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Preparation method and application of Fe3O4/MIL-101(Cr)

A 3.9H2O, NH3.H2O technology, applied in chemical instruments and methods, adsorption water/sewage treatment, alkali metal oxides/hydroxides, etc., can solve the problem of large particle size of magnetic nanoparticles and reduced surface area of ​​composite materials , Magnetic weakening and other problems, to achieve the effect of stable quality, large surface area and strong magnetism

Active Publication Date: 2015-12-30
SHENYANG PHARMA UNIVERSITY
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  • Abstract
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  • Application Information

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Problems solved by technology

Because this method is only applicable to MOFs composed of easily soluble carboxylic acid ligands, it is impossible to encapsulate the large surface area MIL-101 composed of insoluble carboxylic acid ligands on Fe 3 o 4 Surface (F.Ke, L.G. Qiu, Y.P. Yuan, X. Jiang, J.F. Zhu. Fe 3 o 4 MOFcore–shellmagneticmicrosphereswithadesignablemetal–organicframeworkshell.JournalofMaterialsChemistry, 2012, 22, 9497-9500.); (2) In-situ magnetization of MIL-101 by electrostatic attraction
This material only relies on electrostatic force to combine, and the stability is poor (S.H.Huo, X.P.Yan. Facilemagnetizationofmetal-organicframeworkMIL-101formagneticsolid-phaseextractionofpolycycliccarromatichydrocarbonsinenvironmentalwatersamples[J].Analyst,2012,137,3445-3451.); (3) pre-synthesized The magnetic nanoparticles are mixed with the raw materials for synthesizing MOFs, and magnetic MOFs materials are prepared by hydrothermal method
But the size of the pre-synthesized magnetic nanoparticles is large, which reduces the surface area of ​​the composite material, weakens the magnetism, and the yield is low (Y.F.Huang, Y.QWang, Q.S.Zhao, YLi, J.M.Zhang, FacileinsituhydrothermalsynthesisofFe 3 o 4 MIL-101 composites for removing textile dyes [J]. RSCAdvances, 2014, 4, 47921-47924.)

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  • Preparation method and application of Fe3O4/MIL-101(Cr)
  • Preparation method and application of Fe3O4/MIL-101(Cr)
  • Preparation method and application of Fe3O4/MIL-101(Cr)

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Experimental program
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Effect test

Embodiment 1

[0031] (1) MIL-101(Cr) was synthesized by hydrothermal method. Weigh 800mgCr(NO 3 ) 3 9H 2 O and 332mg of terephthalic acid, placed in a polytetrafluoroethylene liner, add 0.4mL of hydrofluoric acid with a mass fraction of 35% and 9.5mL of pure water, ultrasonic for 15min, after mixing evenly, cover and move to a stainless steel reaction kettle After inner sealing, place in an oven at 215° C., react for 9 hours, and then cool down to room temperature naturally. The product is a green powder, which is washed three times with N,N-dimethylformamide, ethanol and pure water respectively, centrifuged at high speed and dried for use.

[0032] (2) Preparation of Fe by reduction precipitation method 3 o 4 / MIL-101 (Cr) composite material. Weigh 0.125g of MIL-101(Cr), place it in a 100mL three-necked flask, add 60mL of 0.05mol / L FeCl 3 After the solution was shaken and mixed evenly, it was sonicated at room temperature 25°C for 30 minutes, and then nitrogen gas was passed into th...

Embodiment 2

[0035] (1) MIL-101(Cr) was synthesized by hydrothermal method. Weigh 800mgCr(NO 3 ) 3 9H 2 O and 332mg of terephthalic acid, placed in a polytetrafluoroethylene liner, add 0.4mL of hydrofluoric acid with a mass fraction of 35% and 9.5mL of pure water, ultrasonic for 15min, after mixing evenly, cover and move to a stainless steel reaction kettle After inner sealing, place in an oven at 220° C., react for 8 hours, and then cool to room temperature naturally. The product is a green powder, which is washed three times with N,N-dimethylformamide, ethanol and pure water respectively, centrifuged at high speed and dried for use.

[0036] (2) Preparation of Fe by reduction precipitation method 3 o 4 / MIL-101 (Cr) composite material. Weigh 0.500g MIL-101(Cr), place it in a 100mL three-necked flask, add 30mL FeCl with a concentration of 0.1mol / L 3 After the solution was shaken and mixed evenly, it was sonicated at room temperature 25°C for 30 minutes, then nitrogen gas was passed...

Embodiment 3

[0039] (1) MIL-101(Cr) was synthesized by hydrothermal method. Weigh 800mgCr(NO 3 ) 3 9H 2 O and 332mg of terephthalic acid, placed in a polytetrafluoroethylene liner, add 0.35mL of hydrofluoric acid with a mass fraction of 40% and 9.5mL of pure water, ultrasonic for 15min, after mixing evenly, cover and move to a stainless steel reaction kettle After inner sealing, place in an oven at 225° C., react for 7 hours, and then cool to room temperature naturally. The product is a green powder, which is washed three times with N,N-dimethylformamide, ethanol and pure water respectively, centrifuged at high speed and dried for use.

[0040] (2) Preparation of Fe by reduction precipitation method 3 o 4 / MIL-101 (Cr) composite material. Weigh 1.000g of MIL-101(Cr), place it in a 100mL three-necked flask, add 15mL of 0.2mol / LFeCl 3 After the solution was oscillated and mixed evenly, it was sonicated at room temperature 25°C for 30 minutes, then nitrogen gas was passed into the thre...

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Abstract

The invention relates to the technical field of magnetic metal organic framework materials, in particular to a preparation method and application of Fe3O4 / MIL-101(Cr). The method includes the steps of preparing MIL-101(Cr) material through a hydrothermal method to serve as a template, and generating Fe3O4 particles in situ in holes of MIL-101(Cr) through a reduction co-precipitation method under the ultrasonic conduction and in a nitrogen protection state. The Fe3O4 / MIL-101(Cr) composite obtained through the method is strong in magnetism, large in surface area, shortened in synthesis time, controllable in synthesis condition, novel in synthesis method, simple and easy to repeat, stable and controllable in prepared material quality, and capable of being synthesized in batches. The Fe3O4 / MIL-101(Cr) composite is good in effect and can be repeatedly used six times or more when used for adsorbing and removing acid dyes in environmental water.

Description

technical field [0001] The invention belongs to the technical field of magnetic metal organic framework materials, and relates to a magnetic metal organic framework material Fe 3 o 4 / MIL-101 (Cr) fast and simple new preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs) are a new class of porous crystalline materials, which consist of metal ions or metal clusters as coordination centers and self-assembled networks with oxygen- or nitrogen-containing organic ligands through coordination. shaped skeleton structure. MOFs have the advantages of large surface area, flexible synthesis method, diverse types and properties, adjustable pore and crystal size, modifiable skeleton, good thermal and solvent stability, etc., making them have great potential for application in gas and liquid phase adsorption related fields. However, most MOFs have poor water resistance, which limits their application in aqueous phase. Only MIL-101(Cr), MIL-10...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/28B01J20/30C02F1/28
Inventor 侯晓虹王婷张聪璐
Owner SHENYANG PHARMA UNIVERSITY
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