CN106475144A - A kind of type Fenton catalyst preparation method based on ferrous metals organic framework material - Google Patents
A kind of type Fenton catalyst preparation method based on ferrous metals organic framework material Download PDFInfo
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- CN106475144A CN106475144A CN201610855682.3A CN201610855682A CN106475144A CN 106475144 A CN106475144 A CN 106475144A CN 201610855682 A CN201610855682 A CN 201610855682A CN 106475144 A CN106475144 A CN 106475144A
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- 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]
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- 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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention discloses a kind of type Fenton catalyst preparation method based on ferrous metals organic framework material.First, by 2 sodium sulfonate of anthraquinone（AQS）Chloride, then with the ferrous metals organic framework material containing amino（NH2‑MIL(Fe)）Generation chemical reaction, by forming S N covalent bond, prepares AQS NH MIL (Fe) catalyst.The catalyst activity is high, environmental friendliness, it is easy to reclaim, and repeats and utilizes, organic pollutants of efficiently degrading in wider pH value range, has great application prospect.
Description
Technical field
The invention belongs to field of waste water treatment, and in particular to a kind of class based on ferrous metals-organic framework material
Fenton method for preparing catalyst.
Background technology
At present, based on potentiometric titrations（SO4 −•）Fenton-like high-level oxidation technology be subject to favor both domestic and external.Cross
Sulfate（S2O8 2−）, can be activated by ultraviolet light, heat, transition metal etc. and produce SO4 −•.In these active modes, transition metal
Ion-activated due to less energy consumption, expense low, application is more universal, but exists and can not recycle, and there is certain poison to environment
The shortcomings of property.Therefore, cause the concern of people based on the different-phase catalyst of transition metal ions.Transition metal ions is loaded to
On the carriers such as activated carbon, zeolite, silica and aluminum oxide, different-phase catalyst is prepared；Magnetic iron ore, Co3O4、RuO2, FeS, Huang Tie
Ore deposit and cobalt acid iron etc. are also highly useful as the catalyst of activation persulfate.These catalyst generally existing transition metal ion content
The problems such as low, catalysis activity has much room for improvement, metal ion is easy to run off, so, the preparation of efficient stable catalyst be people always
The focus of research.
At present, MIL（Materials of the Institute Lavoisier）Series material has become heterogeneous catalysis
The most commonly used metal-organic framework materials of area research（Metal-organic frameworks, MOFs）One of, MIL system
Row material is widely used to catalytic field.Research discovery, iron-based MIL material such as MIL-101 (Fe), MIL-100 (Fe), MIL-
53 (Fe) and MIL-88B (Fe) etc. can efficiently activate acid orange 7 in persulfate degradation water（Applied Surface
Science, 2016, 369: 130-136.）.Fe (II) the@MIL-100 (Fe) of load Fe (II) ion is that a kind of performance is excellent
Good Fenton-like different-phase catalyst, methyl orange in effective catalytic decomposition hydrogen peroxide oxidation degradation water（J. Mol. Catal.
A: Chem. 2015, 400: 81-89.）.
Redox mediators as electron transit mediator, can by the circulation conversion of its oxidation state and reduction-state accelerate electronics by
Primary electron donor is to the transmission of final electron acceptor, so that reaction rate improves one arrives several orders of magnitude.Natural organic
Matter, polyoxometallate, activated carbon and quinones substance etc. all can be processed using Fenton method organic as redox mediators
During waste water, the oxidative degradation of organic matter can be effectively facilitated.In actual applications, dissolvable redox amboceptor constantly must add
It is added to reaction system and the purpose for improving organic pollutant removal rate is can be only achieved, this is by the raising for causing operating cost and secondary dirt
Dye.And study and show, loaded on carrier and can solve the problem that the problems referred to above.
The present invention is by the redox mediators anthraquinone-2-sodium of function admirable（AQS）By way of forming covalent bond
It is bonded on iron-based MIL (Fe) material containing amino, prepares AQS-NH-MIL (Fe) catalyst, activation persulfate oxidation drop
Solution organic pollutants.NH2- MIL (Fe) material energy efficient absorption is enriched with organic pollutants, is conducive to active metal point
Position contact of the iron with organic pollution；Meanwhile, AQS accelerates the transfer of electronics as redox mediators, promotes Fe3+To Fe2+Hurry up
Speed conversion, so as to effectively facilitate the catalyzing oxidizing degrading of Organic substance in water.So, the present invention is wide for processing organic wastewater offer
Prospect.
Content of the invention
The invention aims to solving the deficiencies in the prior art, provide a kind of based on ferrous metals-organic backbone material
The type Fenton catalyst preparation method of material, the catalyst has that catalysis activity is high, has good stability, easily reclaims, environmental friendliness
And inexpensive the advantages of.
The technical scheme is that：First by anthraquinone-2-sodium（AQS）Chloride, then with the iron containing amino
Base MIL material（NH2-MIL(Fe)）Generation chemical reaction, by forming S-N covalent bond, prepares AQS-NH-MIL (Fe) catalysis
Agent.
A kind of preparation method of the type Fenton catalyst based on ferrous metals-organic framework material, comprises the following steps：
（1）Anthraquinone-2-sodium（AQS）Chloride：0.279 g AQS is scattered in 20 mL thionyl chloride solution, is added
0.5 mL N,N-dimethylformamide（DMF）As catalyst, 12 h are heated to reflux, with Rotary Evaporators by said mixture
In solvent remove, you can obtain the AQS of chloride（AQSCl）.
（2）NH2The preparation of-MIL (Fe)：By 2- amino terephthalic acid (TPA) ultrasonic disperse in N,N-dimethylformamide
（DMF）In, pH value is adjusted with a certain amount of NaOH solution, add FeCl3·6H2O or Fe (NO3)3·9H2One kind in O, has made
Machine part and Fe3+Concentration is respectively 15.0～36.2 g/L and 9.3～11.2 g/L, and 15 min of magnetic agitation, makes at room temperature
Which mixes, and is then encapsulated in, with teflon-lined reactor, reacting 5～24 h at 100～160 DEG C,
It is cooled to room temperature；Centrifugation, is washed with water, ethanol at 25～60 DEG C, is finally vacuum dried 24 h at 60 DEG C
, prepared NH2- MIL (Fe) is NH2-MIL-53(Fe)、NH2- MIL-88B (Fe) or NH2In-MIL-101 (Fe)
A kind of.
（3）AQS-NH-MIL (Fe) catalyst preparation：By 0.356 g NH2- MIL (Fe) is scattered in 10 mL acetonitriles, plus
Enter 2 mL pyridines, 5 min of magnetic agitation；10 mL acetonitriles are added in 0.05～1.0 g AQSCl, instill NH at 0 DEG C2-
In MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, finally at 60 DEG C
Lower vacuum drying 24h.
Usefulness of the present invention is mainly reflected in：
（1）NH2- MIL (Fe) with huge specific surface area and larger aperture, organic matter that can be in adsorption and enrichment water,
NH2The loose structure of-MIL (Fe) makes its own have good permeability, is conducive to the mass transfer of reactant and product, so as to promote
Enter the reaction of free radical and organic matter；
（2）In AQS-NH-MIL (Fe) catalyst, AQS is a kind of redox mediators of good performance, and electronics quickly occurs
Transfer, promotes Fe3+To Fe2+Rapid conversion, so as to accelerate the circulation of iron, promotes the carrying out of embryonic stem-like cells, is conducive in water
The degraded of organic pollution.
（3）AQS-NH-MIL (Fe) catalyst gives full play to the absorption property of MIL (Fe) and the electricity of catalytic performance and AQS
Sub- transfer performance, had both had higher catalysis activity, overcame water-soluble AQS to be easy to the shortcoming being lost in again.
（4）Catalyst preparation process is simple, and reaction condition is gentle, low cost, and is easily recycled, and repeats and utilizes, ring
Border is friendly, and can be mass-produced application.
Description of the drawings
Fig. 1 is the x-ray diffraction pattern of prepared AQS-NH-MIL-101 (Fe) in the embodiment of the present invention 1.
Fig. 2 is the scanning electron microscope (SEM) photograph of prepared AQS-NH-MIL-101 (Fe) in the embodiment of the present invention 1.
Specific embodiment
The specific embodiment of the present invention is further explained with reference to embodiment, but application claims
The scope of protection is not limited to that.
Embodiment 1
（1）The preparation of AQS-NH-MIL-101 (Fe) catalyst
Anthraquinone-2-sodium（AQS）Chloride：0.279 g AQS is scattered in 20 mL thionyl chloride solution, adds 0.5
ML N,N-dimethylformamide（DMF）As catalyst, 12 h are heated to reflux, will be molten in said mixture with Rotary Evaporators
Agent is removed, you can obtain the AQS of chloride（AQSCl）.
NH2The preparation of-MIL-101 (Fe)：By 0.225 g ultrasonic disperse of 2- amino terephthalic acid (TPA) in 15 mL DMF,
It is subsequently adding 0.675 g FeCl3·6H2O, 15 min of magnetic agitation；In teflon-lined autoclave, 110
24 h are reacted at DEG C；It is cooled to room temperature, centrifugation, washed with water, ethanol, at 60 DEG C, be finally vacuum dried 24 h.
The preparation of AQS-NH-MIL-101 (Fe) catalyst：By 0.356 g NH2- MIL-101 (Fe) is scattered in 10 mL second
In nitrile solution, 2 mL pyridines, 5 min of magnetic agitation is added；10 mL acetonitriles are added in 0.2 g AQSCl, are instilled at 0 DEG C
NH2In-MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, is finally existed
24 h are vacuum dried at 60 DEG C.
（2）Catalyst performance evaluation
Organic pollution bisphenol-A is selected to study the performance of prepared catalyst as probe molecule.By 5 mg catalyst and over cure
Sour potassium solution is added in bisphenol-A waste water, and reactant liquor cumulative volume is 25 mL, and wherein bisphenol-A and potassium peroxydisulfate concentration is respectively 60
Mg/L and mg/L, magnetic agitation under room temperature, organic pollutants are degraded；Separated in time is sampled, and water sample is passed through
After filter, its concentration is determined using high performance liquid chromatograph, finally calculate bisphenol-A degradation rate.
5 mg AQS-NH-MIL-101 (Fe) and NH are separately added in bisphenol-A waste water2- MIL-101 (Fe) is used as catalysis
Agent, after 120 min of reaction, bisphenol-A degradation rate is respectively 97.57% and 60.56%.
Embodiment 2
（1）The preparation of AQS-NH-MIL-53 (Fe) catalyst
Anthraquinone-2-sodium（AQS）Chloride：With embodiment 1.
NH2The preparation of-MIL-53 (Fe)：By 0.543 g ultrasonic disperse of 2- amino terephthalic acid (TPA) in 15 mL DMF,
It is subsequently adding 0.8109 g FeCl3·6H2O, 15 min of magnetic agitation；In teflon-lined autoclave, 150
5 h are reacted at DEG C；It is cooled to room temperature, centrifugation, washed with water, ethanol, at 60 DEG C, be finally vacuum dried 24 h obtain
NH2-MIL-53（Fe）.
The preparation of AQS-NH-MIL-53 (Fe) catalyst：By 0.356 g NH2- MIL-53 (Fe) is scattered in 10 mL acetonitriles
In solution, 2 mL pyridines, 5 min of magnetic agitation is added；10 mL acetonitriles are added in 0.2 g AQSCl, are instilled at 0 DEG C
NH2In-MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, is finally existed
24 h are vacuum dried at 60 DEG C.
（2）Catalyst performance evaluation
With embodiment 1.
5 mg AQS-NH-MIL-53 (Fe) and NH are separately added in bisphenol-A waste water2- MIL-53 (Fe) is used as catalysis
Agent, after 120 min of reaction, bisphenol-A degradation rate is respectively 92.49% and 67.37%.
Embodiment 3
（1）The preparation of AQS-NH-MIL-88B (Fe) composite
Anthraquinone-2-sodium（AQS）Chloride：With embodiment 1.
NH2The preparation of-MIL-88B (Fe)：By 0.379 g NH2- BDC ultrasonic disperse is in 15 mL DMF and 1.2 mL 2
In mol/L NaOH mixed solution, 1.212 g Fe (NO are subsequently adding3)3·9H2O, 15 min of magnetic agitation；In polytetrafluoroethyl-ne
In the autoclave of alkene liner, 12 h at 100 DEG C, are reacted；It is cooled to room temperature, centrifugation, washed with water, ethanol, finally
24 h are vacuum dried at 60 DEG C.
The preparation of AQS-NH-MIL-88B (Fe) catalyst：By 0.356 g NH2- MIL-88B (Fe) is scattered in 10 mL second
In nitrile solution, 2 mL pyridines, 5 min of magnetic agitation is added；10 mL acetonitriles are added in 0.2 g AQSCl, are instilled at 0 DEG C
NH2In-MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, is finally existed
24 h are vacuum dried at 60 DEG C.
（2）Catalyst performance evaluation
With embodiment 1.
5 mg AQS-NH-MIL-88B (Fe) and NH are separately added in bisphenol-A waste water2- MIL-88B (Fe) is used as catalysis
Agent, after 120 min of reaction, bisphenol-A degradation rate is respectively 88.65% and 62.74%.
Embodiment 4
（1）The preparation of AQS-NH-MIL-101 (Fe) catalyst
Anthraquinone-2-sodium（AQS）Chloride：With embodiment 1.
NH2The preparation of-MIL-101 (Fe)：By 0.225 g ultrasonic disperse of 2- amino terephthalic acid (TPA) in 15 mL DMF,
It is subsequently adding 0.675 g FeCl3·6H2O, 15 min of magnetic agitation；In teflon-lined autoclave, 110
24 h are reacted at DEG C；It is cooled to room temperature, centrifugation, washed with water, ethanol, at 60 DEG C, be finally vacuum dried 24 h.
The preparation of AQS-NH-MIL-101 (Fe) catalyst：By 0.356 g NH2- MIL-101 (Fe) is scattered in 10 mL second
In nitrile solution, 2 mL pyridines, 5 min of magnetic agitation is added；10 mL acetonitriles are added in 0.05 g AQSCl, are dripped at 0 DEG C
Enter NH2In-MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, finally
24 h are vacuum dried at 60 DEG C.
（2）Catalyst performance evaluation
With embodiment 1.
5 mg AQS-NH-MIL-101 (Fe) and NH are separately added in bisphenol-A waste water2- MIL-101 (Fe) is used as catalysis
Agent, after 120 min of reaction, bisphenol-A degradation rate is respectively 85.39% and 60.56%.
Embodiment 5
（1）The preparation of AQS-NH-MIL-101 (Fe) catalyst
Anthraquinone-2-sodium（AQS）Chloride：With embodiment 1.
NH2The preparation of-MIL-101 (Fe)：By 0.225 g ultrasonic disperse of 2- amino terephthalic acid (TPA) in 15 mL DMF,
It is subsequently adding 0.675 g FeCl3·6H2O, 15 min of magnetic agitation；In teflon-lined autoclave, 110
24 h are reacted at DEG C；It is cooled to room temperature, centrifugation, washed with water, ethanol, at 60 DEG C, be finally vacuum dried 24 h.
The preparation of AQS-NH-MIL-101 (Fe) catalyst：By 0.356 g NH2- MIL-101 (Fe) is scattered in 10 mL second
In nitrile solution, 2 mL pyridines, 5 min of magnetic agitation is added；10 mL acetonitriles are added in 1.0 g AQSCl, are instilled at 0 DEG C
NH2In-MIL (Fe), acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, is finally existed
24 h are vacuum dried at 60 DEG C.
（2）Catalyst performance evaluation
With embodiment 1.
5 mg AQS-NH-MIL-101 (Fe) and NH are separately added in bisphenol-A waste water2- MIL-101 (Fe) is used as catalysis
Agent, after 120 min of reaction, bisphenol-A degradation rate is respectively 90.28% and 60.56%.
Claims (1)
1. a kind of type Fenton catalyst preparation method based on ferrous metals-organic framework material, it is characterised in that：By following
Step is carried out,
（1）Anthraquinone-2-sodium（AQS）Chloride：0.279 g AQS is scattered in 20 mL thionyl chloride solution, is added
0.5 mL N,N-dimethylformamide（DMF）As catalyst, 12 h are heated to reflux, with Rotary Evaporators by said mixture
In solvent remove, you can obtain the AQS of chloride（AQSCl）；
（2）NH2The preparation of-MIL (Fe)：By 2- amino terephthalic acid (TPA) ultrasonic disperse in N,N-dimethylformamide（DMF）In,
PH value is adjusted with a certain amount of NaOH solution, add FeCl3·6H2O or Fe (NO3)3·9H2One kind in O, make organic ligand and
Fe3+Concentration is respectively 15.0～36.2 g/L and 9.3～11.2 g/L, at room temperature 15 min of magnetic agitation so as to which mixing is all
Even, it is then encapsulated in, with teflon-lined reactor, reacting 5～24 h at 100～160 DEG C, being cooled to room
Temperature；Centrifugation, is washed with water, ethanol at 25～60 DEG C, is finally vacuum dried 24 h at 60 DEG C, made
Standby NH2- MIL (Fe) is NH2-MIL-53(Fe)、NH2- MIL-88B (Fe) or NH2One kind in-MIL-101 (Fe)；
（3）AQS-NH-MIL (Fe) catalyst preparation：By 0.356 g NH2- MIL (Fe) is scattered in 10 mL acetonitriles, adds 2
ML pyridine, 5 min of magnetic agitation；10 mL acetonitriles are added in 0.05～1.0 g AQSCl, instill NH at 0 DEG C2-MIL
(Fe), in acetonitrile and pyridine mixtures, 24 h of magnetic agitation under normal temperature；Centrifugation, is washed with ethanol, finally at 60 DEG C
Vacuum drying 24h.
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Cited By (11)
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| CN107008507A (en) * | 2017-06-08 | 2017-08-04 | 合肥工业大学 | A kind of mesoporous Fe bases MOF@AgI high efficiency composition visible-light photocatalysis materials and its preparation method and application |
| CN107519934A (en) * | 2017-07-21 | 2017-12-29 | 济南大学 | A kind of ferrous metals organic framework material type Fenton catalyst preparation method of ferrocene modification |
| CN107917910A (en) * | 2017-11-16 | 2018-04-17 | 武汉轻工大学 | It is a kind of to be used to detect class enzyme test peper of hydrogen peroxide and its preparation method and application |
| CN108176414A (en) * | 2017-12-12 | 2018-06-19 | 上海大学 | Catalyst MnFe2O4- MIL-53 (Al) magnetic composite, preparation method and application |
| CN108393097A (en) * | 2018-05-15 | 2018-08-14 | 济南大学 | A kind of ferrous metals containing redox mediators-organic framework material type Fenton catalyst preparation method |
| CN110331001A (en) * | 2019-07-11 | 2019-10-15 | 福建师范大学福清分校 | The preparation method and applications of the immobilized ionic liquid of ferrous metals organic backbone |
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| CN107519934B (en) * | 2017-07-21 | 2020-06-05 | 济南大学 | Preparation method of iron-based metal-organic framework material Fenton-like catalyst modified by ferrocene |
| CN107519934A (en) * | 2017-07-21 | 2017-12-29 | 济南大学 | A kind of ferrous metals organic framework material type Fenton catalyst preparation method of ferrocene modification |
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| CN110803754A (en) * | 2019-10-25 | 2020-02-18 | 南昌大学 | Fenton reagent capable of efficiently degrading organic pollutants in alkaline environment and application thereof |
| CN110803754B (en) * | 2019-10-25 | 2022-03-29 | 南昌大学 | Fenton reagent capable of efficiently degrading organic pollutants in alkaline environment and application thereof |
| CN111408413A (en) * | 2020-03-30 | 2020-07-14 | 浙江工商大学 | Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof |
| CN111408413B (en) * | 2020-03-30 | 2022-09-20 | 浙江工商大学 | Modified carbon nitride/Fe-based MOF composite material and preparation method and application thereof |
| CN112661253A (en) * | 2020-12-18 | 2021-04-16 | 长沙理工大学 | Application of iron-based metal organic framework material in degradation of imidacloprid |
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