CN111111639A - ZnO/InOOH heterogeneous Z-type photocatalytic material and preparation method thereof - Google Patents
ZnO/InOOH heterogeneous Z-type photocatalytic material and preparation method thereof Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 title claims abstract description 62
- 239000000463 material Substances 0.000 title claims abstract description 48
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 11
- 239000012266 salt solution Substances 0.000 claims abstract description 10
- 150000002471 indium Chemical class 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 150000003751 zinc Chemical class 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 6
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 239000011592 zinc chloride Substances 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 125000005842 heteroatom Chemical group 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000005215 recombination Methods 0.000 description 6
- 230000006798 recombination Effects 0.000 description 6
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 4
- 229960000907 methylthioninium chloride Drugs 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000004044 response Effects 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000031700 light absorption Effects 0.000 description 2
- 239000011941 photocatalyst Substances 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 239000012716 precipitator Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/08—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of gallium, indium or thallium
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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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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Abstract
A ZnO/InOOH heterogeneous Z-type photocatalytic material has the following ZnO energy band edges: eCB＝‑0.31eV,EVB+2.89eV, InOOH band edge: eCB＝‑0.29eV,EVBAnd the two are matched to form a Z-type ZnO/InOOH photocatalytic system at +3.21 eV. The preparation method comprises the following steps: 1) dissolving zinc salt and indium salt in water to obtain a mixed salt solution; 2) under the condition of stirring, dripping a precipitant solution into the mixed salt solution to react until the pH value is 9-9.5 to obtain a reaction system mixed solution; 3) transferring the mixed solution of the reaction system to a high-pressure reaction kettle for hydrothermal reaction; 4) and cooling the hydrothermal reaction product to room temperature, centrifuging, washing and drying to obtain the ZnO/InOOH heterogeneous Z-type photocatalytic material. The ZnO/InOOH heterogeneous Z-type photocatalytic material has the advantages of small composite powder particles, high repeated utilization rate, good dispersibility, high photocatalytic efficiency, simple synthesis method, easy operation and low reaction cost.
Description
Technical Field
The invention belongs to the technical field of photocatalytic degradation of dye wastewater, and particularly relates to a ZnO/InOOH heterogeneous Z-shaped photocatalytic material and a preparation method thereof.
Background
Semiconductor photocatalytic materials have gained wide attention from researchers in different fields due to their unique properties in the fields of solar energy conversion and catalytic degradation. Although it is known from the current research progress that ZnO has relatively high photocatalytic activity or photocatalytic degradation speed, the use ratio of the ZnO-based photocatalytic material to sunlight is limited due to the large forbidden band width. In general, the narrower the forbidden band width of a semiconductor, the wider the spectral response range of the semiconductor, the more the solar light is utilized, but the weaker the photohole and electron redox capabilities are, therefore, the balance between the following two aspects should be considered for improving the photocatalytic performance of ZnO: namely, the band gap width is reduced, and the spectral response range of the semiconductor is expanded; and simultaneously makes the valence band potential more positive and the conduction band potential more negative. However, these two points are contradictory to each other, and thus it is difficult to simultaneously realize these two points in a single component photocatalyst.
However, the Z-type photocatalytic material can satisfy these two requirements at the same time, namely: the Z-type photocatalytic material can not only retain photogenerated electrons with higher reduction capability and photogenerated holes with higher oxidation capability, but also can be more and more widely applied to the field of photocatalysis due to the specific advantages of the Z-type photocatalytic material.
Disclosure of Invention
In order to overcome the defects of the prior art and solve the problem of environmental pollution, the invention aims to provide a ZnO/InOOH heterogeneous Z-type photocatalytic material and a preparation method thereof, and the ZnO/InOOH heterogeneous Z-type photocatalytic material has the advantages of low cost, high removal efficiency, short treatment time and no secondary pollution; it is another object of the present invention to provide a new method for introducing conductive channels for constructing a high-efficiency Z-type photocatalytic system.
In order to achieve the purpose, the invention adopts the technical scheme that:
a ZnO/InOOH heterogeneous Z-type photocatalytic material has the following ZnO energy band edges: eCB＝-0.31eV,EVB+2.89eV, InOOH band edge: eCB＝-0.29eV,EVBAnd the two are matched to form a Z-type ZnO/InOOH photocatalytic system at +3.21 eV.
Preferably, the ZnO corresponds to two forms of PDF #36-1451 and PDF #21-1486 in an XRD standard card.
Preferably, the molar ratio of ZnO to InOOH is 1 (1-5), especially 1: 1; 1: 2; 1: 3; 1: 4; 1:5 can produce ZnO/InOOH heterogeneous Z-type photocatalytic materials, and the molar ratio is about 1: 2.
the ZnO is cylindrical, and the InOOH is cubic.
The invention also provides a preparation method of the ZnO/InOOH heterogeneous Z-type photocatalytic material, which comprises the following steps:
1) dissolving zinc salt and indium salt in water to obtain a mixed salt solution;
2) under the condition of stirring, dripping a precipitant solution into the mixed salt solution to react until the pH value is 9-9.5 to obtain a reaction system mixed solution;
3) transferring the mixed solution of the reaction system to a high-pressure reaction kettle for hydrothermal reaction;
4) and cooling the hydrothermal reaction product to room temperature, centrifuging, washing and drying to obtain the ZnO/InOOH heterogeneous Z-type photocatalytic material.
Preferably, in the step 1), the zinc salt is ZnCl2The indium salt is InCl3And (2) taking deionized water as a solution, and magnetically stirring at room temperature to prepare a mixed salt solution, wherein the molar ratio of zinc salt to indium salt is 1: 2.
preferably, in the step 2), ammonia water is used as a precipitant solution.
Preferably, in the step 3), the hydrothermal reaction temperature is 300 ℃ and the reaction time is 24 h.
Preferably, in the step 4), the centrifugation speed is 8000rpm, the centrifugation time is 8min, and deionized water and ethanol are adopted for washing.
Preferably, in the step 4), the drying temperature is 80 ℃ and the drying time is 10 h.
Compared with the prior art, the invention has the beneficial effects that:
(1) the novel ZnO/InOOH heterogeneous Z-type photocatalytic material is synthesized by adopting a one-step hydrothermal method, the method has the advantages of simplicity in operation, environmental friendliness, low energy consumption and the like, and the adopted ZnCl2，InCl3And raw materials such as ammonia water and the like, is cheap and easy to obtain, and has low toxicity.
(2) The ZnO selected by the invention has proper energy band edge (E)CB＝-0.31eV,EVB= 2.89eV), it may be reacted with InOOH (E)CB＝-0.29eV,EVB+3.21eV) to form a Z-type ZnO/InOOH photocatalytic system. In the Z-type photocatalytic system, the recombination of photo-generated electron-hole pairs can be effectively inhibited, and the response range of light is expanded.
Drawings
FIG. 1 is a diagram of the photocatalytic mechanism of the heterogeneous Z-type photocatalytic material of the present invention.
FIG. 2 is an XRD diffraction pattern of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the method of the present invention.
FIG. 3 is a UV-Vis spectrum of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the method of the present invention.
FIG. 4 is a PL map of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the method of the present invention.
FIG. 5 is a graph showing the relationship between the degradation efficiency of methylene blue and the photocatalytic time of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the method of the present invention, wherein the amount of the catalyst is 0.5g/L, and the concentration of the methylene blue is 10 mg/L.
Detailed Description
The embodiments of the present invention will be described in detail below with reference to the drawings and examples.
Referring to fig. 1, the principle of the present invention is: under the irradiation of visible light, valence bands of ZnO and InOOH respectively generate electrons to jump to a conduction band, and positive holes are left in the valence bands; when the two materials are heterogeneous Z-type composite photocatalysts, electrons of an InOOH conduction band are combined with holes of a ZnO valence band, and dye molecules generate O & lt + & gt with electrons of a ZnO conduction band2 -A chemical reaction occurs; meanwhile, the compound can also chemically react with OH & generated by a cavity of an InOOH valence band to achieve the purpose of dye degradation, and the electron transfer path of the Z-type heterogeneous photocatalytic material can effectively avoid the problem of high electron-hole recombination rate in the photocatalytic process, thereby improving the photocatalytic efficiency.
In one embodiment of the present invention, a method for preparing a ZnO/InOOH heterogeneous Z-type photocatalytic material is provided, which comprises the following steps:
1) mixing a mixture of 1:2 zinc salt ZnCl2And indium salt InCl3Dissolving in deionized water, and magnetically stirring to obtain a mixed salt solution;
2) under the condition of stirring, dropwise adding ammonia water of a precipitator solution into the mixed salt solution to react until the pH value is 9-9.5 to obtain a reaction system mixed solution;
3) transferring the mixed solution of the reaction system into a high-pressure reaction kettle, and keeping hydrothermal reaction for 24 hours at 300 ℃;
4) and cooling the hydrothermal reaction product to room temperature, centrifuging for 8min at 8000rmp, washing with deionized water and ethanol, and drying at 80 ℃ for 10h to obtain the ZnO/InOOH heterogeneous Z-type photocatalytic material.
FIG. 2 is an XRD spectrum of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the above steps. It can be seen from the figure that it has good crystallinity. Indium salts exist as InOOH oxides, with unusual phases of ZnO (PDF #21-1486) being present in addition to the conventional wurtzite ZnO (PDF # 36-1451).
FIG. 3 is a UV-VIS spectrum of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the above steps. The light absorption range of the material is larger than that of ZnO, which shows that the ZnO/InOOH heterogeneous Z-shaped photocatalytic material can more effectively utilize solar energy. This variation is caused by the variation of the energy band width.
FIG. 4 is a PL diagram of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the above steps. The intensity of PL indicates the rate of electron-hole recombination. The stronger the peak, the higher the electron-hole recombination rate. The peak of ZnO is obviously higher than that of ZnO/InOOH, which shows that the ZnO/InOOH heterogeneous Z-type photocatalytic material obviously inhibits the recombination rate of electrons and holes due to the existence of an internal electric field.
FIG. 5 is a graph showing the relationship between the degradation efficiency of methylene blue and the photocatalytic time of the ZnO/InOOH heterogeneous Z-type photocatalytic material prepared by the above steps. The catalyst amount is 0.5g/L, and the methylene blue concentration is 10 mg/L. The degradation experiments all occur under visible light. The construction of the heterogeneous Z-shaped photocatalytic material can effectively expand the light absorption range and inhibit the recombination of electrons and holes, so that the degradation efficiency of the ZnO/InOOH heterogeneous Z-shaped photocatalytic material is obviously due to ZnO.
In conclusion, the ZnO/InOOH heterogeneous Z-type photocatalytic material has the advantages of small composite powder particles, high repeated utilization rate, good dispersibility, high photocatalytic efficiency, simple synthesis method, easy operation and low reaction cost.
Claims (10)
1. A ZnO/InOOH heterogeneous Z-type photocatalytic material is characterized in that the ZnO energy band edge: eCB＝-0.31eV,EVB+2.89eV, InOOH band edge: eCB＝-0.29eV,EVBAnd the two are matched to form a Z-type ZnO/InOOH photocatalytic system at +3.21 eV.
2. The ZnO/InOOH heterogeneous Z-type photocatalytic material of claim 1, wherein the ZnO corresponds to two forms of PDF #36-1451 and PDF #21-1486 in XRD standard card, and the InOOH corresponds to PDF # 71-2283.
3. The ZnO/InOOH heterogeneous Z-type photocatalytic material of claim 1, wherein the molar ratio of ZnO to InOOH is 1 (1-5).
4. The ZnO/InOOH hetero Z-type photocatalytic material of claim 1, wherein the ZnO is cylindrical and the InOOH is cubic.
5. A preparation method of a ZnO/InOOH heterogeneous Z-type photocatalytic material is characterized by comprising the following steps:
1) dissolving zinc salt and indium salt in water to obtain a mixed salt solution;
2) under the condition of stirring, dripping a precipitant solution into the mixed salt solution to react until the pH value is 9-9.5 to obtain a reaction system mixed solution;
3) transferring the mixed solution of the reaction system to a high-pressure reaction kettle for hydrothermal reaction;
4) and cooling the hydrothermal reaction product to room temperature, centrifuging, washing and drying to obtain the ZnO/InOOH heterogeneous Z-type photocatalytic material.
6. The ZnO/InOOH heterogeneous Z-type photocatalytic material of claim 4 and preparation method thereof, wherein in the step 1), the zinc salt is ZnCl2The indium salt is InCl3And using deionized water as a solution, and magnetically stirring at room temperature to prepare a mixed salt solution.
7. The ZnO/InOOH heterogeneous Z-type photocatalytic material and the preparation method thereof according to claim 4 or 5, characterized in that the molar ratio of the zinc salt to the indium salt is 1: 2.
8. the ZnO/InOOH heterogeneous Z-type photocatalytic material and the preparation method thereof according to claim 4, wherein in the step 2), ammonia water is used as a precipitant solution.
9. The ZnO/InOOH heterogeneous Z-type photocatalytic material and the preparation method thereof according to claim 4, wherein in the step 3), the hydrothermal reaction temperature is 300 ℃ and the reaction time is 24 hours, and in the step 4), the drying temperature is 80 ℃ and the drying time is 10 hours.
10. The ZnO/InOOH heterogeneous Z-type photocatalytic material and the preparation method thereof according to claim 4, wherein in the step 4), the centrifugation speed is 8000rpm, the centrifugation time is 8min, and deionized water and ethanol are adopted for washing.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113877556A (en) * | 2021-10-18 | 2022-01-04 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113877556A (en) * | 2021-10-18 | 2022-01-04 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
| CN113877556B (en) * | 2021-10-18 | 2023-01-17 | 常州大学 | Indium oxyhydroxide/modified attapulgite photocatalytic composite material and preparation method and application thereof |
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