CN110550657A - Method for preparing square bismuth oxychloride with adjustable thickness by hydrothermal method - Google Patents
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229940073609 bismuth oxychloride Drugs 0.000 title claims abstract description 34
- 238000001027 hydrothermal synthesis Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title abstract description 9
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 19
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 12
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000002244 precipitate Substances 0.000 claims abstract description 10
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 claims abstract description 9
- 229930195725 Mannitol Natural products 0.000 claims abstract description 9
- 239000000594 mannitol Substances 0.000 claims abstract description 9
- 235000010355 mannitol Nutrition 0.000 claims abstract description 9
- 239000000463 material Substances 0.000 claims abstract description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 4
- 229960001180 norfloxacin Drugs 0.000 claims description 16
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002336 sorption--desorption measurement Methods 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 2
- 238000013032 photocatalytic reaction Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 abstract description 2
- 238000005406 washing Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 description 12
- 238000002360 preparation method Methods 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 5
- 239000002135 nanosheet Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 3
- 229940088710 antibiotic agent Drugs 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 230000000593 degrading effect Effects 0.000 description 3
- 229940124307 fluoroquinolone Drugs 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000003115 biocidal effect Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 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 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 210000002700 urine Anatomy 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
- C01P2004/24—Nanoplates, i.e. plate-like particles with a thickness from 1-100 nanometer
-
- 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
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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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Abstract
the invention discloses a method for preparing square bismuth oxychloride with adjustable thickness by a hydrothermal method, which comprises the steps of dispersing Bi (NO 3) 3.5H 2 O and mannitol in 50-100mL of ultrapure water according to a molar ratio of 1:50, stirring for 10-30 minutes until the two are completely dissolved, then adding polyvinylpyrrolidone, stirring until the two are fully dissolved for 10-20 minutes, then adding 5-10mL of saturated sodium chloride solution, stirring for 10-20 minutes, transferring the mixture into a hydrothermal kettle, heating the mixture at 180 ℃ for 2-5 hours, cooling, centrifuging the obtained precipitate, repeatedly washing the precipitate with ultrapure water and ethanol, and drying the precipitate at 60-80 ℃ to obtain BiOCl photocatalytic materials with different thicknesses.
Description
Technical Field
The invention belongs to the field of semiconductor material preparation technology and application, and particularly relates to a method for preparing a square bismuth oxychloride photocatalyst with adjustable thickness by a hydrothermal method, which can be used for degrading norfloxacin pollution under visible light.
Background
the increase of microbial resistance and antibiotic resistance caused by antibiotics contained in natural water has attracted great attention. Many antibiotics detected in aquatic environments, even at varying concentrations, can cause antibiotic resistance and have adverse effects on aquatic wildlife, ecosystem, and human health. Fluoroquinolone (FQ) is one of the most consumed antibiotics in the world, with a total consumption of about 4 million 4 kilotons per year. Norfloxacin is the second generation synthetic FQ, widely used in veterinary and human infection treatment. Since only a small fraction of the drug is absorbed by humans and animals and the vast majority is excreted via urine or feces, a large amount of norfloxacin is released into the environment.
In the research process of norfloxacin degradation, several photocatalytic materials are reported, including TiO 2, BiOCl, CdS, Bi 2 WO 6 and g-C 3 N 4 bismuth oxychloride (BiOCl) is a novel photocatalyst developed in recent years, is cheap, easy to obtain and environment-friendly, is a photocatalyst material with potential, has the characteristics of special two-dimensional lamellar structure, easy modulation of crystal face, strong hole oxidation capability and the like, and has a good application prospect in the field of photoelectrocatalytic oxidation, the well-known feature size, structure and the like of the photocatalyst material can greatly influence the photocatalytic performance of the photocatalyst material, for example, patent CN201610101729.7, provides a preparation method of a pine needle biological carbon supported flower-shaped composite photocatalyst, the photocatalytic degradation of rhodamine B under visible light is successfully applied, the photocatalytic performance and the like of the photocatalyst can be greatly improved, the utilization rate of visible light is greatly increased, the hydroxyl radical of visible light can be further degraded, oxygen radical of oxygen can be promoted to generate transition, and oxygen radical can be further generated under visible light irradiation.
BiOCl is a typical two-dimensional layered material, and the thickness of BiOCl has a great influence on the photocatalytic performance of BiOCl. For example, patent CN201510019624.2 discloses a preparation method for preparing BiOCl ultrathin nanosheets by high-temperature calcination, and the preparation method has better photocatalytic degradation efficiency of organic dye rhodamine B. At present, the methods all have the defects of long time consumption, complicated preparation and the like. A preparation method of ultrathin BiOCl with low energy consumption and low cost is urgently needed.
Disclosure of Invention
The invention aims to provide a simple and rapid synthesis method for preparing a BiOCl photocatalyst with adjustable thickness by a hydrothermal method, which can be used for decomposing norfloxacin pollution under visible light conditions.
The invention adopts the following technical scheme:
A hydrothermal method for preparing square bismuth oxychloride with adjustable thickness comprises the steps of dispersing Bi (NO 3) 3.5H 2 O and mannitol in 50-100mL of ultrapure water according to a molar ratio of 1:50, stirring for 10-30 minutes until the Bi and the mannitol are completely dissolved, then adding polyvinylpyrrolidone, stirring until the polyvinylpyrrolidone is fully dissolved for 10-20 minutes, then adding 5-10mL of saturated sodium chloride solution, stirring for 10-20 minutes, transferring to a hydrothermal kettle, carrying out hydrothermal treatment at the temperature of 150 ℃ and 180 ℃ for 2-5 hours, cooling, centrifuging the obtained precipitate, repeatedly washing with ultrapure water and ethanol, and drying at the temperature of 60-80 ℃ to obtain BiOCl photocatalytic materials with different thicknesses.
Preferably, 0.9g of mannitol is dispersed in 60mL of ultrapure water, sufficiently stirred to dissolve the mannitol, 0.97g of Bi (NO 3) 3.5H 2 O is added thereto, the mixture is stirred for 20 minutes, PVP is added, the mixture is stirred for 10 to 20 minutes, a saturated sodium chloride solution is added, the mixture is stirred for 30 minutes, the homogeneous suspension is transferred to a 100mL Teflon-lined stainless steel autoclave and kept at 160 ℃ for 3 hours, the precipitate is obtained after cooling to room temperature, the precipitate is centrifuged, and then repeatedly washed with ultrapure water and ethanol, and dried at 80 ℃ to obtain bismuth oxychloride.
As an example, PVP was added in an amount of 0.1 g.
As another example, PVP was added in an amount of 0.4 g.
Taking 100mL of norfloxacin solution of 20mg/L, adding 0.05g of bismuth oxychloride, placing the mixture into a photocatalysis instrument, carrying out dark reaction for 30min to achieve adsorption-desorption balance, and then turning on a lamp to carry out photocatalysis reaction under visible light.
The invention has the beneficial effects that:
The nanosheet with adjustable BiOCl thickness prepared by a simple and rapid method disclosed by the invention has excellent photocatalytic activity when norfloxacin is degraded under visible light. The method has the advantages of simple process, low price, easy obtainment, low cost and short reaction time, thereby reducing the energy consumption and the reaction cost, being convenient for batch production, having no toxicity or harm, and meeting the environment-friendly requirement.
Drawings
FIG. 1 is an X-ray diffraction pattern (XRD) of the prepared sample.
FIG. 2 is a Scanning Electron Microscope (SEM) image of the prepared sample, wherein (a) is a global image of the added PVP concentration of 0g, (b) is a local image of the added PVP concentration of 0g, and (c) is a global image of the added PVP concentration of 0.1 g; (d) as a local plot of 0.1g of added PVP concentration, (e) as a global plot of 0.4g of added PVP concentration; (f) a local plot of 0.4g of PVP added was obtained.
Fig. 3 is a graph comparing the effect of the prepared samples on degrading norfloxacin under visible light.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1: preparation of thickness-adjustable BiOCl photocatalyst
0.9g of mannitol was dispersed in 60mL of ultrapure water, sufficiently stirred to dissolve it, then 0.97g of Bi (NO 3) 3.5H 2 O was added thereto, after stirring for 20 minutes, different amounts of PVP (0, 0.1, 0.4g) were added, after stirring for 10-20 minutes, a saturated sodium chloride solution was added, after stirring for 30 minutes, the above homogeneous suspension was transferred to a 100mL Teflon-lined stainless steel autoclave and kept at 160 ℃ for 3 hours, after cooling to room temperature, the resulting precipitate was centrifuged, washed repeatedly with ultrapure water and ethanol, and dried at 80 ℃ to obtain BiOCl of different thicknesses, which in the present invention was determined by X-ray diffraction (XRD), as shown in FIG. 1, characteristic peaks of BiOCl in XRD correspond one-to-one with standard cards 85-0861, and NO other miscellaneous peaks were observed, and thus the XRD pattern indicates that BiOCl was successfully prepared.
The SEM is shown in FIG. 2(a), the partial view is shown in FIG. 2(b), the SEM of BiOCl-0.1 is shown in FIG. 2(c), the partial view is shown in FIG. 2(d), the SEM of BiOCl-0.4 is shown in FIG. 2(e), and the partial view is shown in FIG. 2(f) nanosheet. The morphology composition of BiOCl is determined by a Scanning Electron Microscope (SEM), as shown in FIG. 2, BiOCl is of a nanosheet structure, and the BiOCl nanosheets become thinner with the increase of PVP content.
Example 2: the photocatalyst can degrade norfloxacin by visible light.
The experiment for degrading norfloxacin was performed on the photocatalyst samples obtained in the above examples, wherein different thicknesses of BiOCl were used to degrade norfloxacin under visible light for 60min, 100mL of norfloxacin solution of 20mg/L was taken, 0.05g of photocatalyst was added, the mixture was placed in a photocatalytic apparatus, dark reaction was performed for 30min to achieve adsorption-desorption equilibrium, a lamp was turned on to perform photocatalytic reaction under visible light, 4mL of sample was taken every 20min, the solution was immediately filtered through an aqueous phase filter of 0.45 μm, the total sampling was performed for 7 times, and the concentration of the obtained sample was measured by liquid chromatography, and the concentration of norfloxacin in the solution after photocatalytic degradation was calculated by the following formula, wherein R is the removal rate (C 0 -C X)/C 0, C 0 is the initial concentration of norfloxacin in the solution, and C X is the X-th sampling (X is 1, 2, 3, 4, 5, 6 or 7) of norfloxacin in the solution after photocatalytic degradation.
As shown in FIG. 3, BiOCl-0.4 has the best degradation effect, that is, BiOCl obtained by adding 0.4g PVP has the best degradation effect, and the adsorption performance is stronger and stronger because the thickness is thinner continuously.
Claims (5)
1. A hydrothermal method for preparing square bismuth oxychloride with adjustable thickness is characterized in that Bi (NO 3) 3.5H 2 O and mannitol are dispersed in 50-100mL of ultrapure water according to a molar ratio of 1:50, stirred for 10-30 minutes until the two are completely dissolved, then polyvinylpyrrolidone is added, stirred for 10-20 minutes after the two are fully dissolved, then 5-10mL of saturated sodium chloride solution is added, stirred for 10-20 minutes and then transferred into a hydrothermal kettle for hydrothermal treatment at 180 ℃ for 2-5 hours, the obtained precipitate is centrifuged after cooling, washed repeatedly with ultrapure water and ethanol, and dried at 60-80 ℃ to obtain BiOCl photocatalytic materials with different thicknesses.
2. The hydrothermal process for preparing square bismuth oxychloride with adjustable thickness of claim 1, wherein 0.9g of mannitol is dispersed in 60mL of ultrapure water, and the mixture is stirred sufficiently to dissolve the mannitol, then 0.97g of Bi (NO 3) 3.5H 2 O is added thereto, after stirring for 20 minutes, PVP is added, after stirring for 10-20 minutes, a saturated sodium chloride solution is added, after stirring for 30 minutes, the homogeneous suspension is transferred to a 100mL Teflon-lined stainless steel autoclave and kept at 160 ℃ for 3 hours, after cooling to room temperature, a precipitate is obtained, the precipitate is centrifuged, and then washed repeatedly with ultrapure water and ethanol, and dried at 80 ℃ to obtain bismuth oxychloride.
3. The hydrothermal process for preparing square bismuth oxychloride of adjustable thickness according to claim 1, wherein the amount of PVP added is 0.1 g.
4. The hydrothermal process for preparing square bismuth oxychloride of adjustable thickness according to claim 1, wherein the amount of PVP added is 0.4 g.
5. The hydrothermal method for preparing square bismuth oxychloride with adjustable thickness according to claim 1, wherein 100mL of norfloxacin solution with 20mg/L is taken, 0.05g of bismuth oxychloride is added, the mixture is placed in a photocatalytic instrument, the dark reaction is carried out for 30min, and after the adsorption-desorption balance is achieved, the photocatalytic reaction is carried out under visible light by turning on a lamp.
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