CN108704638A - A kind of silk ball-shaped Bi2WO6Nano material and its preparation method and application - Google Patents
A kind of silk ball-shaped Bi2WO6Nano material and its preparation method and application Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002086 nanomaterial Substances 0.000 claims abstract description 41
- 238000006731 degradation reaction Methods 0.000 claims abstract description 27
- 230000015556 catabolic process Effects 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 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 18
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 18
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 18
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- WPZFLQRLSGVIAA-UHFFFAOYSA-N sodium tungstate dihydrate Chemical compound O.O.[Na+].[Na+].[O-][W]([O-])(=O)=O WPZFLQRLSGVIAA-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002245 particle Substances 0.000 claims abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 3
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 claims abstract description 3
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract 2
- 238000012805 post-processing Methods 0.000 claims abstract 2
- 239000000243 solution Substances 0.000 claims description 14
- 238000013019 agitation Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 7
- 230000036571 hydration Effects 0.000 claims description 3
- 238000006703 hydration reaction Methods 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 2
- 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 claims 2
- BDJYZEWQEALFKK-UHFFFAOYSA-N bismuth;hydrate Chemical compound O.[Bi] BDJYZEWQEALFKK-UHFFFAOYSA-N 0.000 claims 2
- 229910052708 sodium Inorganic materials 0.000 claims 2
- 239000011734 sodium Substances 0.000 claims 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims 2
- 229910052721 tungsten Inorganic materials 0.000 claims 2
- 239000010937 tungsten Substances 0.000 claims 2
- 239000004698 Polyethylene Substances 0.000 claims 1
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 150000004040 pyrrolidinones Chemical class 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 230000003197 catalytic effect Effects 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract 1
- 238000006555 catalytic reaction Methods 0.000 description 7
- 206010001497 Agitation Diseases 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 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 description 3
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 238000003911 water pollution Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 230000012010 growth Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000005909 ethyl alcohol group Chemical group 0.000 description 1
- 230000007773 growth pattern Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 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 1
- 238000002156 mixing Methods 0.000 description 1
- 150000005181 nitrobenzenes Chemical class 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of silk ball-shaped Bi2WO6Nano material, using five nitric hydrate bismuths and Disodium tungstate (Na2WO4) dihydrate as raw material, using surfactant polyvinylpyrrolidone(PVP)As the hot method synthesis of structure directing agent secondary solvent, through alcohol, water washing, dry obtained silk ball-shaped Bi after reaction2WO6Nano material, the Bi2WO6The microscopic appearance of nano material is silk ball-shaped, 600 ~ 1100 nm of particle size.Preparation method includes the following steps:1)The preparation of pre-reaction material;2)Silk ball-shaped Bi2WO6The preparation of nano material;3)Silk ball-shaped Bi2WO6The post-processing of nano material.As the application of photocatalytic degradation methylene blue catalyst, methylene blue degradation is catalyzed under the conditions of simulated visible light, degradation rate is up to 95 ~ 99% in 120min.The present invention prepares material novelty, and simple for process, catalytic degradation activity is high, therefore has broad application prospects in catalytic degradation, environmental protection etc..
Description
Technical field
The present invention relates to photocatalysis fields, and in particular to a kind of silk ball-shaped Bi2WO6It nano material and preparation method thereof and answers
With.
Background technology
With the development of industry, environmental pollution especially water pollution is increasingly severe, and water pollution mostlys come from dyeing
It is remaining in the COD concentration and the more benzene ring compounds of a large amount of aromatic series, pesticide of the superelevation discharged in technique and paper-making industry to have
Machine chlorine and nitrobenzene class pollutant in organophosphor, pharmaceuticals industry and hospital wastewater, the alkyl chloride hydro carbons generated in petroleum refining
And the waste water etc. containing heavy metal generated in inorganic chemical production.Their serious pollutions and murder by poisoning environment, if depositing for a long time
Serious pollution will be caused to entire ecology, the health even life of the mankind can be caused greatly in biological chain
Harm.It cannot completely degrade using traditional method, such as general chemical method, Physical and bioanalysis and administer these pollutions
Object, and be also faced with many problems during the treatment, such as secondary pollution, cost are big etc., therefore seek a kind of honest and clean
The method of valence efficient process waste water is particularly necessary.
Therefore, novel photochemical catalyst developmental research is particularly important.Bi2WO6For perovskite layer structure, contain in molecule
WO6Octahedral structure lamella and Bi2O2Layer.With TiO2It compares, Bi2WO6Energy gap is relatively narrow, only 2.7eV.Therefore, Bi2WO6It can
Carry out degradation of dye to effectively utilize big sunlight energy, is a more promising photochemical catalyst.The pattern of photochemical catalyst is not
The adsorption ability to pollutant is only affected, but also affects the utilization rate to light, regulates and controls answering for photo-generate electron-hole
It closes, to influence photocatalytic activity.Therefore, Bi2WO6The microscopic appearance regulation and control of photochemical catalyst are early to have become photocatalysis research field
One of emphasis.Surfactant plays the role of the regulation and control of microscopic appearance prodigious.
Wu etc. adds PVP, and the photochemical catalyst of nido structure is successfully prepared using hydro-thermal method, and this nido configuration is by more
Layer nanometer sheet rule arrangement assembling and formed.For being catalyzed 100ml, 1.0*10-5When M rhodamine Bs, it is seen that illumination 6 is small
When after rhodamine B degradation 95%.(The Journal of Physical Chemistry C, 2007, 111(34),
12866-12871)。
Invention content
The object of the present invention is to provide a kind of silk ball-shaped Bi2WO6Nano material and its preparation method and application, with five hydrations
Bismuth nitrate and Disodium tungstate (Na2WO4) dihydrate are raw material, and playing the role of structure directing agent using PVP makes five nitric hydrate bismuths and two be hydrated
Sodium tungstate is forming Bi2WO6When crystal, growth pattern be it is outside reunite with embracing be built up by sheet spherical, eventually form silk ball
Type Bi2WO6Nano material.To obtain stable structure and with high specific surface area material.Effectively improve catalysis dyestuff degradation
Performance, solve current water pollution problems.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention is:
A kind of silk ball-shaped Bi2WO6Nano material is lived using five nitric hydrate bismuths and Disodium tungstate (Na2WO4) dihydrate as raw material using surface
Property agent polyvinylpyrrolidone(PVP)It is done through alcohol, water washing after reaction as the hot method synthesis of structure directing agent secondary solvent
Dry obtained silk ball-shaped Bi2WO6Nano material, the Bi2WO6The microscopic appearance of nano material be silk ball-shaped, particle size 600 ~
1100 nm。
Silk ball-shaped Bi2WO6The preparation method of nano material, includes the following steps:
Step 1)The preparation of pre-reaction material:Magnetic agitation in distilled water is added in five nitric hydrate bismuths and obtains five muddy hydrations
Bismuth nitrate solution, then magnetic agitation in absolute ethyl alcohol is added in Disodium tungstate (Na2WO4) dihydrate and structure directing agent PVP and obtains muddy mix
Solution is closed, while the ratio between amount for meeting five nitric hydrate bismuths, Disodium tungstate (Na2WO4) dihydrate and PVP substances is (1 ~ 4):1:1, distilled water
Volume ratio with absolute ethyl alcohol is 1:The relationship of (1 ~ 3), by above two solution magnetic agitation 1-2h at ambient temperature, fully
It is mixed to get pre-reaction material.
Step 2)Silk ball-shaped Bi2WO6The preparation of nano material, by step 1)Pre-reaction material be packed into reaction kettle be placed in 160
~ 200 DEG C of baking ovens react 2 ~ 4 d.
Step 3)After reaction, control baking oven is down to room temperature, 2 ~ 4 d of stewing process, filtration product with 5 ~ 10 DEG C/min
It is washed respectively 1 ~ 5 time through distilled water and absolute ethyl alcohol again, is placed in 50 ~ 100 DEG C of 6 ~ 12 h of oven drying, obtains silk ball-shaped Bi2WO6
Nano material.
Silk ball-shaped Bi2WO6Application of micron is in the methylene blue solution of a concentration of 10 mg/L of 100 mL of catalytic degradation
When methylenum careuleum, the degradation rate of methylene is up to 96.43% after 120min.Its performance is compared with the prior art, after visible light was according to 6 hours
Rhodamine B degradation 95% increases significantly.
The technique effect that the present invention has is confirmed by following experiment:
X-ray powder diffraction is analyzed:Silk ball-shaped Bi of the present invention2WO6Nano material X-ray powder diffraction analysis be
It is carried out on Bruker D8 Advance type x-ray diffractometers.Experiment condition is:Voltage is 40 kV, and electric current is 40 mA, scanning
Ranging from 20 ~ 80 °.In 2 θ=28 o, 33 o, 47 o, 56o, 58 o, 69.0 o, 76 o, 78 oAll there is obvious diffraction maximum,
It corresponds respectively to(113),(200),(220)(313),(226),(333),(260)The diffraction maximum of crystal face.And these diffraction maximums with
The Bi of perovskite layer structure2WO6PDF standard cards(JCPDS NO.73-1126)It coincide.
Catalyst is catalyzed methylene blue degradation experiment under visible light illumination:The present invention utilizes silk ball-shaped Bi2WO6Nanometer material
Catalysis methylene blue degradation experiment carries out material as follows under visible light illumination:1)By 10 mg silk ball-shapeds Bi2WO6Nanometer
Material is added in the methylene blue solution of a concentration of 10 mg/L of 100 mL, and mixture stirs under the conditions of dark situation
60min reaches suction-desorption equilibrium;2)Mixed liquor is put into self-control photo catalysis reactor, with 150W xenon lamp irradiating samples;3)
Methylene blue solution absorbance change is surveyed after 20min takes supernatant liquor to filter.Experimental results show that the present invention is made
Standby silk ball-shaped Bi2WO6Nano material shows very high catalytic degradation methylene blue activity under simulated visible light irradiation,
Degradation rate is up to 95 ~ 99% in 120 min.
The present invention is successfully synthesized by regulating and controlling reaction temperature using PVP as structure directing agent assisted hydrothermal synthesis method
Go out the silk ball-shaped Bi of silk ball-shaped2WO6Nano material, in the methylene blue solution methylene of catalysis a concentration of 10 mg/L of 100 mL
The degradation rate of methylene is up to 96.43% after Lan Shi, 120min.Its performance is compared with the prior art, the Luo Dan after visible light was according to 6 hours
Bright B degradations 95% increase significantly.
The present invention compared with the existing technology, has the following advantages:
One, the present invention utilizes solvent structure, and experimental implementation is simple, and yield is up to 85 ~ 90%;
Two, patent of the present invention synthesizes silk ball-shaped Bi by regulating and controlling reaction condition2WO6Nano material, crystal growth are to roll into a ball outward
Poly- embrace is built up spherical by sheet, is conducive to increase Bi in this way2WO6Surface area promotes light-catalyzed reaction, improves photocatalysis
The performance of reaction;
Three, for the present invention when being catalyzed methylene blue degradation, at ambient temperature, 120min degradation rates are up to 95 ~ 99%.
Therefore, the present invention has more excellent catalytic efficiency compared with prior art, has wide answer in catalytic field
Use foreground.
Description of the drawings:
Fig. 1 is silk ball-shaped Bi in embodiment2WO6Nano material X-ray powder diffraction collection;
Fig. 2 is silk ball-shaped Bi in embodiment2WO6Nano material SEM spectrum;
Fig. 3 is the Bi that structure directing agent PVP is added without in embodiment2WO6Nano material SEM spectrum;
Fig. 4 is silk ball-shaped Bi prepared in embodiment2WO6Nano material is catalyzed sub- catalysis methyl blue drop under visible light illumination
Solution preocess changes over time curve graph;
Fig. 5 is silk ball-shaped Bi prepared in embodiment2WO6Nano material is catalyzed methylene blue degradation speed under visible light illumination
Rate figure.
Specific implementation mode
The present invention is described in further detail the content of present invention by embodiment, in conjunction with Figure of description, but is not pair
The limitation of the present invention.
A kind of silk ball-shaped Bi of embodiment2WO6Preparation method of nano material:
Step 1)The preparation of pre-reaction material weighs 485.07 mg, five nitric hydrate bismuths and 10 ml distilled water magnetic agitations is added
Muddy bismuth nitrate solution is obtained, then weighs 329.85 mg Disodium tungstate (Na2WO4) dihydrates and 1g PVP are added in 15ml absolute ethyl alcohols
Magnetic agitation obtains muddy mixed solution solution, and then magnetic agitation 1.5h is obtained the mixing of above two solution at ambient temperature
To pre-reaction material.
Step 2)Silk ball-shaped Bi2WO6The preparation of nano material, by step(1)Pre-reaction material be put into reaction kettle and be placed in
180 DEG C of baking ovens react 3d.
Step 3)After reaction, control baking oven is down to room temperature, 3 d of stewing process with 5 DEG C/min, and filtration product passes through again
Distilled water and absolute ethyl alcohol wash 4 times respectively, are placed in 80 DEG C of oven drying 8h, obtain flaxen silk ball-shaped Bi2WO6Nanometer material
Material.
Silk ball-shaped Bi in embodiment2WO6Nano material phase structure is tested, and the results are shown in Figure 1, diffraction maximum and calcium titanium ore bed
The Bi of shape structure2WO6PDF standard cards(JCPDS NO.73-1126)It coincide.And cutting edge of a knife or a sword shape is sharp, without other miscellaneous peaks
Illustrate prepared silk ball-shaped Bi2WO6Nano material is pure phase.
Silk ball-shaped Bi in embodiment2WO6Test results are shown in figure 2 for nano material SEM spectrum, is by many regular morphologies
Spherical little particle, that is, lace ball like silk ball shape form, these particle sizes are in 600-1100nm.Soilless sticking phenomenon, point
The degree of dissipating is good.Illustrate the crystal growth of the sample be it is outside reunite with embracing be built up by sheet spherical, be conducive to increase in this way
Bi2WO6Surface area promotes light-catalyzed reaction, improves the performance of light-catalyzed reaction.
In order to prove that PVP has the function of structure directing agent, it is prepared for being added without the Bi of structure directing agent PVP2WO6Nanometer
Material, the not specified step of preparation method and the above-mentioned silk ball-shaped Bi of the present embodiment2WO6The preparation method phase of nano material
Together.
The difference is that:The step 1 does not add surfactant polyvinylpyrrolidone(PVP).
It is added without the Bi of structure directing agent PVP2WO6Nano material SEM spectrum is as shown in figure 3, it is by many sheets
Structure composition is reunited than more serious.Show that silk ball-shaped Bi can not be formed by being not added with structure directing agent PVP2WO6Nano material.
Silk ball-shaped Bi in embodiment2WO6Nano material is polished to be used for catalytic degradation methylene blue, and degradation process is at any time
Between change curve as shown in figure 4, the characteristic absorption peak of methylene blue in 663 nm, as time increases, the suction of methylene blue
Luminosity continuously decreases, and characteristic absorption peak red shift, shows gradually being degraded for methylene blue, degradation rate is up to after 120 min
96.43%。
Silk ball-shaped Bi in embodiment2WO6Nano material is catalyzed methylene blue degradation rate curve such as under visible light illumination
Shown in Fig. 5, the linear reduction of degradation rate in 60min illustrates that the present invention has faster degradation rate.
Claims (6)
1. a kind of silk ball-shaped Bi2WO6Nano material, it is characterised in that:Using five nitric hydrate bismuths and Disodium tungstate (Na2WO4) dihydrate as former material
Material, using surfactant polyvinylpyrrolidone(PVP)As the hot method synthesis of structure directing agent secondary solvent, through wine after reaction
Essence, water washing, dry obtained silk ball-shaped Bi2WO6Nano material, the Bi2WO6The microscopic appearance of nano material is silk ball-shaped,
600 ~ 1100 nm of particle size.
2. silk ball-shaped Bi according to claim 12WO6The preparation method of nano material, it is characterised in that including following step
Suddenly:
Step 1)The preparation of pre-reaction material, by five nitric hydrate bismuth of raw material, Disodium tungstate (Na2WO4) dihydrate and surfactant polyethylene
Pre-reaction material is prepared as structure directing agent in pyrrolidones under certain condition;
Step 2)Silk ball-shaped Bi2WO6The preparation of nano material, by step 1)Gained pre-reaction material reacts under certain condition;
Step 3)Silk ball-shaped Bi2WO6The post-processing of nano material, by step 2)Gained reaction product is filtered, is washed under certain condition
It washs, dry, obtain silk ball-shaped Bi2WO6Nano material.
3. preparation method according to claim 2, it is characterised in that:The step 1)The preparation condition of pre-reaction material
For magnetic agitation in distilled water is added in five nitric hydrate bismuths and obtains five muddy nitric hydrate bismuth solution, then tungsten is hydrated by two
Sour sodium and PVP are added magnetic agitation in absolute ethyl alcohol and obtain muddy mixed solution, to meet five nitric hydrate bismuths, two hydration tungsten
The ratio between amount of sour sodium and PVP substances is (1 ~ 4):1:1, the volume ratio of distilled water and absolute ethyl alcohol is 1:The relationship of (1 ~ 3), will
Above two solution magnetic agitation 1-2 h at ambient temperature, are sufficiently mixed to obtain pre-reaction material.
4. preparation method according to claim 2, it is characterised in that:The step 2)Reaction condition be reaction temperature
It it is 160 ~ 200 DEG C, the reaction time is 2 ~ 4d, and after reaction, control baking oven is down to room temperature with 5 ~ 10 DEG C/min.
5. preparation method according to claim 2, it is characterised in that:The step 3)The condition be filtered, washed, dried
First to stand 2 ~ 4 d, then filter, dry 6 ~ 12 h under the conditions of 50 ~ 100 DEG C.
6. silk ball-shaped Bi according to claim 12WO6Nano material is answered as photocatalytic degradation methylene blue catalyst
With, it is characterised in that:Methylene blue degradation is catalyzed under the conditions of simulated visible light, degradation rate is up to 95 ~ 99% in 120 min.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810525142.8A CN108704638A (en) | 2018-05-28 | 2018-05-28 | A kind of silk ball-shaped Bi2WO6Nano material and its preparation method and application |
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CN110711591A (en) * | 2019-07-12 | 2020-01-21 | 盐城工学院 | Preparation method and application of catalyst for photocatalytic degradation of VOCs (volatile organic compounds) |
CN112206767A (en) * | 2020-08-31 | 2021-01-12 | 盐城工学院 | Morphological structure regulation method of bismuth tungstate, product and application thereof |
CN113231099A (en) * | 2021-05-21 | 2021-08-10 | 吉林大学 | Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst |
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Cited By (4)
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CN110711591A (en) * | 2019-07-12 | 2020-01-21 | 盐城工学院 | Preparation method and application of catalyst for photocatalytic degradation of VOCs (volatile organic compounds) |
CN112206767A (en) * | 2020-08-31 | 2021-01-12 | 盐城工学院 | Morphological structure regulation method of bismuth tungstate, product and application thereof |
CN113231099A (en) * | 2021-05-21 | 2021-08-10 | 吉林大学 | Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst |
CN113231099B (en) * | 2021-05-21 | 2022-05-17 | 吉林大学 | Preparation and application of Z-type polypyrrole-bismuth tungstate photocatalyst |
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