CN108906033A - The method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system - Google Patents
The method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system Download PDFInfo
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- CN108906033A CN108906033A CN201810780119.3A CN201810780119A CN108906033A CN 108906033 A CN108906033 A CN 108906033A CN 201810780119 A CN201810780119 A CN 201810780119A CN 108906033 A CN108906033 A CN 108906033A
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- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 37
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 37
- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000006555 catalytic reaction Methods 0.000 title claims abstract description 25
- 239000000463 material Substances 0.000 title claims abstract description 25
- 239000002135 nanosheet Substances 0.000 title claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 19
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000002194 synthesizing effect Effects 0.000 title claims abstract 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229960003431 cetrimonium Drugs 0.000 claims abstract description 7
- RLGQACBPNDBWTB-UHFFFAOYSA-N cetyltrimethylammonium ion Chemical compound CCCCCCCCCCCCCCCC[N+](C)(C)C RLGQACBPNDBWTB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- 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 7
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 abstract description 5
- 238000003786 synthesis reaction Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010189 synthetic method Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000001699 photocatalysis Effects 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 239000003054 catalyst Substances 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000000758 substrate Substances 0.000 description 6
- 239000000356 contaminant Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 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 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 235000012054 meals Nutrition 0.000 description 1
- 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 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G41/00—Compounds of tungsten
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- 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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Hydrology & Water Resources (AREA)
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Abstract
The invention discloses a kind of methods for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system, 16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and are uniformly mixed to obtain clear solution, add five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；The sodium hydroxide solution that 4mol/L is added into solution A adjusts the pH value of reaction system and obtains solution B for 2 ~ 8；Solution B is placed in autoclave and is reacted for 24 hours in 120 DEG C, cooled to room temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of different-thickness after taking out product.The present invention is by the two-dimentional Bismuth tungstate nano-sheet of the pH value controlledly synthesis different-thickness of regulation reaction system, and synthetic method is easy to operate, raw material is green, low in cost, and product manufacturing cycle is shorter, reproducible, easy to promote and utilize.
Description
Technical field
The invention belongs to the synthesis technical fields of inorganic two-dimentional catalysis material, and in particular to one kind passes through regulation reactant
It is the method for pH value synthesis different-thickness Bismuth tungstate nano-sheet catalysis material.
Background technique
Water pollution is the environmental problem for seriously affecting people's life that China's rapid industrial development is supervened in the process,
Such as aromatics organic pollutant, heavy metal contaminants.Use sunlight as light during photocatalysis technology degradation of contaminant
Source, for inorganic semiconductor material as photochemical catalyst, product is environmental-friendly substance, and photocatalytic pollutant degradation have at
Sheet is low, does not cause the features such as secondary pollution.It is largely visible light in sunlight, therefore develops efficient visible light-responded light
Catalyst is current photocatalytic pollutant degradation field critical issue urgently to be resolved.
Bismuth tungstate（Bi2WO6）Band gap width be ~ 2.7eV, in visible region（λ>420nm）With stronger response energy
Power.And bismuth tungstate has the characteristics such as stability is good, have no toxic side effect, physical and chemical performance is excellent as photochemical catalyst, and it is wide
It is general be used for photocatalytic degradation environmental contaminants, such as the various organic dyestuff of RhB, methyl orange, methylene blue, tetracycline, contain phenyl ring
Pollutant.The more surface atom of two-dimensional ultrathin nanometer chip architecture exposure, is capable of providing more activity in the photocatalytic process
Site is used for adsorption reaction molecule and promotes the generation of light-catalyzed reaction.The thickness of two-dimensional nano piece is to influence bismuth tungstate energy band knot
Structure, electricity, the principal element of chemical property, therefore the controllable bismuth tungstate two-dimensional nano piece of thickness is prepared for preparation with bloom
The catalyst of catalytic activity is very crucial.
The patent of Publication No. 104561979A discloses a kind of preparation method of bismuth tungstate film, this method by tungsten plate or
Surface has the substrate of tungsten layer to be placed in reaction solution as substrate, grows bismuth tungstate film in substrate surface by hydro-thermal reaction.
Notification number is that the patent of 104923214B discloses a kind of preparation method of bismuth tungstate photocatalysis film, and this method synthesizes tungsten first
Sour bismuth meal end, obtains briquet by dry-pressing, and high temperature sintering obtains sputtering required target, then with the method for magnetron sputtering in quartz
Bismuth tungstate photocatalysis film is prepared on sheet glass substrate.Two dimension bismuth tungstate film obtained in report is on long substrate, due to
It is influenced by substrate dimension and film thickness, in light-catalyzed reaction, the amount of photochemical catalyst is fewer, influences the effect of degradation of contaminant
Rate.The two-dimentional Bismuth tungstate nano-sheet photochemical catalyst of dispersion can measure increase and decrease catalysis according to actual needs during light-catalyzed reaction
The dosage of agent reaches best degradation of contaminant effect.It is controllable that the present invention by the pH value of regulation reaction system synthesizes thickness
Two-dimentional Bismuth tungstate nano-sheet photochemical catalyst provides new thinking for synthesis bismuth tungstate two dimension catalysis material.
Summary of the invention
Different-thickness wolframic acid is synthesized by regulation pH value of reaction system the technical problem to be solved by the present invention is to provide a kind of
The method of bismuth nanosheet photocatalytic material, this method synthesize the two-dimentional bismuth tungstate of different-thickness by the pH value of control reaction system
Nanometer sheet.
The present invention adopts the following technical scheme that solve above-mentioned technical problem, different by regulation pH value of reaction system synthesis
The method of thickness Bismuth tungstate nano-sheet catalysis material, it is characterised in that the specific steps are：
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 2 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
~ 8 obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of different-thickness after taking out product.
The present invention has the advantages that compared with prior art：The present invention is controllable by the pH value of regulation reaction system
The two-dimentional Bismuth tungstate nano-sheet of different-thickness is synthesized, synthetic method is easy to operate, raw material is green, low in cost, product preparation week
Phase is shorter, reproducible, easy to promote and utilize.
Detailed description of the invention
A, b, c are respectively the Flied emission scanning of two dimension Bismuth tungstate nano-sheet catalysis material made from embodiment 1-3 in Fig. 1
Electron microscope, catalysis material obtained is the aggregation of laminated structure as seen from the figure, and d, e, f are respectively that embodiment 1-3 is made
Two-dimentional Bismuth tungstate nano-sheet catalysis material transmission electron microscope picture, as seen from the figure condition of different pH preparation Bismuth tungstate nano-sheet
The size of catalysis material is different；
Fig. 2 is the X-ray diffracting spectrum of two dimension Bismuth tungstate nano-sheet catalysis material made from embodiment 1-4, is spread out as seen from the figure
Penetrate the orthorhombic crystal phase that peak corresponds to bismuth tungstate；
Fig. 3 is two dimension Bismuth tungstate nano-sheet catalysis material photocatalytic degradation Cr made from embodiment 1-4（VI）Degradation curve,
The two-dimentional Bismuth tungstate nano-sheet catalysis material prepared as seen from the figure is to Cr（VI）With preferable degradation efficiency.
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this
The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair
Bright range.
Embodiment 1
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 2 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
Obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of specific thicknesses after taking out product.
Embodiment 2
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 4 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
Obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of specific thicknesses after taking out product.
Embodiment 3
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 6 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
Obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of specific thicknesses after taking out product.
Embodiment 4
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 8 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
Obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of specific thicknesses after taking out product.
Embodiment above describes basic principles and main features of the invention and advantage, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, and the above embodiments and description only describe originals of the invention
Reason, under the range for not departing from the principle of the invention, various changes and improvements may be made to the invention, these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (1)
1. the method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system, it is characterised in that
The specific steps are：
Step S1：16.5mg sodium tungstate and 25mg cetrimonium bronmide are added in 50mL deionized water and stirred mixed
Conjunction uniformly obtains clear solution, adds five water bismuth nitrate of 485mg and is uniformly mixed to obtain solution A；
Step S2：It is 2 that the sodium hydroxide solution that 4mol/L is added in the solution A obtained to step S1, which adjusts the pH value of reaction system,
~ 8 obtain solution B；
Step S3：The obtained solution B of step S2 is placed in autoclave and is reacted for 24 hours in 120 DEG C, room is naturally cooled to
Temperature is centrifugated, is dried to obtain the two-dimentional Bismuth tungstate nano-sheet catalysis material of different-thickness after taking out product.
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| CN201810780119.3A CN108906033A (en) | 2018-07-16 | 2018-07-16 | The method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system |
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| CN201810780119.3A CN108906033A (en) | 2018-07-16 | 2018-07-16 | The method for synthesizing different-thickness Bismuth tungstate nano-sheet catalysis material by regulation pH value of reaction system |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951557A (en) * | 2006-11-03 | 2007-04-25 | 中国科学院上海硅酸盐研究所 | Hydrothermal method for preparing superstructure visible light responsive Bi2WO6 photcatalyst |
| CN102992406A (en) * | 2011-09-15 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Bismuth tungstate nano-sheet and preparation method thereof |
| CN107376899A (en) * | 2017-07-19 | 2017-11-24 | 河南师范大学 | The method that one step hydro thermal method synthesizes different-shape bismuth tungstate two dimension catalysis material |
-
2018
- 2018-07-16 CN CN201810780119.3A patent/CN108906033A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1951557A (en) * | 2006-11-03 | 2007-04-25 | 中国科学院上海硅酸盐研究所 | Hydrothermal method for preparing superstructure visible light responsive Bi2WO6 photcatalyst |
| CN102992406A (en) * | 2011-09-15 | 2013-03-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Bismuth tungstate nano-sheet and preparation method thereof |
| CN107376899A (en) * | 2017-07-19 | 2017-11-24 | 河南师范大学 | The method that one step hydro thermal method synthesizes different-shape bismuth tungstate two dimension catalysis material |
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