CN109261171A - A kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its preparation method and application - Google Patents
A kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its preparation method and application Download PDFInfo
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- SBCLYZJAWPMPDE-UHFFFAOYSA-N O(I)I.[Bi].[Cl] Chemical compound O(I)I.[Bi].[Cl] SBCLYZJAWPMPDE-UHFFFAOYSA-N 0.000 title claims abstract description 78
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims description 23
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000013078 crystal Substances 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 5
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 4
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 4
- 229960004756 ethanol Drugs 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 6
- OAAKZKGKPMPJIF-UHFFFAOYSA-N [Cl].[I] Chemical compound [Cl].[I] OAAKZKGKPMPJIF-UHFFFAOYSA-N 0.000 claims 1
- 239000011259 mixed solution Substances 0.000 claims 1
- 238000002791 soaking Methods 0.000 claims 1
- CBACFHTXHGHTMH-UHFFFAOYSA-N 2-piperidin-1-ylethyl 2-phenyl-2-piperidin-1-ylacetate;dihydrochloride Chemical compound Cl.Cl.C1CCCCN1C(C=1C=CC=CC=1)C(=O)OCCN1CCCCC1 CBACFHTXHGHTMH-UHFFFAOYSA-N 0.000 abstract description 19
- 230000001699 photocatalysis Effects 0.000 abstract description 13
- 238000007146 photocatalysis Methods 0.000 abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 4
- 239000000843 powder Substances 0.000 abstract description 4
- -1 compound chlorine bismuth oxyiodide Chemical class 0.000 abstract description 2
- 238000005215 recombination Methods 0.000 abstract description 2
- 230000006798 recombination Effects 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 2
- 239000002243 precursor Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 11
- 238000006731 degradation reaction Methods 0.000 description 11
- 239000000460 chlorine Substances 0.000 description 7
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 6
- 229910052801 chlorine Inorganic materials 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 230000008859 change Effects 0.000 description 3
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical group [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 239000002355 dual-layer Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B01J35/33—
-
- B01J35/39—
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/40—Organic compounds containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its preparation method and application.The present invention solve the problems, such as existing bismuth oxyiodide (001) legibility from, absorbing properties are weak, photocatalysis efficiency is low.The dispersion liquid of graphene is prepared first, then the dispersion liquid of graphene is mixed with the precursor solution of chlorine bismuth oxyiodide (010), and chlorine bismuth oxyiodide and compound chlorine bismuth oxyiodide (the 010)/graphene powder of graphene are generated by hydro-thermal method.Promote efficiently separating for chlorine bismuth oxyiodide (010) light induced electron and hole using graphene conductive ability, the recombination probability of light induced electron and hole is reduced, to improve the photo-catalysis capability of bismuth oxyiodide (010).
Description
Technical field
The invention belongs to photocatalysis water process skill field, be related to a kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its
Preparation method and application.
Background technique
Photocatalysis pollutant process, which refers to, occurs photocatalysis degradation organic contaminant under the action of light by catalyst, and
Mineralising processing can be realized to organic pollutant poisonous and harmful in environment, be that a kind of solution human society environmental problem is most latent
One of technology of power.The semiconductor light-catalyst technology of emerging development can generate clean energy resource hydrogen and oxygen using sunlight, can also
Removal organic polluter is removed in degradation.But the research of catalysis material at present still suffers from the problem of limiting its practical application, light is rung
Narrow range is answered, the conventional semiconductors catalysis material with high activity, such as titanium dioxide, energy band is wider (3.2eV), can only
The ultraviolet light for accounting for solar spectrum gross energy 4% or so is absorbed, causes solar energy utilization ratio lower.In view of the above-mentioned problems, development is new
Type efficient visible light catalysis material is a trend.Bismuth oxyiodide (BiOI) is a kind of with the photoactive photocatalysis of visible light
Agent, for BiOI because forbidden bandwidth is relatively narrow (1.63-1.94 eV), crystal structure is PbFCl type, D4hAxial symmetry, P4/nmm space group,
Belong to tetragonal crystal system.Because the forbidden bandwidth of BiOI is smaller, bismuth oxyiodide is asked there are photo-generate electron-hole is low to separative efficiency etc.
Topic, so as to cause the reduction of its photocatalytic activity.Therefore many scholars are by being modified the photocatalytic activity to enhance it to it.
Liu etc. (AppliedCatalysis B:Environmental, 2015,163:547-553) first uses solvent heat legal system
Standby BiOI is reacted 24 hours at 180 DEG C using hydrothermal process then using sodium dihydrogen phosphate as primary raw material and obtains BiPO4/
BiOI hetero-junctions.The purer BiOI of heterojunction photocatalysis activity of preparation is greatly improved.The disadvantage is that preparation process is complicated, reaction
Time is long, increases preparation cost.The crystal structure of BiOI is also considered as along c-axis direction, double I–Sheath and [Bi2O2]2+Layer
It is alternately arranged, forms layer structure, but dual layer arrangement I–The non-bonding force of belonging to combine, binding force is weaker, is easy dissociation, therefore
The bismuth oxyiodide (010) that (010) face of exploration preferentially exposes is a kind of important means for improving its stability.Chlorine bismuth oxyiodide
(BiOI1-xClx) it is chlorine ion doped bismuth oxyiodide, graphene is a kind of two-dimentional carbon material of layer structure, due to its energy band
Gap is almost 0, and charge carrier transport efficiency is high, and adsorption capacity is strong, becomes good carrier of photocatalyst material, and can
Effectively facilitate the separative efficiency of photo-generated carrier.
In view of the above-mentioned problems, development is based on the catalysis material of chlorine bismuth oxyiodide (010)/graphene, semiconductor light is urged
Change technology is of great significance in environmental improvement and in terms of solving energy crisis.
Summary of the invention
The purpose of the present invention is to provide a kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and preparation method thereof and answer
With compound using hydro-thermal method progress two-phase, the more other chemical synthesis of process flow are simple, have high photocatalysis performance.
In order to achieve the above object, the present invention adopts the following technical scheme:
A kind of preparation method and application of chlorine bismuth oxyiodide (010)/graphene hetero-junctions, comprising the following steps:
Step 1, graphene is taken to be added in ethyl alcohol and the mixed liquor of deionized water, ultrasonic disperse simultaneously stirs evenly, at 30~50 DEG C
15~30min of lower ultrasonic disperse, is made into A liquid；
Step 2, by Bi (NO3)3·5H2O is added to dilute HNO3In, it is stirred at 70~90 DEG C to being completely dissolved, is made into B liquid；
Step 3, it takes KI and KCl to be dissolved in deionized water, obtains C liquid, wherein Bi (NO3)3·5H2The molar ratio of O and (KI+KCl)
For 1:1；
Step 4, A drop will be prepared to be added in B liquid, forms D liquid；
Step 5, the NaOH solution of 2~4 mol/L is added drop-wise in D liquid, the pH value for adjusting D liquid is 6；
Step 6, C liquid is added in D liquid, forms E liquid；
Step 7, E liquid is poured into reaction kettle, reaction kettle is heated to 160~180 DEG C, keeps the temperature 12~24 h；
Step 8, after reaction kettle is cooling, the dehydrated alcohol of the precipitating in reaction kettle and deionized water is washed, is dry, uses Ma
Nao mortar obtains the heterogeneous crystal plane of chlorine bismuth oxyiodide (010)/graphene/graphene hetero-junctions after being ground.
Compared with prior art, the invention has the following advantages:
Chlorine bismuth oxyiodide (010)/graphene hetero-junctions provided by the invention and its preparation method and application, is synthesized by hydro-thermal method
Chlorine bismuth oxyiodide (010) powder is compound with graphene, it is prepared for chlorine bismuth oxyiodide (010)/graphene hetero-junctions.This method tool
Have the advantages that reaction condition is mild, low in cost, simple process.Since (010) crystal face of chlorine bismuth oxyiodide is formed with graphene
It is good compound, it can use the good carrier transport performance of graphene and promote light induced electron can from chlorine bismuth oxyiodide
(010) conduction band of crystal face is transferred in reaction solution, and photohole can directly be reacted with organic pollutant.The formation of hetero-junctions
The separation rate for improving photo-generate electron-hole pair can be improved the photocatalysis performance of chlorine bismuth oxyiodide (010).
In chlorine bismuth oxyiodide (010)/graphene hetero-junctions prepared by the present invention, Cl-Introducing with graphene does not change
The object phase for becoming bismuth oxyiodide still maintains as tetragonal phase, and (010) the crystal face exposure of chlorine bismuth oxyiodide is good, and the knot of crystal
It is brilliant in good condition.Chlorine bismuth oxyiodide (010) crystal face and graphene two-phase coexistent, the high specific surface area of graphene can increase after compound
To the adsorption capacity of organic pollutant, the good electric conductivity of graphene can also improve the migration of light induced electron, improve photoproduction electricity
Son-hole pair separation rate.
And the hetero-junctions that chlorine bismuth oxyiodide (010) crystal face and graphene are formed is after visible light is according to 150min to methylene
Blue percent of decolourization is up to 96%, and pure bismuth oxyiodide (010) powder is 20% according to the degradation rate after 150min in visible light, compound
The photocatalysis efficiency of chlorine bismuth oxyiodide (010)/graphene hetero-junctions degradation rate purer bismuth oxyiodide (010) powder obviously mentions afterwards
It rises.
Detailed description of the invention
Fig. 1 is chlorine bismuth oxyiodide (010)/graphene hetero-junctions XRD diffracting spectrum prepared by the embodiment of the present invention 1；
Fig. 2 is chlorine bismuth oxyiodide (010)/graphene hetero-junctions TEM figure prepared by the embodiment of the present invention 1；
Fig. 3 is the photocatalytic degradation map of sample prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3；
Fig. 4 is that chlorine bismuth oxyiodide (010)/graphene hetero-junctions prepared by the embodiment of the present invention 1, embodiment 2 and embodiment 3 is glimmering
Light spectrogram.
Specific embodiment
The present invention is described further with currently preferred specific embodiment with reference to the accompanying drawing, raw material is analysis
It is pure.
Embodiment 1:
Step 1,0.07g commercial graphite alkene is taken to be added in deionized water, the ultrasonic disperse 20min at 30 DEG C is made into A liquid；
Step 2, by the Bi (NO of 5mmol3)3·5H2O is added to the HNO of 2.0 mol/L3In, it is stirred at 80 DEG C to completely molten
Solution, is made into B liquid；
Step 3, it takes 4.94mmolKI and 0.06mmol KCl to be dissolved in deionized water, is made into C liquid；
Step 4, A drop will be prepared and is added to B liquid, be made into D liquid, wherein Bi (NO3)3·5H2The molar ratio of O and (KI+KCl) is
1:1；
Step 5,2.0 mol/L NaOH solutions are slowly dropped in D liquid, the pH value for adjusting D liquid is 6；
Step 6, C liquid is added in D liquid, forms E liquid；
Step 7, E liquid is poured into reaction kettle, reaction kettle is heated to 170 DEG C, heat preservation is for 24 hours；
Step 8, after reaction kettle is cooling, the precipitating in reaction kettle is successively washed, at 80 DEG C with dehydrated alcohol and deionized water
It is dry to obtain chlorine bismuth oxyiodide (010)/graphene hetero-junctions afterwards for 24 hours.
Embodiment 2:
Step 1, by the Bi (NO of 5mmol3)3·5H2O is added to the HNO of 2.0 mol/L3In, it is stirred at 80 DEG C to completely molten
Solution, is made into A liquid；
Step 2, it takes 4.94mmolKI and 0.06mmol KCl to be dissolved in deionized water, is made into B liquid；
Step 4, A drop will be prepared and is added to B liquid, be made into C liquid, wherein Bi (NO3)3·5H2The molar ratio of O and (KI+KCl) is
1:1；
Step 5,2.0 mol/L NaOH solutions are slowly dropped in C liquid, the pH value for adjusting C liquid is 6；
Step 6, B liquid is added in C liquid, forms D liquid；
Step 7, D liquid is poured into reaction kettle, reaction kettle is heated to 170 DEG C, heat preservation is for 24 hours；
Step 8, after reaction kettle is cooling, the precipitating in reaction kettle is successively washed, at 80 DEG C with dehydrated alcohol and deionized water
It is dry to obtain chlorine bismuth oxyiodide (010) afterwards for 24 hours.
Embodiment 3:
Step 1, by the Bi (NO of 5mmol3)3·5H2O is added to the HNO of 2.0 mol/L3In, it is stirred at 80 DEG C to completely molten
Solution, is made into A liquid；
Step 2,5mmolKI is dissolved in deionized water, is made into B liquid；
Step 4, A drop will be prepared and is added to B liquid, be made into C liquid, wherein Bi (NO3)3·5H2The molar ratio of O and KI is 1:1；
Step 5,2.0 mol/L NaOH solutions are slowly dropped in C liquid, the pH value for adjusting C liquid is 6；
Step 6, B liquid is added in C liquid, forms D liquid；
Step 7, D liquid is poured into reaction kettle, reaction kettle is heated to 170 DEG C, heat preservation is for 24 hours；
Step 8, after reaction kettle is cooling, the precipitating in reaction kettle is successively washed, at 80 DEG C with dehydrated alcohol and deionized water
It is dry to obtain bismuth oxyiodide (010) afterwards for 24 hours.
Application examples 1:
The Asia for being 15 mg/L using photochemical catalyst photocatalytic degradation concentration prepared by the present embodiment 1, embodiment 2 and embodiment 3
Methyl blue solution, the photochemical catalyst for taking 0.1 g to prepare are mixed with the methylene blue solution of 100 mL, and dark 60 min of stirring reach
To after adsorption equilibrium, it is then turned on the irradiation of 300 W simulated solar irradiations.A certain amount of aforesaid liquid was extracted every 30 minutes, was centrifuged
Its photocatalysis efficiency is characterized using the absorbance under spectrophotometer measurement 662nm afterwards.
Fig. 1 is chlorine bismuth oxyiodide (the 010)/graphene hetero-junctions XRD diagram prepared in the embodiment of the present invention 1, from figure
It is found that the appearance of strong (102) diffraction maximum, shows that chlorine bismuth oxyiodide is in chlorine bismuth oxyiodide (010)/graphene hetero-junctions
(010) face preferentially exposes.The introducing of chlorine causes the angular high angle direction of the diffraction of bismuth oxyiodide (102) to have displacement to generate, and does not have
There is generation impurity phase, shows that chlorine is successfully adulterated into the lattice of bismuth oxyiodide (010), the introducing of chlorine and graphene does not change
The object phase for becoming bismuth oxyiodide, is still tetragonal phase.
Fig. 2 is chlorine bismuth oxyiodide (the 010)/graphene hetero-junctions TEM figure prepared in the embodiment of the present invention 1, from figure
It is found that the thin slice crimped is graphene, shape more rule, color is deeper for chlorine bismuth oxyiodide (010), to know
It is successfully prepared out chlorine bismuth oxyiodide (010)/graphene hetero-junctions.
Fig. 3 is chlorine bismuth oxyiodide (the 010)/graphene hetero-junctions degradation of methylene blue prepared in the embodiment of the present invention 1
Degradation map, it can be seen that chlorine bismuth oxyiodide (010)/graphene hetero-junctions degradation rate after visible light is according to 150min is reachable
96% or more, the degradation rate of chlorine bismuth oxyiodide (010) is 42%, and the degradation rate of bismuth oxyiodide (010) is only 20%.Chlorine iodine oxidation
Bismuth (010)/graphene hetero-junctions degradation rate improves 4.8 times than the degradation rate of bismuth oxyiodide (010).
Fig. 4 is chlorine bismuth oxyiodide (the 010)/graphene hetero-junctions fluorescence spectra prepared in the embodiment of the present invention 1, from
It is found that chlorine bismuth oxyiodide (010)/graphene hetero-junctions Carrier recombination probability is significantly lower than chlorine bismuth oxyiodide (010) in figure
With bismuth oxyiodide (010).
Above said content is only the basic explanation under present inventive concept, by reading description of the invention to the present invention
Any equivalent transformation that technical solution is taken, should all belong to protection scope of the present invention.
Claims (7)
1. a kind of chlorine bismuth oxyiodide (010)/graphene hetero-junctions and its preparation method and application, which is characterized in that chlorine iodine oxidation
The preparation of bismuth (010)/graphene hetero-junctions the following steps are included:
Step 1, graphene is taken to be added in ethyl alcohol and the mixed liquor of deionized water, ultrasonic disperse simultaneously stirs evenly, at 30~50 DEG C
15~30min of lower ultrasonic disperse, is made into A liquid；
Step 2, by Bi (NO3)3·5H2O is added to dilute HNO3In, it is stirred at 70~90 DEG C to being completely dissolved, is made into B liquid；
Step 3, it takes KI and KCl to be dissolved in deionized water, obtains C liquid, wherein Bi (NO3)3·5H2The molar ratio of O and (KI+KCl)
For 1:1；
Step 4, A drop will be prepared to be added in B liquid, forms D liquid；
Step 5, the NaOH solution of 2~4 mol/L is added drop-wise in D liquid, the pH value for adjusting D liquid is 6；
Step 6, C liquid is added in D liquid, forms E liquid；
Step 7, E liquid is poured into reaction kettle, reaction kettle is heated to 160~180 DEG C, keeps the temperature 12~24 h；
Step 8, after reaction kettle is cooling, the dehydrated alcohol of the precipitating in reaction kettle and deionized water is washed, is dry, uses Ma
Nao mortar obtains the heterogeneous crystal plane of chlorine bismuth oxyiodide (010)/graphene/graphene hetero-junctions after being ground.
2. chlorine bismuth oxyiodide (010)/graphene hetero-junctions according to claim 1 and its preparation method and application, special
Sign is that in step 1, the volume ratio of ethyl alcohol and deionized water is 1:1, and the concentration of graphene is 0.2~0.8g/ in solution A
L。
3. chlorine bismuth oxyiodide (010)/graphene hetero-junctions according to claim 1 and its preparation method and application, special
Sign is, in step 2, HNO3Concentration be 2~4mol/L, Bi (NO3)3Concentration be 0.15~0.35mol/.
4. chlorine bismuth oxyiodide (010)/graphene hetero-junctions according to claim 1 and its preparation method and application, special
Sign is that in step 3, the concentration of KI is 0.15~0.35mol/L in KI solution, and the concentration of KCl solution is 0 .15~0
.35mol/L, wherein the molar ratio of KI and KCl is (1~0.90): (0 ~ 0.10).
5. chlorine bismuth oxyiodide (010)/graphene hetero-junctions according to claim 1 and its preparation method and application, special
Sign is that in step 4, the concentration of NaOH solution is 2~4 mol/L, and the mixed solution pH value after dripping NaOH solution is
6。
6. chlorine bismuth oxyiodide (010)/graphene hetero-junctions according to claim 1 and its preparation method and application, special
Sign is that the temperature of reaction kettle in the step 5 is 160~180 DEG C, and soaking time is 12~24 h.
7. chlorine bismuth oxyiodide (010)/graphene hetero-junctions is in terms of photocatalytic degradation methylene blue described in claim 1-6
Using.
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