CN113289681A - Immobilized BiOI nano microsphere photocatalytic material and preparation method thereof - Google Patents
Immobilized BiOI nano microsphere photocatalytic material and preparation method thereof Download PDFInfo
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- CN113289681A CN113289681A CN202110589142.6A CN202110589142A CN113289681A CN 113289681 A CN113289681 A CN 113289681A CN 202110589142 A CN202110589142 A CN 202110589142A CN 113289681 A CN113289681 A CN 113289681A
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- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 7
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 3
- 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 3
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
- B01J31/069—Hybrid organic-inorganic polymers, e.g. silica derivatized with organic groups
-
- 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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- B01J35/23—
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- B01J35/39—
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- B01J35/51—
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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 an immobilized BiOI nano microsphere photocatalytic material and a preparation method thereof, wherein 15g of PVA (polyvinyl alcohol) and 0.3g of sodium alginate are accurately weighed in a beaker, 100mL of distilled water is added, water bath heating is carried out at 100 ℃ until a mixture in the beaker is gelatinous and has no PVA solid small particles, heating is stopped, 0.3g of BiOI powder is added after the gelatinous mixture is slightly cooled, and the mixture is slowly stirred to be uniformly distributed to obtain an immobilized BiOI nano microsphere mixed solution; and (3) sucking the immobilized BiOI nano microsphere mixed solution by using a dropper, slowly and uniformly dropping the solution into the cross-linking agent solution which is continuously stirred, stirring the solution for 30 min after all the mixed solution is dropped, standing the solution for 24 h to solidify the mixed solution into balls, washing the balls to be neutral by using distilled water after solidification is finished, and drying the balls in an oven at 50 ℃ for 12h to obtain the immobilized BiOI nano microsphere photocatalytic material. The photocatalysis performance can be recycled after being stably recovered, and the cycle service life is longer.
Description
Technical Field
The invention relates to the technical field of photocatalytic materials, in particular to an immobilized BiOI nano microsphere photocatalytic material and a preparation method thereof.
Background
The development of science and technology and industry promotes social progress and simultaneously brings about the problems of energy shortage, environmental pollution and the like. Therefore, in the current society, sustainable development is particularly important, development of novel renewable energy sources is bound to become the mainstream direction of scientific research under the current situation, and the photocatalytic technology is a novel green and environment-friendly technology for converting solar energy into chemical energy. The mechanism of the photocatalytic reaction is that under the irradiation of light, the semiconductor photocatalytic material is excited to generate photoproduction electron-hole pairs, and the photoproduction electron-hole pairs and substances adsorbed on the surface of the material or in the environment undergo an oxidation-reduction reaction so as to degrade pollutants. Therefore, the photocatalysis technology has wide application prospect in the aspect of treating environmental pollution, and particularly has prominent performance in the aspect of treating persistent pollutants in wastewater.
In recent years, bismuth-based semiconductor photocatalytic materials have proved promising in terms of environmental purification. The BiOI has high photocatalytic activity and good visible light absorption performance, and is widely applied to the aspects of degrading dyes, organic pollutants and the like. However, the BiOI is powdery and is difficult to recover after the photocatalytic reaction is finished, so that the BiOI cannot be recycled, and secondary pollution of a water body is caused.
Disclosure of Invention
The invention aims to provide an immobilized BiOI nano microsphere photocatalytic material and a preparation method thereof, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: an immobilized BiOI nano microsphere photocatalytic material comprises the following raw materials: the photocatalytic material is in a nano microsphere shape, and the average particle size of the microsphere is 1-5 mu m.
A preparation method of an immobilized BiOI nano microsphere photocatalytic material comprises the following steps:
s1 preparation of BiOI
S101, accurately weighing 2.43g of pentahydrate bismuth nitrate and 0.83g of potassium iodide in a beaker, adding 40mL of ethylene glycol, stirring and dissolving until a uniform solution is formed, draining the uniform solution into a reaction kettle by using a glass rod, and reacting for 12 hours at 160 ℃;
s102, after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out centrifugal separation to obtain all solids, washing the solids, and after the washing is finished, putting the wet solids into an oven to be dried at the temperature of 80 ℃ to finally obtain the BiOI for later use;
s2 preparation of crosslinker solution
Accurately weighing 11.2g of boric acid and 6g of calcium chloride in a beaker, adding 200mL of distilled water, stirring and dissolving until the solution is clear and transparent, then adding a small amount of anhydrous sodium carbonate for multiple times, and adjusting the pH value of the solution to be neutral to obtain a cross-linking agent solution for later use;
s3 preparation of immobilized BiOI nano-microspheres
S301, accurately weighing 15g of PVA (polyvinyl alcohol) and 0.3g of sodium alginate in a beaker, adding 100mL of distilled water, heating in a water bath at 100 ℃ until the mixture in the beaker is gelatinous and has no PVA solid small particles, stopping heating, adding 0.3g of BiOI powder after the gelatinous mixture is slightly cooled, and slowly stirring to uniformly distribute the mixture to obtain an immobilized BiOI nano microsphere mixed solution;
s302, sucking the immobilized BiOI nano microsphere mixed solution by using a dropper, slowly and uniformly dropping the immobilized BiOI nano microsphere mixed solution into the continuously stirred cross-linking agent solution, stirring the mixed solution for 30 min, stopping stirring, standing for 24 h to solidify the mixed solution into balls, washing the balls to be neutral by using distilled water after solidification, and drying the balls in an oven at 50 ℃ for 12h to obtain the immobilized BiOI nano microsphere photocatalytic material.
In a preferred embodiment, in step S101, the stirring rate is 500-; in step S102, the solid-liquid mixture is centrifuged in batches, the centrifugation operation is repeated until all solids are obtained, the solids are repeatedly washed with distilled water and the centrifugation operation is repeated until the color of the solids is uniform.
In a preferred embodiment, in step S301, the concentration of PVA is in the range of 0.1-2g/L, the gelatinous mixture is cooled to 85-90 ℃, and then BiOI powder is added while stirring until the mixture is uniformly mixed.
In a preferred embodiment, the photocatalytic material is used for photocatalytic degradation of organic dyes.
In a preferred embodiment, the photocatalytic material is used for photocatalytic decomposition of pollutants in sewage treatment.
Compared with the prior art, the invention has the beneficial effects that: the BiOI is added into PVA and sodium alginate to form a colloid, and then the colloid is solidified into balls through the cross-linking agent, so that the immobilized BiOI nano microsphere photocatalytic material is obtained, and pure BiOI is formed into nano microspheres.
Drawings
FIG. 1 is a schematic diagram of the XRD pattern structure of the immobilized BiOI nano microsphere photocatalytic material prepared by the invention and pure BiOI;
FIG. 2 is a schematic view of FT-IR spectrum structures of the immobilized BiOI nano-microsphere photocatalytic material prepared by the present invention and pure BiOI;
FIG. 3 is a graph of photocatalytic degradation at different pH;
FIG. 4 is a graph showing the experimental results of recycling photocatalytic materials according to the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, 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.
Referring to fig. 1-4, the present invention provides a technical solution: an immobilized BiOI nano microsphere photocatalytic material comprises the following raw materials: BiOI, a cross-linking agent solution, PVA and sodium alginate, wherein the photocatalytic material is in a nano microsphere shape, and the average particle size of the microsphere is 1-5 mu m.
A preparation method of an immobilized BiOI nano microsphere photocatalytic material comprises the following steps:
s1 preparation of BiOI
S101, accurately weighing 2.43g of pentahydrate bismuth nitrate and 0.83g of potassium iodide in a beaker, adding 40mL of ethylene glycol, stirring and dissolving until a uniform solution is formed, draining the uniform solution into a reaction kettle by using a glass rod, and reacting for 12 hours at 160 ℃;
s102, after the reaction is finished, naturally cooling the reaction kettle to room temperature, centrifuging the solid-liquid mixture in batches, repeating the centrifuging operation until all solids are obtained, repeatedly washing the solids with distilled water and repeating the centrifuging operation until the solids are uniform in color, and drying the wet solids in an oven at 80 ℃ to finally obtain BiOI for later use;
s2 preparation of crosslinker solution
Accurately weighing 11.2g of boric acid and 6g of calcium chloride in a beaker, adding 200mL of distilled water, stirring and dissolving until the solution is clear and transparent, then adding a small amount of anhydrous sodium carbonate for multiple times, and adjusting the pH value of the solution to be neutral to obtain a cross-linking agent solution for later use;
s3 preparation of immobilized BiOI nano-microspheres
S301, accurately weighing 15g of PVA (polyvinyl alcohol) and 0.3g of sodium alginate in a beaker, adding 100mL of distilled water, heating in a water bath at 100 ℃ until the mixture in the beaker is gelatinous and has no PVA solid small particles, stopping heating, adding 0.3g of BiOI powder after the gelatinous mixture is slightly cooled, and slowly stirring to uniformly distribute the mixture to obtain an immobilized BiOI nano microsphere mixed solution;
s302, sucking the immobilized BiOI nano microsphere mixed solution by using a dropper, slowly and uniformly dropping the immobilized BiOI nano microsphere mixed solution into the continuously stirred cross-linking agent solution, stirring the mixed solution for 30 min, stopping stirring, standing for 24 h to solidify the mixed solution into balls, washing the balls to be neutral by using distilled water after solidification, and drying the balls in an oven at 50 ℃ for 12h to obtain the immobilized BiOI nano microsphere photocatalytic material.
Further, in step S101, the stirring rate is 500-600 r/min.
Further, in step S301, the concentration of PVA is in the range of 0.1-2g/L, the gelatinous mixture is cooled to 85-90 ℃, and then BiOI powder is added while stirring until the mixture is uniformly mixed.
The immobilized BiOI nano microsphere photocatalytic material prepared by the invention is subjected to the following experiments:
experiment 1: a BiOI component experiment in the immobilized BiOI nano microsphere photocatalytic material is carried out by respectively carrying out XRD (X-ray diffraction) and FT-IR (FT-IR) spectrum experiments on a pure BiOI material and the immobilized BiOI nano microsphere photocatalytic material prepared by the invention, and the results are as follows,
fig. 1 is an XRD pattern of pure bio i and the immobilized bio i nano microsphere photocatalytic material prepared by the present invention, and for a bio i sample, diffraction peaks appearing at diffraction angles 2 θ =9.24 °, 29.38 °, 31.78 °, 45.53 ° and 55.11 ° correspond to characteristic diffraction peaks of (001), (012), (110), (020) and (122) crystal planes of a tetragonal crystal form bio i standard card (JCPDS No. 73-2062). For the sample of the immobilized BiOI nano-microspheres, characteristic diffraction peaks of BiOI appear at diffraction angles of 2 theta =29.22 degrees, 31.77 degrees and 55.12 degrees, which indicates that BiOI exists in the immobilized BiOI nano-microspheres;
FIG. 2 is an FT-IR spectrum of pure BiOI and the immobilized BiOI nano microsphere photocatalytic material prepared by the present invention. The absorption peak of both samples appearing near 520 cm < -1 > is the Bi-O characteristic absorption peak of the sample, which indicates that the BiOI component exists in the immobilized BiOI nano microspheres and has a photocatalytic effect.
Experiment 2: the immobilized BiOI nano-microsphere photocatalytic material prepared by the method is used for carrying out photocatalytic experiments on dyes and tetracycline in sewage, and the results are as follows,
the tetracycline solution (10 mg/L) was adjusted to pH 6, 7.5, 8.5, 9.6, 10.5 (10 mg/L tetracycline solution initial pH 7.5) using a pH buffer, and 100mL portions were weighed and poured into five Erlenmeyer flasks numbered A, B, C, D, E in sequence. 0.06g (the relative content of the BiOI) of the immobilized BiOI nano microspheres prepared by the method is put into five conical flasks in sequence to react for 30 min in a dark reaction, so as to achieve the adsorption-desorption balance. And after the dark reaction for 30 min is finished, placing the conical flask under the sunlight for carrying out the photocatalytic reaction for 70 min. During the photocatalytic reaction, 4 mL of the reaction solution was aspirated from the flask at 5 min intervals. Then, the absorbance of the reaction solution was measured at 357 nm using an ultraviolet spectrophotometer (UV-vis) and recorded.
As can be seen from FIG. 3, the immobilized BiOI nano-microspheres prepared by the invention have excellent photocatalytic degradation effect on tetracycline, wherein when the pH value is 6, the overall change rule is different from that of the rest four groups, and when sampling is carried out in the middle and later periods of an experiment, the color of reaction liquid is changed from original transparency to slight faint yellow, part of BiOI possibly breaks away from the immobilized material due to analysis reasons, the influence of acidic pH on the photocatalytic performance of the material is large, and the material is more suitable for neutral or alkaline environments, and is particularly suitable for alkaline sewage treatment in printing and dyeing.
The microspheres in experiment 2, in which the tetracycline solution had a pH of 7.5, were recovered and the dark reaction + photocatalytic reaction was repeated four times.
Fig. 4 is a bar graph of cycle number-degradation rate of five photocatalytic degradation of tetracycline using immobilized bio i nanospheres. As can be seen from fig. 4, after five times of recycling, the immobilized bio i nano-microspheres still exhibit high-efficiency photocatalytic performance, and the degradation efficiency after five times of recycling still reaches 70%, which indicates that the immobilized bio i nano-microspheres of the present invention have stable photocatalytic performance and high tetracycline degradation efficiency, and are a photocatalytic material with good recycling performance, good stability and long cycle life. In addition, the immobilized BiOI nano microspheres have no deformation under multiple times of stirring, have high mechanical strength and are suitable for industrial popularization and use.
In conclusion, the BiOI is added into PVA and sodium alginate to form colloid, and then the colloid is solidified into balls through the cross-linking agent, so that the immobilized BiOI nano microsphere photocatalytic material is obtained, and the pure BiOI is formed into nano microspheres, so that the nano microsphere has stable photocatalytic performance in use, high tetracycline degradation efficiency, no deformation under multiple stirring, high mechanical strength, low loss in photocatalysis, reusability after recovery and long cycle service life.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. An immobilized BiOI nano microsphere photocatalytic material is characterized by comprising the following raw materials: the photocatalytic material is in a nano microsphere shape, and the average particle size of the microsphere is 1-5 mu m.
2. A preparation method of an immobilized BiOI nano microsphere photocatalytic material is characterized by comprising the following steps:
s1 preparation of BiOI
S101, accurately weighing 2.43g of pentahydrate bismuth nitrate and 0.83g of potassium iodide in a beaker, adding 40mL of ethylene glycol, stirring and dissolving until a uniform solution is formed, draining the uniform solution into a reaction kettle by using a glass rod, and reacting for 12 hours at 160 ℃;
s102, after the reaction is finished, naturally cooling the reaction kettle to room temperature, carrying out centrifugal separation to obtain all solids, washing the solids, and after the washing is finished, putting the wet solids into an oven to be dried at the temperature of 80 ℃ to finally obtain the BiOI for later use;
s2 preparation of crosslinker solution
Accurately weighing 11.2g of boric acid and 6g of calcium chloride in a beaker, adding 200mL of distilled water, stirring and dissolving until the solution is clear and transparent, then adding a small amount of anhydrous sodium carbonate for multiple times, and adjusting the pH value of the solution to be neutral to obtain a cross-linking agent solution for later use;
s3 preparation of immobilized BiOI nano-microspheres
S301, accurately weighing 15g of PVA (polyvinyl alcohol) and 0.3g of sodium alginate in a beaker, adding 100mL of distilled water, heating in a water bath at 100 ℃ until the mixture in the beaker is gelatinous and has no PVA solid small particles, stopping heating, adding 0.3g of BiOI powder after the gelatinous mixture is slightly cooled, and slowly stirring to uniformly distribute the mixture to obtain an immobilized BiOI nano microsphere mixed solution;
s302, sucking the immobilized BiOI nano microsphere mixed solution by using a dropper, slowly and uniformly dropping the immobilized BiOI nano microsphere mixed solution into the continuously stirred cross-linking agent solution, stirring the mixed solution for 30 min, stopping stirring, standing for 24 h to solidify the mixed solution into balls, washing the balls to be neutral by using distilled water after solidification, and drying the balls in an oven at 50 ℃ for 12h to obtain the immobilized BiOI nano microsphere photocatalytic material.
3. The preparation method of the immobilized BiOI nano microsphere photocatalytic material as claimed in claim 2, wherein: in the step S101, the stirring speed is 500-; in step S102, the solid-liquid mixture is centrifuged in batches, the centrifugation operation is repeated until all solids are obtained, the solids are repeatedly washed with distilled water and the centrifugation operation is repeated until the color of the solids is uniform.
4. The preparation method of the immobilized BiOI nano microsphere photocatalytic material as claimed in claim 2, wherein: in step S301, the concentration range of PVA is 0.1-2g/L, the gelatinous mixture is cooled to 85-90 ℃, and then BiOI powder is added while stirring until the mixture is uniformly mixed.
5. An immobilized BiOI nano microsphere photocatalytic material is characterized in that: the photocatalytic material is used for photocatalytic degradation of organic dyes.
6. An immobilized BiOI nano microsphere photocatalytic material is characterized in that: the photocatalytic material is used for photocatalytic decomposition of pollutants in sewage treatment.
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| CN202110589142.6A Pending CN113289681A (en) | 2021-05-28 | 2021-05-28 | Immobilized BiOI nano microsphere photocatalytic material and preparation method thereof |
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Citations (4)
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| CN102302924A (en) * | 2011-08-18 | 2012-01-04 | 江苏科技大学 | Preparation method of microsphere adsorbent based on rectorite |
| WO2012066545A2 (en) * | 2010-11-16 | 2012-05-24 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Bismuth oxyhalide compounds useful as photocatalysts |
| US20180008953A1 (en) * | 2016-07-08 | 2018-01-11 | Soochow University | Composite with synergistic effect of adsorption and visible light catalytic degradation and preparation method and application thereof |
| CN109550512A (en) * | 2018-11-02 | 2019-04-02 | 河南师范大学 | A kind of preparation method of the flower-shaped ball tungsten sulfide/bismuthino composite material of micron |
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Patent Citations (4)
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| WO2012066545A2 (en) * | 2010-11-16 | 2012-05-24 | Yissum Research Development Company Of The Hebrew University Of Jerusalem Ltd. | Bismuth oxyhalide compounds useful as photocatalysts |
| CN102302924A (en) * | 2011-08-18 | 2012-01-04 | 江苏科技大学 | Preparation method of microsphere adsorbent based on rectorite |
| US20180008953A1 (en) * | 2016-07-08 | 2018-01-11 | Soochow University | Composite with synergistic effect of adsorption and visible light catalytic degradation and preparation method and application thereof |
| CN109550512A (en) * | 2018-11-02 | 2019-04-02 | 河南师范大学 | A kind of preparation method of the flower-shaped ball tungsten sulfide/bismuthino composite material of micron |
Non-Patent Citations (1)
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| 王磊;张新欣;薛芒;董晓丽;: "分级微球BiOI的制备及其可见光光催化性能", 大连工业大学学报, no. 03, pages 180 - 184 * |
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