CN110327948A - A kind of tri compound nano heterojunction photocatalysis agent and preparation method, application - Google Patents
A kind of tri compound nano heterojunction photocatalysis agent and preparation method, application Download PDFInfo
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- CN110327948A CN110327948A CN201910758011.9A CN201910758011A CN110327948A CN 110327948 A CN110327948 A CN 110327948A CN 201910758011 A CN201910758011 A CN 201910758011A CN 110327948 A CN110327948 A CN 110327948A
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- 150000001875 compounds Chemical class 0.000 title claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 25
- 238000007146 photocatalysis Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910015667 MoO4 Inorganic materials 0.000 claims abstract description 35
- 229910002900 Bi2MoO6 Inorganic materials 0.000 claims abstract description 25
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 23
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- 230000003197 catalytic effect Effects 0.000 claims abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 81
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 60
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 51
- 239000006185 dispersion Substances 0.000 claims description 40
- 239000000243 solution Substances 0.000 claims description 33
- 239000007788 liquid Substances 0.000 claims description 29
- 238000003756 stirring Methods 0.000 claims description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 18
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 18
- 235000009518 sodium iodide Nutrition 0.000 claims description 17
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims description 10
- 239000012456 homogeneous solution Substances 0.000 claims description 9
- 229910019626 (NH4)6Mo7O24 Inorganic materials 0.000 claims description 8
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 6
- 239000011941 photocatalyst Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 150000004677 hydrates Chemical class 0.000 claims description 4
- 239000002105 nanoparticle Substances 0.000 claims description 4
- 101710134784 Agnoprotein Proteins 0.000 claims description 3
- 230000003111 delayed effect Effects 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000002243 precursor Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005457 optimization Methods 0.000 claims 4
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims 1
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 21
- 229910021641 deionized water Inorganic materials 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 229910002651 NO3 Inorganic materials 0.000 description 7
- -1 after stirring 20min Substances 0.000 description 7
- 238000003760 magnetic stirring Methods 0.000 description 7
- 238000001556 precipitation Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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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
- B01J27/132—Halogens; Compounds thereof with chromium, molybdenum, tungsten or polonium
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- 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
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- 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
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- 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
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Abstract
The present invention relates to catalysis material technical fields, and in particular to one kind is by AgI/Bi2MoO6/AgBi(MoO4)2Tri compound nano heterojunction photocatalysis agent of composition and preparation method thereof, application.The photochemical catalyst is to pass through AgI/Bi2MoO6/AgBi(MoO4)2Three-phase composite forms.Preparation process of the present invention is simple and environmentally-friendly, is easy to produce in batches；It can be by adjusting AgI, Bi2MoO6With AgBi (MoO4)2The ratio of ingredient is optimal its catalytic performance；AgI/Bi prepared by the present invention2MoO6/AgBi(MoO4)2The agent of tri compound nano heterojunction photocatalysis has preferable degradation effect to quadracycline, in terms of visible light photocatalytic degradation of organic pollutants with good application prospect.
Description
Technical field
The present invention relates to catalysis material technical fields, and in particular to one kind is by AgI/Bi2MoO6/AgBi(MoO4)2Composition
Tri compound nano heterojunction photocatalysis agent and preparation method thereof, application.
Background technique
In recent years, with the acceleration of industrialization and urbanization, demand of the people to resource promptly increases, this gives nature ring
Border brings the increasing pressure.Wherein environmental problem relevant with water pollution to atmosphere pollution is the most prominent.Due to water body
Pollution causes water environment degradation, and then threatens the existence of the mankind and the ecological balance of the earth.Therefore, administer and control water body dirt
The problem of dying for environmental improvement urgent need to resolve.
Photocatalysis technology has in terms of the environmental contaminants processing such as catalytic degradation organic pollutant, reducing heavy metal ion
Unique advantage and broad prospect of application have great research significance in terms of environmental improvement.Currently, conductor photocatalysis skill
For art due to having low cost, high efficiency and the advantages such as environmental-friendly, oneself has been obtained extensive concern.Numerous semiconductor lights are urged
In agent, wide band gap semiconducter TiO2, ZnO etc. as typical photochemical catalyst receive extensive research.TiO2, the photochemical catalysts such as ZnO
Wider band gap width causes its photoresponse wavelength region to be concentrated mainly on UV light region, and the ultraviolet light ingredient in sunlight
Less than 5%, thus such photochemical catalyst cannot efficiently use sunlight.In addition, TiO2, higher light inside the photochemical catalysts such as ZnO
Raw Carrier recombination rate, is also unfavorable for its photocatalysis performance.In order to more effectively utilize solar energy, explore it is new, have it is visible
The semiconductor light-catalyst material of photoresponse is simultaneously modified the important research direction studied as current photochemical catalyst to it.?
In numerous Photocatalyst means, it is common in recent years and highly effective that different semiconductor materials, which are compounded to form hetero-junctions,
Means.
Summary of the invention
The present invention provides one kind by AgI/Bi2MoO6/AgBi(MoO4)2The tri compound nano heterojunction light of composition is urged
Agent.
The present invention also provides a kind of preparation methods of tri compound nano heterojunction photocatalysis agent.
The present invention also provides a kind of applications of tri compound nano heterojunction photocatalysis agent.
Used technical solution to achieve the goals above are as follows:
The present invention provides a kind of tri compound nano heterojunction photocatalysis agent, which is to pass through AgI/Bi2MoO6/
AgBi(MoO4)2It is combined.
The present invention also provides a kind of preparation methods of tri compound nano heterojunction photocatalysis agent, comprising the following steps:
(1) five nitric hydrate bismuths and sodium iodide difference are soluble in water, it stirs evenly, obtains homogeneous solution；By IodineSodium Solution
It is added drop-wise in five nitric hydrate bismuth solution, stirs, react it sufficiently；After after reaction, being separated, washed, being dried
The product arrived is to get BiOI nanometer sheet；
(2) the resulting BiOI nanometer sheet of step (1) is dispersed in water, forms BiOI aqueous dispersions, ammonium molybdate aqueous solution is delayed
It is slow to be added in BiOI aqueous dispersions, it stirs evenly, obtains mixed dispersion liquid；
(3) silver nitrate aqueous solution is slowly added in step (2) resulting mixed dispersion liquid, is stirred at room temperature anti-
It answers, is then separated, washed, dried, obtained powder is composite precursor；It is finally heat-treated, is obtained in Muffle furnace
To AgI/Bi2MoO6/AgBi(MoO4)2Tri compound nano heterojunction photocatalysis agent.
Further, in step (1), the molal volume ratio of the five nitric hydrates bismuth and water is (1 ~ 3) mmol:20mL；
The molal volume of the sodium iodide and water ratio is (1 ~ 3) mmol:20mL；The molar ratio of the five nitric hydrates bismuth and sodium iodide is
1:1；The abundant reaction, which refers to, to be stirred at room temperature, reaction time 3.5h；The washing refers to distilled water and dehydrated alcohol
Alternately wash；The drying refers to 60 DEG C of dry 12h；Most preferably, the molal volume ratio with water of the five nitric hydrates bismuth
Preferably 2mmol:20mL；The molal volume of sodium iodide and water ratio is 2mmol:20mL；Five nitric hydrate bismuths and sodium iodide rub
Your ratio is 1:1.
Further, in step (2), in the BiOI dispersion liquid, the molal volume ratio of BiOI and water is 0.5mmol:
20mL；(NH in the ammonium molybdate aqueous solution4)6Mo7O24·4H2The molal volume of O and water ratio is (0.086 ~ 0.114) mmol:
10mL；Most preferably, the molal volume of the BiOI and water ratio is 0.5mmol:20mL；(the NH4)6Mo7O24·4H2O and water
Molal volume ratio be 0.114mmol:10mL.
Further, in step (3), AgNO in the silver nitrate aqueous solution3Molal volume ratio with water is (1.2 ~ 1.6)
Mmol:10mL；The time being stirred to react is 1~10min；Most preferably, the AgNO3Molal volume ratio with water is
1.6mmol:10mL；It is described to be stirred to react the time as 2min.
AgNO in above-mentioned steps (3), in the silver nitrate aqueous solution3With (the NH in mixed dispersion liquid4)6Mo7O24·
4H2The molar ratio of O is 14:1, and wherein the molar ratio of Mo and Bi is (1.2 ~ 1.6): 1.
Further, in step (3), the heat treatment condition is that 1 ~ 5h is kept the temperature at 350 ~ 450 DEG C；The washing refers to
It is alternately washed with distilled water and dehydrated alcohol；The drying refers in 60 DEG C of dry 12h；Most preferably, the heat treatment item
Part is to keep the temperature 2h at 400 DEG C.
AgI/Bi prepared by the present invention2MoO6/AgBi(MoO4)2Tri compound nano heterojunction photocatalysis agent is two-dimensional slice
Shape structure, piece size is 1 ~ 5 μm, with a thickness of 0.1 ~ 0.2 μm；The AgI nano particle is evenly dispersed in two-dimensional slice surface,
AgI nanoparticle size is 2 ~ 25 nm.
The present invention also provides a kind of AgI/Bi2MoO6/AgBi(MoO4)2Tri compound nano heterojunction photocatalysis agent exists
Application in catalytic degradation organic pollutant.
Preparation method of the invention and resulting product have the following advantages that and the utility model has the advantages that
(1) preparation process of the present invention is simple and environmentally-friendly, is easy to produce in batches；
(2) AgI/Bi prepared by the present invention2MoO6/AgBi(MoO4)2Photochemical catalyst, can be by adjusting AgI, Bi2MoO6With
AgBi(MoO4)2The ratio of ingredient is optimal its catalytic performance；
(3) AgI/Bi prepared by the present invention2MoO6/AgBi(MoO4)2The agent of tri compound nano heterojunction photocatalysis is to hydrochloric acid Fourth Ring
Element has preferable degradation effect, in terms of visible light photocatalytic degradation of organic pollutants with good application prospect.
Detailed description of the invention
Fig. 1 is embodiment 1,4 gained AgI/Bi2MoO6/AgBi(MoO4)2The agent of tri compound nano heterojunction photocatalysis and
The XRD diagram of comparative example 1~3；
Fig. 2 is 4 gained AgI/Bi of embodiment2MoO6/AgBi(MoO4)2The scanning electricity of tri compound nano heterojunction photocatalysis agent
Mirror figure；
Fig. 3 is 4 gained AgI/Bi of embodiment2MoO6/AgBi(MoO4)2The transmission electricity of tri compound nano heterojunction photocatalysis agent
Mirror figure；
Fig. 4 is embodiment 1,4 gained AgI/Bi2MoO6/AgBi(MoO4)2Ternary nano heterojunction photocatalyst and comparative example 1
~3, AgI, Bi2MoO6、AgBi(MoO4)2Under visible light to the degradation curve figure of quadracycline；AgI/Bi2MoO6/AgBi
(MoO4)2- 1~AgI/Bi2MoO6/AgBi(MoO4)2- 4 respectively correspond Examples 1 to 4.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 2mmol Bi (NO3)3·5H2O and 2mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.086mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 1.2mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution slowly adds
Enter into the mixed dispersion liquid of step (2), after 2min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 2h is heat-treated at 400 DEG C, i.e. acquisition tri compound nano heterojunction light
Catalyst AgI/Bi2MoO6/AgBi(MoO4)2-1。
Embodiment 2
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 1mmol Bi (NO3)3·5H2O and 1mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.095mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 1.33mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution is slow
It is added in the mixed dispersion liquid of step (2), after 1min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 5h is heat-treated at 350 DEG C, i.e. acquisition tri compound nano heterojunction light
Catalyst AgI/Bi2MoO6/AgBi(MoO4)2-2。
Embodiment 3
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 3mmol Bi (NO3)3·5H2O and 3mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.105mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 1.47mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution is slow
It is added in the mixed dispersion liquid of step (2), after 10min is stirred at room temperature, is alternately washed with dehydrated alcohol and deionized water
For several times, it is placed in 60 DEG C of vacuum ovens dry 12h, and is heat-treated 1h at 450 DEG C, is i.e. acquisition tri compound nano heterojunction
Photochemical catalyst AgI/Bi2MoO6/AgBi(MoO4)2-3。
Embodiment 4
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 2mmol Bi (NO3)3·5H2O and 2mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.114mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 1.6mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution slowly adds
Enter into the mixed dispersion liquid of step (2), after 2min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 2h is heat-treated at 400 DEG C, i.e. acquisition tri compound nano heterojunction light
Catalyst AgI/Bi2MoO6/AgBi(MoO4)2-4。
Comparative example 1
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 2mmol Bi (NO3)3·5H2O and 2mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.029mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 0.4mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution slowly adds
Enter into the mixed dispersion liquid of step (2), after 2min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 2h is heat-treated at 400 DEG C, i.e. acquisition sample (comparative example 1), through XRD
Test analysis shows that sample composition is Bi2O3/Bi2MoO6/AgBi(MoO4)2。
Comparative example 2
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 2mmol Bi (NO3)3·5H2O and 2mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.057mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 0.8mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution slowly adds
Enter into the mixed dispersion liquid of step (2), after 2min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 2h is heat-treated at 400 DEG C, i.e. acquisition sample (comparative example 2), through XRD
Test analysis shows that sample composition is Bi2O3/AgI/Bi2MoO6/AgBi(MoO4)2。
Comparative example 3
(1) the room temperature precipitation method prepare BiOI nanometer sheet: by 2mmol Bi (NO3)3·5H2O and 2mmol NaI is dissolved in 20mL respectively
In water, after stirring 20min, homogeneous solution is obtained；IodineSodium Solution is added drop-wise in five nitric hydrate bismuth solution, 3.5h is stirred,
React it sufficiently；After reaction, after being washed three times with dehydrated alcohol and deionized water respectively, 60 DEG C of vacuum ovens are placed in
Middle dry 12h is to get BiOI nanometer sheet.
(2) it takes 0.5mmol BiOI obtained by step (1) to be dispersed in the deionized water of 20mL, obtains the water dispersion of BiOI
Liquid；By 0.143mmol (NH4)6Mo7O24·4H2It after O is dissolved in 10mL water, adds it in the aqueous dispersions of BiOI, stirs
It mixes, obtains mixed dispersion liquid；
(3) by 2.0mmol AgNO3It is dissolved in 10mL water, obtains AgNO3Solution；Under magnetic stirring by AgNO3Solution slowly adds
Enter into the mixed dispersion liquid of step (2), after 2min is stirred at room temperature, alternately washs number with dehydrated alcohol and deionized water
It is secondary, dry 12h is placed in 60 DEG C of vacuum ovens, and 2h is heat-treated at 400 DEG C, i.e. acquisition sample (comparative example 3), through XRD
Test analysis shows that sample composition is AgI/AgBi (MoO4)2。
The AgI/Bi that embodiment 1 ~ 4 obtains2MoO6/AgBi(MoO4)2Ternary nano heterojunction photocatalyst is used for visible light
Catalytic degradation quadracycline, specific test method and condition: using 300W xenon lamp as light source (being equipped with optical filter λ >=400nm),
It is 5 × 10 by 35mL concentration−5M quadracycline aqueous solution is added in quartz glass reactor, and 30mg photocatalysis is added
Agent, dark treatment 30min reach adsorption equilibrium；It turns on light illumination, takes 2mL quadracycline aqueous solution every 15min, measure it
Residual concentration obtains its photocatalytic degradation efficiency curve, as shown in Figure 4.Fig. 4 is embodiment 1,4 gained AgI/Bi2MoO6/
AgBi(MoO4)2Heterojunction photocatalyst is under visible light to the degradation curve figure of quadracycline.As shown in Figure 4, work as Mo/Bi
Molar ratio be 1.6:1 when, catalyst is best to the degradation effect of quadracycline.Compared to pure AgI, Bi2MoO6、AgBi
(MoO4)2And comparative example 1~3, AgI/Bi prepared by the present invention2MoO6/AgBi(MoO4)2Tri compound nano heterojunction light is urged
The catalytic activity of agent significantly increases, before showing that it has good application in terms of the Photocatalytic Activity for Degradation organic pollutant
Scape.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (9)
1. a kind of tri compound nano heterojunction photocatalysis agent, which is characterized in that the photochemical catalyst is to pass through AgI/Bi2MoO6/
AgBi(MoO4)2It is combined.
2. a kind of preparation method of tri compound nano heterojunction photocatalysis agent as described in claim 1, which is characterized in that packet
Include following steps:
(1) five nitric hydrate bismuths and sodium iodide difference are soluble in water, it stirs evenly, obtains homogeneous solution；By IodineSodium Solution
It is added drop-wise in five nitric hydrate bismuth solution, stirs, react it sufficiently；After after reaction, being separated, washed, being dried
The product arrived is to get BiOI nanometer sheet；
(2) the resulting BiOI nanometer sheet of step (1) is dispersed in water, forms BiOI aqueous dispersions, ammonium molybdate aqueous solution is delayed
It is slow to be added in BiOI aqueous dispersions, it stirs evenly, obtains mixed dispersion liquid；
(3) silver nitrate aqueous solution is slowly added in step (2) resulting mixed dispersion liquid, is stirred at room temperature anti-
It answers, is then separated, washed, dried, obtained powder is composite precursor；It is finally heat-treated, is obtained in Muffle furnace
To AgI/Bi2MoO6/AgBi(MoO4)2Tri compound nano heterojunction photocatalysis agent.
3. preparation method according to claim 2, which is characterized in that in step (1), the five nitric hydrates bismuth and water
Molal volume ratio is (1 ~ 3) mmol:20mL；The molal volume of the sodium iodide and water ratio is (1 ~ 3) mmol:20mL；Described five
The molar ratio of nitric hydrate bismuth and sodium iodide is 1:1；The abundant reaction, which refers to, to be stirred at room temperature, reaction time 3.5h；Institute
Washing is stated to refer to the alternately washing of distilled water and dehydrated alcohol；The drying refers to 60 DEG C of dry 12h；Optimization, five water
The molal volume ratio preferably 2mmol:20mL with water of conjunction bismuth nitrate；The molal volume of sodium iodide and water ratio is 2mmol:
20mL；The molar ratio of five nitric hydrate bismuths and sodium iodide is 1:1.
4. preparation method according to claim 2, which is characterized in that in step (2), in the BiOI dispersion liquid, BiOI
Molal volume ratio with water is 0.5mmol:20mL；(NH in the ammonium molybdate aqueous solution4)6Mo7O24·4H2Mole body of O and water
Product is than being (0.086 ~ 0.114) mmol:10mL；Optimization, the molal volume ratio of the BiOI and water is 0.5mmol:20mL；Institute
State (NH4)6Mo7O24·4H2The molal volume of O and water ratio is 0.114mmol:10mL.
5. preparation method according to claim 2, which is characterized in that in step (3), AgNO in the silver nitrate aqueous solution3
Molal volume ratio with water is (1.2 ~ 1.6) mmol:10mL；The time being stirred to react is 1~10min；Optimization, it is described
AgNO3Molal volume ratio with water is 1.6mmol:10mL；It is described to be stirred to react the time as 2min.
6. preparation method according to claim 2 or 5, which is characterized in that in step (3), in the silver nitrate aqueous solution
AgNO3With (the NH in mixed dispersion liquid4)6Mo7O24·4H2The molar ratio of O is 14:1, and wherein the molar ratio of Mo and Bi is
(1.2 ~ 1.6): 1.
7. according to preparation method described in claim 2,5 or 6, which is characterized in that in step (3), the heat treatment condition is
1 ~ 5h is kept the temperature at 350 ~ 450 DEG C；The washing refers to alternately is washed with distilled water and dehydrated alcohol；The drying refer in
60 DEG C of dry 12h；Optimization, the heat treatment condition is to keep the temperature 2h at 400 DEG C.
8. according to the described in any item preparation methods of claim 2-7, which is characterized in that the AgI/Bi2MoO6/AgBi
(MoO4)2Tri compound nano heterojunction photocatalysis agent is two-dimensional sheet structure, and piece size is 1 ~ 5 μm, with a thickness of 0.1 ~ 0.2 μ
m；The AgI nano particle is evenly dispersed in two-dimensional slice surface, and AgI nanoparticle size is 2 ~ 25 nm.
9. a kind of AgI/Bi by the described in any item preparation method preparations of claim 2-72MoO6/AgBi(MoO4)2Ternary
Application of the composite Nano heterojunction photocatalyst in catalytic degradation organic pollutant.
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