CN109569732B - Method for preparing MIL-100(Fe)/BiOCl composite photocatalyst by one-pot method - Google Patents
Method for preparing MIL-100(Fe)/BiOCl composite photocatalyst by one-pot method Download PDFInfo
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- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 239000013144 Fe-MIL-100 Substances 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005580 one pot reaction Methods 0.000 title claims abstract description 9
- QMKYBPDZANOJGF-UHFFFAOYSA-N benzene-1,3,5-tricarboxylic acid Chemical compound OC(=O)C1=CC(C(O)=O)=CC(C(O)=O)=C1 QMKYBPDZANOJGF-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 10
- 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 abstract description 10
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 10
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 239000007787 solid Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000463 material Substances 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- 238000001308 synthesis method Methods 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 2
- AEDZKIACDBYJLQ-UHFFFAOYSA-N ethane-1,2-diol;hydrate Chemical compound O.OCCO AEDZKIACDBYJLQ-UHFFFAOYSA-N 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 35
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 4
- 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 4
- 229940043267 rhodamine b Drugs 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000012621 metal-organic framework Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical compound [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 229910001447 ferric ion Inorganic materials 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- -1 iron ions Chemical class 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000011206 ternary composite Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 238000001291 vacuum drying Methods 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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- 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
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
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- B01J35/39—
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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
- C02F2101/34—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
- C02F2101/36—Organic compounds containing halogen
-
- 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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- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention relates to an MIL-100(Fe)/BiOCl composite photocatalyst and a preparation method thereof, belonging to the field of preparation of novel nano catalytic materials. The material synthesis method used in the invention is a one-step reaction solution method. The method comprises the following specific steps: firstly, dissolving trimesic acid and ferric chloride in DMF (dimethyl formamide) and ethylene glycol water respectively, transferring the solution into a round-bottom flask, adding bismuth nitrate pentahydrate into the round-bottom flask, mixing the solution and the solution, and transferring the mixture into an oil bath for reaction. And centrifuging, washing and drying the obtained product to obtain a light red powdery solid, namely the MIL-100(Fe)/BiOCl composite photocatalyst. The preparation method is simple and easy to implement, the synthesized catalytic material has stable performance, the experimental conditions are green and environment-friendly, and the experimental conditions are mild and suitable for large-scale production.
Description
Technical Field
The invention relates to an MIL-100(Fe)/BiOCl composite photocatalyst prepared by a one-pot method and a preparation method thereof, belonging to the technical field of novel inorganic nano functional materials.
Background
Bismuth oxychloride (BiOCl) is an important branch of bismuth-based semiconductor photocatalytic materials and is a V-VI-VII family ternary composite semiconductor material. Scientists have found in recent years that bismuth oxychloride (BiOCl) is an indirect transition bandgap semiconductor, and when the bismuth oxychloride (BiOCl) is excited by light to generate a photo-generated electron-hole pair, the layered structure of BiOCl provides sufficient space for polarization of corresponding atoms and atom orbitals, induced dipole moment can effectively separate holes from electrons, and the indirect transition bandgap semiconductor reduces the recombination rate of photo-generated carriers, and bismuth oxychloride (BiOCl) is easily perpendicular to [ Bi ]2O2]An internal electric field is formed in the direction of the layer and the halogen layer, further promoting the separation of the photo-generated electrons from the holes. However, the band gap of bismuth oxychloride is generally wide (Eg. about.3.2 eV), and visible light cannot be effectively utilized for photocatalytic reaction; meanwhile, the specific surface area is small, the adsorption capacity to pollutants is weak, and the application range of the bismuth oxychloride is limited. The MIL-100(Fe) complex constructed by the iron ions and the trimesic acid ligand has the characteristics of large specific surface area, high porosity and the like, has a good absorption effect in a visible light range, and simultaneously, the ferric ions in the structure can be used as Lewis acid sites to accept electrons so as to have proper interaction with a target object, so that the complex has good photocatalytic performance.
In some reports, BiOCl and Metal Organic Frameworks (MOFs) are combined, so that the adsorption capacity and the degradation efficiency of pollutant molecules are effectively improved. But the synthesis method is often complicated. According to the invention, two materials with excellent photocatalytic potential, namely the MIL-100(Fe) complex and the BiOCl, are organically combined through a one-pot method, so that the MIL-100(Fe)/BiOCl composite photocatalyst is prepared, and the defects of complex preparation method, non-uniform product components, high cost and the like of the existing composite material are overcome. The MIL-100(Fe)/BiOCl composite photocatalyst can be prepared in one reaction, and has the advantages of large specific surface area, high porosity and wide light absorption range of the MIL-100(Fe) complex, low recombination rate of the BiOCl photo-generated electrons and holes and high density of the photo-generated electron-hole pairs, fully exerts the synergistic effect of the MIL-100(Fe) complex and the BiOCl in the photocatalytic reaction, and provides wide prospects in the aspect of photocatalytic treatment of organic wastewater.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing an MIL-100(Fe)/BiOCl composite photocatalyst by a one-pot method, and the MIL-100(Fe)/BiOCl composite photocatalyst with uniform size and regular appearance can be prepared by one-pot reaction by adopting a solution method. The preparation process is simple, rapid, efficient and low in cost, and is suitable for large-scale industrial production.
The purpose of the invention is realized by the following technical scheme:
1) weighing ferric chloride in a round-bottom flask according to a certain molar ratio, weighing trimesic acid (btc) in a beaker A, and weighing bismuth nitrate pentahydrate solid in a beaker B;
2) adding N, N-Dimethylformamide (DMF) into the round-bottom flask used in the step 1), and performing ultrasonic treatment to promote the dissolution of the trimesic acid into the DMF;
3) adding Ethylene Glycol (EG) into the beaker A in the step 1) and stirring to dissolve ferric chloride;
4) adding the solution obtained in the step 3) and the bismuth nitrate pentahydrate solid in the beaker B into the solution obtained in the step 2), and stirring to uniformly mix the solution, the bismuth nitrate pentahydrate solid and the solution;
5) putting the mixed solution obtained in the step 4) to 90oC, heating in an oil bath for 3 hours for reaction;
6) centrifuging the reaction mixture obtained in step 5), washing with deionized water, DMF and ethanol, and then washing at 60 deg.CoAnd C, vacuum drying to obtain a final product.
The invention has the beneficial effects that:
(1) the invention provides a method for preparing an MIL-100(Fe)/BiOCl composite photocatalyst by a one-pot method, which is simple and easy to operate, does not need special equipment, has low cost, is suitable for large-scale preparation, can prepare the MIL-100(Fe)/BiOCl composite photocatalyst by only one-time reaction, and can meet the requirements of practical application;
(2) the MIL-100(Fe)/BiOCl composite photocatalyst prepared by the method is high in preparation speed and product purity, and the preparation efficiency is improved;
(3) the MIL-100(Fe)/BiOCl composite photocatalyst prepared by the invention has good photocatalytic degradation effect on organic pollutants;
(4) the method is simple and easy to implement, and does not need special equipment;
(5) the raw materials used in the invention are cheap, the material synthesis cost is low, and the method is suitable for mass production.
Drawings
FIG. 1 is one of a plurality of Transmission Electron Microscope (TEM) photographs of the MIL-100(Fe)/BiOCl composite photocatalyst prepared by the method of the present invention taken after observation by a Japanese electron JEOL-1400 TEM; wherein, FIG. 1a is a low-power TEM image of the MIL-100(Fe)/BiOCl composite photocatalyst, and FIG. 1b is a high-power TEM image of the MIL-100(Fe)/BiOCl composite photocatalyst;
FIG. 2 is an X-ray diffraction (XRD) pattern of the MIL-100(Fe)/BiOCl composite photocatalyst prepared by the method.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments, which are not intended to limit the scope of the present invention.
Example 1
Firstly weighing 0.32 mmol of ferric chloride to be dissolved in 8 ml of EG, weighing 0.36 mmol of trimesic acid to be dissolved in 8 ml of DMF, weighing 0.32 mmol of bismuth nitrate pentahydrate solid, mixing the three, putting the mixture into a 90 ℃ oil bath kettle to react for 3 hours, then carrying out centrifugal separation, respectively carrying out ultrasonic cleaning by deionized water and ethanol, and drying at 60 ℃ to obtain the MIL-100(Fe)/BiOCl composite photocatalyst.
Example 2
Firstly weighing 0.32 mmol of ferric chloride to be dissolved in 8 ml of EG, weighing 0.36 mmol of trimesic acid to be dissolved in 8 ml of DMF, weighing 0.32 mmol of bismuth nitrate pentahydrate solid, mixing the three, putting the mixture into an oil bath kettle at 80 ℃ for reaction for 5 hours, then carrying out centrifugal separation, respectively carrying out ultrasonic cleaning by deionized water and ethanol, and drying at 50 ℃ to obtain the MIL-100(Fe)/BiOCl composite photocatalyst.
Example 3
Firstly weighing 0.64 mmol of ferric chloride to be dissolved in 15 ml of EG, weighing 0.72 mmol of trimesic acid to be dissolved in 15 ml of DMF, weighing 0.64 mmol of bismuth nitrate pentahydrate solid, mixing the three, putting the mixture into a 90 ℃ oil bath kettle to react for 3 hours, then carrying out centrifugal separation, respectively carrying out ultrasonic cleaning by deionized water and ethanol, and drying at 60 ℃ to obtain the MIL-100(Fe)/BiOCl composite photocatalyst.
Example 4
Firstly weighing 0.32 mmol of ferric chloride to be dissolved in 8 ml of EG, weighing 0.36 mmol of trimesic acid to be dissolved in 8 ml of DMF, weighing 0.40 mmol of bismuth nitrate pentahydrate solid, mixing the three, putting the mixture into an oil bath kettle at 120 ℃ for reaction for 1 hour, then carrying out centrifugal separation, respectively carrying out ultrasonic cleaning by deionized water and ethanol, and drying at 60 ℃ to obtain the MIL-100(Fe)/BiOCl composite photocatalyst.
Example 5
The photocatalytic degradation organic dye rhodamine B (RhB) is selected as a degradation model to study the performance of the prepared MIL-100(Fe)/BiOCl composite photocatalyst for photocatalytic degradation of organic pollutants. Preparing 100 mL of rhodamine B dye wastewater with the concentration of 10 mg/L, adding 20 mg of MIL-100(Fe)/BiOCl composite photocatalyst, magnetically stirring at room temperature, degrading pollutants in water under the irradiation of a xenon lamp with the light power of 165 mW and the wavelength of more than or equal to 420 nm, sampling at certain intervals, centrifuging to remove the catalyst, measuring the absorbance of the sample by using an ultraviolet-visible spectrophotometer, and finally calculating the degradation rate of rhodamine B.
Claims (3)
1. A preparation method of an MIL-100(Fe)/BiOCl composite photocatalyst by a one-pot method is characterized by comprising the following steps:
1) weighing ferric chloride and trimesic acid (btc) with a molar ratio of 8:9, and respectively dissolving the ferric chloride and the trimesic acid (btc) into solvents of EG and DMF;
2) mixing the solution obtained in the step 1), transferring the mixed solution into a round-bottom flask, adding a certain amount of bismuth nitrate pentahydrate solid, and reacting in an oil bath kettle;
3) centrifuging, washing and drying to obtain light red powder product.
2. The method for preparing the MIL-100(Fe)/BiOCl composite photocatalyst as claimed in claim 1, wherein the molar ratio of bismuth nitrate pentahydrate to ferric chloride is 1: 1 to 1: 2.
3. The method for preparing the MIL-100(Fe)/BiOCl composite photocatalyst as claimed in claim 1, wherein the reaction temperature in the step 2) is 80-120 ℃ and the reaction time is 1-5 hours.
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| CN110773206A (en) * | 2019-11-27 | 2020-02-11 | 中国科学院青岛生物能源与过程研究所 | Fe with high catalytic degradation activity 2O 3BiOCl composite photocatalyst and preparation method and application thereof |
| CN113058655A (en) * | 2021-03-29 | 2021-07-02 | 杭州朗迈新材料有限公司 | Preparation method and application of BiOCl/Fe-MOFs composite catalytic material |
| CN114892210A (en) * | 2022-06-07 | 2022-08-12 | 济南大学 | Method for preparing Ni @ Ru nano electrocatalyst with sandwich-like structure by one-pot method |
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| CN105170186A (en) * | 2015-09-09 | 2015-12-23 | 济南大学 | Preparation method of core-shell structure BiOX@MTL(Fe) photocatalyst |
| CN107670695A (en) * | 2017-09-18 | 2018-02-09 | 上海应用技术大学 | A kind of preparation method of nucleocapsid heterogeneous structure material |
| CN109095546A (en) * | 2018-09-29 | 2018-12-28 | 吴洋洋 | A kind of method of photocatalysis treatment of waste water collaboration hydrogen making |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105170186A (en) * | 2015-09-09 | 2015-12-23 | 济南大学 | Preparation method of core-shell structure BiOX@MTL(Fe) photocatalyst |
| CN107670695A (en) * | 2017-09-18 | 2018-02-09 | 上海应用技术大学 | A kind of preparation method of nucleocapsid heterogeneous structure material |
| CN109095546A (en) * | 2018-09-29 | 2018-12-28 | 吴洋洋 | A kind of method of photocatalysis treatment of waste water collaboration hydrogen making |
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