CN107088407A - A kind of nano-sheet tungstic acid high efficiency photocatalyst and preparation method thereof - Google Patents
A kind of nano-sheet tungstic acid high efficiency photocatalyst and preparation method thereof Download PDFInfo
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- CN107088407A CN107088407A CN201710272337.1A CN201710272337A CN107088407A CN 107088407 A CN107088407 A CN 107088407A CN 201710272337 A CN201710272337 A CN 201710272337A CN 107088407 A CN107088407 A CN 107088407A
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- 239000002135 nanosheet Substances 0.000 title claims abstract description 24
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 19
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000243 solution Substances 0.000 claims abstract description 51
- 239000011259 mixed solution Substances 0.000 claims abstract description 34
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 27
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000010937 tungsten Substances 0.000 claims abstract description 11
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 6
- LPQOADBMXVRBNX-UHFFFAOYSA-N ac1ldcw0 Chemical compound Cl.C1CN(C)CCN1C1=C(F)C=C2C(=O)C(C(O)=O)=CN3CCSC1=C32 LPQOADBMXVRBNX-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 150000002772 monosaccharides Chemical class 0.000 claims abstract description 5
- 229930006000 Sucrose Natural products 0.000 claims description 11
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 11
- 239000005720 sucrose Substances 0.000 claims description 11
- 239000003054 catalyst Substances 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 4
- -1 sucrose fatty ester Chemical class 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 17
- 238000006731 degradation reaction Methods 0.000 abstract description 17
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 239000000975 dye Substances 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 36
- 239000012153 distilled water Substances 0.000 description 20
- 229910001868 water Inorganic materials 0.000 description 11
- 229910020350 Na2WO4 Inorganic materials 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 10
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 9
- 150000002194 fatty esters Chemical class 0.000 description 9
- 239000000463 material Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 239000012467 final product Substances 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 230000035484 reaction time Effects 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
- 229910052724 xenon Inorganic materials 0.000 description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910001930 tungsten oxide Inorganic materials 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 240000000111 Saccharum officinarum Species 0.000 description 1
- 235000007201 Saccharum officinarum Nutrition 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000027 toxicology Toxicity 0.000 description 1
- 238000003911 water pollution Methods 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
- B01J23/16—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
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/10—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
- A62D3/17—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
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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
- 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
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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
- 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
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
- C01G41/02—Oxides; Hydroxides
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- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
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- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/20—Organic substances
- A62D2101/28—Organic substances containing oxygen, sulfur, selenium or tellurium, i.e. chalcogen
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Abstract
The present invention relates to a kind of nano-sheet tungstic acid high efficiency photocatalyst and preparation method thereof, first monosaccharide solutions and tungsten source solution are well mixed, the mol ratio for obtaining monose and tungsten source in mixed solution A, mixed solution A is (1~4):1；Then the surfactant solution for accounting for mixed solution A volume 1%~2% is added into mixed solution A, it is well mixed to obtain mixed solution B；Mixed solution B pH value is adjusted 0.5~2.5, homogeneous hydro-thermal reaction is carried out at 150~200 DEG C；Homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains nano-sheet tungstic acid high efficiency photocatalyst.Product produced by the present invention is nano-sheet, bigger than surface, can fully be contacted with dyestuff；In addition, the WO prepared by the present invention3There are a small amount of C residuals, the band gap that it can be induced above valence band is overlapping, reduces band gap, makes photo-generated carrier be more easy to move at avtive spot, improves the degradation rate of light-catalyzed reaction.
Description
Technical field
The invention belongs to catalyst material field, and in particular to a kind of nano-sheet tungstic acid high efficiency photocatalyst and its
Preparation method.
Background technology
In recent years, developing rapidly with social economy, influence of the mankind's activity to the earth is increasing so that the earth is dirty
Dye problem is increasingly severe, and wherein water pollution is particularly acute, and has jeopardized daily life.Therefore, in order to solve
This problem, people begin one's study photochemical catalyst, it is desirable to which it can make environmental pollution be eased, and improve the living environment of people.
Photochemical catalyst be under the irradiation of ultraviolet light and visible ray, can will be degradable in the pollutant short time or be mineralized into ring
The harmless product in border, or convert light energy into chemical energy, and promote the synthesis of organic matter with decompose a class material [J.Carey,
J.Lawrence,H.Tosine.Photodechlorination of PCB’s in the presence of titanium
dioxide in aqueous suspensions[J].Bulletin of Environmental Contamination and
Toxicology,1976,16:697-701.].The most commonly used photochemical catalyst is mainly TiO2, but be due to it in light degradation
During can only be using the ultraviolet light of sunshine very small part be accounted for, the utilization rate to sunshine is too low, therefore, and people start to visit
Suo Xin photochemical catalyst [Yueqi Kong, Honggang Sun, Xian Zhao, et al.Fabrication of
hexagonal/cubic tungsten oxide homojunction with improved photocatalytic
activity[J].Applied Catalysis A:General,2015,505:447-455.]。
Tungsten oxide due to its good electrical and optical properties, and is widely used in lithium as a kind of n-type semiconductor
The fields such as ion battery, electrochromic device, gas sensor and photocatalysis [Yi Zheng, Gang Chen, Yaoguang
Yu,et al.Synthesis of carbon doped WO3·0.33H2O hierarchical photocatalyst
with improved photocatalytic activity[J].Applied Surface Science,2016,362:
182-190.].But, WO3Band gap it is too big and solar energy can not be effectively utilized, and its conduction band positions it is too low and can not
Pair production effectively is utilized, so as to cause WO3It can not be used by effective exploitation.
The content of the invention
It is an object of the invention to overcome problems of the prior art, there is provided a kind of nano-sheet tungstic acid is efficient
Photochemical catalyst and preparation method thereof, catalytic performance is good.
In order to achieve the above object, the present invention is adopted the following technical scheme that：
Comprise the following steps：
(1) monosaccharide solutions and tungsten source solution are well mixed, obtain monose and tungsten source in mixed solution A, mixed solution A
Mol ratio is (1~4):1；Then into mixed solution A add account for mixed solution A volume 1%~2% surfactant it is molten
Liquid, it is well mixed to obtain mixed solution B；
(2) regulation mixed solution B pH value obtains mixed solution C 0.5~2.5；
(3) mixed solution C is subjected to homogeneous hydro-thermal reaction at 150~200 DEG C；
(4) homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains the oxygen of nano-sheet three
Change tungsten high efficiency photocatalyst.
Further, the concentration of monosaccharide solutions is 0.5~1mol/L in step (1), the concentration of tungsten source solution for 0.5~
1mol/L, the concentration of surfactant solution is 0.01~0.05mol/L.
Further, monose uses C in step (1)6H12O6·H2O。
Further, tungsten source uses Na in step (1)2WO4·2H2O, surfactant uses sucrose fatty ester.
Further, it is to be well mixed by stirring 10~20min at 30~40 DEG C in step (1).
Further, pH value is adjusted using 2~3mol/L HCl solution in step (2).
Further, mixed solution C is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle in step (3), and volume is filled out
Fill than 35%~65%, then sealing polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, be put into homogeneous hydro-thermal reaction instrument
Carry out homogeneous hydro-thermal reaction.
Further, the time of homogeneous hydro-thermal reaction is 20~30h in step (3).
Further, the drying in step (4) is to dry 12~20h in 40~60 DEG C of vacuum drying ovens.
One kind utilizes nano-sheet tungstic acid high efficiency photocatalyst, the photochemical catalyst made from preparation method as described above
Thickness in 80~150nm.
Compared with prior art, the present invention has following beneficial technique effect：
The present invention provides a kind of nano-sheet WO by hydro-thermal method3Preparation method, obtained product crystal property is good,
Size is controllable；Raw material is simple, it is easy to synthesize；Cost is relatively low, and yield is up to more than 85%, available for factory's large-scale production.This
Invent the nano-sheet WO of synthesis3Ratio surface it is big, can fully be contacted with dyestuff, increase active area.In addition, of the invention
Prepared WO3There are a small amount of C residuals, the band gap that it can be induced above valence band is overlapping, so as to reduce band gap, makes photo-generated carrier
It is more easy to move at avtive spot, improves the degradation rate of light-catalyzed reaction.
Nano-sheet WO synthesized by the present invention3Thickness is in 80~150nm, with preferable photocatalysis performance, in 1000W
Xenon lamp under the light degradation rhodamine B time be 90min, degradation rate can reach 78~92.5%；Under the same conditions, it is commercialized
P25 degradation rates are 45%, and degradation rate of the present invention can lift one times or so.
Brief description of the drawings
Fig. 1 is WO prepared by the embodiment of the present invention 13XRD spectrum.
Fig. 2 is nano-sheet WO prepared by the embodiment of the present invention 13SEM photograph under 100k multiplication factors.
Embodiment
The present invention is described in further details below in conjunction with the accompanying drawings.
1) 0.5~1M C is prepared6H12O6·H2O distilled water solutions, 0.5~1M Na2WO4·2H2O distilled water solutions with
And 0.01~0.05M sucrose fatty ester distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2WO4·2H2O=(1~4):1 ratio mixing, 30~
10~20min is stirred at 40 DEG C.Then the sucrose fatty ester distilled water that volume ratio is 1%~2% is added into resulting solution
Solution, stirs 10~20min at 30~40 DEG C.
3) pH=0.5~2.5 of above-mentioned mixed solution are adjusted for 2~3M HCl solution with concentration.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
35%~65%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 150~200 DEG C to set temperature parameter, reaction
Time is 20~30h.
6) reaction is cooled to room temperature after terminating, after end reaction thing is centrifuged, respectively with deionized water and anhydrous second
Alcohol respectively washing 3 times.Powder material after centrifuging, washing is put into 40~60 DEG C of vacuum drying ovens and dries 12~20h, that is, obtains final
Product.
Embodiment 1
1) 0.5M C is prepared6H12O6·H2O distilled water solutions, 0.5M Na2WO4·2H2O distilled water solutions and 0.01M
Sucrose fatty ester distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2WO4·2H2O=2:1 ratio mixing, is stirred at 30 DEG C
Mix 20min.Then the sucrose fatty ester distilled water solution that volume ratio is 1% is added into resulting solution, in 30 times stirrings
20min。
3) HCl solution for being 2M with concentration adjusts the pH=0.5 of above-mentioned mixed solution.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
35%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 150 DEG C to set temperature parameter, and the reaction time is
30h。
6) reaction is cooled to room temperature after terminating, after end reaction thing is centrifuged, respectively with deionized water and anhydrous second
Alcohol respectively washing 3 times.Powder material after centrifuging, washing is put into 40 DEG C of vacuum drying ovens and dries 20h, that is, obtains final product.
Yield is 88%.
As seen from Figure 1：Product prepared by the present invention is six side WO of pure phase3。
As seen from Figure 2：The WO that the present invention is obtained3Be thickness be about 100nm flaky nanometer structure.
The light degradation rhodamine B time is 90min under 1000W xenon lamp, and degradation rate can reach 92.5%.It is commercialized
Degradation rate under P25 the same terms is 45%.Compared with commercialized P25, degradation rate of the present invention is greatly promoted.
Embodiment 2
1) 1M C is prepared6H12O6·H2O distilled water solutions, 1M Na2WO4·2H2The sugarcane of O distilled water solutions and 0.05M
Sugar fatty acid ester distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2WO4·2H2O=1:1 ratio mixing, is stirred at 40 DEG C
Mix 10min.Then the sucrose fatty ester distilled water solution that volume ratio is 2% is added into resulting solution, is stirred at 40 DEG C
10min。
3) HCl solution for being 3M with concentration adjusts the pH=2.5 of above-mentioned mixed solution.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
65%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 200 DEG C to set temperature parameter, and the reaction time is
20h。
6) reaction is cooled to room temperature after terminating, each with deionized water and absolute ethyl alcohol after end reaction thing is centrifuged
Washing 3 times.Powder material after centrifuging, washing is put into 60 DEG C of vacuum drying ovens and dries 12h, that is, obtains final product.Yield
85.6%.
The light degradation rhodamine B time is 90min under 1000W xenon lamp, and degradation rate can reach 85%.
The WO that the present invention is obtained3Be thickness be about 80nm flaky nanometer structure.
Embodiment 3
1) 0.8M C is prepared6H12O6·H2O distilled water solutions, 0.8M Na2WO4·2H2O distilled water solutions and 0.03M
Sucrose fatty ester distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2WO4·2H2O=3:1 ratio mixing, is stirred at 35 DEG C
Mix 15min.Then the sucrose fatty ester distilled water solution that volume ratio is 1.5% is added into resulting solution, is stirred at 35 DEG C
Mix 15min.
3) HCl solution for being 2M with concentration adjusts the pH=1 of above-mentioned mixed solution.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
50%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 180 DEG C to set temperature parameter, and the reaction time is
24h。
6) reaction is cooled to room temperature after terminating, each with deionized water and absolute ethyl alcohol after end reaction thing is centrifuged
Washing 3 times.Powder material after centrifuging, washing is put into 50 DEG C of vacuum drying ovens or freeze drying box and dries 16h, that is, is obtained
Final product.Yield is 92%.
The light degradation rhodamine B time is 90min under 1000W xenon lamp, and degradation rate can reach 80%.
The WO that the present invention is obtained3Be thickness be about 125nm flaky nanometer structure.
Embodiment 4
1) 0.9M C is prepared6H12O6·H2O distilled water solutions, 0.9M Na2WO4·2H2O distilled water solutions and 0.02M
Sucrose fatty ester distilled water solution.
2) by above-mentioned solution C by volume6H12O6·H2O:Na2WO4·2H2O=4:1 ratio mixing, is stirred at 32 DEG C
Mix 12min.Then the sucrose fatty ester distilled water solution that volume ratio is 1.2% is added into resulting solution, is stirred at 32 DEG C
Mix 12min.
3) HCl solution for being 3M with concentration adjusts the pH=2 of above-mentioned mixed solution.
4) well mixed solution is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle, keeps volume packing ratio to exist
40%.
5) reactor of good seal is put into homogeneous hydro-thermal reaction instrument, it is 160 DEG C to set temperature parameter, and the reaction time is
28h。
6) reaction is cooled to room temperature after terminating, each with deionized water and absolute ethyl alcohol after end reaction thing is centrifuged
Washing 3 times.Powder material after centrifuging, washing is put into 45 DEG C of vacuum drying ovens or freeze drying box and dries 18h, that is, is obtained
Final product.Yield is 91.5%.
The light degradation rhodamine B time is 90min under 1000W xenon lamp, and degradation rate can reach 78%.
The WO that the present invention is obtained3Be thickness be about 150nm flaky nanometer structure.
Sample throughput prepared by the present invention is big, and good crystallinity, purity is high, with excellent photocatalytic.In addition, this hair
Bright device therefor is simple, is easy to operation, and raw materials used cost is relatively low, is conducive to factory to mass produce.
Claims (10)
1. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst, it is characterised in that：Comprise the following steps：
(1) monosaccharide solutions and tungsten source solution are well mixed, obtain monose and mole in tungsten source in mixed solution A, mixed solution A
Than for (1~4):1；Then the surfactant solution for accounting for mixed solution A volume 1%~2% is added into mixed solution A, is mixed
Conjunction uniformly obtains mixed solution B；
(2) regulation mixed solution B pH value obtains mixed solution C 0.5~2.5；
(3) mixed solution C is subjected to homogeneous hydro-thermal reaction at 150~200 DEG C；
(4) homogeneous hydro-thermal reaction is cooled to room temperature after terminating, and isolates product and washs drying, obtains nano-sheet tungstic acid
High efficiency photocatalyst.
2. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：The concentration of monosaccharide solutions is 0.5~1mol/L in step (1), and the concentration of tungsten source solution is 0.5~1mol/L, surface-active
The concentration of agent solution is 0.01~0.05mol/L.
3. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：Monose uses C in step (1)6H12O6·H2O。
4. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：Tungsten source uses Na in step (1)2WO4·2H2O, surfactant uses sucrose fatty ester.
5. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：It is to be well mixed by stirring 10~20min at 30~40 DEG C in step (1).
6. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：Using 2~3mol/L HCl solution regulation pH value in step (2).
7. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：Mixed solution C is poured into polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle in step (3), volume packing ratio 35%~
65%, then polytetrafluoroethyllining lining high-pressure hydrothermal reaction kettle is sealed, is put into homogeneous hydro-thermal reaction instrument and carries out homogeneous hydro-thermal
Reaction.
8. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：The time of homogeneous hydro-thermal reaction is 20~30h in step (3).
9. a kind of preparation method of nano-sheet tungstic acid high efficiency photocatalyst according to claim 1, its feature exists
In：Drying in step (4) is to dry 12~20h in 40~60 DEG C of vacuum drying ovens.
10. one kind utilizes nano-sheet tungstic acid high efficiency photocatalyst made from preparation method, its feature described in claim 1
It is：The thickness of the photochemical catalyst is in 80~150nm.
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| CN101805023A (en) * | 2010-04-01 | 2010-08-18 | 中国科学院宁波材料技术与工程研究所 | Method for preparing tungstic oxide nano-sheets |
| CN103030179A (en) * | 2013-01-08 | 2013-04-10 | 江苏大学 | Tungsten trioxide nano-sheet prepared by hydrothermal method and application of tungsten trioxide nano-sheet |
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| CN103030179A (en) * | 2013-01-08 | 2013-04-10 | 江苏大学 | Tungsten trioxide nano-sheet prepared by hydrothermal method and application of tungsten trioxide nano-sheet |
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