CN111204804B - BiVO4Preparation method of nano material - Google Patents
BiVO4Preparation method of nano material Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 7
- 238000000034 method Methods 0.000 title abstract description 5
- 229910002915 BiVO4 Inorganic materials 0.000 claims abstract description 16
- 239000013078 crystal Substances 0.000 claims abstract description 13
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 11
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 34
- 229910003206 NH4VO3 Inorganic materials 0.000 claims description 23
- 239000011259 mixed solution Substances 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 10
- 125000002091 cationic group Chemical group 0.000 claims description 9
- 229920002401 polyacrylamide Polymers 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- -1 polytetrafluoroethylene Polymers 0.000 claims description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 7
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 7
- 239000002244 precipitate Substances 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 7
- 239000010935 stainless steel Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 5
- 125000003917 carbamoyl group Chemical group [H]N([H])C(*)=O 0.000 claims description 2
- 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 abstract description 5
- 229940043267 rhodamine b Drugs 0.000 abstract description 5
- 230000000593 degrading effect Effects 0.000 abstract description 4
- 239000002159 nanocrystal Substances 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 3
- 239000003431 cross linking reagent Substances 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 7
- 238000006731 degradation reaction Methods 0.000 description 7
- 239000011941 photocatalyst Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical group C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001045 blue dye Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
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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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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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
- 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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- 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
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C02F2101/00—Nature of the contaminant
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- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- 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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Abstract
The invention discloses a BiVO4A method for preparing nano material. The invention adopts hydrophilic high molecular polymer sodium polyacrylate and a crosslinking agent in aqueous solution to form a hydrophilic nano reactor with a network structure, thereby limiting BiVO4The crystal growth preparation method can obtain BiVO with the size of 12-18 nm and good dispersibility4The nano crystal has excellent performance of catalyzing and degrading rhodamine B.
Description
Technical Field
The invention belongs to the technical field of environmental photocatalysis, relates to preparation of visible light response photocatalyst, and particularly relates to BiVO4A method for preparing nano material.
Background
The photocatalysis technology for degrading organic pollutants by utilizing the semiconductor photocatalyst under the action of sunlight has the characteristics of high efficiency, energy conservation and cleanness, and is widely concerned in the aspects of environmental management and the like. Semiconductor photocatalysts such as TiO2And ZnO and the like are widely applied to catalytic degradation of organic matters, but can only absorb ultraviolet light accounting for less than 5% of sunlight due to high forbidden energy level, and has poor response to visible light. Monoclinic phase BiVO4The catalyst is a semiconductor material with stable performance, has the forbidden band width of about 2.4eV, has the characteristics of no toxicity, no harm, stable property, safety, environmental protection and the like, and can be used as a novel inorganic nonmetal semiconductor catalyst with high visible light activity to be applied to removing organic pollutants. Yanjianji et al (Yulin academy of education (Nature science) at 5 th stage of 2018, pages 55-64]With Bi (NO)3)3·5H2O and NH4VO3Adopts a hydrothermal method as a raw material, and prepares BiVO by regulating and controlling the pH value of a reaction solution and adding a surfactant sodium dodecyl sulfate4A visible light photocatalyst. BiVO4The visible light catalyst is a dendritic structure formed by agglomeration of a plurality of nanocrystals with the average grain size of 27.7nm, and the visible light catalyst is BiVO4In the presence of the dye, the decomposition of the methylene blue dye is accelerated, and the highest degradation rate is 89% after 2 hours of visible light irradiation. Lijie et al (inorganic materials journal, 164-172 p 2 2019) of Henan university of science and technology adopts a microwave hydrothermal method to produce BiVO3·5H2O and NH4VO3As a raw material, and a visible light catalyst BiVO with a monoclinic system structure can be controllably synthesized by regulating and controlling the pH of a precursor solution to be 94The crystal size is about 1-2 mu, and the degradation rate of methylene blue is 84.6%. The former has serious agglomeration, and the crystals obtained by the latter are all micron-sized large crystals, which affects the catalytic performance of the catalyst.
Disclosure of Invention
The invention aims to provide a BiVO (BiVO) aiming at the defects of the prior art4The preparation method of the nano material adopts the hydrophilic high molecular polymer sodium polyacrylate to form a hydrophilic nano reactor with a network structure with a cross-linking agent in aqueous solution, so that BiVO is limited4Preparation method for crystal growthBy the method, BiVO with the size of 12-18 nm and good dispersibility can be obtained4The nano crystal has excellent performance of catalyzing and degrading rhodamine B.
BiVO of the invention4The preparation method of the nano material comprises the following specific steps:
0.01 to 0.03mol of Bi (NO)3)3·5H2Dissolving O in 30-50 ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
adding 0.01 to 0.03mol NH4VO3Dissolving the mixture in 30-50 ml of deionized water to obtain NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring uniformly in the ethylene glycol solution to obtain a mixed solution; sequentially adding 0.4-1.0 g of sodium polyacrylate and 0.01-0.03 g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 12-24 hours at 120-150 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 60-80 ℃ to obtain BiVO4And (4) crystals.
The molecular formula of the cationic polyacrylamide is ([ CH)2CH(CONH2)]m[(CH2CH)COO-CH2CH2N+(CH3)3Cl]n) The molecular weight is 100-300 ten thousand;
the molecular weight of the sodium polyacrylate is 500-700 ten thousand.
The invention has the beneficial effects that:
the invention adopts hydrophilic high molecular polymer sodium polyacrylate and cross-linking agent cationic polyacrylamide in aqueous solution to form a hydrophilic nano-reactor with a network structure, thereby limiting BiVO4The crystal growth preparation method can obtain BiVO with the size of 12-18 nm and good dispersibility4The nano crystal has excellent performance of catalyzing and degrading rhodamine B.
Detailed Description
The invention is further analyzed with reference to the following specific examples.
Comparative example 1
0.01mol of Bi (NO)3)3·5H2Dissolving O in 30ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
adding 0.01mol NH4VO3Dissolved in 30ml of deionized water to obtain NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring the mixture evenly in the glycol solution to obtain a mixed solution; placing the mixed solution in a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 24 hours at 120 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 60 ℃ to obtain BiVO4And (4) crystals.
Example 1:
0.01mol of Bi (NO)3)3·5H2Dissolving O in 30ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
adding 0.01mol NH4VO3Dissolved in 30ml of deionized water to obtain NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring the mixture evenly in the glycol solution to obtain a mixed solution; sequentially adding 0.4g of sodium polyacrylate and 0.01g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 24 hours at 120 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 60 ℃ to obtain BiVO4And (4) crystals.
Example 2:
0.03mol of Bi (NO)3)3·5H2Dissolving O in 50ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
0.03mol NH4VO3Dissolved in 50ml of deionized water to give NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring the mixture evenly in glycol solution to obtain mixed solutionLiquid; sequentially adding 1.0g of sodium polyacrylate and 0.03g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 12 hours at 150 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 80 ℃ to obtain BiVO4And (4) crystals.
Example 3:
0.02mol of Bi (NO)3)3·5H2Dissolving O in 40ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
0.02mol NH4VO3Dissolved in 40ml of deionized water to give NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring uniformly in the ethylene glycol solution to obtain a mixed solution; sequentially adding 0.6g of sodium polyacrylate and 0.02g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 18 hours at 140 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 70 ℃ to obtain BiVO4And (4) crystals.
Example 4:
0.02mol of Bi (NO)3)3·5H2Dissolving O in 45ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
0.02mol NH4VO3Dissolved in 45ml of deionized water to give NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring uniformly in the ethylene glycol solution to obtain a mixed solution; sequentially adding 0.8g of sodium polyacrylate and 0.02g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 16 hours at 140 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 75 ℃ to obtain BiVO4And (4) crystals.
Photocatalytic degradation experiment
At 300WThe xenon lamp is used as a light source, and an optical filter is arranged between the light source and the reactor to filter ultraviolet light below 420 nm. 20mg of the catalyst BiVO prepared in comparative example 1 and examples 1 to 4 were weighed out4Adding the solution into 100mL of 5mg/L rhodamine B solution, placing a light source above a reaction kettle, and fixing the distance between the light source and the liquid level of the RhB solution in the reaction kettle to be 6.5 cm. Stirring for 30min in dark to ensure that the sample is dispersed uniformly and fully absorbed. The light source was then turned on and the magnetic stirring was continued, maintaining the temperature at 25 ℃. Detecting the change of the RhB concentration in the solution by adopting an ultraviolet-visible spectrometer, and calculating the degradation rate of RhB according to the formula: (Co-C)/Co 100%.
Table 1 catalyst BiVO4Catalytic degradation rate of rhodamine B under visible light
| Degradation Rate/illumination 100Min (%) | Degradation/illumination of RhB 180Min (%) | |
| Example 1 | 73.5 | 97.5 |
| Example 2 | 76.2 | 98.3 |
| Example 3 | 70.5 | 95.4 |
| Example 4 | 70.7 | 95.5 |
| Comparative example 1 | 55.5 | 83.5 |
Claims (1)
1. BiVO4The preparation method of the nano material is characterized by comprising the following steps:
0.01 to 0.03mol of Bi (NO)3)3·5H2Dissolving O in 30-50 ml of ethylene glycol to obtain Bi (NO)3)3A glycol solution;
adding 0.01 to 0.03mol NH4VO3Dissolving the mixture in 30-50 ml of deionized water to obtain NH4VO3A solution;
reacting NH4VO3Slowly adding Bi (NO) into the solution3)3Stirring uniformly in the ethylene glycol solution to obtain a mixed solution; sequentially adding 0.4-1.0 g of sodium polyacrylate and 0.01-0.03 g of cationic polyacrylamide into the mixed solution, then placing the mixed solution into a stainless steel reaction kettle with a polytetrafluoroethylene lining, reacting for 12-24 hours at 120-150 ℃, and naturally cooling to room temperature after the reaction is finished; separating and washing the obtained precipitate, and drying at 60-80 ℃ to obtain BiVO4A crystal;
the molecular weight of the cationic polyacrylamide is 100-300 ten thousand, and the molecular formula is as follows:
（ [CH2CH(CONH2)]m[(CH2CH)COO-CH2CH2N+(CH3)3Cl]n）；
the molecular weight of the sodium polyacrylate is 500-700 ten thousand.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104108753A (en) * | 2013-04-22 | 2014-10-22 | 海南师范大学 | Preparation for visible-light responsible BiVO4 catalyst |
| CN103224251A (en) * | 2013-05-15 | 2013-07-31 | 湛江师范学院 | Preparation method of microwave-synthesized monoclinic system olivary pucherite BiVO4 |
| CN105731538B (en) * | 2014-12-08 | 2018-01-05 | 青岛农业大学 | A kind of high pressure hydro-thermal method prepares BiVO4The method of photochemical catalyst |
| CN106268760A (en) * | 2016-08-11 | 2017-01-04 | 广西南宁胜祺安科技开发有限公司 | A kind of method preparing pucherite base composite photocatalyst |
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