CN106268776A - A kind of doped nano photocatalyst, preparation method and application - Google Patents
A kind of doped nano photocatalyst, preparation method and application Download PDFInfo
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- CN106268776A CN106268776A CN201610562907.6A CN201610562907A CN106268776A CN 106268776 A CN106268776 A CN 106268776A CN 201610562907 A CN201610562907 A CN 201610562907A CN 106268776 A CN106268776 A CN 106268776A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000011259 mixed solution Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 26
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 22
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 18
- 230000003197 catalytic effect Effects 0.000 claims abstract description 11
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 8
- 239000001119 stannous chloride Substances 0.000 claims abstract description 8
- 235000011150 stannous chloride Nutrition 0.000 claims abstract description 8
- 239000003513 alkali Substances 0.000 claims abstract description 7
- 239000002253 acid Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 38
- 239000000047 product Substances 0.000 claims description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 230000015556 catabolic process Effects 0.000 claims description 11
- 238000006731 degradation reaction Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims description 10
- 239000012065 filter cake Substances 0.000 claims description 10
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 10
- 238000006703 hydration reaction Methods 0.000 claims description 8
- 239000000126 substance Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 12
- 230000000694 effects Effects 0.000 description 8
- 230000001699 photocatalysis Effects 0.000 description 8
- 238000007146 photocatalysis Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 5
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 4
- 229910004619 Na2MoO4 Inorganic materials 0.000 description 4
- 229910020350 Na2WO4 Inorganic materials 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 238000001000 micrograph Methods 0.000 description 4
- VLAPMBHFAWRUQP-UHFFFAOYSA-L molybdic acid Chemical compound O[Mo](O)(=O)=O VLAPMBHFAWRUQP-UHFFFAOYSA-L 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- 239000007787 solid Substances 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 230000004931 aggregating effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 2
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 241001062009 Indigofera Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/30—Tungsten
-
- 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
-
- 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
-
- 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
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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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
- C02F2101/308—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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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Abstract
The invention provides the preparation method of a kind of doped nano photocatalyst, comprise the following steps: step one, weigh sodium tungstate and sodium molybdate and be dissolved in deionized water, stirring, to dissolving completely, obtains mixed solution；Step 2, adds stannous chloride to mixed solution, with acid or alkali regulation pH after stirring, obtains the mixed solution after pH regulator；Step 3, carries out hydro-thermal reaction by the mixed solution after pH regulator in step 2, obtains reacted mixed solution；Step 4, treats the reacted mixed solution cooling that step 3 obtains, is filtered by reacted mixed solution, washs, is dried, obtain dry products；Step 5, grinds dry products, obtains doped nano photocatalyst.The doped nano photocatalyst environmental protection of the present invention, composition simply, have highlight catalytic active the most under visible light, and have strong physical absorption performance.Preparation method is simple, low cost, and environmentally safe, it is adaptable to industrial applications.
Description
Technical field
The present invention relates to photocatalysis technology field, be specifically related to a kind of doped nano photocatalyst, preparation method and answer
With.
Background technology
Along with environmental pollution and energy crisis are increasingly sharpened, people are constantly searching for Environment control and are utilizing solar energy
Method.Owing to photocatalysis technology has simple to operate, green non-pollution and can directly utilize the advantages such as solar energy, therefore light is urged
Change technology becomes one of current research focus.Traditional photocatalyst material TiO2At the ultraviolet light being less than 400nm by wavelength
Exciting and lower just demonstrate photocatalytic activity, the energy of this part wavelength light only accounts for solar energy gross energy about 4%, and do not utilize
Visible light energy accounts for about 43%, and the visible light responsive photocatalyst therefore developing efficient stable becomes photocatalysis field
Study hotspot.
2009, IS Cho, CH Kwak research report first α-SnWO4Certain photocatalysis is had to live under visible light
Property.2011, Zhu G and Que W research report water heat transfer α-SnWO4Reaction mechanism, preparation condition etc..Scientist
Attempted with different ions doping improve α-SnWO4Activity, achieves certain effect, but activity improves limited, it is impossible to meet
Efficiently utilize the needs of solar energy.
Not yet it is related at present by doping Mo6+Improve α-SnWO4The relevant report of visible light photocatalysis active.
Summary of the invention
The present invention is carried out to solve the problems referred to above, and the present invention is with methylene blue as target contaminant, by black
Under dark condition, methylene blue is characterized the physical absorption performance of catalyst by the absorbance after Catalyst Adsorption, by calculating visible ray
Excite lower catalyst to the degradation rate of methylene blue to characterize its visible light photocatalysis active, it is provided that one is catalyzed under visible light
Activity is high, physical absorption performance is strong doped nano photocatalyst and the preparation method and application of this catalyst, be catalyzed fall
Solve the organic pollution in environment.
The invention provides the preparation method of a kind of doped nano photocatalyst, have the feature that, including following
Step:
Step one, weighs sodium tungstate and sodium molybdate and is dissolved in deionized water, and stirring, to dissolving completely, obtains mixing molten
Liquid；
Step 2, adds stannous chloride to mixed solution, with acid or alkali regulation pH=3-10 after stirring, obtains pH and adjusts
Mixed solution after joint；
Step 3, carries out hydro-thermal in the reactor under high-temperature and high-pressure conditions by the mixed solution after pH regulator in step 2
Reaction, obtains reacted mixed solution；
Step 4, after the reacted mixed solution obtained until step 3 is cooled to room temperature, by reacted mixed solution
It is filtrated to get filter cake, to Cake Wash, is dried, obtains dry products；
Step 5, grinds dry products, obtains doped nano photocatalyst.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in step one, the preparation method of mixed solution includes following sub-step:
Sub-step one, weighs sodium tungstate and sodium molybdate respectively and is dissolved in deionized water, and stirring is complete to dissolving, difference
Obtain sodium tungstate solution and sodium molybdate solution；
Sub-step two, is mixed and added into deionized water by sodium tungstate solution and sodium molybdate solution, obtains mixed solution.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in step one, in mixed solution, W:Mo atomic molar is than for 0:10～10:0.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in step 2, acid is salpeter solution, and alkali is sodium hydroxide solution.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in described step 2, with acid or alkali regulation pH=3.5-4.5 after stirring.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in step 3, high-temperature and high-pressure conditions is temperature 100～300 DEG C, pressure 20～50MPa.
In the preparation method of the doped nano photocatalyst of present invention offer, it is also possible to have a feature in that it
In, in step 3, the time of hydration reaction is 6～12h.
Present invention also offers a kind of doped nano photocatalyst, by the doped nano photocatalysis of above-mentioned any one
The preparation method of agent prepares, it is characterised in that: the chemical formula of doped nano photocatalyst is SnW(1-x)MoxO4, the wherein model of X
Enclosing is 0≤X≤1, and the quantivalence of Mo is+6 valencys.
Present invention also offers a kind of above-mentioned doped nano photocatalyst answering in catalytic degradation organic pollution
With.
In the doped nano photocatalyst application in catalytic degradation organic pollution that the present invention provides, it is also possible to
Having a feature in that wherein, organic pollution is methylene blue.
Invention effect and effect
The invention provides a kind of doped nano photocatalyst, preparation method and application, the doped nano of the present invention
Photocatalyst SnW(1-x)MoxO4Environmental protection, composition simply, have highlight catalytic active the most under visible light, and have
Strong physical absorption performance.
Sodium tungstate is mixed by the preparation method of the doped nano photocatalyst of the present invention with sodium molybdate, and adds protochloride
Stannum, carries out hydration reaction under high-temperature and high-pressure conditions, more dry by filtering reacted mixed solution, wash, being dried to obtain
Dry product, is finally ground dry products, obtains doped nano photocatalyst, and this preparation method is simple, cost
Low, and environmentally safe, it is adaptable to industrial applications.
The application of the doped nano photocatalyst of the present invention is by photocatalyst SnW(1-x)MoxO4Under the exciting of visible ray
Catalytic degradation methylene blue, catalytic degradation efficiency is high.
Accompanying drawing explanation
Fig. 1 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4X-ray diffractogram；
Fig. 2 (a) is doped nano photocatalyst α-SnMoO in embodiments of the invention four4Scanning electron microscope image, figure
2 (b) is doped nano photocatalyst SnW in embodiments of the invention one0.7Mo0.3O4Scanning electron microscope image；
Fig. 3 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4Absorption Asia under dark condition
Methyl blue absorption-time graph；And
Fig. 4 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4Under the conditions of radiation of visible light
To methylene blue degraded-time graph.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, doped nano photocatalyst, the preparation method and application of the present invention are entered
One step explanation.
Embodiment one
The preparation method of the doped nano photocatalyst of the present embodiment comprises the following steps:
Step one, weighs 0.04mol (13.1940g) sodium tungstate (Na2WO4·2H2O), dissolved in 200ml deionization
In water, stirring, to dissolving completely, obtains the sodium tungstate solution that concentration is 0.2mol/L；And weigh 0.04mol (9.6780g) molybdic acid
Sodium (Na2MoO4·2H2O), dissolved in 200ml deionized water, stirring is to dissolving completely, and obtaining concentration is 0.2mol/L
Sodium molybdate solution；Take 0.2mol/L sodium tungstate solution 14ml and 0.2mol/L sodium molybdate solution 6ml and add deionized water
20ml obtains mixed solution.
Step 2, weighs the stannous chloride (SnCl of 0.004mol (0.9026g)2·2H2O) solid, adds to above-mentioned mixing
In solution, stirring mixing under room temperature, regulate pH=3 with dilute nitric acid solution, stirring, to dissolving completely, obtains the mixing after pH regulator
Solution.
Step 3, the mixed solution after pH regulator is put into temperature be 100 DEG C, pressure be anti-under conditions of 20MPa
Answer and still carries out hydration reaction 6h, obtain reacted mixed solution.
Step 4, after reacted mixed solution is cooled to room temperature, obtains by circulating water type multiplex vacuum pump filtered sample
To filter cake, washing and filtering abundant to filter cake deionized water, it is dried, obtains dry products.
Step 5, grinds dry products, obtains doped nano photocatalyst SnW0.7Mo0.3O4。
Fig. 1 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4X-ray diffractogram.
Fig. 2 (b) is doped nano photocatalyst SnW in embodiments of the invention one0.7Mo0.3O4Scanning electron microscope image
As it is shown in figure 1, the doped nano photocatalyst SnW that the present embodiment obtains0.7Mo0.3O4It it is 27.6 ° in the angle of diffraction
Diffracted intensity corresponding to diffraction maximum the strongest.
As shown in Fig. 2 (b), doped nano photocatalyst SnW0.7Mo0.3O4Become aggregating state, α-SnWO4With Mo6+Can enter
Row well combines.
Embodiment two
The preparation method of the doped nano photocatalyst of the present embodiment comprises the following steps:
Step one, weighs 0.04mol (13.1940g) sodium tungstate (Na2WO4·2H2O), dissolved in 200ml deionization
In water, stirring, to dissolving completely, obtains the sodium tungstate solution that concentration is 0.2mol/L；And weigh 0.04mol (9.6780g) molybdic acid
Sodium (Na2MoO4·2H2O), dissolved in 200ml deionized water, stirring is to dissolving completely, and obtaining concentration is 0.2mol/L
Sodium molybdate solution；Take 0.2mol/L sodium tungstate solution 8ml and 0.2mol/L sodium molybdate solution 12ml and add deionized water
20ml obtains mixed solution.
Step 2, weighs the stannous chloride (SnCl of 0.004mol (0.9026g)2·2H2O) solid, adds to above-mentioned mixing
In solution, under room temperature, stirring mixes, and regulates pH=4.5 with dilute nitric acid solution, and stirring, to dissolving completely, obtains mixing after pH regulator
Close solution.
Step 3, the mixed solution after pH regulator is put into temperature be 200 DEG C, pressure be anti-under conditions of 35MPa
Answer and still carries out hydration reaction 8h, obtain reacted mixed solution.
Step 4, after reacted mixed solution is cooled to room temperature, obtains by circulating water type multiplex vacuum pump filtered sample
To filter cake, washing and filtering abundant to filter cake deionized water, it is dried, obtains dry products.
Step 5, grinds dry products, obtains doped nano photocatalyst SnW0.4Mo0.6O4。
Again as it is shown in figure 1, the doped nano photocatalyst SnW of the present embodiment0.4Mo0.6O4It it is 27.6 ° in the angle of diffraction
Diffracted intensity corresponding to diffraction maximum is the strongest.
Embodiment three
The preparation method of the doped nano photocatalyst of the present embodiment comprises the following steps:
Step one, weighs 0.04mol (13.1940g) sodium tungstate (Na2WO4·2H2O), dissolved in 200ml deionization
In water, stirring, to dissolving completely, obtains the sodium tungstate solution that concentration is 0.2mol/L；And weigh 0.04mol (9.6780g) molybdic acid
Sodium (Na2MoO4·2H2O), dissolved in 200ml deionized water, stirring is to dissolving completely, and obtaining concentration is 0.2mol/L
Sodium molybdate solution；Take 0.2mol/L sodium molybdate solution 20ml and add deionized water 20ml and obtain mixed solution.
Step 2, weighs the stannous chloride (SnCl of 0.004mol (0.9026g)2·2H2O) solid, adds to above-mentioned mixing
In solution, under room temperature, stirring mixes, and regulates pH=8 with sodium hydroxide solution, and stirring, to dissolving completely, obtains mixing after pH regulator
Close solution.
Step 3, the mixed solution after pH regulator is put into temperature be 250 DEG C, pressure be anti-under conditions of 40MPa
Answer and still carries out hydration reaction 10h, obtain reacted mixed solution.
Step 4, after reacted mixed solution is cooled to room temperature, obtains by circulating water type multiplex vacuum pump filtered sample
To filter cake, washing and filtering abundant to filter cake deionized water, it is dried, obtains dry products.
Step 5, grinds dry products, obtains doped nano photocatalyst α-SnMoO4。
Again as it is shown in figure 1, the doped nano photocatalyst α-SnMoO of the present embodiment4At the diffraction that the angle of diffraction is 27.6 °
The diffracted intensity that peak is corresponding is the strongest.
Fig. 2 (a) is doped nano photocatalyst α-SnMoO in embodiments of the invention four4Scanning electron microscope image.
As shown in Fig. 2 (a), doped nano photocatalyst α-SnMoO4Also aggregating state is become.
Embodiment four
The preparation method of the doped nano photocatalyst of the present embodiment comprises the following steps:
Step one, weighs 0.04mol (13.1940g) sodium tungstate (Na2WO4·2H2O), dissolved in 200ml deionization
In water, stirring, to dissolving completely, obtains the sodium tungstate solution that concentration is 0.2mol/L；And weigh 0.04mol (9.6780g) molybdic acid
Sodium (Na2MoO4·2H2O), dissolved in 200ml deionized water, stirring is to dissolving completely, and obtaining concentration is 0.2mol/L
Sodium molybdate solution；Take 0.2mol/L sodium tungstate solution 20ml and add deionized water 20ml and obtain mixed solution.
Step 2, weighs the stannous chloride (SnCl of 0.004mol (0.9026g)2·2H2O) solid, adds to above-mentioned mixing
In solution, stirring mixing under room temperature, regulate pH=10 with sodium hydroxide solution, stirring is to dissolving completely, after obtaining pH regulator
Mixed solution.
Step 3, the mixed solution after pH regulator is put into temperature be 300 DEG C, pressure be anti-under conditions of 50MPa
Answer and still carries out hydration reaction 12h, obtain reacted mixed solution.
Step 4, after reacted mixed solution is cooled to room temperature, obtains by circulating water type multiplex vacuum pump filtered sample
To filter cake, washing and filtering abundant to filter cake deionized water, it is dried, obtains dry products.
Step 5, grinds dry products, obtains doped nano photocatalyst α-SnWO4。
Degradation experiment
With methylene blue as target contaminant, under excited by visible light, it is separately added into embodiment one to embodiment four preparation
The doped nano photocatalyst SnW obtained(1-x)MoxO4(0≤X≤1)。
Fig. 3 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4Absorption Asia under dark condition
Methyl blue absorption-time graph.
As it is shown on figure 3, when W:Mo atomic molar ratio is during for 4:6, doped nano photocatalyst SnW0.4Mo0.6O4In dark
Under the conditions of absorbability the strongest.
Fig. 4 is doped nano photocatalyst SnW in embodiments of the invention(1-x)MoxO4Under the conditions of radiation of visible light
To methylene blue degraded-time graph.
As shown in Figure 4, when W:Mo atomic molar ratio is during for 7:3, doped nano photocatalyst SnW0.7Mo0.3O4To methylene
The degradation effect of base indigo plant is best, and it possesses high visible light catalytic activity.
Embodiment effect and effect
Embodiment one to embodiment four provides a kind of doped nano photocatalyst, preparation method, embodiment one to reality
Execute the doped nano photocatalyst SnW that example four prepares(1-x)MoxO4Environmental protection, composition are simple, the most under visible light
There is highlight catalytic active, and there is strong physical absorption performance.
Sodium tungstate is mixed by the preparation method of the doped nano photocatalyst of embodiment one to embodiment four with sodium molybdate,
And add stannous chloride, under high-temperature and high-pressure conditions, carry out hydration reaction, then by reacted mixed solution is filtered, washes
Wash, be dried to obtain dry products, finally dry products is ground, obtain doped nano photocatalyst, this preparation method
Simple, low cost, and environmentally safe, it is adaptable to industrial applications.
The application of the doped nano photocatalyst of embodiment one to embodiment four is by photocatalyst SnW(1-x)MoxO4Can
See catalytic degradation methylene blue under the exciting of light, and under dark condition, adsorb methylene, photocatalyst SnW(1-x)MoxO4Catalysis
Degradation efficiency is high, high adsorption capacity.
Above example is only the basic explanation under present inventive concept, does not limits the invention.And according to the present invention
Any equivalent transformation of being made of technical scheme, belong to protection scope of the present invention.
Claims (10)
1. the preparation method of a doped nano photocatalyst, it is characterised in that comprise the following steps:
Step one, weighs sodium tungstate and sodium molybdate and is dissolved in deionized water, and stirring, to dissolving completely, obtains mixed solution；
Step 2, adds stannous chloride to described mixed solution, with acid or alkali regulation pH=3-10 after stirring, obtains pH and adjusts
Mixed solution after joint；
Step 3, carries out hydro-thermal anti-in the reactor under high-temperature and high-pressure conditions by the mixed solution after pH regulator in step 2
Should, obtain reacted mixed solution；
Step 4, after the reacted mixed solution obtained until step 3 is cooled to room temperature, by described reacted mixed solution
It is filtrated to get filter cake, to described Cake Wash, is dried, obtains dry products；
Step 5, grinds described dry products, obtains described doped nano photocatalyst.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step one, the preparation method of described mixed solution includes following sub-step:
Sub-step one, weighs described sodium tungstate and sodium molybdate respectively and is dissolved in deionized water, and stirring is complete to dissolving, difference
Obtain described sodium tungstate solution and described sodium molybdate solution；
Sub-step two, is mixed and added into deionized water by described sodium tungstate solution and described sodium molybdate solution, obtains described mixing
Solution.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step one, in described mixed solution, W:Mo atomic molar is than for 0:10～10:0.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step 2, described acid is salpeter solution, and described alkali is sodium hydroxide solution.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step 2, after stirring, regulate pH=3.5-4.5 with described sour or described alkali.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step 3, described high-temperature and high-pressure conditions is temperature 100～300 DEG C, pressure 20～50MPa.
The preparation method of doped nano photocatalyst the most according to claim 1, it is characterised in that:
Wherein, in described step 3, the time of described hydration reaction is 6～12h.
8. a doped nano photocatalyst, by the doped nano photocatalyst described in any one in claim 1～7
Preparation method prepare, it is characterised in that:
The chemical formula of described doped nano photocatalyst is SnW(1-x)MoxO4,
Wherein X is in the range of 0≤X≤1, and the quantivalence of Mo is+6 valencys.
9. doped nano photocatalyst application in catalytic degradation organic pollution as claimed in claim 8.
10., according to the application in catalytic degradation organic pollution of the doped nano photocatalyst described in right 9, its feature exists
In:
Wherein, described organic pollution is methylene blue.
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Citations (3)
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| CN101690891A (en) * | 2009-09-25 | 2010-04-07 | 南京大学 | Synthetic method of visible light catalyst SnWO4 |
| CN101745381A (en) * | 2009-10-27 | 2010-06-23 | 南京大学 | Hydrothermal method for synthesizing visible light catalyst SnWO4 |
| WO2012031645A1 (en) * | 2010-09-07 | 2012-03-15 | Karlsruher Institut Für Technologie (Kit) | Tin tungstate-based photocatalyst and production thereof |
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| CN101690891A (en) * | 2009-09-25 | 2010-04-07 | 南京大学 | Synthetic method of visible light catalyst SnWO4 |
| CN101745381A (en) * | 2009-10-27 | 2010-06-23 | 南京大学 | Hydrothermal method for synthesizing visible light catalyst SnWO4 |
| WO2012031645A1 (en) * | 2010-09-07 | 2012-03-15 | Karlsruher Institut Für Technologie (Kit) | Tin tungstate-based photocatalyst and production thereof |
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