CN108654599B - Hexagonal phase hydrated molybdenum trioxide photocatalyst and preparation method and application thereof - Google Patents
Hexagonal phase hydrated molybdenum trioxide photocatalyst and preparation method and application thereof Download PDFInfo
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- CN108654599B CN108654599B CN201810617943.7A CN201810617943A CN108654599B CN 108654599 B CN108654599 B CN 108654599B CN 201810617943 A CN201810617943 A CN 201810617943A CN 108654599 B CN108654599 B CN 108654599B
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- molybdenum trioxide
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 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 abstract description 20
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 20
- 239000002351 wastewater Substances 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims description 13
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000000356 contaminant Substances 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 239000000243 solution Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical group 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- B01J35/39—
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/28—Molybdenum
-
- B01J35/51—
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- 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 hexagonal phase hydrated molybdenum trioxide photocatalyst, the chemical formula of which is MoO3·0.55H2O; the hexagonal phase hydrated molybdenum trioxide photocatalyst is in a flower ball shape and is formed by assembling a plurality of regular hexagonal prisms; the side length of the regular hexagonal prism is 600nm, and the height of the regular hexagonal prism is 5-8 mu m. The hydrated molybdenum trioxide photocatalyst is simple in preparation method and low in cost; and can efficiently degrade Methylene Blue (MB) dye wastewater solution under indoor weak light.
Description
Technical Field
The invention relates to a novel hexagonal phase hydrated molybdenum trioxide photocatalyst, a simple preparation method thereof and photocatalytic activity.
Background
In the 21 st century, human beings have faced two very serious problems of energy and environment, especially the environmental problem caused by toxic and non-degradable organic pollutants (such as polycyclic aromatic hydrocarbon, polychlorinated biphenyl, pesticide, dye, etc.), which has become a significant problem affecting human survival and health. Organic pollutants can be effectively oxidized and decomposed by utilizing the characteristic that the surface of the semiconductor oxide material can be activated under the irradiation of sunlight. Compared with the traditional environment purification treatment method, the semiconductor photocatalysis technology has the advantages of mild reaction conditions, no secondary pollution, simple operation, obvious degradation effect and the like. However, many degradation reactions occur under ultraviolet irradiation, and the solar energy utilization rate is low; the degradation reaction efficiency under visible light is not high, which limits the practical application of photocatalysis.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a novel material which is simple in preparation method and excellent in photocatalytic performance.
In order to achieve the above object, the present invention provides a hexagonal phase hydrated molybdenum trioxide photocatalyst having a chemical formula of MoO3·0.55H2O; the hexagonal phase hydrated molybdenum trioxide photocatalyst is in a flower ball shape and is formed by assembling a plurality of regular hexagonal prisms; the side length of the regular hexagonal prism is 600nm, and the height of the regular hexagonal prism is 5-8 mu m.
The invention also provides a preparation method of the hexagonal phase hydrated molybdenum trioxide photocatalyst, which comprises the following steps:
1) adding 10mL of water into a beaker, and adding 2.46g of ammonium paramolybdate under the stirring condition; (ii) a
2) Heating in a water bath for 60-80 ℃;
3) adding 2ml of nitric acid with the mass fraction of 68%, and continuously stirring for one hour;
4) centrifugally washing and drying.
The invention also provides application of the hexagonal phase hydrated molybdenum trioxide photocatalyst in photocatalytic degradation of organic pollutants.
Specifically, when the photocatalytic degradation of organic pollutants is carried out, adding the hexagonal-phase hydrated molybdenum trioxide photocatalyst into an organic pollutant wastewater solution when the photocatalytic degradation of organic pollutants is carried out, stirring for 60min in a dark place, and carrying out catalytic reaction for 120-150min in indoor weak light; wherein the concentration of the organic pollutant wastewater solution is not higher than 4.5 mg/L; the addition amount of the hexagonal phase hydrated molybdenum trioxide photocatalyst is 0.1g per 200mL of the organic pollutant wastewater solution.
The organic contaminant subjected to photocatalytic degradation is preferably methylene blue.
Compared with the prior art, the invention has the following advantages:
the hydrated molybdenum trioxide photocatalyst is simple in preparation method and low in cost; and can efficiently degrade Methylene Blue (MB) dye wastewater solution under indoor weak light.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a hydrated molybdenum trioxide prepared in example one and a non-hydrated molybdenum trioxide photocatalyst prepared in comparative example two;
FIG. 2 is a Scanning Electron Micrograph (SEM) comparison of a hydrated molybdenum trioxide photocatalyst prepared in example one and a non-hydrated molybdenum trioxide photocatalyst prepared in comparative example two;
in FIG. 2, the left side is the hydrated molybdenum trioxide photocatalyst prepared in example one, and the right side is the non-hydrated molybdenum trioxide photocatalyst prepared in comparative example two;
FIG. 3 is a graph comparing the activity of hydrated molybdenum trioxide and non-hydrated molybdenum trioxide photocatalysts in Effect example III in degrading wastewater solutions containing Methylene Blue (MB) dye.
In FIG. 3, C0The initial concentration of MB, the concentration of MB measured after a period of indoor low-light irradiation, and the time t.
As can be seen from FIG. 3, under indoor weak light irradiation, the hydrated molybdenum trioxide photocatalyst can efficiently catalyze and degrade MB dye wastewater solution, and the activity is much higher than that of a non-hydrated molybdenum trioxide catalyst.
Detailed Description
The present invention will be described in detail with reference to specific examples.
The first embodiment is as follows:
10mL of water was added to the beaker, and 2.46g of ammonium paramolybdate was added with stirring. The mixture was heated in a water bath to 80 ℃ and 2ml of nitric acid with a mass fraction of 68% was added and stirring was continued for one hour. Centrifugally washing and drying at 60 ℃ to obtain a hydrated molybdenum trioxide product.
As shown in the lower part of FIG. 1, the hydrated molybdenum trioxide photocatalyst prepared completely conformed to the standard card for XRD (JCPDS: 48-0399).
Comparative example two:
50mL of water was added to a beaker, and 0.62g of ammonium paramolybdate was added with stirring. The mixture was heated in a water bath to 80 ℃ and 1.6ml of 2.2mol/L nitric acid was added thereto and stirred for 3 minutes. Transfer to a teflon liner and hold at 180 ℃ for 96 hours. Naturally cooling to room temperature, centrifugally washing, and drying at 60 ℃ to obtain a non-hydrated molybdenum trioxide product.
As shown in the upper part of FIG. 1, the prepared non-hydrated molybdenum trioxide completely conformed to the standard card of XRD (JCPDS: 21-0569).
As shown in fig. 2, the hydrated molybdenum trioxide (fig. 2, left) prepared in the first embodiment of the present invention has a regular columnar morphology, similar to the non-hydrated molybdenum trioxide (fig. 2, right) prepared in the second embodiment of the present invention. The specific differences are as follows: the side length of the hydrated molybdenum trioxide regular hexagonal prism prepared by the method is 600nm, the height of the hydrated molybdenum trioxide regular hexagonal prism is 5-8 mu m, and the hydrated molybdenum trioxide regular hexagonal prism is assembled into a flower ball shape. And the side length of the non-hydrated molybdenum trioxide prepared in the second comparative example is 800nm, and the height of the non-hydrated molybdenum trioxide is 4 mu m.
Effect example three:
the test procedure was as follows:
the hydrated molybdenum trioxide photocatalyst prepared in example one and the non-hydrated molybdenum trioxide photocatalyst prepared in comparative example two were used to degrade a waste aqueous solution of MB.
Weighing 0.1g of sample, respectively adding 200ml of MB aqueous solution, wherein the MB concentration is 4.5mg/L, and stirring for 60min in a dark place to ensure that the dye is adsorbed/desorbed on the surface of the catalyst to be balanced. Then, the catalytic reaction is carried out under indoor weak light, and the supernatant is detected by a spectrophotometer. According to the Lambert-Beer law, the concentration change of the organic matter can be quantitatively calculated according to the change of the characteristic absorption peak intensity of the organic matter. When the light-absorbing substances are the same and the thicknesses are the same, the change in the concentration of the solution can be directly expressed by the change in absorbance. Since MB has a characteristic absorption peak at 664 nm, the change in concentration of MB in the solution can be measured by the change in absorbance (abscissa: time of weak light irradiation; ordinate: ratio of MB concentration value measured after a lapse of time of weak light irradiation to initial concentration of MB).
As shown in fig. 3, after 120min of low light irradiation, the hydrated molybdenum trioxide photocatalyst degraded MB up to 86%, and the hydrated molybdenum trioxide photocatalyst had a higher catalytic activity for MB than non-hydrated molybdenum trioxide).
Claims (4)
1. A hexagonal phase hydrated molybdenum trioxide photocatalyst is characterized in that: the chemical formula of the photocatalyst is MoO3·0.55H2O; the hexagonal phase hydrated molybdenum trioxide photocatalyst is in a flower ball shape and is formed by assembling a plurality of regular hexagonal prisms; the side length of the regular hexagonal prism is 600nm, and the height of the regular hexagonal prism is 5-8 mu m; the photocatalyst is prepared by the following steps:
1) adding 10mL of water into a beaker, and adding 2.46g of ammonium paramolybdate under the stirring condition;
2) heating in a water bath for 60-80 ℃;
3) adding 2mL of nitric acid with the mass fraction of 68%, and continuously stirring for one hour;
4) centrifugally washing and drying.
2. Use of the hexagonal-phase hydrated molybdenum trioxide photocatalyst of claim 1 for photocatalytic degradation of organic pollutants.
3. Use according to claim 2, characterized in that: when the hexagonal phase hydrated molybdenum trioxide photocatalyst is used for photocatalytic degradation of organic pollutants, the hexagonal phase hydrated molybdenum trioxide photocatalyst is added into an organic pollutant wastewater solution, and after the mixture is stirred for 60min in a dark place, the mixture is subjected to catalytic reaction for 120-150min under indoor weak light; the concentration of the organic pollutant wastewater solution is not higher than 4.5 mg/L; the addition amount of the hexagonal phase hydrated molybdenum trioxide photocatalyst is 0.1g per 200mL of organic pollutant wastewater solution.
4. Use according to claim 3, characterized in that: the organic contaminant is methylene blue.
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| CN110921708B (en) * | 2019-12-16 | 2021-12-24 | 济南大学 | MoO (MoO)3Preparation method and application of self-assembled hexagonal prism structure |
| CN111298786B (en) * | 2020-01-07 | 2024-03-12 | 重庆化工职业学院 | Micrometer hexagonal prism MoO 3-x Preparation method of photocatalytic material |
| CN111704166B (en) * | 2020-06-28 | 2024-02-09 | 南京信息工程大学 | Application of hydrated molybdenum trioxide in nitrogen fixation reaction |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921402A (en) * | 2012-11-15 | 2013-02-13 | 合肥工业大学 | Normal temperature preparation method of hydrated molybdenum trioxide photocatalyst |
| CN104709943A (en) * | 2015-03-13 | 2015-06-17 | 济南大学 | Preparation method of molybdenum trioxide microsphere in three-dimensional hierarchical structure |
| CA2962296C (en) * | 2015-06-08 | 2018-11-13 | University Of Waterloo | Electrode materials for rechargeable zinc cells and batteries produced therefrom |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102921402A (en) * | 2012-11-15 | 2013-02-13 | 合肥工业大学 | Normal temperature preparation method of hydrated molybdenum trioxide photocatalyst |
| CN104709943A (en) * | 2015-03-13 | 2015-06-17 | 济南大学 | Preparation method of molybdenum trioxide microsphere in three-dimensional hierarchical structure |
| CA2962296C (en) * | 2015-06-08 | 2018-11-13 | University Of Waterloo | Electrode materials for rechargeable zinc cells and batteries produced therefrom |
Non-Patent Citations (3)
| Title |
|---|
| Thermal stability and photoluminescence property of hexagonal MoO3•0.55H2O microrods;Ke Ma etal.;《PHASE TRANSITIONS》;20160622;第342-350页 * |
| 低温液相合成路线制备六方相MoO3 纳米棒;杨保俊等;《中国钼业》;20090430;第29-32页 * |
| 氧化钼微结构控制合成及气敏性能;祁晴晴;《万方数据》;20150728;第30-38页 * |
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