CN111841584B - Preparation method of BiVO4/NiSe2/Bi compound - Google Patents
Preparation method of BiVO4/NiSe2/Bi compound Download PDFInfo
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- CN111841584B CN111841584B CN202010889977.9A CN202010889977A CN111841584B CN 111841584 B CN111841584 B CN 111841584B CN 202010889977 A CN202010889977 A CN 202010889977A CN 111841584 B CN111841584 B CN 111841584B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 150000001875 compounds Chemical class 0.000 title claims abstract description 8
- 229910002915 BiVO4 Inorganic materials 0.000 title abstract description 16
- 239000002243 precursor Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 5
- 239000012279 sodium borohydride Substances 0.000 claims description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 4
- 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 description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000007789 sealing Methods 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims description 3
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 2
- QHASIAZYSXZCGO-UHFFFAOYSA-N selanylidenenickel Chemical compound [Se]=[Ni] QHASIAZYSXZCGO-UHFFFAOYSA-N 0.000 claims 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 4
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 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 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000000969 carrier Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 230000002195 synergetic effect Effects 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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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; Compounds thereof
-
- 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
- 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
-
- 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
- C02F2101/34—Organic compounds containing oxygen
-
- 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
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a preparation method of a BiVO4/NiSe2/Bi compound, which comprises the steps of precursor preparation, hydrothermal reaction and the like. The prepared compound has excellent performance of photocatalytic degradation of organic matters.
Description
Technical Field
The invention relates to a preparation method of a BiVO4/NiSe2/Bi composite.
Technical Field
The rapid development of the human society brings convenience and rich physical life. However, with the development of economy, environmental pollution has become increasingly serious. In order to be sustainable, the problem of environmental pollution must be solved. Organic pollution is one of the pollution sources of environmental pollution. The photocatalytic technology is utilized to degrade the organic pollutants into water and carbon dioxide, which is an effective way to solve the organic pollutants.
The photocatalytic technology requires the use of semiconductor photocatalysts. The single semiconductor photocatalyst faces the problem of low photocatalytic efficiency due to low separation efficiency of photo-generated carriers. The compound of various semiconductors or metals can rapidly and effectively separate photon-generated carriers, thereby having excellent performance. However, the preparation of these complexes is often complicated. Therefore, it is a problem to be solved to develop a simple process for preparing a composite photocatalyst having excellent properties.
Disclosure of Invention
The invention aims to provide a BiVO4/NiSe2/Bi composite photocatalyst with simple process and excellent performance.
The preparation method of the BiVO4/NiSe2/Bi composite comprises the following steps: 2.9104g of pentahydrate bismuth nitrate is weighed and dissolved in 32mL of 1mol/L nitric acid solution, and the mixture is stirred until clear solution is obtained; 0.7019g ammonium metavanadate is weighed into the solution; until the solution turns orange; adding 3g of urea into the solution; then placing the solution in an oil bath at 80 ℃ and stirring for 24 hours; washing the precipitate with deionized water for 5 times, and drying in an oven at 60 deg.C to obtain precursor; 0.3239g of the precursor, 0.0079g of selenium powder and 0.0047g of sodium borohydride are weighed; dissolving the above 3 substances in 30mL of DMF, and continuously stirring for 20min until no solid precipitate exists; adding 0.0119g nickel chloride hexahydrate and stirring for 20min; transferring the solution into a 50ml reaction kettle; sealing the reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, washing the precipitate in the reaction kettle with deionized water for 3 times, and then washing with ethanol for 2 times; then the mixture is placed at 60 ℃ for vacuum drying for 12 hours to obtain the BiVO4/NiSe2/Bi compound.
Compared with the prior art, the sample provided by the invention has the following advantages: the prepared photocatalyst has excellent performance and simple preparation process.
Drawings
Figure 1 is an XRD pattern of the example sample.
FIG. 2 is a performance curve of photocatalytic degradation of rhodamine B of example samples.
FIG. 3 is a performance curve of pure BiVO4 for photocatalytic degradation of rhodamine B.
Fig. 4 is a plot of the rate of photocatalytic degradation of rhodamine B for the example samples and pure BiVO 4.
Figure 5 is an XRD pattern of the comparative example.
Detailed Description
The following detailed description of implementations of the invention refers to specific embodiments.
The preparation method of the BiVO4/NiSe2/Bi composite comprises the following steps: weighing 2.9104g of bismuth nitrate pentahydrate, dissolving in 32mL of 1mol/L nitric acid solution, and stirring until a clear solution is obtained; 0.7019g ammonium metavanadate is weighed into the solution; until the solution turns orange; adding 3g of urea into the solution; then placing the solution in an oil bath at 80 ℃ and stirring for 24 hours; washing the precipitate with deionized water for 5 times, and drying in an oven at 60 deg.C to obtain precursor; 0.3239g of the precursor, 0.0079g of selenium powder and 0.0047g of sodium borohydride are weighed; dissolving the above 3 materials in 30mL of DMF, and continuously stirring for 20min until no solid precipitate exists; adding 0.0119g nickel chloride hexahydrate and stirring for 20min; transferring the solution into a 50ml reaction kettle; sealing the reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, washing the precipitate in the reaction kettle with deionized water for 3 times, and then washing with ethanol for 2 times; then the mixture is placed at 60 ℃ for vacuum drying for 12 hours to obtain the BiVO4/NiSe2/Bi compound.
In order to illustrate the technical effects of the examples, samples of the examples were characterized. FIG. 1 is the XRD pattern of the sample of the example, and it can be seen that the diffraction peaks of the sample closely match the standard data for BiVO4, bi, niSe2, indicating that the sample is a BiVO4/NiSe2/Bi composite. FIG. 2 is a degradation curve of the sample of the example on rhodamine B under illumination with a xenon lamp (cut-off wavelength of 420 nm) at 300W, and the solution is taken out at intervals of 30 minutes for testing. FIG. 3 is a degradation curve of pure BiVO4 to rhodamine B under the same illumination condition. It can be seen that the degradation of the example samples is significantly faster. The data in fig. 2 and 3 were extracted to produce the degradation rate curve of fig. 4. Wherein the ordinate in figure 4 represents the initial rhodamine B concentration divided by the real-time concentration, followed by the logarithm. The degradation rate of the sample obtained in the example was 0.00443/min, while that of pure BiVO4 was 0.00126/min, which is about 3.5 times the latter.
To illustrate the method steps of the examples, a synergistic effect was produced to produce a BiVO4/NiSe2/Bi complex, rather than a simple reduction of sodium borohydride. The following comparative examples were made: weighing 2.9104g of bismuth nitrate pentahydrate, dissolving in 32mL of 1mol/L nitric acid solution, and stirring until a clear solution is obtained; 0.7019g ammonium metavanadate is weighed into the solution; until the solution turns orange; adding 3g of urea into the solution; then placing the solution in an oil bath at 80 ℃ and stirring for 24 hours; washing the precipitate with deionized water for 5 times, and drying in an oven at 60 deg.C to obtain precursor; 0.3239g of the precursor, and 0.0047g of sodium borohydride were weighed; dissolving the 2 substances in 30mL of DMF, and continuously stirring for 20min until no solid precipitate exists; transferring the solution into a 50ml reaction kettle; sealing the reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, washing the precipitate in the reaction kettle with deionized water for 3 times, and then washing with ethanol for 2 times; after further drying at 60 ℃ for 12 hours under vacuum, the comparative product is obtained.
The XRD results of the comparative sample are shown in fig. 5, and it can be seen that the product has BiVO4 only and no Bi.
It should be noted that the above description is only a preferred embodiment of the present invention, and the present invention is not limited to the above examples. It is to be understood that other modifications and variations, which may be directly derived or suggested to one skilled in the art without departing from the basic concept of the invention, are to be considered as included within the scope of the invention.
Claims (1)
1. BiVO 4 /NiSe 2 The preparation method of the/Bi compound is characterized by comprising the following steps: weighing 2.9104g of bismuth nitrate pentahydrate, dissolving in 32mL of 1mol/L nitric acid solution, and stirring until a clear solution is obtained; 0.7019g ammonium metavanadate is weighed into the solution; until the solution turns orange; adding 3g of urea into the solution; then placing the solution in an oil bath at 80 ℃ and stirring for 24 hours; washing the precipitate with deionized water for 5 times, and drying in an oven at 60 deg.C to obtain precursor; 0.3239g of the precursor, 0.0079g of selenium powder and 0.0047g of sodium borohydride are weighed; dissolving the above 3 materials in 30mL of DMF, and continuously stirring for 20min until no solid precipitate exists; adding 0.0119g of nickel chloride hexahydrate and stirring for 20min; transferring the solution into a 50ml reaction kettle; sealing the reaction kettle, and heating at 160 ℃ for 24 hours; cooling to room temperature, washing the precipitate in the reaction kettle with deionized water for 3 times, and then washing with ethanol for 2 times; then the mixture is placed at 60 ℃ for vacuum drying for 12 hours to obtain BiVO 4 /NiSe 2 a/Bi composite.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075875A (en) * | 2019-05-08 | 2019-08-02 | 福州大学 | It is a kind of using NiSe as efficient heterojunction photocatalyst of auxiliary agent and its preparation method and application |
| CN110280276A (en) * | 2019-07-08 | 2019-09-27 | 福州大学 | Loaded photocatalyst NiSe2The preparation method and applications of/CdS |
| CN110354840A (en) * | 2019-08-02 | 2019-10-22 | 重庆大学 | It is a kind of to prepare β-Bi2O3/BiVO4The new method of composite photocatalyst material |
| CN111359638A (en) * | 2020-03-31 | 2020-07-03 | 中北大学 | Photocatalytic carbon dioxide reduction catalyst and preparation method and application thereof |
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2020
- 2020-08-28 CN CN202010889977.9A patent/CN111841584B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110075875A (en) * | 2019-05-08 | 2019-08-02 | 福州大学 | It is a kind of using NiSe as efficient heterojunction photocatalyst of auxiliary agent and its preparation method and application |
| CN110280276A (en) * | 2019-07-08 | 2019-09-27 | 福州大学 | Loaded photocatalyst NiSe2The preparation method and applications of/CdS |
| CN110354840A (en) * | 2019-08-02 | 2019-10-22 | 重庆大学 | It is a kind of to prepare β-Bi2O3/BiVO4The new method of composite photocatalyst material |
| CN111359638A (en) * | 2020-03-31 | 2020-07-03 | 中北大学 | Photocatalytic carbon dioxide reduction catalyst and preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| Bifunctional S-scheme g-C3N4/Bi/BiVO4 hybrid photocatalysts toward artificial carbon cycling;Quan Xie et al;《Chinese Journal of Catalysis》;20200105;第41卷;摘要，第2.1-2.3节，第4节 * |
| Function of NiSe2 over CdS nanorods for enhancement of photocatalytic hydrogen production — From preparation to mechanism;Guorong Wang et al;《Applied Surface Science》;20181030;第467–468卷;摘要，第2.1-2.3节，第3.8节，第4节 * |
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