CN107983336A - A kind of praseodymium doped bismuth tungstate light urges agent and preparation method thereof - Google Patents
A kind of praseodymium doped bismuth tungstate light urges agent and preparation method thereof Download PDFInfo
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- CN107983336A CN107983336A CN201711305728.5A CN201711305728A CN107983336A CN 107983336 A CN107983336 A CN 107983336A CN 201711305728 A CN201711305728 A CN 201711305728A CN 107983336 A CN107983336 A CN 107983336A
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 44
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 44
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052777 Praseodymium Inorganic materials 0.000 title claims abstract description 41
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000243 solution Substances 0.000 claims abstract description 53
- 241000446313 Lamella Species 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 10
- 239000002245 particle Substances 0.000 claims abstract description 9
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 239000003643 water by type Substances 0.000 claims description 14
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 12
- 229910017604 nitric acid Inorganic materials 0.000 claims description 12
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- 229910020350 Na2WO4 Inorganic materials 0.000 claims description 7
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 7
- 229910002828 Pr(NO3)3·6H2O Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 3
- 239000004094 surface-active agent Substances 0.000 abstract description 7
- 239000006185 dispersion Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 3
- YWECOPREQNXXBZ-UHFFFAOYSA-N praseodymium(3+);trinitrate Chemical compound [Pr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O YWECOPREQNXXBZ-UHFFFAOYSA-N 0.000 abstract description 2
- 206010013786 Dry skin Diseases 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 230000003321 amplification Effects 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 6
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 6
- 229940012189 methyl orange Drugs 0.000 description 6
- 238000003199 nucleic acid amplification method Methods 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 238000006555 catalytic reaction Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000007146 photocatalysis 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
- 150000001875 compounds Chemical class 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- 229910052708 sodium Inorganic materials 0.000 description 4
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 4
- 229910052721 tungsten Inorganic materials 0.000 description 4
- 239000010937 tungsten Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical compound [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 241001198704 Aurivillius Species 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 150000003114 praseodymium compounds Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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
- 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
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
-
- 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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
-
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of praseodymium doped bismuth tungstate light to urge agent and preparation method thereof.It accumulates the three-dimensional flower-shaped structure to be formed for lamella, and the thickness of lamella is 50 80nm, and a diameter of 2 4um of flower-shaped particle, its crystal structure is orthorhombic phase, and its preparation method seals and stirs, obtain bismuth nitrate acid solution for bismuth nitrate is dissolved in salpeter solution；Sodium tungstate solution is added dropwise in bismuth nitrate acid solution, seals and stirs to obtain mixed solution, then praseodymium nitrate is dissolved in mixed solution, seals and stirs；Resulting solution is transferred in autoclave, in 120~200 DEG C of insulations, cooled to room temperature, then filters and centrifuge, after washes of absolute alcohol, in 60~80 DEG C of dryings.Cost of the present invention is low, and the uniformity of obtained product is good, and without extra addition surfactant, obtained praseodymium doped bismuth tungstate product accumulates the three-dimensional flower-shaped structure to be formed for lamella, good dispersion and has visible light catalytic effect.
Description
Technical field
The present invention relates to a kind of praseodymium doped bismuth tungstate light to urge agent and preparation method thereof, belongs to photocatalysis technology field.
Background technology
Bismuth tungstate Bi2WO6It is a kind of Aurivillius type oxides with layer structure, the accumulation of its atomic layer is compact easily
In the lamellar structure of formation rule.Its forbidden band is relatively narrow, about 2.7eV, can absorb some visible light and is excited, and is dropped in pollutant
The fields such as solution, new energy development have higher application value.And bismuth tungstate catalysis material stability is good, has no toxic side effect,
It is a kind of environmentally friendly material, receives extensive concern in field of photocatalytic material in recent years.However, Bi2WO6It is visible light-responded
Narrow range, photo-generate electron-hole is easily compound, photo-generated carrier short life, therefore photocatalysis efficiency and the TiO of mature2
Etc. system compared to still there is certain gap.People by using catalyst it is compound, addition surfactant the methods of change its pattern,
Particle size, improves Bi to a certain extent2WO6The catalytic capability of photocatalytic system.But compound method adds catalysis
Agent production cost, the method for adding surfactant are difficult to control the final pattern of product, thus develop a kind of preparation process it is simple,
The bismuth tungstate nano-powder of microstructure even structure, good dispersion, improves its photocatalysis efficiency, to promoting bismuth tungstate to be urged in light
The long term growth in change field has positive effect.
The content of the invention
In view of this, it is an object of the invention to provide one kind to utilize bismuth nitrate, sodium tungstate and praseodymium nitrate raw material, prepares
Journey is simple, and preparation process need not add surfactant, without other compound species catalyst, obtains even structure, dispersiveness
Good rear-earth-doped Bi2WO6Photochemical catalyst, products obtained therefrom have good crystallinity and visible light catalysis activity.
For achieving the above object, a kind of praseodymium doped bismuth tungstate light of the invention urges agent, it accumulates what is formed for lamella
Three-dimensional flower-shaped structure composition, the thickness of lamella is 50-80nm, and a diameter of 2-4um of flower-shaped particle, its crystal structure is orthogonal
Phase, praseodymium doped concentration are 0.5~10%.
A kind of praseodymium doped bismuth tungstate light urges the preparation method of agent, it is following steps：
(1) 200~500 μ L nitric acid are dissolved in 20~60mL deionized waters, seal and stir 10~30min and obtain nitric acid
Solution, by 0.5~2.0 gram of Bi (NO3)3·5H2O is dissolved in salpeter solution, is sealed and is stirred 10~30min, obtains nitric acid bismuthic acid
Property solution；
(2) by 0.5~2.0 gram of Na2WO4·2H2O is dissolved in 20~60mL deionized waters, is stirred 10~30min, is obtained tungsten
Acid sodium solution, sodium tungstate solution is added dropwise in bismuth nitrate acid solution, seal and stir 10~30min obtain mixing it is molten
Liquid, then by 0.01~0.03 gram of Pr (NO3)3·6H2O is dissolved in mixed solution, is sealed and is stirred 10~30min；
(3) step (2) resulting solution is transferred in autoclave, 12~24h is kept the temperature at 120~200 DEG C, it is naturally cold
But to room temperature, then filter and centrifuge, then with washes of absolute alcohol 3~5 times, in 60~80 DEG C of dry 6~12h.
The present invention synthesizes a kind of preparation method of the flower-shaped praseodymium doped bismuth tungstate formed with lamella accumulation using hydro-thermal method,
Preparation process is without surfactant, and prepared bismuth tungstate has good crystallinity and visible light catalysis activity.Utilize
Rare earth element Pr is adulterated, and on the premise of bismuth tungstate catalyst morphology is not influenced, without in addition addition surfactant, can be obtained
Even structure, good dispersion and the bismuth tungstate with visible light catalytic effect.This method also has the cost low, reproducible excellent
Gesture.
Compared with prior art, the present invention has the advantages that：Cost of the present invention is low, the uniformity of product is good, system
For standby process without additionally adding surfactant, the bismuth tungstate photocatalyst of the praseodymium doped finally obtained accumulates what is formed for lamella
Flower-like structure, and good dispersion, there is photocatalysis effect.
Brief description of the drawings
Fig. 1 is X-ray diffraction (XRD) figure of the praseodymium doped wolframic acid bismuth catalyst prepared by embodiment 1,2, and wherein a is real
X-ray diffraction (XRD) figure of the praseodymium doped bismuth tungstate prepared by example 1 is applied, b is the X of the praseodymium doped bismuth tungstate prepared by embodiment 2
X ray diffraction (XRD) figure.
Fig. 2 is the stereoscan photograph of the praseodymium doped bismuth tungstate prepared by the embodiment of the present invention 1, and wherein a is amplification 5000
Stereoscan photograph again, b are the stereoscan photographs of 20000 times of amplification.
Fig. 3 is the energy spectrum diagram of the praseodymium doped bismuth tungstate prepared by embodiment 1.
Fig. 4 is the stereoscan photograph of praseodymium doped bismuth tungstate prepared by embodiment 2, and wherein a is the scanning of 5000 times of amplification
Electromicroscopic photograph, b are the stereoscan photographs of 20000 times of amplification.
Fig. 5 is to be catalyzed methyl orange degradation under the praseodymium doped bismuth tungstate visible light conditions prepared by the embodiment of the present invention 1,2
Curve map, wherein a are the degradation curve figures of embodiment 1, and b is the degradation curve figure of embodiment 2.
Embodiment
The present invention is described in further detail with reference to the accompanying drawings and examples.
A kind of praseodymium doped bismuth tungstate light of the present invention urges agent, it accumulates the three-dimensional flower-shaped structure to be formed for lamella, lamella
Thickness is 50-80nm, a diameter of 2-4um of flower-shaped particle, its crystal structure is orthorhombic phase, and praseodymium doped concentration is 0.5~10%.
A kind of praseodymium doped bismuth tungstate light urges the preparation method of agent, it is following steps：
(1) 200~500 μ L nitric acid are dissolved in 20~60mL deionized waters, seal and stir 10~30min and obtain nitric acid
Solution, by 0.5~2.0 gram of Bi (NO3)3·5H2O is dissolved in salpeter solution, is sealed and is stirred 10~30min, obtains nitric acid bismuthic acid
Property solution；
(2) by 0.5~2.0 gram of Na2WO4·2H2O is dissolved in 20~60mL deionized waters, is stirred 10~30min, is obtained tungsten
Acid sodium solution, sodium tungstate solution is added dropwise in bismuth nitrate acid solution, seal and stir 10~30min obtain mixing it is molten
Liquid, then by 0.01~0.03 gram of Pr (NO3)3·6H2O is dissolved in mixed solution, is sealed and is stirred 10~30min；
(3) step (2) resulting solution is transferred in autoclave, 12~24h is kept the temperature at 120~200 DEG C, it is naturally cold
But to room temperature, then filter and centrifuge, then with washes of absolute alcohol 3~5 times, in 60~80 DEG C of dry 6~12h.
Embodiment 1
(1) 200 μ L nitric acid are dissolved in 30 ml deionized waters, seal and stir 30 minutes；
(2) by 1.0 grams of Bi (NO3)3·5H2O is dissolved in step (1) resulting solution, is sealed and is stirred 30 minutes；
(3) by 0.6 gram of Na2WO4·2H2O is dissolved in 30 ml deionized waters, is stirred 20 minutes；
(4) step (3) resulting solution is added dropwise in step (2) resulting solution, seals and stir 15 minutes；
(5) by 0.01 gram of Pr (NO3)3·6H2O is dissolved in step (4) resulting solution, is sealed and is stirred 30 minutes；
(6) step (5) resulting solution is transferred in autoclave, when 180 DEG C of insulations 12 are small, naturally cools to room
Temperature.
(7) reaction product filtered, centrifuged, washes of absolute alcohol 4 times, 60 DEG C it is dry 8 it is small when.
It is the XRD diagram for passing through dried praseodymium doped bismuth tungstate sample in the present embodiment as shown in Fig. 1 (a).Pass through contrast
PDF standard cards, it is found that the bismuth tungstate obtained by the present embodiment coincide with card number for the orthorhombic phase bismuth tungstate of No.39-0256.
And the diffraction maximum without praseodymium simple substance or praseodymium compound in figure, show that Pr ions enter BiNa2WO6Lattice.
Fig. 2 is the SEM figures for the praseodymium doped bismuth tungstate sample that the present embodiment obtains.From the figure, it can be seen that sample is by lamella
Structure is accumulated, and forms three-dimensional flower-shaped structure.It is 50-80nm wherein from the thickness of the amplification it can be seen from the figure that lamella of Fig. 2 (b),
A diameter of 2-4um of flower-shaped particle.
Fig. 3 is the energy spectrum analysis figure for the praseodymium doped bismuth tungstate sample that the present embodiment obtains.There are obvious Pr elements in figure
Peak, shows to contain Pr in the sample prepared by the present embodiment.
Embodiment 2
(1) 200 μ L nitric acid are dissolved in 30 ml deionized waters, seal and stir 30 minutes；
(2) by 1.0 grams of Bi (NO3)3·5H2O is dissolved in step (1) resulting solution, is sealed and is stirred 30 minutes；
(3) by 0.6 gram of Na2WO4·2H2O is dissolved in 30 ml deionized waters, is stirred 20 minutes；
(4) step (3) resulting solution is added dropwise in step (2) resulting solution, seals and stir 15 minutes；
(5) 0.02 gram of Pr (NO3) 36H2O is dissolved in step (4) resulting solution, seals and stir 30 minutes；
(6) step (5) resulting solution is transferred in autoclave, when 200 DEG C of insulations 12 are small, naturally cools to room
Temperature.
(7) reaction product filtered, centrifuged, washes of absolute alcohol 4 times, 60 DEG C it is dry 8 it is small when.
(8) 30mg samples are added into the quartz ampoule of the methyl orange solution for the 10mg/L for having 250ml.Stirred under dark condition
Mix 30 minutes and reach adsorption equilibrium.300W xenon lamps are opened, and are kept stirring, carry out visible light photocatalytic degradation.Every 20 points
Clock takes a solution, and centrifugation, separate, and tests the absorbance of supernatant.Catalyst is to the degradation rate of methyl orange according to the following formula
Calculate：
In formula, C, C0The absorbance of methyl orange before and after respectively degrading.
It is the XRD diagram for passing through dried praseodymium doped bismuth tungstate sample in the present embodiment as shown in Fig. 1 (b).Pass through contrast
PDF standard cards, it is found that the bismuth tungstate obtained by the present embodiment coincide with No.39-0256.And without praseodymium simple substance or praseodymium chemical combination in figure
The diffraction maximum of thing, shows that Pr ions enter bismuth tungstate lattice.
Fig. 4 is the SEM figures for the praseodymium doped bismuth tungstate sample that the present embodiment obtains.From the figure, it can be seen that sample is by lamella
Structure is accumulated, and forms three-dimensional flower-shaped structure.It is 50-80nm wherein from the thickness of the amplification it can be seen from the figure that lamella of Fig. 2 (b),
A diameter of 2-4um of flower-shaped particle.
Fig. 5 is the praseodymium doped bismuth tungstate obtained with embodiment 1,2, to the degradation curve of methyl orange under visible light conditions
Figure, under praseodymium doped bismuth tungstate photocatalysis, 2 it is small when after the degradation efficiency of methyl orange reach more than 90%, wherein embodiment 1
The praseodymium doped bismuth tungstate of acquisition reaches 95% to the degradation efficiency of methyl orange after 2 hours.Show prepared praseodymium doped wolframic acid
Bismuth has good visible light catalysis activity.
Embodiment 3
A kind of praseodymium doped bismuth tungstate light urges agent, it accumulates the three-dimensional flower-shaped structure composition to be formed, the thickness of lamella for lamella
For 55nm, a diameter of 2.5um of flower-shaped particle, its crystal structure is orthorhombic phase, and praseodymium doped concentration is 1.5%.
A kind of praseodymium doped bismuth tungstate light urges the preparation method of agent, it is following steps：
(1) 400 μ L nitric acid are dissolved in 40mL deionized waters, seal and stir 25min and obtain salpeter solution, by 1.5 grams
Bi (NO3) 35H2O is dissolved in salpeter solution, is sealed and is stirred 25min, obtains bismuth nitrate acid solution；
(2) by 1.5 grams of Na2WO4·2H2O is dissolved in 30mL deionized waters, is stirred 20min, sodium tungstate solution is obtained, by tungsten
Acid sodium solution is added dropwise in bismuth nitrate acid solution, is sealed and is stirred 20min and obtains mixed solution, then by 0.021 gram of Pr
(NO3)3·6H2O is dissolved in mixed solution, is sealed and is stirred 20min；
(3) step (2) resulting solution is transferred in autoclave, 180 DEG C keep the temperature 20h, cooled to room temperature,
Then filter and centrifuge, then with washes of absolute alcohol 4 times, in 70 DEG C of dry 10h.
Embodiment 4
A kind of praseodymium doped bismuth tungstate light urges agent, it accumulates the three-dimensional flower-shaped structure composition to be formed, the thickness of lamella for lamella
For 70nm, a diameter of 3.2um of flower-shaped particle, its crystal structure is orthorhombic phase, and praseodymium doped concentration is 5%.
A kind of praseodymium doped bismuth tungstate light urges the preparation method of agent, it is following steps：
(1) 400 μ L nitric acid are dissolved in 40mL deionized waters, seal and stir 20min and obtain salpeter solution, by 1.2 grams
Bi(NO3)3·5H2O is dissolved in salpeter solution, is sealed and is stirred 20min, obtains bismuth nitrate acid solution；
(2) by 1.3 grams of Na2WO4·2H2O is dissolved in 40mL deionized waters, is stirred 20min, sodium tungstate solution is obtained, by tungsten
Acid sodium solution is added dropwise in bismuth nitrate acid solution, is sealed and is stirred 20min and obtains mixed solution, then by 0.02 gram of Pr
(NO3)3·6H2O is dissolved in mixed solution, is sealed and is stirred 20min；
(3) step (2) resulting solution is transferred in autoclave, 180 DEG C keep the temperature 21h, cooled to room temperature,
Then filter and centrifuge, then with washes of absolute alcohol 5 times, in 72 DEG C of dry 10h.
Finally illustrate, the above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to compared with
The present invention is described in detail in good embodiment, it will be understood by those of ordinary skill in the art that, can be to the skill of the present invention
Art scheme technical scheme is modified or replaced equivalently, without departing from the objective and scope of technical solution of the present invention, it should all cover at this
Among the right of invention.
Claims (2)
1. a kind of praseodymium doped bismuth tungstate light urges agent, it is characterised in that it accumulates the three-dimensional flower-shaped structure to be formed for lamella, lamella
Thickness is 50-80nm, a diameter of 2-4um of flower-shaped particle, its crystal structure is orthorhombic phase, and praseodymium doped concentration is 0.5~10%.
2. a kind of praseodymium doped bismuth tungstate light urges the preparation method of agent, it is characterised in that is following steps：
(1) 200~500 μ L nitric acid are dissolved in 20~60mL deionized waters, seal and stir 10~30min to obtain nitric acid molten
Liquid, by 0.5~2.0 gram of Bi (NO3)3·5H2O is dissolved in salpeter solution, is sealed and is stirred 10~30min, obtains bismuth nitrate acidity
Solution；
(2) by 0.5~2.0 gram of Na2WO4·2H2O is dissolved in 20~60mL deionized waters, is stirred 10~30min, is obtained sodium tungstate
Solution, sodium tungstate solution is added dropwise in bismuth nitrate acid solution, is sealed and is stirred 10~30min and obtains mixed solution, then
By 0.01~0.03 gram of Pr (NO3)3·6H2O is dissolved in mixed solution, is sealed and is stirred 10~30min；
(3) step (2) resulting solution is transferred in autoclave, keeps the temperature 12~24h at 120~200 DEG C, naturally cool to
Room temperature, then filters and centrifuges, then with washes of absolute alcohol 3~5 times, in 60~80 DEG C of dry 6~12h.
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| CN113083287A (en) * | 2021-04-29 | 2021-07-09 | 沈阳工业大学 | Bismuth and bismuth tungstate composite powder with nano-particle stacked lamellar structure and preparation method thereof |
| CN114408973A (en) * | 2021-12-15 | 2022-04-29 | 深圳大学 | Nuclear radiation shielding material and preparation method thereof |
| CN114768792A (en) * | 2022-05-21 | 2022-07-22 | 李广强 | Purifying agent for sewage treatment and preparation method thereof |
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| CN111841529A (en) * | 2020-07-30 | 2020-10-30 | 陕西科技大学 | Rare earth doped flaky Tb/Bi2WO6Nano material and preparation method and application thereof |
| CN112007633A (en) * | 2020-09-15 | 2020-12-01 | 西北矿冶研究院 | La/Bi2WO6Preparation method and application of photocatalyst |
| CN113083287A (en) * | 2021-04-29 | 2021-07-09 | 沈阳工业大学 | Bismuth and bismuth tungstate composite powder with nano-particle stacked lamellar structure and preparation method thereof |
| CN113083287B (en) * | 2021-04-29 | 2023-09-19 | 沈阳工业大学 | Bismuth and bismuth tungstate composite powder with nano-particle stacking lamellar structure and preparation method thereof |
| CN114408973A (en) * | 2021-12-15 | 2022-04-29 | 深圳大学 | Nuclear radiation shielding material and preparation method thereof |
| CN114408973B (en) * | 2021-12-15 | 2023-11-17 | 深圳大学 | Nuclear radiation shielding material and preparation method thereof |
| CN114768792A (en) * | 2022-05-21 | 2022-07-22 | 李广强 | Purifying agent for sewage treatment and preparation method thereof |
| CN114768792B (en) * | 2022-05-21 | 2023-10-10 | 济宁市盈润环保助剂有限公司 | Purifying agent for sewage treatment and preparation method thereof |
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