CN110947425A - Photocatalytic performance research of double rare earth metal organic framework constructed based on 2,2 '-bipyridine-4, 4' -dicarboxylic acid - Google Patents
Photocatalytic performance research of double rare earth metal organic framework constructed based on 2,2 '-bipyridine-4, 4' -dicarboxylic acid Download PDFInfo
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- CN110947425A CN110947425A CN201811118200.1A CN201811118200A CN110947425A CN 110947425 A CN110947425 A CN 110947425A CN 201811118200 A CN201811118200 A CN 201811118200A CN 110947425 A CN110947425 A CN 110947425A
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- 239000012621 metal-organic framework Substances 0.000 title claims abstract description 23
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 17
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 17
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 11
- FXPLCAKVOYHAJA-UHFFFAOYSA-N 2-(4-carboxypyridin-2-yl)pyridine-4-carboxylic acid Chemical compound OC(=O)C1=CC=NC(C=2N=CC=C(C=2)C(O)=O)=C1 FXPLCAKVOYHAJA-UHFFFAOYSA-N 0.000 title claims abstract description 9
- 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 abstract description 15
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 14
- 238000006731 degradation reaction Methods 0.000 claims abstract description 13
- 230000015556 catabolic process Effects 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 6
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 239000013078 crystal Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 238000002835 absorbance Methods 0.000 claims description 6
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 5
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 claims description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 5
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 claims description 5
- 230000000593 degrading effect Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 239000011941 photocatalyst Substances 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000010453 quartz Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 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
- 238000000870 ultraviolet spectroscopy Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 238000004065 wastewater treatment Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 10
- 239000000975 dye Substances 0.000 description 6
- 238000004043 dyeing Methods 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 239000010842 industrial wastewater Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000013110 organic ligand Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000004729 solvothermal method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910002538 Eu(NO3)3·6H2O Inorganic materials 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 231100000518 lethal Toxicity 0.000 description 1
- 230000001665 lethal effect Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000036284 oxygen consumption Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 231100000378 teratogenic Toxicity 0.000 description 1
- 230000003390 teratogenic effect Effects 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
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0213—Complexes without C-metal linkages
- B01J2531/0216—Bi- or polynuclear complexes, i.e. comprising two or more metal coordination centres, without metal-metal bonds, e.g. Cp(Lx)Zr-imidazole-Zr(Lx)Cp
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/30—Complexes comprising metals of Group III (IIIA or IIIB) as the central metal
- B01J2531/38—Lanthanides other than lanthanum
-
- 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
- C02F2101/36—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
-
- 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 photocatalytic performance of a double rare earth metal organic framework constructed based on 2,2 '-bipyridine-4, 4' -dicarboxylic acid is researched. The invention particularly relates to preparation of a double rare earth metal organic framework and research on photocatalytic performance of rhodamine B under an ultraviolet light condition. Experimental research results show that under the irradiation of ultraviolet light, the rare earth metal organic framework can enable the degradation rate of rhodamine B to reach 53.12% within 6 hours. The rare earth metal organic framework can be used as an ideal photocatalytic material and has potential application in the aspect of organic dye wastewater treatment.
Description
Technical Field
The invention relates to a preparation method of a double rare earth metal organic framework and application of the double rare earth metal organic framework in photocatalytic degradation of organic dyes.
Background
The printing and dyeing industry wastewater is one of the pollution sources of environmental water, and restricts the sustainable development of the printing and dyeing industry. Most of chemical substances contained in the wastewater are refractory organic substances, and the wastewater has the characteristics of high oxygen consumption and high toxicity and has teratogenic, carcinogenic and even lethal hazards. However, the traditional treatment methods for the printing and dyeing industrial wastewater, such as biological treatment, coagulating sedimentation, adsorption, membrane technology and other processes, have high operation cost, long reaction time, incomplete removal of colored dyes and easy secondary pollution, so that a novel, environment-friendly, economic and efficient method for treating the printing and dyeing industrial wastewater is urgently needed to be found. Solar energy, as a clean and inexhaustible energy source, may be a good alternative to solving these problems. The photocatalytic technology rapidly developed in recent ten years can photolyze organic pollutants into micromolecular non-toxic organic matters or carbon dioxide and water, and is one of green, environment-friendly, novel, efficient and energy-saving methods for treating printing and dyeing industrial wastewater.
Metal-organic frameworks (MOFs) are a new type of organic-inorganic hybrid material, and have become a hot spot for research in the field of photocatalysis due to their characteristics of large specific surface area, high porosity, structural diversity, controllable synthesis, and the like. MOFs have many advantages in degrading organic pollutants: 1. the pore channel is adjustable, and can selectively adsorb reactants and products; 2. the controllability of the structure and the function can obtain a material with high visible light response; 3. the topological structure of the MOFs determines that active sites are relatively dispersed and are not easy to agglomerate, and the stability of the catalyst is high. Therefore, the invention takes 2,2 '-bipyridine-4, 4' -dicarboxylic acid as an organic ligand, and forms a double rare earth metal organic framework together with rare earth metal europium and terbium ions: (Eu)0.01Tb0.09(dcbpy)(DMF)2(NO3) (MOF1) and the structure and photocatalytic properties thereof were studied.
Disclosure of Invention
The invention aims to provide a novel technology capable of degrading organic dye. The metal organic framework is prepared by a solvothermal method and is used as a photocatalyst for photocatalytic degradation of organic dyes.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention adopts a solvothermal method, uses 2,2 '-bipyridine-4, 4' -dicarboxylic acid as an organic ligand and metal ionsEuropium and terbium prepare MOF1 with a molecular formula of (Eu)0.01Tb0.09(dcbpy)(DMF)2(NO3) The concrete preparation process comprises the following steps:
tb (NO)3)3·6H2O、Eu(NO3)3·6H2O, 2 '-bipyridine-4, 4' -dicarboxylic acid (H)2dcbpy) and N, N-Dimethylformamide (DMF), placing the mixture into a closed stainless steel reaction kettle with a polytetrafluoroethylene lining, stirring the mixture until the mixture is uniform, placing the mixture into a constant-temperature oven, heating the mixture for three days at the temperature of 100 ℃, then cooling the mixture to room temperature, and filtering the mixture to obtain colorless transparent crystals.
The double rare earth metal organic framework is prepared by adopting the method.
The invention relates to a method for degrading rhodamine B by double rare earth metal organic framework MOF1 through photocatalysis, which comprises the following steps: selecting better crystal, drying, grinding into powder, weighing 20mg of crystal powder, and dispersing in 80mL of rhodamine B water solution (10 mg of crystal powder)-5M), stirring for 40min under dark condition to make the reaction reach adsorption-desorption equilibrium, then irradiating for 6h under an ultraviolet lamp (xenon lamp, 280W), and sampling once every 0.5 h. And centrifuging the taken sample, sucking the supernatant liquid, placing the supernatant liquid in a quartz cuvette, and measuring the absorbance by using an ultraviolet-visible spectrophotometer. Because the concentration of rhodamine B is relatively low, the concentration and the absorbance of the solution follow the Lambert beer law, and the degradation rate can be calculated. The degradation rate is shown in figure 1. The degradation experiment process under the conditions of natural light, darkness and no photocatalyst is the same as the above, and the comparative graph of the degradation effect under different conditions is shown in the attached figure 2.
The application of the MOF provided by the invention has the following characteristics: (1) the preparation method of the MOF1 is simple, high in material purity and good in stability. (2) The synthesized MOF1 has the advantages of simplicity, convenience, no pollution and the like in the aspect of organic dye pollution degradation.
Drawings
Fig. 1 is a graph of the photocatalytic degradation rate of synthesized MOF1 to RhB under uv light conditions;
FIG. 2 is a graph comparing the degradation effect of rhodamine B under different conditions.
Detailed Description
Example 1 synthesis of MOF 1:
eu (NO)3)3·6H2O(4.46mg，0.01mmol)、Tb(NO3)3·6H2O (40.77mg, 0.09mmol), 2 '-bipyridine-4, 4' -dicarboxylic acid (H2dcbpy) (24.5mg, 0.1mmol) and N, N-Dimethylformamide (DMF) (10mL) were mixed and placed in a sealed stainless steel reaction vessel lined with polytetrafluoroethylene, stirred until uniform, placed in a constant temperature oven, heated at 100 ℃ for three days, then cooled to room temperature, and filtered to obtain colorless transparent crystals.
Example 2 photocatalytic degradation of rhodamine B by MOF1 under uv light conditions:
selecting crystals with good quality, drying, grinding into powder, weighing 20mg of crystal powder, and dispersing in 80mL of RhB (10)- 5M) in the aqueous solution, stirring the mixture in the dark for 40 minutes to allow the reaction to reach an adsorption-desorption equilibrium, irradiating the mixture under an ultraviolet lamp (xenon lamp, 280W) for 6 hours, sampling the mixture every half hour, centrifuging the sampled sample, sucking the supernatant, placing the supernatant in a quartz cuvette, and measuring the absorbance by an ultraviolet-visible spectrophotometer (C) of η ═ ini-C0)/C0＝(Ai-A0)/A0Formula (A in formula)0And AiRespectively representing the initial absorbance of rhodamine B and the absorbance of degradation time i, C0And CiRespectively representing the initial concentration and the concentration of degradation time i) of the rhodamine B, the degradation rate of the MOF1 on the rhodamine B reaches 53.12 percent after 6 hours of illumination, and the graph is shown in figure 1.
The degradation process of MOF1 under natural light and dark conditions and without photocatalyst is the same, and the degradation rates are 12.11%, 9.67% and 6.32% respectively. In conclusion, the double rare earth metal organic framework can also be used as an ideal photocatalytic material and has potential application in the aspect of organic dye wastewater treatment.
Claims (4)
1. The photocatalytic performance research of a metal organic framework constructed by 2,2 '-bipyridyl-4, 4' -dicarboxylic acid and rare earth metal europium and terbium. The preparation method of the complex constructed by the 2,2 '-bipyridyl-4, 4' -dicarboxylic acid and the rare earth metal europium and terbium comprises the following steps:
eu (NO)3)3·6H2O(4.46mg，0.01mmol)、Tb(NO3)3·6H2O (40.77mg, 0.09mmol), 2 '-bipyridine-4, 4' -dicarboxylic acid (H)2dcbpy) (24.5mg, 0.1mmol) and N, N-Dimethylformamide (DMF) (10mL) were mixed and placed in a sealed stainless steel reaction vessel lined with polytetrafluoroethylene, stirred until uniform and placed in a constant temperature oven, heated at 100 ℃ for three days, then cooled to room temperature and filtered to give colorless transparent crystals.
2. The metal-organic framework material of claim 1, applied to photocatalytic degradation of rhodamine B.
3. The method for degrading rhodamine B by using the metal-organic framework constructed by 2,2 '-bipyridine-4, 4' -dicarboxylic acid and rare earth metal europium and terbium in claim 2 comprises the following specific steps:
selecting better grown crystal, drying, grinding into powder, weighing 20mg of crystal powder, and dispersing in 80mL of rhodamine B (10)- 5M) in the aqueous solution, stirring for 40 minutes under dark conditions to allow the reaction to reach adsorption-desorption equilibrium, and then irradiating under an ultraviolet lamp (xenon lamp, 280W) for 6 hours to take samples every half an hour. And centrifuging the taken sample, sucking supernatant liquid, placing the supernatant liquid in a quartz cuvette, and measuring absorbance by using an ultraviolet-visible spectrophotometer. The specific steps of other conditions were the same as above.
4. The application of the compound of claim 3, wherein a metal organic framework constructed by 2,2 '-bipyridine-4, 4' -dicarboxylic acid and rare earth metal europium and terbium is used as a photocatalyst, and the degradation rate of rhodamine B under ultraviolet light is 53.12% within 6 hours.
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| CN201811118200.1A CN110947425A (en) | 2018-09-26 | 2018-09-26 | Photocatalytic performance research of double rare earth metal organic framework constructed based on 2,2 '-bipyridine-4, 4' -dicarboxylic acid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536855A (en) * | 2022-08-12 | 2022-12-30 | 吉林化工学院 | Preparation method and application of polyacid-based europium complex |
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| CN101531672A (en) * | 2008-03-12 | 2009-09-16 | 安徽大学 | Metal-organic framework material with nano pores and preparation method and application thereof |
| CN102153578A (en) * | 2011-02-28 | 2011-08-17 | 华南理工大学 | Rare-earth organic coordination polymer taking 4,4'-bipyridyl as template, and preparation method and application thereof |
| CN102757453A (en) * | 2012-07-16 | 2012-10-31 | 南开大学 | Multifunctional rare earth metal-organic framework and preparation method thereof |
| US20140284829A1 (en) * | 2011-10-04 | 2014-09-25 | Fundació Institut Catalá De Nanociéncia I Nanotecnologia | Method for the preparation of metal organic frameworks |
| CN107335470A (en) * | 2017-06-20 | 2017-11-10 | 安徽师范大学 | Rare earth neodymium metal organic frame catalysis material and preparation method thereof and application |
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Patent Citations (5)
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|---|---|---|---|---|
| CN101531672A (en) * | 2008-03-12 | 2009-09-16 | 安徽大学 | Metal-organic framework material with nano pores and preparation method and application thereof |
| CN102153578A (en) * | 2011-02-28 | 2011-08-17 | 华南理工大学 | Rare-earth organic coordination polymer taking 4,4'-bipyridyl as template, and preparation method and application thereof |
| US20140284829A1 (en) * | 2011-10-04 | 2014-09-25 | Fundació Institut Catalá De Nanociéncia I Nanotecnologia | Method for the preparation of metal organic frameworks |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115536855A (en) * | 2022-08-12 | 2022-12-30 | 吉林化工学院 | Preparation method and application of polyacid-based europium complex |
| CN115536855B (en) * | 2022-08-12 | 2024-01-26 | 吉林化工学院 | Preparation method and application of polyacid-based europium complex |
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