of 0.05:1-1:1 and pucherite are compounded to form heterojunction structure by mol ratio, pucherite nano particle is dispersed in bismuth oxyiodide nano grain surface, and wherein the thing of pucherite is monocline scheelite type mutually.
The mol ratio of described bismuth oxyiodide and described pucherite is 0.1:1-0.5:1.
A preparation method for bismuth oxyiodide-pucherite heterojunction photocatalyst, adopts following steps to carry out:
(1) by Bi (NO 3) 35H 2o and C 6h 8o 7h 2o is dissolved in 1mol/L dust technology according to the mol ratio of 1:1-1:3, adds ammoniacal liquor adjust ph to 6.5-7.5, is designated as solution A;
(2) will with Bi (NO described in step (1) 3) 35H 2the NH of O equimolar amounts 4vO 3and with C described in step (1) 6h 8o 7h 2the C of O equimolar amounts 6h 8o 7h 2o is dissolved in distilled water, is designated as B solution;
(3), after B solution being stirred 30-50min under 60-90 DEG C of heating condition, solution becomes blackish green, more slowly adds solution A, is mixed to form C solution;
(4) mole is taken for 0.05-1 is doubly to Bi (NO described in step (1) 3) 35H 2bi (the NO of O 3) 35H 2o, and be dissolved in ethylene glycol, be designated as solution D;
(5) will with Bi (NO described in step (4) 3) 35H 2the KI of O equimolar amounts is dissolved in distilled water, is designated as E solution;
(6) by solution D and E solution mix and blend after 12-24 hour, join in the C solution that step (3) obtains, Keep agitation 6-14h is to forming navy blue gel, ageing 24-48h, be placed in 100-120 DEG C of baking oven to dry, then be fired in 300-400 DEG C and become solid, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst.
Preferably, Bi (NO in step (1) 3) 35H 2o and C 6h 8o 7h 2the mol ratio of O is 1:2.
Preferably, the pH in step (1) is 7.
Preferably, the heating-up temperature in step (3) is 80 DEG C.
Preferably, in step (6), the mix and blend time is 12-15h.
Preferably, in step (6), digestion time is 24-36h.
Preferably, the calcining heat in step (6) is 350 DEG C.
The invention has the beneficial effects as follows:
(1) BiOI/BiVO for preparing of the present invention 4photochemical catalyst has typical heterojunction structure, BiVO 4, BiOI is when being subject to illumination, produce electron-hole pair, because the difference that energy gap is different, can there is directional migration to BiVO in the photoelectron of BiOI under the effect of internal electric field simultaneously 4valence band on, and then can suppress the compound again of electron-hole, effectively improve quantum efficiency, heterojunction structure meets the requirement of high activity, wide spectral response.
(2) BiOI/BiVO for preparing of the present invention 4during photochemical catalyst light degradation organic dyestuff rhodamine B, compared to monomer pucherite BiVO 4, photocatalytic activity is better, and stability is higher.
(3) preparation method of the present invention is simple to operation, and do not need large-scale, complicated experimental facilities, cost is low, and environmental protection can be applicable to industrialization.
Accompanying drawing explanation
The BiOI/BiVO that Fig. 1 is embodiment 1, prepared by embodiment 2 4x-ray diffraction (XRD) spectrogram of heterojunction photocatalyst;
Fig. 2 is BiOI/BiVO prepared by embodiment 1 4sEM (SEM) image of photochemical catalyst, with reference to monomers B iVO 4;
Wherein, (A), (B) are the monomers B iVO of reference 4, (C), (D) are BiOI/BiVO prepared by embodiment 1 4heterojunction photocatalyst;
Fig. 3 is BiOI/BiVO prepared by embodiment 1 4fTIR spectrum (FT-IR) analysis chart of heterojunction photocatalyst, with reference to pure BiOI and pure BiVO 4;
Fig. 4 is BiOI/BiVO 4the forming process figure of photochemical catalyst heterojunction structure;
The BiOI/BiVO that Fig. 5 is embodiment 1, prepared by embodiment 2 4the clearance trend graph of heterojunction photocatalyst rhodamine B degradation, with reference to the degradation curve figure of pure pucherite.
Detailed description of the invention
Below by specific embodiment, the present invention is described in further detail, and following examples can make those skilled in the art more fully understand the present invention, but do not limit the present invention in any way.
The five water bismuth nitrate (Bi (NO adopted in following examples 3) 35H 2o), ammonium metavanadate (NH 4vO 3), citric acid (C 6h 8o 7h 2o), nitric acid (HNO 3), ammoniacal liquor (NH 4oH), KI (KI), ethylene glycol, rhodamine B (RhB), be analyze pure.
Embodiment 1
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL1mol/L dust technology, stirs 30min and makes it dissolve completely, add ammoniacal liquor adjust ph to 7, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL distilled water, stirs 30min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 40min under 80 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.001mol (0.4851g) Bi (NO 3) 35H 2o is dissolved in 15ml ethylene glycol, is designated as solution D;
5th step: get 0.001mol (0.166g) KI and be dissolved in 50mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 15 hours, join in the C solution that the 3rd step obtains, after Keep agitation 10h, navy blue gel will be formed, ageing 32h, is placed in 110 DEG C of baking ovens and dries, and then puts into Muffle furnace at 350 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.1:1).
As can be seen from X-ray diffraction (XRD) spectrogram of Fig. 1, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 1-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
As can be seen from SEM (SEM) image of Fig. 2, the bismuth oxyiodide prepared by the present embodiment 1-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
As can be seen from the Fourier transform infrared spectroscopy figure (FT-IR) of Fig. 3, the bismuth oxyiodide prepared by the present embodiment 1-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
By the BiOI/BiVO of Fig. 4 4the forming process figure of photochemical catalyst heterojunction structure can know the transition process seeing electronics, BiVO 4, BiOI is when being subject to illumination, produce electron-hole pair, because the difference that energy gap is different, can there is directional migration to BiVO in the photoelectron of BiOI under the effect of internal electric field simultaneously 4valence band on, and then effectively can suppress the compound again of electron-hole, improve quantum efficiency, strengthen the photocatalytic activity of photochemical catalyst.
The photocatalysis performance of the bismuth oxyiodide prepared by the present embodiment 1-pucherite heterojunction photocatalyst can be evaluated with degraded rhdamine B.Light source is 500w high-pressure sodium lamp, and the concentration of rhodamine B solution is 10mg/L, and the bismuth oxyiodide-pucherite heterojunction photocatalyst 250mg taken prepared by the present embodiment 1 adds in 300mL reaction bulb, then adds the rhodamine B solution 250mL of 10mg/L.First allow catalyst fully adsorb 1h under dark reaction condition, reach adsorption equilibrium; Then open light source, after preheating 5min, start timing, at interval of 10min sample analysis, duration 90min.Result shown in Fig. 5 shows, under experimental conditions, bismuth oxyiodide prepared by the present embodiment 1-pucherite heterojunction photocatalyst is degraded rapidly in front 10min, substantially 60% is reached, all higher than 90% after 30 minutes, after reaction 90min, reach 91.6%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can promote the separation of carrier, contribute to the carrying out of light-catalyzed reaction.
Embodiment 2
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL1mol/L dust technology, stirs 30min and makes it dissolve completely, add ammoniacal liquor adjust ph to 7.1, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL distilled water, stirs 30min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 40min under 80 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.005mol (2.4254g) Bi (NO 3) 35H 2o is dissolved in 20ml ethylene glycol, is designated as solution D;
5th step: get 0.005mol (0.83g) KI and be dissolved in 50mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 18 hours, join in the C solution that the 3rd step obtains, after Keep agitation 11h, navy blue gel will be formed, ageing 39h, is placed in 110 DEG C of baking ovens and dries, and then puts into Muffle furnace at 360 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.5:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 2-pucherite heterojunction photocatalyst.
As can be seen from X-ray diffraction (XRD) spectrogram of Fig. 1, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 2-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 2-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 2-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 2, as shown in Figure 5, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially 60% is reached, higher than 90% after 30 minutes, after reaction 90min, reach 94%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 3
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 40mL1mol/L dust technology, stirs 20min and makes it dissolve completely, add ammoniacal liquor adjust ph to 6.5, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 40mL distilled water, stirs 20min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 50min under 60 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.0005mol (0.2425g) Bi (NO 3) 35H 2o is dissolved in 10ml ethylene glycol, is designated as solution D;
5th step: get 0.0005mol (0.083g) KI and be dissolved in 40mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 12 hours, join in the C solution that the 3rd step obtains, after Keep agitation 6h, navy blue gel will be formed, ageing 24h, is placed in 100 DEG C of baking ovens and dries, and then puts into Muffle furnace at 300 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.05:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 3-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 3-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 3-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 3-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 3, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 90%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 4
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 60mL1mol/L dust technology, stirs 40min and makes it dissolve completely, add ammoniacal liquor adjust ph to 7.5, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 60mL distilled water, stirs 40min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 30min under 90 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o is dissolved in 25ml ethylene glycol, is designated as solution D;
5th step: get 0.01mol (1.66g) KI and be dissolved in 60mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 24 hours, join in the C solution that the 3rd step obtains, after Keep agitation 14h, navy blue gel will be formed, ageing 48h, is placed in 120 DEG C of baking ovens and dries, and then puts into Muffle furnace at 400 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=1:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 4-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 4-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 4-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 4-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 4, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 91%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 5
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 45mL1mol/L dust technology, stirs 25min and makes it dissolve completely, add ammoniacal liquor adjust ph to 6.8, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 45mL distilled water, stirs 25min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 45min under 70 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.001mol (0.4851g) Bi (NO 3) 35H 2o is dissolved in 15ml ethylene glycol, is designated as solution D;
5th step: get 0.001mol (0.166g) KI and be dissolved in 45mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 15 hours, join in the C solution that the 3rd step obtains, after Keep agitation 9h, navy blue gel will be formed, ageing 30h, is placed in 105 DEG C of baking ovens and dries, and then puts into Muffle furnace at 330 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.1:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 5-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 5-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 5-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 5-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 5, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 90%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 6
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 55mL1mol/L dust technology, stirs 35min and makes it dissolve completely, add ammoniacal liquor adjust ph to 7.3, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 55mL distilled water, stirs 35min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 40min under 80 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.005mol (2.4254g) Bi (NO 3) 35H 2o is dissolved in 20ml ethylene glycol, is designated as solution D;
5th step: get 0.005mol (0.83g) KI and be dissolved in 55mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 21 hours, join in the C solution that the 3rd step obtains, after Keep agitation 12h, navy blue gel will be formed, ageing 42h, is placed in 115 DEG C of baking ovens and dries, and then puts into Muffle furnace at 370 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.5:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 6-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 6-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 6-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 6-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 6, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 93%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 7
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 40mL1mol/L dust technology, stirs 20min and makes it dissolve completely, add ammoniacal liquor adjust ph to 6.6, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.01mol (2.1g) C 6h 8o 7h 2o is dissolved in 40mL distilled water, stirs 20min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 45min under 65 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.0008mol (0.3881g) Bi (NO 3) 35H 2o is dissolved in 10ml ethylene glycol, is designated as solution D;
5th step: get 0.0008mol (0.1328g) KI and be dissolved in 40mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 14 hours, join in the C solution that the 3rd step obtains, after Keep agitation 8h, navy blue gel will be formed, ageing 27h, is placed in 102 DEG C of baking ovens and dries, and then puts into Muffle furnace at 320 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.08:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 7-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 7-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 7-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 7-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 7, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 91%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 8
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL1mol/L dust technology, stirs 30min and makes it dissolve completely, add ammoniacal liquor adjust ph to 6.9, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.02mol (4.2g) C 6h 8o 7h 2o is dissolved in 50mL distilled water, stirs 30min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 40min under 75 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.003mol (1.4552g) Bi (NO 3) 35H 2o is dissolved in 15ml ethylene glycol, is designated as solution D;
5th step: get 0.003mol (0.498g) KI and be dissolved in 50mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 16 hours, join in the C solution that the 3rd step obtains, after Keep agitation 10h, navy blue gel will be formed, ageing 33h, is placed in 110 DEG C of baking ovens and dries, and then puts into Muffle furnace at 350 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.3:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 8-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 8-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 8-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 8-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 8, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 95%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Embodiment 9
The first step: get 0.01mol (4.8507g) Bi (NO 3) 35H 2o and 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 60mL1mol/L dust technology, stirs 40min and makes it dissolve completely, add ammoniacal liquor adjust ph to 7.4, be designated as solution A;
Second step: get 0.01mol (1.1698g) NH 4vO 3with 0.03mol (6.3g) C 6h 8o 7h 2o is dissolved in 60mL distilled water, stirs 40min and makes it dissolve completely, be designated as B solution;
3rd step: after B solution is stirred 35min under 85 DEG C of heating conditions, solution can become blackish green by orange-yellow, now slowly adds solution A again, is mixed to form C solution;
4th step: get 0.008mol (3.8806g) Bi (NO 3) 35H 2o is dissolved in 20ml ethylene glycol, is designated as solution D;
5th step: get 0.008mol (1.328g) KI and be dissolved in 60mL distilled water, be designated as E solution;
6th step: by solution D and E solution mix and blend after 22 hours, join in the C solution that the 3rd step obtains, after Keep agitation 12h, navy blue gel will be formed, ageing 45h, is placed in 118 DEG C of baking ovens and dries, and then puts into Muffle furnace at 380 DEG C, calcines the solid of 3h to agglomerating caking, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst (BiOI/BiVO 4mol ratio=0.8:1).
The means of catalysis such as XRD, SEM, FT-IR are adopted to carry out phenetic analysis to the bismuth oxyiodide prepared by the present embodiment 9-pucherite heterojunction photocatalyst.
X-ray diffraction (XRD) spectrogram can be found out, the characteristic peak that the bismuth oxyiodide prepared by the present embodiment 9-pucherite heterojunction photocatalyst has on the position of the angles of diffraction such as 18.6 °, 28.6 °, 19 °, 28.98 °, 30.5 °, 34.5 °, 35.2 °, 40 °, 47.6 °, 53.7 ° is the BiVO of monoclinic phase scheelite type 4absworption peak, illustrates after mixing BiOI, BiVO 4monoclinic phase main body phase structure do not change; Meanwhile, photochemical catalyst is the characteristic peak that position near 12.8 ° detects BiOI in the angle of diffraction, and result shows the existence having bismuth oxyiodide in the photochemical catalyst synthesized.
SEM (SEM) image can be found out, the bismuth oxyiodide prepared by the present embodiment 9-pucherite heterojunction photocatalyst, BiVO 4nano particle uniform fold is on the surface of BiOI nano particle, and both fully contact, combine, and forms composite construction, and it is better dispersed.
Fourier transform infrared spectroscopy figure (FT-IR) can find out, the bismuth oxyiodide prepared by the present embodiment 9-pucherite heterojunction photocatalyst has BiOI and BiVO simultaneously 4characteristic peak, illustrate preparation photochemical catalyst in BiVO 4, BiOI still keeps original chemical combination state, because both form heterojunction structure, the separation of electron-hole can be promoted further, more contribute to the carrying out of light-catalyzed reaction, BiOI and BiVO 4between there is cooperative effect.
With the degradation curve of pure pucherite for reference, utilize the bismuth oxyiodide-pucherite heterojunction photocatalyst photocatalytic degradation rhdamine B prepared by the present embodiment 9, under experimental conditions, photochemical catalyst is degraded rapidly in front 10min, substantially reaches 60%, after reaction 90min, reach 92%, be much better than the catalytic activity of monomer pucherite, this is because the formation of heterojunction structure can improve the migration rate of electronics, greatly promote the carrying out of light-catalyzed reaction.
Although be described the preferred embodiments of the present invention by reference to the accompanying drawings above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make the concrete conversion of a lot of form, these all belong within protection scope of the present invention.

Claims (9)

1. bismuth oxyiodide-pucherite heterojunction photocatalyst, it is characterized in that, be that the bismuth oxyiodide of 0.05:1-1:1 and pucherite are compounded to form heterojunction structure by mol ratio, pucherite nano particle is dispersed in bismuth oxyiodide nano grain surface, and wherein the thing of pucherite is monocline scheelite type mutually.
2. a kind of bismuth oxyiodide-pucherite heterojunction photocatalyst according to claim 1, is characterized in that, the mol ratio of described bismuth oxyiodide and described pucherite is 0.1:1-0.5:1.
3. a preparation method for bismuth oxyiodide-pucherite heterojunction photocatalyst, is characterized in that, adopts following steps to carry out:
(1) by Bi (NO 3) 35H 2o and C 6h 8o 7h 2o is dissolved in 1mol/L dust technology according to the mol ratio of 1:1-1:3, adds ammoniacal liquor adjust ph to 6.5-7.5, is designated as solution A;
(2) will with Bi (NO described in step (1) 3) 35H 2the NH of O equimolar amounts 4vO 3and with C described in step (1) 6h 8o 7h 2the C of O equimolar amounts 6h 8o 7h 2o is dissolved in distilled water, is designated as B solution;
(3), after B solution being stirred 30-50min under 60-90 DEG C of heating condition, solution becomes blackish green, more slowly adds solution A, is mixed to form C solution;
(4) mole is taken for 0.05-1 is doubly to Bi (NO described in step (1) 3) 35H 2bi (the NO of O 3) 35H 2o, and be dissolved in ethylene glycol, be designated as solution D;
(5) will with Bi (NO described in step (4) 3) 35H 2the KI of O equimolar amounts is dissolved in distilled water, is designated as E solution;
(6) by solution D and E solution mix and blend after 12-24 hour, join in the C solution that step (3) obtains, Keep agitation 6-14h is to forming navy blue gel, ageing 24-48h, be placed in 100-120 DEG C of baking oven to dry, then be fired in 300-400 DEG C and become solid, take out grinding after cooling, obtain bismuth oxyiodide-pucherite heterojunction photocatalyst.
4. the preparation method of a kind of bismuth oxyiodide-pucherite heterojunction photocatalyst according to claim 3, is characterized in that, Bi (NO in step (1) 3) 35H 2o and C 6h 8o 7h 2the mol ratio of O is 1:2.
5. the preparation method of a kind of bismuth oxyiodide-pucherite heterojunction photocatalyst according to claim 3, is characterized in that, the pH in step (1) is 7.
6. the preparation method of a kind of bismuth oxyiodide-pucherite heterojunction photocatalyst according to claim 3, is characterized in that, the heating-up temperature in step (3) is 80 DEG C.
7. the preparation method of a kind of bismuth oxyiodide-composite bismuth vanadium photocatalyst according to claim 3, is characterized in that, in step (6), the mix and blend time is 12-15h.
8. the preparation method of a kind of bismuth oxyiodide-composite bismuth vanadium photocatalyst according to claim 3, is characterized in that, in step (6), digestion time is 24-36h.
9. the preparation method of a kind of bismuth oxyiodide-composite bismuth vanadium photocatalyst according to claim 3, is characterized in that, the calcining heat in step (6) is 350 DEG C.
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CN114433107B (en) * 2022-01-11 2024-04-12 西安建筑科技大学 Co (cobalt) 3 O 4 /Bi 4 O 7 /Bi 2 O 3 Heterojunction photocatalyst and application thereof
CN114984990A (en) * 2022-05-16 2022-09-02 湖南大学 Tubular carbon nitride-based Schottky heterojunction photocatalyst and preparation method and application thereof

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