CN114797834A - Alkali etching method for greatly improving photocatalytic performance of bismuth vanadate - Google Patents
Alkali etching method for greatly improving photocatalytic performance of bismuth vanadate Download PDFInfo
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- CN114797834A CN114797834A CN202210431148.5A CN202210431148A CN114797834A CN 114797834 A CN114797834 A CN 114797834A CN 202210431148 A CN202210431148 A CN 202210431148A CN 114797834 A CN114797834 A CN 114797834A
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- bivo
- alkali etching
- bismuth vanadate
- etching method
- photocatalytic performance
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- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000005530 etching Methods 0.000 title claims abstract description 22
- 239000003513 alkali Substances 0.000 title claims abstract description 19
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 19
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 19
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 17
- 238000003756 stirring Methods 0.000 claims abstract description 17
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 11
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 5
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims abstract description 5
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 5
- 238000006243 chemical reaction Methods 0.000 claims description 3
- 239000011941 photocatalyst Substances 0.000 abstract description 19
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 230000008569 process Effects 0.000 abstract description 4
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 15
- 230000008859 change Effects 0.000 description 10
- 239000000047 product Substances 0.000 description 5
- 239000005416 organic matter Substances 0.000 description 4
- 238000002835 absorbance Methods 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 description 1
- 150000003071 polychlorinated biphenyls Chemical class 0.000 description 1
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000005303 weighing Methods 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
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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
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to the technical field of alkali etching, in particular to an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate, which increases the addition of ammonia water in the process of preparing the bismuth vanadate and synthesizes the bismuth vanadate under hydrothermal conditions, and comprises the following specific steps: adding 30mL of nitric acid solution with the concentration of 2mol/L into a beaker, adding 3.6mmol of bismuth nitrate pentahydrate and 3.6mmol of ammonium metavanadate under the stirring condition, and stirring for 60 minutes; dropwise adding 20mL of 25-28% ammonia water into the solution obtained after stirring for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, carrying out hydrothermal reaction at the constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain the BiVO 4 -2, the invention adopts ammonia etching to obtain BiVO 4 The method of the-2 photocatalyst is simple and easy to implement, has low cost and good reproducibility, and can realize BiVO under visible light 4 The photocatalytic performance is improved.
Description
Technical Field
The invention relates to the technical field of alkali etching, in particular to an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate.
Background
Environmental problems caused by organic pollutants difficult to degrade (such as polycyclic aromatic hydrocarbons, polychlorinated biphenyls, pesticides, dyes and the like) become a great problem affecting human survival and health. Compared with the traditional purification treatment method, the semiconductor photocatalysis technology has the advantages of mild reaction conditions, no secondary pollution, simple operation, obvious degradation effect and the like. Bismuth vanadate has attracted extensive attention of researchers due to its characteristics of appropriate forbidden band width (2.4eV), stable properties, and the like.
Through search, Chinese patent publication No. CN 111204804A discloses BiVO with size of 12-18nm and good dispersibility 4 The nanocrystal is used as a photocatalyst, and hydrophilic high molecular polymer sodium polyacrylate and a cross-linking agent are adopted to form a hydrophilic nanoreactor with a network structure in an aqueous solution, so that BiVO is limited 4 The crystal growth preparation method can obtain BiVO with the size of 12-18nm and good dispersibility 4 Nanocrystals, but bismuth vanadate does not have high performance.
Disclosure of Invention
The invention aims to provide an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate so as to solve the problems in the background technology.
The technical scheme of the invention is as follows: an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate comprises the following specific steps:
s1, adding 30mL of nitric acid solution with the concentration of 2mol/L into a beaker, adding 3.6mmol of bismuth nitrate pentahydrate and 3.6mmol of ammonium metavanadate under the stirring condition, and stirring for 60 minutes;
s2, adding the solution obtained in S1 dropwise at a concentration of 25%Stirring ammonia water with concentration of 28 percent for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, carrying out hydrothermal reaction, naturally cooling to room temperature, centrifuging, washing and drying to obtain the product BiVO 4 -2；
Preferably, the alkali etching method is performed under hydrothermal conditions.
Preferably, in S2, 20ml of 25% -28% ammonia water is added dropwise to the solution obtained in S1.
Preferably, the suspension in S2 is hydrothermally reacted in a teflon-lined autoclave for 24 hours at a constant reaction temperature of 180 ℃.
The invention provides an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate through improvement, and compared with the prior art, the alkali etching method has the following improvements and advantages:
one is as follows: the invention adopts ammonia water etching to obtain BiVO 4 The method of the-2 photocatalyst is simple and easy to implement, has low cost and good reproducibility, and can realize BiVO under visible light 4 The photocatalytic performance is improved;
the second step is as follows: the invention adopts waste water solution containing RhB and BiVO respectively 4 Photocatalyst and BiVO 4 -2, comparing the photo-catalytic reactions, quantitatively calculating the concentration change of the organic matter according to the change of the characteristic absorption peak intensity of the organic matter according to the Lambert-Beer law, and directly representing the change of the solution concentration by using the change of absorbance when light absorption substances are the same and the thicknesses are the same, so that the photo-catalytic activity of the bismuth vanadate can be judged more easily.
Drawings
The invention is further explained below with reference to the figures and examples:
FIG. 1 is a scheme for preparing BiVO 4 -2 Process diagram of photocatalyst
FIG. 2 is BiVO prepared in the examples 4 And BiVO 4 -2X-ray diffraction (XRD) pattern of the photocatalyst;
FIG. 3 is BiVO prepared in the examples 4 A Scanning Electron Microscope (SEM) image of the photocatalyst;
FIG. 4 is BiVO prepared in the examples 4 -2 scanning electron microscope (S) of photocatalystEM) map;
FIG. 5 shows BiVO prepared 4 And BiVO 4 -2 photocatalyst in visible light (λ)>420nm) degradation of RhB.
Detailed Description
The present invention is described in detail below, and technical solutions in the embodiments of the present invention are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides an alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate by improvement, and the technical scheme of the invention is as follows:
as shown in figure 1, the alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate increases the addition of ammonia water in the process of preparing the bismuth vanadate, and is synthesized under hydrothermal conditions, and the method specifically comprises the following steps:
s1, adding 30mL of nitric acid solution with the concentration of 2mol/L into a beaker, adding 3.6mmol of bismuth nitrate pentahydrate and 3.6mmol of ammonium metavanadate under the stirring condition, and stirring for 60 minutes;
s2, dropwise adding 20mL of 25-28% ammonia water into the solution obtained in S1, stirring for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, carrying out hydrothermal reaction at the constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain a product, namely BiVO 4 -2。
The experimental process comprises the following steps:
s1, adding 30mL of nitric acid solution with the concentration of 2mol/L into a beaker, adding 3.6mmol of bismuth nitrate pentahydrate and 3.6mmol of ammonium metavanadate under the stirring condition, and stirring for 60 minutes;
s2, dropwise adding 5mL of 25-28% ammonia water into the solution obtained in S1, stirring for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, carrying out hydrothermal reaction at the constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain a product, namely BiVO 4 ；
S3, dropwise adding 20mL of 25-28% ammonia water into the solution obtained in S1, stirring for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, carrying out hydrothermal reaction at the constant temperature of 180 ℃ for 24 hours, naturally cooling to room temperature, centrifuging, washing and drying to obtain a product, namely BiVO 4 -2；
S4, use of BiVO prepared in S2 4 Photocatalyst and BiVO prepared in S3 4 -2, respectively degrading waste water solution containing RhB by using a photocatalyst: separately weighing BiVO 4 Photocatalyst and BiVO 4 -2, adding 0.05g of each photocatalyst into 200ml of RhB aqueous solution respectively, wherein the concentration of RhB is 7.5mg/L, stirring for 30min in a dark place to ensure that the dye is adsorbed/desorbed on the surface of the catalyst to be balanced, then starting a xenon lamp light source provided with a 420nm optical filter to perform photocatalytic reaction under the irradiation of visible light, and detecting the supernatant by using a spectrophotometer.
According to the Lambert-Beer law, the concentration change of the organic matter can be quantitatively calculated according to the change of the characteristic absorption peak intensity of the organic matter. When the light-absorbing substances are the same and the thicknesses are the same, the change in the concentration of the solution can be directly expressed by the change in absorbance. Because RhB has a characteristic absorption peak at 554nm, the change of the absorbance can be used for measuring the change of the concentration of RhB in the solution.
It can be seen from FIG. 5 (abscissa: time of irradiation with visible light; ordinate: ratio of value of concentration of RhB measured after a lapse of time of irradiation with visible light to initial concentration of RhB) that BiVO is relatively unetched 4 BiVO obtained by ammonia etching 4 2 the activity of the photocatalyst is improved by 2.5 times.
To be further explained, FIG. 2 is BiVO prepared in the examples 4 And BiVO 4 -2X-ray diffraction (XRD) pattern of the photocatalyst, as can be seen from FIG. 2, BiVO prepared in the examples 4 And BiVO 4 -2 and BiVO 4 Standard card (JCPDS: 14-0688) is identical, so the product prepared in the examples is a phase-pure BiVO 4 And is still phase-pure BiVO after alkali etching 4 (ii) a FIG. 3 is BiVO prepared in the examples 4 Scanning Electron Microscope (SEM) images of the photocatalyst,as can be seen from FIG. 3, BiVO prepared in the examples 4 The photocatalyst is in the shapes of nanoparticles and nano-blocks, the diameter of the nanoparticles is 400-600nm, the length of the nano-blocks is 4-6 mu m, and the thickness of the nano-blocks is 3-4 mu m; FIG. 4 is BiVO prepared in the examples 4 -2 Scanning Electron Microscope (SEM) picture of photocatalyst, as can be seen from FIG. 4, BiVO prepared in example 4 -2 the photocatalyst is a hollow nanorod with a length of 7-8 μm and a diameter of 800-1000 nm; FIG. 5 is BiVO prepared by testing 4 And BiVO 4 -2 photocatalyst in visible light (λ)>420nm) degradation of RhB, where C 0 Is the initial concentration of RhB, C is the RhB concentration measured after a period of visible light irradiation, t is the time, BiVO 4 -2 is capable of effectively degrading RhB wastewater solution under visible light irradiation and is compared with non-etched BiVO 4 The performance is improved by 2.5 times.
The previous description is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (4)
1. An alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate is characterized in that: the method comprises the following specific steps:
s1, adding 30mL of nitric acid solution with the concentration of 2mol/L into a beaker, adding 3.6mmol of bismuth nitrate pentahydrate and 3.6mmol of ammonium metavanadate under the stirring condition, and stirring for 60 minutes;
s2, dropwise adding 25-28% ammonia water into the solution obtained in S1, stirring for 60 minutes, transferring the obtained suspension into a polytetrafluoroethylene lining autoclave, performing hydrothermal reaction, naturally cooling to room temperature, centrifuging, washing and drying to obtain a product, namely BiVO 4 -2。
2. The alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate according to claim 1, characterized in that: the alkali etching method is carried out under hydrothermal conditions.
3. The alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate according to claim 1, characterized in that: in S2, 20ml of 25% -28% ammonia water was added dropwise to the solution obtained in S1.
4. The alkali etching method for greatly improving the photocatalytic performance of bismuth vanadate according to claim 1, characterized in that: the suspension in S2 was subjected to hydrothermal reaction in a teflon-lined autoclave for 24 hours at a constant reaction temperature of 180 ℃.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950978A (en) * | 2014-04-09 | 2014-07-30 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103950978A (en) * | 2014-04-09 | 2014-07-30 | 河南师范大学 | Biomimetic synthesis method of bismuth vanadate visible-light photocatalyst having hierarchical structure |
Non-Patent Citations (1)
| Title |
|---|
| HAILIN TIAN等: "Hydrothermal synthesis of m-BiVO4/t-BiVO4 heterostructure for organic pollutants degradation: Insight into the photocatalytic mechanism of exposed facets from crystalline phase controlling" * |
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