CN107188234A - A kind of sheet Bi2WO6Preparation method - Google Patents
A kind of sheet Bi2WO6Preparation method Download PDFInfo
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- CN107188234A CN107188234A CN201710444141.6A CN201710444141A CN107188234A CN 107188234 A CN107188234 A CN 107188234A CN 201710444141 A CN201710444141 A CN 201710444141A CN 107188234 A CN107188234 A CN 107188234A
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- 238000000034 method Methods 0.000 title abstract description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 34
- 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 24
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- 230000004044 response Effects 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000052 vinegar Substances 0.000 claims description 8
- 235000021419 vinegar Nutrition 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 claims 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 claims 1
- 229910001950 potassium oxide Inorganic materials 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 239000000243 solution Substances 0.000 description 37
- 239000003643 water by type Substances 0.000 description 14
- 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 10
- 239000011734 sodium Substances 0.000 description 10
- 229910052708 sodium Inorganic materials 0.000 description 10
- -1 tungstate dihydrates Chemical class 0.000 description 10
- 239000002253 acid Substances 0.000 description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 5
- 239000007795 chemical reaction product Substances 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 238000009413 insulation Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 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 5
- 229940043267 rhodamine b Drugs 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-M Bicarbonate Chemical compound OC([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-M 0.000 description 1
- 229910004382 CaIn2O4 Inorganic materials 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000011858 nanopowder Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000008313 sensitization Effects 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of 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
- 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
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- 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
Abstract
The present invention relates to a kind of sheet Bi2WO6Preparation method, comprise the following steps：1) bismuth nitrate solution is added drop-wise in sodium tungstate solution；0.20~0.60mol/L of molar concentration of the bismuth nitrate solution, 0.10~0.30mol/L of molar concentration of the sodium tungstate solution；2) continue that potassium hydroxide solution is added dropwise, mix laggard water-filling thermal response, filter, cleaning obtains sheet Bi2WO6；0.10~2mol/L of molar concentration of the potassium hydroxide solution.The sheet Bi that this method is prepared2WO6Pattern it is good, size uniformity, and with excellent photocatalysis performance.
Description
Technical field
The present invention relates to Bi2WO6Synthesis field, and in particular to a kind of sheet Bi2WO6Preparation method.
Background technology
For many years, researcher is to TiO2The modification or sensitization of various approach have been carried out, has strengthened its response to visible ray, with
Improve its photocatalytic activity.However, due to TiO2The property of itself makes its modified in actual applications, still by very big limit
System.Therefore, researcher starts to visible light-responded Bi2WO6, InVO4, AgAlO2, CaIn2O4And BiVO4Deng novel photocatalysis
Agent is studied.
Bismuth tungstate possesses the WO of perovskite type structure6Octahedra and lamellar structure, Bi6s tracks can be miscellaneous with O2p tracks
Change and form new continuous valence band, new valence band location can effectively reduce the forbidden band of semiconductor on original valence band location
Width, makes compound have visible absorption.Kudo in 1999 etc. has found Bi2WO6Visible ray (>420nm) irradiate lower with light
Since catalytic activity, Bi2WO6It is wide concerned for the catalyst that novel visible is responded.
Microcosmic particle size, specific surface area, the separative efficiency of photo-generate electron-hole due to catalyst etc. can all influence to urge
The catalytic efficiency of agent.Bi is generally prepared using high-temperature roasting method in the prior art2WO6, but the particle diameter of gained sample is larger,
Specific surface area is smaller, pollutant in its table and absorption, cause its photocatalytic activity not high.
At present, sight is focused on Bi by researcher2WO6In the soft chemical method synthesis of material and its Morphological control, it is intended to pass through
Change synthesis condition, to regulate and control Bi2WO6Pattern, and then reach improve its photocatalysis performance purpose.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of sheet Bi2WO6Preparation method, this method
The sheet Bi prepared2WO6Pattern it is good, size uniformity, and with excellent photocatalysis performance.
Technical scheme provided by the present invention is：
A kind of sheet Bi2WO6Preparation method, comprise the following steps：
1) bismuth nitrate solution is added drop-wise in sodium tungstate solution；The molar concentration 0.20 of the bismuth nitrate solution~
0.60mol/L, 0.10~0.30mol/L of molar concentration of the sodium tungstate solution；
2) continue that potassium hydroxide solution is added dropwise, mix laggard water-filling thermal response, filter, cleaning obtains sheet Bi2WO6；Institute
State 0.10~2mol/L of molar concentration of potassium hydroxide solution.
It is final to realize using potassium hydroxide as mineralizer using sodium tungstate and bismuth nitrate as reaction mass in above-mentioned technical proposal
Sheet Bi2WO6Preparation.Sodium tungstate is strong base-weak acid salt, and bismuth nitrate is strong acid weak base salt, adds a certain amount of potassium hydroxide,
So that mixed solution shows certain alkalescent, OH-Ion is more.In more OH-Under ionization, the increase of forming core point quantity,
Be conducive to forming core, finally give the less nanometer sheet of size.
It is preferred that, the volume ratio of the bismuth nitrate solution, sodium tungstate solution and potassium hydroxide solution is 13~17:13~
17:10。
It is preferred that, 0.30~0.40mol/L of molar concentration of the bismuth nitrate solution.
It is preferred that, 0.15~0.20mol/L of molar concentration of the sodium tungstate solution.
It is preferred that, 0.6~1.2mol/L of molar concentration of the potassium hydroxide solution.
It is preferred that, the reaction temperature of the hydro-thermal reaction is 180~250 DEG C, and the reaction time is 12~32h.
It is preferred that, the reaction temperature of the hydro-thermal reaction is 190~200 DEG C, and the reaction time is 20~24h.
It is preferred that, the cleaning is：The product being filtrated to get is repeatedly clear with spirit of vinegar, deionized water and ethanol successively
Wash.Further, preferably three times.It is in order to carbon dioxide will be mixed into presoma to the cleaning of Hydrothermal Synthesiss product with spirit of vinegar
The CO formed3 2-、HCO3 -Remove, clean with deionized water be in order to reaction mass is introduced sodium ion, nitrate ion and
The sheet Bi of synthesis2WO6It is sufficiently separated.
It is preferred that, the step 1) and step 2) in 1~2 drop/sec of rate of addition.
Preferably, 0.19~0.20mol/L of molar concentration of the sodium tungstate solution, the molar concentration of bismuth nitrate solution
0.39~0.40mol/L, 0.7~0.9mol/L of molar concentration of potassium hydroxide solution；The bismuth nitrate solution, sodium tungstate solution
Volume ratio with potassium hydroxide solution is 14~16:14~16:10.The reaction temperature of the hydro-thermal reaction is 195~200 DEG C,
Reaction time is 19~21h.Under the conditions described above, gained sheet Bi2WO6Pattern preferably, steady quality, powder granule point
Dissipate property good.
Compared with the existing technology, beneficial effects of the present invention are embodied in：
(1) preparation process in the present invention is simple, it is easy to control, non-environmental-pollution, cost is low, it is easy to scale metaplasia
Production.
(2) the sheet Bi that the present invention is prepared2WO6Thickness be about 20nm, product quality is stable, and powder granule disperses
Property it is good, and with excellent photocatalysis performance.
Brief description of the drawings
Fig. 1 be embodiment it is 2-in-1 into sheet Bi2WO6X-ray diffractogram；
Fig. 2 be embodiment it is 2-in-1 into sheet Bi2WO6Scanning electron microscope diagram；
Fig. 3 is the Bi that comparative example 1 is synthesized2WO6The scanning electron microscope diagram of self-assembled nanometer ball；
Fig. 4 be comparative example it is 2-in-1 into block Bi2O3Scanning electron microscope diagram；
Fig. 5 be embodiment it is 2-in-1 into sheet Bi2WO6The degradation curve figure of rhodamine B degradation；
Fig. 6 is rhodamine B from degradation curve figure.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
1) the sour sodium of 1.5mmol tungstate dihydrates is dissolved in 15ml deionized waters so that tungstate dihydrate acid sodium solution it is mole dense
Spend 0.10mol/L.
2) the water bismuth nitrates of 3mmol five are dissolved in 15ml deionized waters so that the molar concentration of five water bismuth nitrate solutions
0.20mol/L, a certain amount of KOH tablets are dissolved in 10ml deionized waters so that potassium hydroxide solution molar concentration is
0.4mol/L；
Five water bismuth nitrate solutions are added drop-wise in sodium tungstate solution with 1~2 drop/sec of speed, and by potassium hydroxide solution
It is added drop-wise to identical drop rate in above-mentioned mixed solution, after stirring 30min, insulation carries out hot place in 12 hours at 180 DEG C
Reason.Then, room temperature is down to, reaction product is taken out, filtering is cleaned three times, 60 DEG C of temperature with spirit of vinegar, deionized water and ethanol successively
Degree is lower to dry, and obtains sheet Bi2WO6。
Embodiment 2
1) the sour sodium of 3mmol tungstate dihydrates is dissolved in 15ml deionized waters so that the molar concentration of tungstate dihydrate acid sodium solution
0.20mol/L。
2) the water bismuth nitrates of 6mmol five are dissolved in 15ml deionized waters so that the molar concentration of five water bismuth nitrate solutions
0.40mol/L, a certain amount of KOH tablets are dissolved in 10ml deionized waters so that potassium hydroxide solution molar concentration is
0.8mol/L；
Five water bismuth nitrate solutions are added drop-wise in sodium tungstate solution with 1~2 drop/sec of speed, and by potassium hydroxide solution
It is added drop-wise to identical drop rate in above-mentioned mixed solution, after stirring 30min, insulation carries out hot place in 20 hours at 200 DEG C
Reason.Then, room temperature is down to, reaction product is taken out, filtering is cleaned three times, 60 DEG C of temperature with spirit of vinegar, deionized water and ethanol successively
Degree is lower to dry, and obtains sheet Bi2WO6。
Synthesized sheet Bi2WO6X-ray diffractogram, as shown in Figure 1；SEM SEM photograph such as Fig. 2 institutes
Show, obtained sheet Bi2WO6Thickness is about 20nm.
Embodiment 3
1) the sour sodium of 4.5mmol tungstate dihydrates is dissolved in 15ml deionized waters so that tungstate dihydrate acid sodium solution it is mole dense
Spend 0.30mol/L.
2) the water bismuth nitrates of 9mmol five are dissolved in 15ml deionized waters so that the molar concentration of five water bismuth nitrate solutions
0.60mol/L, a certain amount of KOH tablets are dissolved in 10ml deionized waters so that potassium hydroxide solution molar concentration is 2mol/
L；
Five water bismuth nitrate solutions are added drop-wise in sodium tungstate solution with 1~2 drop/sec of speed, and by potassium hydroxide solution
It is added drop-wise to identical drop rate in above-mentioned mixed solution, after stirring 30min, insulation carries out hot place in 32 hours at 250 DEG C
Reason.Then, room temperature is down to, reaction product is taken out, filtering is cleaned three times, 60 DEG C of temperature with spirit of vinegar, deionized water and ethanol successively
Degree is lower to dry, and obtains sheet Bi2WO6。
Comparative example 1
1) the sour sodium of 4mmol tungstate dihydrates is dissolved in 20ml deionized waters so that the molar concentration of tungstate dihydrate acid sodium solution
0.20mol/L。
2) the water bismuth nitrates of 8mmol five are dissolved in 20ml deionized waters so that the molar concentration of five water bismuth nitrate solutions
0.40mol/L；
Five water bismuth nitrate solutions are added drop-wise in sodium tungstate solution with 1~2 drop/sec of speed, after stirring 30min, 200
Insulation is heat-treated for 20 hours at DEG C.Then, room temperature is down to, reaction product, filtering, successively with spirit of vinegar, deionization is taken out
Water is cleaned, and is dried at a temperature of 60 DEG C, is obtained Bi2WO6Self-assembled nanometer ball nano-powder.
SEM SEM photograph is as shown in figure 3, obtained Bi2WO6Self-assembled nanometer ball nano-scale between 2~
4um, pattern is spherical.Nanometer sheet why can self assembly to be spherical, be because the Bi synthesized under mild alkaline conditions2WO6Nanometer sheet table
Face can be higher, is assembled for reduction system surfaces energy nanometer sheet, so as to form spherical morphology.
Comparative example 2
1) the sour sodium of 3mmol tungstate dihydrates is dissolved in 15ml deionized waters so that the molar concentration of tungstate dihydrate acid sodium solution
0.20mol/L。
2) the water bismuth nitrate ammoniums of 6mmol five are dissolved in 15ml deionized waters so that five water bismuth nitrate solutions it is mole dense
0.40mol/L is spent, a certain amount of KOH tablets are dissolved in 10ml deionized waters so that sodium hydroxide solution molar concentration is
4mol/L；
Five water bismuth nitrate solutions are added drop-wise in sodium tungstate solution with 1~2 drop/sec of speed, and by sodium hydroxide solution
It is added drop-wise to identical drop rate in above-mentioned mixed solution, after stirring 30min, insulation carries out hot place in 20 hours at 200 DEG C
Reason.Then, room temperature is down to, reaction product is taken out, filtering is cleaned three times, 60 DEG C of temperature with spirit of vinegar, deionized water and ethanol successively
Degree is lower to dry, and obtains block Bi2O3。
SEM SEM photograph is as shown in Figure 4.Why block Bi can be generated2O3, it is because with PH increasing
Plus, Bi2O2Hydrolysis can strengthen, WO6Solubility in the solution can increase, for Bi2WO6The WO of crystal growth6It will reduce.
When solution alkaline is very strong, WO6Solubility will be bigger, cause only few even without WO6For crystal growth, crystal
Anisotropic growth is suppressed, thus generation bulk Bi2O3。
Rhodamine B degradation performance test：
10-5The sheet Bi prepared by 0.2g embodiments 2 is added in mol/L 60mL rhodamine B solution2WO6, secretly stir
Mix and irradiated under visible light after 60min, a sample is taken at regular intervals, gained uv-visible absorption spectra is as shown in Figure 5.
Separately to make a blank group, without any catalyst, carry out rhodamine B visible ray from degradation experiment, gained is ultraviolet-and can
See that absorption spectrum is as shown in Figure 6.
By contrast, the sheet Bi prepared by this method2WO6With excellent visible light photocatalysis performance.
Claims (8)
1. a kind of sheet Bi2WO6Preparation method, it is characterised in that comprise the following steps：
1) bismuth nitrate solution is added drop-wise in sodium tungstate solution；0.20~0.60mol/L of molar concentration of the bismuth nitrate solution,
0.10~0.30mol/L of molar concentration of the sodium tungstate solution；
2) continue that potassium hydroxide solution is added dropwise, mix laggard water-filling thermal response, filter, cleaning obtains sheet Bi2WO6；The hydrogen
0.10~2mol/L of molar concentration of potassium oxide solution.
2. sheet Bi according to claim 12WO6Preparation method, it is characterised in that the bismuth nitrate solution, sodium tungstate
The volume ratio of solution and potassium hydroxide solution is 13~17:13~17:10.
3. sheet Bi according to claim 12WO6Preparation method, it is characterised in that mole of the bismuth nitrate solution
0.30~0.40mol/L of concentration.
4. sheet Bi according to claim 12WO6Preparation method, it is characterised in that mole of the sodium tungstate solution
0.15~0.20mol/L of concentration.
5. sheet Bi according to claim 12WO6Preparation method, it is characterised in that the reaction temperature of the hydro-thermal reaction
Spend for 180~250 DEG C, the reaction time is 12~32h.
6. sheet Bi according to claim 12WO6Preparation method, it is characterised in that the reaction temperature of the hydro-thermal reaction
Spend for 190~200 DEG C, the reaction time is 20~24h.
7. sheet Bi according to claim 12WO6Preparation method, it is characterised in that the cleaning is：It will be filtrated to get
Product cleaned repeatedly with spirit of vinegar, deionized water and ethanol successively.
8. sheet Bi according to claim 12WO6Preparation method, it is characterised in that the step 1) and step 2) in
1~2 drop/sec of rate of addition.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108607540A (en) * | 2018-04-12 | 2018-10-02 | 浙江大学 | Niobium adulterates the preparation method of bismuth tungstate catalysis material |
| CN110550661A (en) * | 2019-09-09 | 2019-12-10 | 浙江树人学院（浙江树人大学） | preparation method of bismuth tungstate visible-light-driven photocatalyst and application of bismuth tungstate visible-light-driven photocatalyst |
| CN112973671A (en) * | 2021-03-22 | 2021-06-18 | 合肥工业大学 | Nano bismuth tungstate/zinc oxide heterojunction catalyst, preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN103611526A (en) * | 2013-03-02 | 2014-03-05 | 西北大学 | Preparation method for bismuth tungstate microsphere with core-shell structure |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108607540A (en) * | 2018-04-12 | 2018-10-02 | 浙江大学 | Niobium adulterates the preparation method of bismuth tungstate catalysis material |
| CN108607540B (en) * | 2018-04-12 | 2020-06-19 | 浙江大学 | Preparation method of niobium-doped bismuth tungstate photocatalytic material |
| CN110550661A (en) * | 2019-09-09 | 2019-12-10 | 浙江树人学院（浙江树人大学） | preparation method of bismuth tungstate visible-light-driven photocatalyst and application of bismuth tungstate visible-light-driven photocatalyst |
| CN112973671A (en) * | 2021-03-22 | 2021-06-18 | 合肥工业大学 | Nano bismuth tungstate/zinc oxide heterojunction catalyst, preparation method and application thereof |
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