CN109107608A - A kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and preparation method thereof - Google Patents
A kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and preparation method thereof Download PDFInfo
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- CN109107608A CN109107608A CN201710536281.6A CN201710536281A CN109107608A CN 109107608 A CN109107608 A CN 109107608A CN 201710536281 A CN201710536281 A CN 201710536281A CN 109107608 A CN109107608 A CN 109107608A
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- photochemical catalyst
- uranyl
- paranitrobenzoic acid
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- acid complexes
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- 239000003054 catalyst Substances 0.000 title claims abstract description 44
- 125000005289 uranyl group Chemical group 0.000 title claims abstract description 31
- OTLNPYWUJOZPPA-UHFFFAOYSA-N 4-nitrobenzoic acid Chemical class OC(=O)C1=CC=C([N+]([O-])=O)C=C1 OTLNPYWUJOZPPA-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims description 7
- YCIHPQHVWDULOY-FMZCEJRJSA-N (4s,4as,5as,6s,12ar)-4-(dimethylamino)-1,6,10,11,12a-pentahydroxy-6-methyl-3,12-dioxo-4,4a,5,5a-tetrahydrotetracene-2-carboxamide;hydrochloride Chemical compound Cl.C1=CC=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(=O)C(C(N)=O)=C(O)[C@@]4(O)C(=O)C3=C(O)C2=C1O YCIHPQHVWDULOY-FMZCEJRJSA-N 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 12
- 238000006731 degradation reaction Methods 0.000 claims abstract description 12
- ROFVEXUMMXZLPA-UHFFFAOYSA-N Bipyridyl Chemical compound N1=CC=CC=C1C1=CC=CC=N1 ROFVEXUMMXZLPA-UHFFFAOYSA-N 0.000 claims abstract description 4
- 230000003197 catalytic effect Effects 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims description 5
- ABUBSBSOTTXVPV-UHFFFAOYSA-H [U+6].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O Chemical compound [U+6].CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O.CC([O-])=O ABUBSBSOTTXVPV-UHFFFAOYSA-H 0.000 claims description 4
- MWVTWFVJZLCBMC-UHFFFAOYSA-N 4,4'-bipyridine Chemical compound C1=NC=CC(C=2C=CN=CC=2)=C1 MWVTWFVJZLCBMC-UHFFFAOYSA-N 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000013078 crystal Substances 0.000 claims description 2
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 2
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 238000001914 filtration Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 claims 1
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 claims 1
- 238000005303 weighing Methods 0.000 claims 1
- 229910052724 xenon Inorganic materials 0.000 abstract description 5
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 abstract description 5
- 230000003115 biocidal effect Effects 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 239000002351 wastewater Substances 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 239000003344 environmental pollutant Substances 0.000 description 5
- 231100000719 pollutant Toxicity 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 238000000634 powder X-ray diffraction Methods 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 230000004044 response Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 241000186361 Actinobacteria <class> Species 0.000 description 1
- 208000035143 Bacterial infection Diseases 0.000 description 1
- 239000005711 Benzoic acid Substances 0.000 description 1
- 101150039167 Bex3 gene Proteins 0.000 description 1
- 241001443715 Fusarium oxysporum f. sp. conglutinans Species 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229930182555 Penicillin Natural products 0.000 description 1
- JGSARLDLIJGVTE-MBNYWOFBSA-N Penicillin G Chemical compound N([C@H]1[C@H]2SC([C@@H](N2C1=O)C(O)=O)(C)C)C(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-MBNYWOFBSA-N 0.000 description 1
- 241001655322 Streptomycetales Species 0.000 description 1
- 239000004098 Tetracycline Substances 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 208000022362 bacterial infectious disease Diseases 0.000 description 1
- 235000010233 benzoic acid Nutrition 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- CYDMQBQPVICBEU-UHFFFAOYSA-N chlorotetracycline Natural products C1=CC(Cl)=C2C(O)(C)C3CC4C(N(C)C)C(O)=C(C(N)=O)C(=O)C4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-UHFFFAOYSA-N 0.000 description 1
- 229960004475 chlortetracycline Drugs 0.000 description 1
- CYDMQBQPVICBEU-XRNKAMNCSA-N chlortetracycline Chemical compound C1=CC(Cl)=C2[C@](O)(C)[C@H]3C[C@H]4[C@H](N(C)C)C(O)=C(C(N)=O)C(=O)[C@@]4(O)C(O)=C3C(=O)C2=C1O CYDMQBQPVICBEU-XRNKAMNCSA-N 0.000 description 1
- 235000019365 chlortetracycline Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- WYICGPHECJFCBA-UHFFFAOYSA-N dioxouranium(2+) Chemical compound O=[U+2]=O WYICGPHECJFCBA-UHFFFAOYSA-N 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluic acid Chemical class CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluenecarboxylic acid Natural products CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 description 1
- 229940049954 penicillin Drugs 0.000 description 1
- 230000002186 photoactivation Effects 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 244000144977 poultry Species 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229960002180 tetracycline Drugs 0.000 description 1
- 235000019364 tetracycline Nutrition 0.000 description 1
- 229930101283 tetracycline Natural products 0.000 description 1
- 229940072172 tetracycline antibiotic Drugs 0.000 description 1
- 150000003522 tetracyclines Chemical class 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 1
Classifications
-
- B01J35/39—
-
- 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
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2213—At least two complexing oxygen atoms present in an at least bidentate or bridging ligand
-
- 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/06—Preparation of nitro compounds
- C07C201/12—Preparation of nitro compounds by reactions not involving the formation of nitro groups
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C205/00—Compounds containing nitro groups bound to a carbon skeleton
- C07C205/49—Compounds containing nitro groups bound to a carbon skeleton the carbon skeleton being further substituted by carboxyl groups
- C07C205/57—Compounds containing nitro groups bound to a carbon skeleton the carbon skeleton being further substituted by carboxyl groups having nitro groups and carboxyl groups bound to carbon atoms of six-membered aromatic rings of the carbon skeleton
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F5/00—Compounds containing elements of Groups 3 or 13 of the Periodic System
- C07F5/003—Compounds containing elements of Groups 3 or 13 of the Periodic System without C-Metal linkages
-
- 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
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
-
- 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
- B01J2531/39—Actinides
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst, the molecular formula of the photochemical catalyst is (H2‑bipy)[(UO2)4(μ3‑O)2(p‑nba)6], bipy is 4 in molecular formula, 4 '-bipyridyls, Hp-nba is paranitrobenzoic acid, the catalyst is under the irradiation of xenon source, in 300 minutes by concentration be 40mg/L quadracycline solution degradation to 9.1%, be a kind of Complexes of Uranyl photochemical catalyst for having catalytic degradation performance to quadracycline under visible light.
Description
Technical field
The present invention relates to photochemical catalysts, and in particular to a kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and its preparation
Method.
Background technique
Penicillin is had found from nineteen twenty-eight Alexander Fleming, and William Bei Nade in 1948 is from actinomycetes
Aureomycin is extracted in streptomycete, up to the present, the type of antibiotic has reached thousands of kinds, is widely used in treating human body disease
Disease, prevention livestock and poultry, aquatic products bacterial disease in.However, life and medically antibiotic excessively use and abuse, pharmacy
The discharge of the waste water such as enterprise, animal feed and culture fishery, so that contain a large amount of antibiotic pollutant in water environment at present,
The environmental problem got worse is caused, if not effectively removed, Drinking w ater, ecological environment and human health are generated
Long-term potential threat.The common technique of antibiotic has physical method, chemical method, bioanalysis, photocatalytic method in processing waste water at present
Deng.Wherein, physical method carries out the processing of antibiotic waste water in a manner of adsorbing pollutant, and there are poor selectivities and cannot be continuous
The disadvantages of operation；Biological rule has the function that removal antibiotic using the oxydasis and reduction organic molecule of microorganism,
The problems such as it is not thorough there are operating condition harshness, microorganism poisoning and degradation；The chemistry that chemical rule passes through between substance is anti-
The antibiotic in waste water should be removed, but will cause secondary pollution after treatment, and higher cost, in the industrial production by one
Fixed limitation；And photocatalysis technology is a kind of green technology for having important application prospect in the energy and environmental area, advantage
It is: applied widely, reaction rate is fast；Theoretically with permineralization pollutant and it can will not generate secondary pollution；Operating cost
It is low.Therefore, photocatalysis technology has broad application prospects in terms of removing organic pollutant.Meanwhile the preparation of photochemical catalyst
Also result in the extensive concern of people.
Organic Pollutants in Wastewater can be oxidized to H at room temperature by semiconductor light-catalyst2O、CO2Or inorganic ions etc., and
It is without secondary pollution.Currently, catalyst most commonly used in photocatalysis technology is TiO2Semiconductor material, the material is with it to biology
It is nontoxic, chemical property is stable, high catalytic efficiency under fast light burn into ultraviolet light, it is cheap and easy to get the advantages that, be acknowledged as at present most
Good photochemical catalyst.Such as the application for a patent for invention of Publication No. CN102698727A, discloses and a kind of prepare high thermal stability
Supported titanium2The method of photochemical catalyst；But TiO2There are still fatal disadvantages in practical applications for catalysis material: light
Response range is narrow, because the ultraviolet light of solar energy 4% can only be utilized, and quantum efficiency is low.In order to promote it visible
The photocatalysis performance in light region, people are to TiO2A large amount of study on the modification is expanded, such as dye photoactivation, semiconductors coupling, gold
Belong to doping, nonmetal doping etc., as the patent of invention of Publication No. CN103007938A discloses a kind of Cu doping vario-property
TiO2Photochemical catalyst and preparation method thereof, but these means still have many deficiencies.Therefore, exploitation novel photocatalysis material is
Solve the key of tetracycline antibiotics pollution problem in waste water.Uranyl ion have unique visible light wave range it is strong absorption with
Response has higher photocatalysis efficiency, is expected to solve TiO2Optical response range present in photochemical catalyst is narrow, quantum efficiency is low
The disadvantages of, become the photochemical catalyst for having much application potential, as the patent of invention of Publication No. CN103447090A discloses one kind
P-methyl benzoic acid uranyl complex photocatalyst, the catalyst have excellent degradation property under xenon lamp to rhodamine B.And
And degradation of the uranyl base complex for antibiotic pollutant in waste water, the improvement for antibiotic pollutant in environment provide
One practicable approach, also excellent basis has been established in the exploitation for uranyl based photocatalyst, and therefore, the present invention uses water
Thermal method has synthesized a kind of Complexes of Uranyl photochemical catalyst for having catalytic degradation performance to quadracycline under visible light.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of paranitrobenzoic acid uranyl of degradable quadracycline
Complex photochemical catalyst.
The technical scheme of the invention to solve the technical problem is: a kind of paranitrobenzoic acid Complexes of Uranyl light
Catalyst, molecular formula are (H2-bipy)[(UO2)4(μ3-O)2(p-nba)6], bipy=4 in molecular formula, 4 '-bipyridyls, Hp-
Nba=paranitrobenzoic acid.The cell parameter of the paranitrobenzoic acid Complexes of Uranyl photocatalyst crystals are as follows:α=85.07 (3) °, β=74.65 (3) °, γ (°)=73.38
(3) ° it is, anorthic system, belongs to P-1 space group.
Compared with the prior art, the advantages of the present invention are as follows a kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalysts, should
The molecular formula of photochemical catalyst is (H2-bipy)[(UO2)4(μ3-O)2(p-nba)6], bipy is 4,4'-Bipyridine in molecular formula,
Hp-nba is paranitrobenzoic acid, the degradable quadracycline of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst, and this is right
Methyl benzoic acid Complexes of Uranyl photochemical catalyst can use centrifugal separation method recycling and reusing, and the catalyst is avoided to may cause
Secondary pollution.
Detailed description of the invention
Fig. 1 is the molecular structure of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst of the present invention；
Fig. 2 is that the PXRD map of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst of the present invention and monocrystalline simulate PXRD map
Comparison diagram；
Fig. 3 is photocatalytic degradation curve of the paranitrobenzoic acid Complexes of Uranyl photochemical catalyst of the present invention to quadracycline
Figure.
Specific embodiment
The present invention will be described in further detail below with reference to the embodiments of the drawings.
Embodiment 1
It weighs 0.25mmol uranium acetate and is dissolved in 5mL H2In O, yellow solution is dissolved to obtain, separately weighs 0.5mmol to nitre
The 4,4'-Bipyridine of yl benzoic acid and 0.2mmol are added in above-mentioned mixed solution and stir, and solution becomes cloudy, and continues to stir
30min measures pH=2.11, and mixed solution is transferred in the ptfe autoclave liner of 23mL, sealing, and 140
72h is kept at DEG C.Yellow product is obtained after cooling, which is molecular formula (H2-bipy)[(UO2)4(μ3-O)2(Hp-
nba)6] a kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst.By yellow product grind into powder, weighs 48mg and be placed in
60mL contains in the aqueous solution that concentration is 40mg/L quadracycline, is placed in photochemical catalyst reactor, turn on agitator,
Under xenon lamp 300W radiation of visible light, the xenon lamp for being 300W with light source, it is seen that photocatalytic degradation is carried out to it under light, every 30min
Suitable solution is taken, it, 300 minutes can with the variation of quadracycline in ultraviolet-visible spectrophotometer monitoring solution after centrifugation
By the quadracycline degradation 91.9% in aqueous solution, photocatalytic degradation curve graph as shown in Figure 3 is obtained, control experiment is not
It is carried out under conditions of addition paranitrobenzoic acid Complexes of Uranyl photochemical catalyst, step is same as above.
As seen from Figure 3, it in the case where 300W xenon lamp irradiates no catalyst, does not add and states hydrochloric tetracycline simultaneously
There is no degradations, and after above-mentioned catalyst is added, obvious degradation occurs for quadracycline, after 300min, degradation rate 91.9%,
It is the photochemical catalyst for having degradation to quadracycline.The complex can use the method recycling of centrifuge separation as photochemical catalyst
It recycles.Use 2 θ angular range of Bruker D8 Focus powder diffractometer for 5-50 °, with the scanning speed of 10 °/min to this
Complexes of Uranyl photochemical catalyst is scanned, and collects the powder diffraction spectrum (PXRD) of sample at room temperature, and simulate with monocrystalline
PXRD figure comparison, perfect can be fitted, and illustrate that product is pure phase, purity is not less than 99%.
Embodiment 2
Substantially the same manner as Example 1, different only uranium acetates are substituted by uranyl nitrate.
Claims (3)
1. a kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst, it is characterised in that the molecule of the Complexes of Uranyl photochemical catalyst
Formula is (H2-bipy)[(UO2)4(μ3-O)2(p-nba)6], wherein bipy=4,4 '-bipyridyls, Hp-nba=p-nitrophenyl first
Acid, it is characterised in that the cell parameter of the crystal of the paranitrobenzoic acid Complexes of Uranyl photochemical catalyst are as follows:α (°)=85.07 (3) °, β (°)=74.65 (3) °, γ
(°)=73.38 (3) °, the photochemical catalyst are that can lead to the yellow powder sieved with 100 mesh sieve, and purity is not less than 99%, under visible light
There is the Complexes of Uranyl photochemical catalyst of catalytic degradation performance to quadracycline.
2. the preparation method of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst described in claim 1, it is characterised in that step
It is as follows:
A) it weighs 0.1~0.5mmol uranium acetate and is dissolved in 3~10mL H2In O, dissolve yellow solution is stand-by；
B) above-mentioned steps a) mixing is added in the 4,4'-Bipyridine for weighing 0.2~1mmol paranitrobenzoic acid and 0.1~0.5mmol
It is stirred in solution, solution becomes cloudy, and continues 10~60min of stirring；
C) mixed liquor of step b) is transferred in the ptfe autoclave liner of 23mL, seals 120~160 DEG C of reactions 48
~72h, is cooled to room temperature, and yellow chunked pieces body is ground into the powder sieved with 100 mesh sieve by filtering, obtains purity not less than 99%
Paranitrobenzoic acid uranyl photochemical catalyst.
3. the preparation method of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst as claimed in claim 2, it is characterised in that nitre
Sour uranyl substitutes uranium acetate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710536281.6A CN109107608A (en) | 2017-06-23 | 2017-06-23 | A kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
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| CN109939739A (en) * | 2019-04-03 | 2019-06-28 | 东华理工大学 | A kind of 5- nitro-l,2,3 benzene tricarboxylic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
| CN110003248A (en) * | 2019-04-03 | 2019-07-12 | 东华理工大学 | A kind of polycarboxylic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
| CN111495430A (en) * | 2020-04-21 | 2020-08-07 | 周口师范学院 | Target-uranyl-based poly tungstate photocatalyst and preparation method and application thereof |
| CN114558621A (en) * | 2022-03-08 | 2022-05-31 | 西安医学院 | Bis (2-carboxyethyl) isocyanurate uranyl complex photocatalyst and method |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109939739A (en) * | 2019-04-03 | 2019-06-28 | 东华理工大学 | A kind of 5- nitro-l,2,3 benzene tricarboxylic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
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| CN110003248B (en) * | 2019-04-03 | 2022-09-02 | 东华理工大学 | Polycarboxylic acid uranyl complex photocatalyst and preparation method thereof |
| CN111495430A (en) * | 2020-04-21 | 2020-08-07 | 周口师范学院 | Target-uranyl-based poly tungstate photocatalyst and preparation method and application thereof |
| CN111495430B (en) * | 2020-04-21 | 2023-03-14 | 周口师范学院 | Target-uranyl-based poly tungstate photocatalyst and preparation method and application thereof |
| CN114558621A (en) * | 2022-03-08 | 2022-05-31 | 西安医学院 | Bis (2-carboxyethyl) isocyanurate uranyl complex photocatalyst and method |
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