CN111085227A - CeO2-BiOCl nano material and application thereof in photocatalysis - Google Patents
CeO2-BiOCl nano material and application thereof in photocatalysis Download PDFInfo
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- 239000002086 nanomaterial Substances 0.000 title claims abstract description 33
- 230000001699 photocatalysis Effects 0.000 title abstract description 13
- 238000007146 photocatalysis Methods 0.000 title abstract description 6
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 13
- 239000000243 solution Substances 0.000 claims description 17
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 14
- 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 claims description 13
- 229940043267 rhodamine b Drugs 0.000 claims description 13
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 9
- 239000004202 carbamide Substances 0.000 claims description 9
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 9
- 239000001509 sodium citrate Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 8
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 claims 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 description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 4
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 23
- 239000002105 nanoparticle Substances 0.000 abstract description 9
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 6
- 230000006798 recombination Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 239000013078 crystal Substances 0.000 abstract description 2
- 238000001782 photodegradation Methods 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 description 11
- 239000002131 composite material Substances 0.000 description 7
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000003917 TEM image Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
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- 230000005284 excitation Effects 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 229910021642 ultra pure water Inorganic materials 0.000 description 2
- 239000012498 ultrapure water Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000004847 absorption spectroscopy Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000012295 chemical reaction liquid Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 238000005260 corrosion Methods 0.000 description 1
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- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-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
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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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
- 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
Abstract
The invention discloses CeO2the-BiOCl nano material and the application thereof in photocatalysis have the advantages that the nano CeO with good crystal form, obviously improved conductivity and obviously enhanced degradation performance is synthesized by a simple and convenient method2-BiOCl material. The invention takes a sheet BiOCl nano material as a template and adopts a traditional hydrothermal method to mix CeO2The nano particles are loaded on the surface of the sheet BiOCl nano material, so that the band gap of the nano material is narrowed, the excited electrons are increased, and the recombination of the photo-generated electrons and holes is reduced, thereby exciting the potential of the material in photodegradation application on the basis of the principle.
Description
Technical Field
The invention belongs to the field of catalytic chemistry, and particularly relates to a photocatalytic material as well as a preparation method and application thereof.
Background
In recent years, photocatalytic technology, an advanced oxidation method, has been widely used to degrade wastewater because it can generate reducing electrons and oxidizing holes to effectively degrade intractable organic pollutants. Although some conventional photocatalysts have been used for degrading wastewater under simulated sunlight, unfortunately, the photocatalytic activity of these conventional materials is affected by their wide band gap and high recombination of photo-generated electron holes, resulting in limited practical applications.
To obtain a good photocatalyst, the material constituting the photocatalyst should have good solar utilization, have a fast electron transport rate, and have a suitable band gap energy. When the material is illuminated, the light rays in each waveband can be fully utilized to excite electrons in the material, more electrons can be excited to jump, and simultaneously, photo-generated electrons can be timely transmitted to the outside after being excited, so that recombination with electron holes is avoided.
If a good degradation effect is to be obtained, the nanoparticles are combined with a proper material, so that the red shift of the absorption band boundary of the material can be promoted or the absorption strength of the material in a visible light region can be improved, the internal band gap energy and the internal resistance of the material can be reduced as much as possible, the excitation of electrons can be promoted, the speed of electron transmission can be accelerated, the recombination of carriers in the conduction process can be inhibited, and the degradation capability of the material can be improved. Some studies have shown that CeO2Can be activated by light through ultraviolet-visible light irradiation, and decomposes organic matters in the water phase under the irradiation of visible light or sunlight so as to improve the utilization rate of the sunlight.
The technology of using photocatalysts to degrade pollutants still has some defects at present: the green color of the photocatalyst is still difficult, and the reuse of the photocatalyst, the harmless treatment of the material and the like have long-term needs.
Disclosure of Invention
The invention aims to provide CeO capable of effectively improving the utilization rate of sunlight and reducing the band gap energy of a photocatalyst2-BiOCl nanomaterial.
The technical scheme of the invention comprises the following steps: CeO (CeO)2-BiOCl nano material and preparation method thereof, comprising the following steps:
(1) adding a sodium citrate solution into the urea solution to obtain a mixed solution of urea and sodium citrate;
(2) adding cerous chloride into the mixed solution obtained in the step (1), uniformly stirring, slowly adding hydrogen peroxide, and stirring;
(3) carrying out reaction on the mixed solution obtained in the step (2) by adopting a hydrothermal method, cooling, centrifugally cleaning and drying after the reaction is finished to obtain CeO2；
(4) The CeO obtained in the step (3)2Adding the mixture into an aqueous solution of sodium chloride, performing ultrasonic dispersion for 15 minutes, adding an ethanol solution of bismuth nitrate, and stirring for 30 minutes;
(5) carrying out reaction on the mixed solution obtained in the step (4) by adopting a hydrothermal method, cooling, centrifugally cleaning and drying after the reaction is finished to obtain CeO2-BiOCl nanomaterial.
Preferably, the mass ratio of the urea to the sodium citrate to the cerous chloride is 5:1: 4.
Preferably, the mass ratio of the cerous chloride to the hydrogen peroxide is 4: 5.
Preferably, in step (3), the hydrothermal reaction is carried out at 180 ℃ for 22 hours.
Preferably, CeO2The mass ratio of the sodium chloride to the bismuth nitrate is 10:1: 5.
Preferably, in the step (5), the hydrothermal reaction is carried out at 150 ℃ for 8 hours.
The invention also provides CeO2Application of the BiOCl nano material in photocatalytic degradation of RhB (rhodamine B).
Compared with the prior art, the method takes oxyhalide with low cost, no toxicity and corrosion resistance as the basis to synthesize the flaky BiOCl with better dispersity and uses CeO2The nano particles are loaded on the nano particles to form a novel sheet-shaped composite material. When CeO is loaded on the flaky BiOCl2Then, due to the difference of the band gaps of the two materials, the photo-generated electrons and the holes are transmitted between the two materials and participate in the reaction, so that the whole band gap of the composite material is reduced, the excitation of the photo-generated electrons is facilitated, more electrons are excited to a forbidden band from a conduction band, and the whole degradation process is accelerated by participating in the whole degradation reaction. Second CeO2CeO formed after nanoparticles are loaded on BiOCl2the-BiOCl composite material enhances the utilization of visible light by the photocatalyst, and the photocatalyst is moreThe compound has good reaction with RhB, so that the compound has good photocatalytic performance and finally realizes degradation of RhB.
Drawings
FIG. 1 is a TEM image of BiOCl.
FIG. 2 shows CeO2TEM images of BiOCl nanomaterials.
FIG. 3 is an SEM image of BiOCl.
FIG. 4 shows CeO2SEM picture of BiOCl nanomaterial.
FIG. 5 shows CeO2-X-ray diffraction XRD pattern of BiOCl nanomaterial.
FIG. 6 shows BiOCl and CeO2-band gap energy diagram of BiOCl nanomaterial.
FIG. 7 shows BiOCl and CeO2And the BiOCl nano material can degrade RhB in a photocatalysis way under the irradiation of visible light.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and embodiments.
The invention loads CeO on the flaky BiOCl2The nano particles change the internal band gap energy through the compounding of the two materials, so that the quantity of excited electrons is increased, and the propagation of photo-generated electrons is accelerated.
CeO of the invention2-a method for preparing a BiOCl nanomaterial comprising the steps of:
(1) preparing a urea aqueous solution, and adding a sodium citrate solution to obtain a mixed solution of urea and sodium citrate;
(2) adding cerium chloride into the mixed solution, uniformly stirring, slowly adding hydrogen peroxide, and stirring to obtain a light yellow mixed solution;
(3) reacting the mixed solution at 180 ℃ for 22 hours by a hydrothermal method;
(4) cooling, centrifugally cleaning, and drying;
(5) adding the dried sample into an aqueous solution of sodium chloride, ultrasonically dispersing for 15 minutes, slowly adding an ethanol solution of bismuth nitrate, and stirring for 30 minutes to obtain a white mixed solution;
(6) reacting the mixed solution at 150 ℃ for 8 hours by a hydrothermal method;
(7) cooling, centrifugally cleaning and drying to obtain CeO2-BiOCl nanomaterial.
The application process is as follows2And adding the BiOCl nano material into the RhB solution according to the feeding ratio of 0.5g/L, after dark reaction for 30 minutes, turning on a light source, taking reaction liquid at certain intervals, filtering out solids, and measuring ultraviolet absorption spectrum data of the liquid. The composite material prepared by the invention has better photocatalytic performance, and the degradation rate of the composite material is greatly improved compared with that of pure BiOCl. Under the dark reaction of 30 minutes, the photocatalyst is dispersed in the RhB solution uniformly under the condition of vigorous stirring, the influence of the dispersion unevenness of materials on the experiment is eliminated, and the measured data are in line with the linear condition. The light source is a 300W xenon lamp with a UVCUT420nm type filter. The data are recorded as UV absorption Spectroscopy data recording absorbance at wavelength 553 nm.
Examples
1、CeO2Preparation of-BiOCl nano material
(1) 1.3g of urea is placed in 200mL of ultrapure water for ultrasonic dispersion for 8min, 95mL of 10mM/L sodium citrate solution is added, reaction is carried out for 15min under vigorous stirring, 1g of cerous chloride is added, stirring is carried out for 20min, 1.2mL of hydrogen peroxide is dripped at a constant speed of 10mL/min, and stirring is carried out continuously for 30 min. Adding the light yellow mixed solution formed by the reaction into a 50mL polytetrafluoroethylene high-pressure hydrothermal reaction kettle, reacting for 22h at 180 ℃, naturally cooling, centrifugally cleaning and drying at 70 ℃ to obtain light yellow CeO2And (3) sampling.
(2) Adding 2g of the dried sample and 0.2g of sodium chloride into 340mL of ultrapure water, and completely performing ultrasonic dispersion to obtain a solution A; dissolving 1g of bismuth nitrate in 340mL of ethanol to prepare a solution B; the solution B was slowly added to the solution A and stirred for 30 minutes to complete the reaction. Adding the reaction solution into a high-pressure hydrothermal reaction kettle, keeping the temperature at 150 ℃ for 8h, naturally cooling, centrifugally cleaning for several times, and drying at 60 ℃ for later use.
2、CeO2Characterization of BiOCl nanomaterials
FIGS. 1 and 2 show BiOCl and CeO prepared by the present invention, respectively2TEM image of field emission transmission electron microscope of BiOCl nanomaterial, from which it is clearly observed that the prepared BiOCl is in sheet form and CeO2Nanoparticles were well supported on BiOCl sheets.
FIGS. 3 and 4 show the preparation of BiOCl and CeO according to the invention2SEM image of field emission scanning electron microscope of-BiOCl nano material, it is obvious from the image that synthesized BiOCl presents excellent dispersity, does not agglomerate, and CeO can also be observed2The loading of the nanoparticles, the results obtained and the results obtained with a field emission transmission electron microscope are mutually verified.
FIG. 5 shows the sheet BiOCl nano material prepared by the invention and CeO with different loading ratios2-X-ray diffraction XRD pattern of BiOCl nanomaterial. Wherein curve A is a flaky BiOCl nano material XRD curve, and curve B is CeO2-XRD profile of BiOCl nanomaterial. From the figure, it is obvious that BiOCl is doped with CeO2The characteristic diffraction peaks (PDF #73-2060) of BiOCl appear at 2theta =12.0 °, 24.2 °, 25.9 °,32.5 °, 33.6 °, 34.9 °, 36.7 °, 41.0 °, 46.8 °, 49.9 °, 54.2 °, 55.2 °, 58.8 °, 60.8 °, 75.2 ° and 77.7 ° of the rear material, and the CeO appears at 2theta =28.5 ° of the rear material2Characteristic diffraction peak (PDF #89-8436) of (1), corresponding to CeO2The (111) crystal plane of (a).
FIG. 6 shows BiOCl and CeO prepared according to the present invention2Band gap energy diagram of BiOCl nano material, it is found from the diagram that when BiOCl is loaded with CeO2After nanoparticles, the band gap energy of the material was initially reduced from about 3.2eV to about 2.0eV, indicating that when BiOCl and CeO were used2After recombination, the band gap energy of the material is reduced, so that more electrons are excited and the electrons participating in the reaction are increased.
3. Nano material photocatalysis performance test
100mL of RhB (C) was taken0= 1×10-5M), adding 50mg of photocatalyst into the suspension, and continuously stirring the suspension for 30min under dark conditions to ensure that the catalyst and the RhB reach adsorption-desorption equilibrium. At regular intervals, 4mL of the suspension was taken, centrifuged to remove the precipitate and the RhB concentration was further analyzed using a uv spectrophotometer to record absorbance at 553 nm.
FIG. 7 shows the photocatalytic performance curves of different comparative materials, from which it is clearly observed that 10% CeO compared to pure BiOCl2-BiOCl composite material with relatively pure CeO photocatalytic activity2Remarkably improved by 10 percent of CeO2Under the irradiation of a xenon lamp with the wavelength of more than or equal to 420nm for 8 minutes, the degradation rate of the BiOCl composite material to RhB reaches 93.9 percent.
The results of these experiments show that: CeO prepared by the method of the invention2The BiOCl nano material effectively changes the band gap energy in the material, increases the excitation quantity of electrons, improves the propagation speed of the electrons, and obviously enhances the speed of degrading RhB by photocatalysis.
Claims (8)
1. CeO (CeO)2The preparation method of the BiOCl nano material is characterized by comprising the following steps:
(1) adding a sodium citrate solution into the urea solution to obtain a mixed solution of urea and sodium citrate;
(2) adding cerous chloride into the mixed solution obtained in the step (1), uniformly stirring, slowly adding hydrogen peroxide, and stirring;
(3) carrying out hydrothermal reaction on the mixed solution obtained in the step (2), cooling, centrifugally cleaning and drying after the reaction is finished to obtain CeO2；
(4) The CeO obtained in the step (3)2Adding the mixture into an aqueous solution of sodium chloride, performing ultrasonic dispersion for 15 minutes, adding an ethanol solution of bismuth nitrate, and stirring for 30 minutes;
(5) carrying out hydrothermal reaction on the mixed solution obtained in the step (4), cooling, centrifugally cleaning and drying after the reaction is finished to obtain CeO2-BiOCl nanomaterial.
2. The method of claim 1, wherein the mass ratio of urea to sodium citrate to cerous chloride is 5:1: 4.
3. The method according to claim 1, wherein the mass ratio of the cerous chloride to the hydrogen peroxide is 4: 5.
4. The method according to claim 1, wherein in the step (3), the hydrothermal reaction is carried out at 180 ℃ for 22 hours.
5. The method of claim 1 wherein CeO2The mass ratio of the sodium chloride to the bismuth nitrate is 10:1: 5.
6. The method according to claim 1, wherein in the step (5), the hydrothermal reaction is carried out at a temperature of 150 ℃ for 8 hours.
7. CeO prepared by the method of any one of claims 1 to 62-BiOCl nanomaterial.
8. CeO prepared by the method of any one of claims 1 to 62Application of the BiOCl nano material in photocatalytic degradation of rhodamine B.
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| CN114160164A (en) * | 2021-12-09 | 2022-03-11 | 扬州大学 | CeO2-xSxPreparation method and application of/CdZnS/ZnO nano material |
| CN114160164B (en) * | 2021-12-09 | 2023-05-02 | 扬州大学 | CeO 2-x S x Preparation method and application of/CdZnS/ZnO nano material |
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