CN108654599A - A kind of hexagonal phase hydration molybdenum trioxide photocatalyst and the preparation method and application thereof - Google Patents
A kind of hexagonal phase hydration molybdenum trioxide photocatalyst and the preparation method and application thereof Download PDFInfo
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- CN108654599A CN108654599A CN201810617943.7A CN201810617943A CN108654599A CN 108654599 A CN108654599 A CN 108654599A CN 201810617943 A CN201810617943 A CN 201810617943A CN 108654599 A CN108654599 A CN 108654599A
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- molybdenum trioxide
- hexagonal phase
- photocatalyst
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- trioxide photocatalyst
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- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 28
- 230000036571 hydration Effects 0.000 title claims abstract description 22
- 238000006703 hydration reaction Methods 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims description 6
- 239000002351 wastewater Substances 0.000 claims abstract description 11
- 239000003054 catalyst Substances 0.000 claims 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 4
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 4
- 239000000126 substance Substances 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 11
- 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
- 239000002253 acid Substances 0.000 claims description 4
- 239000008236 heating water Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002957 persistent organic pollutant Substances 0.000 claims description 4
- 230000001699 photocatalysis Effects 0.000 claims description 4
- 238000007146 photocatalysis Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 239000000975 dye Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001795 light effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000003672 processing method Methods 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
- 238000010408 sweeping Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
- B01J35/51—Spheres
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Water Supply & Treatment (AREA)
- Health & Medical Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Hydrology & Water Resources (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Toxicology (AREA)
- Catalysts (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of hexagonal phases to be hydrated molybdenum trioxide photocatalyst, and the chemical formula of the photochemical catalyst is MoO3·0.55H2O;Hexagonal phase hydration molybdenum trioxide photocatalyst of the present invention is in flower ball-shaped, is assembled by multiple regular hexagonal prisms;The regular hexagonal prism length of side be 600nm, a height of 58 μm.The hydration molybdenum trioxide photocatalyst production method of the present invention is simple, of low cost;It, can efficiently degradation of methylene blue and indoors under dim light(MB)Waste water from dyestuff solution.
Description
Technical field
The present invention relates to a kind of novel hexagonal phase hydration molybdenum trioxide photocatalysts and its simple preparation method and light to urge
Change activity.
Background technology
In the 21st century, facing mankind two very severe problems of the energy and environment, especially toxic and difficult to degrade
Environmental problem caused by organic pollution (such as polycyclic aromatic hydrocarbon, Polychlorinated biphenyls, pesticide, dyestuff etc.), it has also become influence human survival
With the significant problem of health.Can be had by the characteristic of activation in sunlight irradiation lower surface using semiconductor oxide materials
Effect ground oxygenolysis organic pollution.Compared with traditional environment purification processing method, Photocatalitic Technique of Semiconductor possesses reaction
Mild condition, non-secondary pollution, easy to operate and the degradation effect advantages such as significantly.However, many degradation reactions are shone in ultraviolet light
It is low to penetrate lower just generation, solar energy utilization ratio;And the degradation reaction efficiency occurred under visible light is not also high, which has limited photocatalysis
Practical application.
Invention content
The purpose of the present invention is to solve defect existing in the prior art, it is simple to provide a kind of preparation method, and light
The excellent new material of catalytic performance.
In order to achieve the above object, the present invention provides a kind of hexagonal phases to be hydrated molybdenum trioxide photocatalyst, the photocatalysis
The chemical formula of agent is MoO3·0.55H2O;Hexagonal phase hydration molybdenum trioxide photocatalyst of the present invention is in flower ball-shaped, by multiple positive six
Prism assembles;The length of side of the regular hexagonal prism be 600nm, a height of 5-8 μm.
The present invention also provides the preparation methods that above-mentioned hexagonal phase is hydrated molybdenum trioxide photocatalyst, include the following steps:
1)10mL water is added in beaker, under stirring condition, the metamolybdic acid ammonium of 2.46g is added;;
2)60 ~ 80 DEG C of heating water bath;
3)The nitric acid that 2ml mass fractions are 68% is added, persistently stirs one hour;
4)Centrifuge washing, it is dry.
The present invention also provides above-mentioned hexagonal phases to be hydrated molybdenum trioxide photocatalyst in organic pollution photocatalytic degradation side
The application in face.
Specifically when carrying out organic pollution photocatalytic degradation, it is organic in progress that hexagonal phase is hydrated molybdenum trioxide photocatalyst
When pollutant photocatalytic degradation, hexagonal phase hydration molybdenum trioxide photocatalysis of the present invention is added in organic pollutant wastewater solution
Agent, after being protected from light stirring 60min, 120-150min is reacted in catalysis under dim light indoors, you can;Wherein, organic pollutant wastewater is molten
The concentration of liquid is not higher than in 4.5mg/L;The addition that hexagonal phase is hydrated molybdenum trioxide photocatalyst is per 200mL organic pollutions
0.1g is added in waste water solution.
Carry out the preferred methylene blue of organic pollution of photocatalytic degradation.
The present invention has the following advantages compared with prior art:
The hydration molybdenum trioxide photocatalyst production method of the present invention is simple, of low cost;It, can be high and indoors under dim light
Effect ground degradation of methylene blue(MB)Waste water from dyestuff solution.
Description of the drawings
Fig. 1 is hydrated molybdenum trioxide light non-hydrated made from molybdenum trioxide and comparative example two for prepared by embodiment one
Catalyst and its X-ray diffraction(XRD)Figure;
Fig. 2 is non-hydrated molybdenum trioxide prepared by hydration molybdenum trioxide photocatalyst prepared by embodiment one and comparative example two
The surface sweeping electron microscope of photochemical catalyst(SEM)Comparison;
In Fig. 2, left side, which is that embodiment one is obtained, is hydrated molybdenum trioxide photocatalyst, and right side is non-made from comparative example two
It is hydrated molybdenum trioxide photocatalyst;
Fig. 3 is that hydration molybdenum trioxide and non-hydrated molybdenum trioxide photocatalyst contain methylene in degradation in effect example three
It is blue(MB)The active comparison diagram of waste water from dyestuff solution.
In Fig. 3, C0For the initial concentration of MB, C is the MB concentration measured after indoor weak light irradiates a period of time, and t is
Time.
As seen from Figure 3, under indoor weak light irradiation, hydration molybdenum trioxide photocatalyst energy efficient catalytic degradation MB dyestuffs
Waste water solution, activity are far above the performance of non-hydrated molybdenum trioxide catalyst.
Specific implementation mode
With reference to specific embodiment, the present invention is described in detail.
Embodiment one:
10mL water is added in beaker, under stirring condition, the metamolybdic acid ammonium of 2.46g is added.2ml is added to 80 DEG C in heating water bath
The nitric acid of mass fraction 68% persistently stirs one hour.Centrifuge washing, 60 DEG C of dryings, the molybdenum trioxide product being hydrated.
As shown in the lower part of Figure 1, the standard card of the hydration molybdenum trioxide photocatalyst and XRD that are prepared(JCPDS:48-
0399)It is consistent completely.
Comparative example two:
50mL water is added in beaker, under stirring condition, the metamolybdic acid ammonium of 0.62g is added.Heating water bath is added to 80 DEG C
The nitric acid of 1.6ml 2.2mol/L stirs 3 minutes.It is transferred in polytetrafluoroethyllining lining, 180 DEG C are kept for 96 hours.Naturally cold
But to room temperature, centrifuge washing, 60 DEG C of dryings obtain non-hydrated molybdenum trioxide product.
As shown in the tops Fig. 1, the standard card for the non-hydrated molybdenum trioxide and XRD being prepared(JCPDS:21-0569)
It is consistent completely.
As shown in Fig. 2, hydration molybdenum trioxide prepared by the embodiment of the present invention one(Fig. 2 is left), it is in regular columnar pattern, and it is right
The non-hydrated molybdenum trioxide than made from embodiment two(Fig. 2 is right)It is similar.Specifically it is distinguished as:The hydration three that the present invention is prepared
The regular hexagonal prism length of side of molybdenum oxide be 600nm, a height of 5-8 μm, and assemble be in flower ball-shaped.And what comparative example two was prepared
The regular hexagonal prism length of side of non-hydrated molybdenum trioxide be 800nm, a height of 4 μm.
Effect example three:
Test process is as follows:
By molybdenum trioxide non-hydrated made from the hydration molybdenum trioxide photocatalyst obtained of embodiment one and comparative example two
Photochemical catalyst, the waste water solution for the MB that degrades.
Sample 0.1g is weighed, 200ml MB aqueous solutions, wherein MB concentration all 4.5mg/L is separately added into, is first protected from light stirring
60min makes dyestuff reach absorption/desorption equilibrium in catalyst surface.Then it carries out being catalyzed reaction under indoor weak light, supernatant is used
Spectrophotometer detects.According to Lambert-Beer laws, the variation of organic matter characteristic absorption peak intensity can quantify and calculate it
Concentration changes.When extinction material is identical, thickness is identical, the variation of solution concentration can be directly indicated with the variation of absorbance.
Because there are one characteristic absorption peaks at 664 nm by MB, it is possible to weigh the concentration of MB in solution using the variation of absorbance
Variation(Abscissa:The low light irradiation time;Ordinate:The MB concentration values that are measured after for a period of time by low light irradiation and MB just
The ratio of beginning concentration).
As shown in figure 3, after low light irradiation 120min, hydration molybdenum trioxide photocatalyst degradation MB is up to 86%, and non-hydrated
Molybdenum trioxide compare, hydration molybdenum trioxide photocatalyst to MB have higher catalytic activity).
Claims (5)
1. a kind of novel hexagonal phase is hydrated molybdenum trioxide photocatalyst, it is characterised in that:The chemical formula of the photochemical catalyst is
MoO3·0.55H2O;The hexagonal phase hydration molybdenum trioxide photocatalyst is in flower ball-shaped, is assembled by multiple regular hexagonal prisms;Institute
State regular hexagonal prism the length of side be 600nm, a height of 5-8 μm.
2. the preparation method of hexagonal phase hydration molybdenum trioxide photocatalyst described in claim 1, it is characterised in that:Including following step
Suddenly:
1)10mL water is added in beaker, under stirring condition, the metamolybdic acid ammonium of 2.46g is added;;
2)60 ~ 80 DEG C of heating water bath;
3)The nitric acid that 2ml mass fractions are 68% is added, persistently stirs one hour;
4)Centrifuge washing, it is dry.
3. hexagonal phase described in claim 1 is hydrated molybdenum trioxide photocatalyst answering in terms of organic pollution photocatalytic degradation
With.
4. application according to claim 3, it is characterised in that:The hexagonal phase hydration molybdenum trioxide photocatalyst is carrying out
When organic pollution photocatalytic degradation, the hexagonal phase hydration molybdenum trioxide photocatalysis is added in organic pollutant wastewater solution
Agent, after being protected from light stirring 60min, 120-150min is reacted in catalysis under dim light indoors, you can;The organic pollutant wastewater solution
Concentration be not higher than 4.5mg/L;The addition of the hexagonal phase hydration molybdenum trioxide photocatalyst is per 200mL organic pollutions
0.1g is added in waste water solution.
5. application according to claim 4, it is characterised in that:The organic pollution is methylene blue.
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Cited By (3)
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---|---|---|---|---|
CN110921708A (en) * | 2019-12-16 | 2020-03-27 | 济南大学 | MoO (MoO)3Preparation method and application of self-assembled hexagonal prism structure |
CN111298786A (en) * | 2020-01-07 | 2020-06-19 | 重庆化工职业学院 | Micron hexagonal prism MoO3-xPreparation method of photocatalytic material |
CN111704166A (en) * | 2020-06-28 | 2020-09-25 | 南京信息工程大学 | Application of hydrated molybdenum trioxide in nitrogen fixation reaction |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110921708A (en) * | 2019-12-16 | 2020-03-27 | 济南大学 | MoO (MoO)3Preparation method and application of self-assembled hexagonal prism structure |
CN110921708B (en) * | 2019-12-16 | 2021-12-24 | 济南大学 | MoO (MoO)3Preparation method and application of self-assembled hexagonal prism structure |
CN111298786A (en) * | 2020-01-07 | 2020-06-19 | 重庆化工职业学院 | Micron hexagonal prism MoO3-xPreparation method of photocatalytic material |
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 |
CN111704166A (en) * | 2020-06-28 | 2020-09-25 | 南京信息工程大学 | Application of hydrated molybdenum trioxide in nitrogen fixation reaction |
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 |
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