CN107042087A - A kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material - Google Patents
A kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material Download PDFInfo
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- CN107042087A CN107042087A CN201710044504.7A CN201710044504A CN107042087A CN 107042087 A CN107042087 A CN 107042087A CN 201710044504 A CN201710044504 A CN 201710044504A CN 107042087 A CN107042087 A CN 107042087A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28009—Magnetic properties
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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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
- B01J20/3214—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating characterised by the method for obtaining this coating or impregnating
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
Abstract
A kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material, is related to the preparation of core-shell material.The method for having the advantages that a kind of Situ Hydrothermal convieniently synthesized, without added metal ion gun prepares magnetic metal organic framework core-shell material is provided.FeCl is sequentially added into container3·6H2O, anhydrous sodium acetate and ethylene glycol, after mixing, are transferred in reactor, and heating response is cooled to after room temperature, and gained black product is washed with ethanol, after drying, produce Fe3O4Micron ball；Successively by obtained Fe3O4Micron ball, trimesic acid, water add reactor, mix, and after heating response, obtain brown solid sample, are cooled to after room temperature, dry under nitrogen atmosphere, and gained sample is magnetic metal organic framework core-shell material, as Fe3O4@MIL 101 (Fe) core-shell material.
Description
Technical field
The present invention relates to the preparation of core-shell material, magnetic metal organic framework core is prepared more particularly, to a kind of Situ Hydrothermal
The method of shell material.
Background technology
Metal-organic framework materials (Metal organic frameworks, MOFs) be using metal ion as tie point,
Organic ligand for support Special composition 3D extended structures a class Porous coordination polymer, with regulatable aperture size and can
The advantages of channel surfaces of modification, extremely-low density, superhigh specific surface area, in hydrogen storage, CO2Capture, Chemical Decomposition, urge
The fields such as change, drug delivery, biomedical imaging and chemical sensor are widely used.However, metal organic framework
The application of material there are problems that separating and reclaim, it usually needs realize that the separation to material is returned using the operation such as centrifugation
Receive.In order to solve the above problems, the organic bone of magnetic metal that researcher is prepared for nucleocapsid structure by layer-by-layer
Frame material, in the method, typically first by Fe3O4Micron ball carries out TGA functionalization, further adds metal ion, profit
With it Fe is coated on carboxyl formation coordinate bond3O4Micron ball, is eventually adding organic ligand, is formed with nucleocapsid structure
Fe3O4@MOFs, such as Fe3O4@MIL-101(Fe)(J.Mater.Chem.2012,22,9497-9500)、Fe3O4@Cu3(BTC)2-
NH2(catalysis journal, 2016,37 (3), 420-427), Fe3O4@IRMOF-3 (functional material, 2015,46,6039-6041),
Fe3O4@UiO-66 (Chinese Journal of Inorganic Chemistry, 2016,32 (4), 609-616).Fe3O4@MOFs materials had both had what MOFs had
High-specific surface area and porosity, have the easy recycle and reuse characteristic that magnetic material has again.It is slightly inadequate, these
Fe3O4@MOFs materials need relatively complicated LBL self-assembly step in preparation process, but also need to carry out function to magnetic core
Change and added metal ion.
The content of the invention
It is an object of the invention to for existing Fe3O4To Fe the need for the preparation of@MOFs materials is existing3O4Carry out work(
Energyization, added metal ion gun, cumbersome LBL self-assembly etc. are not enough there is provided with it is convieniently synthesized, without added metal ion
The method that a kind of Situ Hydrothermal of the advantages of source prepares magnetic metal organic framework core-shell material.
The magnetic metal organic framework core-shell material is Fe3O4@MIL-101 (Fe) core-shell material, its preparation method includes
Following steps：
1) Fe is prepared3O4Micron ball；
2) magnetic metal organic framework core-shell material, i.e. Fe are prepared3O4@MIL-101 (Fe) core-shell material.
In step 1) in, the preparation Fe3O4The specific method of micron ball can be：FeCl is sequentially added into container3·
6H2O, anhydrous sodium acetate and ethylene glycol, after mixing, are transferred in reactor, and heating response is cooled to after room temperature, by gained
Black product is washed with ethanol, after drying, produces Fe3O4Micron ball；
The FeCl3·6H2O, ethylene glycol, the proportioning of sodium acetate can be 1.6g: 60mL: 4.3g, wherein FeCl3·6H2O
Calculated by mass with sodium acetate, ethylene glycol is in terms of volume；The temperature of the heating response can be 200 DEG C, heating response when
Between can be 8h, the number of times of the washing can be 6~8 times；The drying can be using vacuum drying, and the temperature of the drying can be 60
DEG C, the dry time can be 8h；Gained Fe3O4A diameter of 200~400nm of micron ball.
In step 2) in, the specific steps of the preparation magnetic metal organic framework core-shell material can be：
Successively by step 1) obtained Fe3O4Micron ball, trimesic acid, water add reactor, mix, after heating response,
Brown solid sample is obtained, is cooled to after room temperature, is dried under nitrogen atmosphere, gained sample is magnetic metal organic framework nucleocapsid
Material, i.e. Fe3O4@MIL-101 (Fe) core-shell material；The Fe3O4Micron ball, trimesic acid, the proportioning of water are 0.2g:
0.3g: 4.28mL, wherein Fe3O4Micron ball, trimesic acid are calculated by mass, and water is in terms of volume；The water can use ultrapure
Water；The temperature of the heating response can be 150~180 DEG C, and time of heating response can be and 12~18h；The temperature of the drying
Degree can be 60 DEG C, and the dry time can be 8h；Obtained magnetic metal organic framework core-shell material is with nucleocapsid structure
Spherical micro particles, Fe3O4Micron ball is core, a diameter of 200~400nm, and MIL-101 (Fe) is shell, and thickness is 40~100nm,
The particle diameter of magnetic metal organic framework core-shell material is 240~500nm.
The present invention has advantages below：
1) Fe of synthesis3O4@MIL-101 (Fe) only need one step hydro thermal method to can be achieved, simple synthetic method, and can be with
The thickness of MIL-101 (Fe) shell is controlled simply by the control reaction time, without carrying out functionalization, additional gold to magnetic core
Belong to the step such as ion gun and LBL self-assembly.
2) Fe of synthesis3O4@MIL-101 (Fe) have higher adsorption efficiency to organic dyestuff and magnetic response is fast, easily return
Receive and utilize, be expected to be used widely in water treatment field.
Brief description of the drawings
Fig. 1 is Fe of the present invention3O4@MIL-101's (Fe) prepares schematic diagram.
Fig. 2 is Fe of the present invention3O4Micron ball and Fe3O4@MIL-101 (Fe) ESEM and transmission electron microscope picture.In Fig. 1
In, a, d are respectively Fe3O4The ESEM and transmission electron microscope picture of micron ball；B, c and e, f are respectively Fe3O4@MIL-101(Fe)
ESEM and transmission electron microscope picture.
Fig. 3 is MIL-101 (Fe) simulation XRD spectra and Fe3O4@MIL-101 (Fe) actual XRD spectra.
The Fe that Fig. 4 is prepared for the present invention3O4@MIL-101 (Fe) Fe3O4@MIL-101 (Fe) transmission electron microscope picture.In figure
In 4, a, reaction time are 12h, and b, reaction time are 16h, and c, reaction time are 18h.
Fig. 5 is Fe of the present invention3O4Micron ball and Fe3O4@MIL-101 (Fe) N2Adsorption-desorption isothermal curve.
Fig. 6 is Fe of the present invention3O4Micron ball and Fe3O4@MIL-101 (Fe) graph of pore diameter distribution.
Fig. 7 is Fe3O4Micron ball and Fe3O4(insertion figure represents Fe to@MIL-101 (Fe) magnetization curve3O4@MIL-101
(Fe) magnetic response characteristic of the material under additional magnetic fields)
Fig. 8 is Fe of the present invention3O4Adsorption capacities of the@MIL-101 (Fe) to different organic dyestuff.In Fig. 8 abscissa,
1. alkali blue 6B；2. eriochrome black T；3. rhodamine B；4. acid chromium blue k；5. it is indigo；6. acid fuchsin；7. methylene blue.
Fig. 9 is Fe of the present invention3O4Adsorption efficiency values of the@MIL-101 (Fe) after recycling for several times to methylene blue.
Embodiment
Following examples will the present invention is further illustrated with reference to accompanying drawing.
Fig. 1 provides Fe of the present invention3O4@MIL-101's (Fe) prepares schematic diagram.The method comprises the steps of firstly, preparing Fe3O4It is micro-
Rice ball, adds trimesic acid, using the strong coordination ability of carboxylic acid, with Fe3O4Fe in micron ball3+Directly occurs coordination anti-
Should, growth in situ Fe3O4@MIL-101(Fe).The reaction only needs a step to complete, without being modified magnetic core, additional gold
Category source, and without tedious steps such as LBL self-assemblies.
Fig. 2 provides Fe of the present invention3O4Micron ball and Fe3O4@MIL-101 (Fe) ESEM and transmission electron microscope picture.In figure
In 2, a, d are respectively Fe3O4The ESEM and transmission electron microscope picture of micron ball；B, c and e, f are respectively Fe3O4@MIL-101(Fe)
ESEM and transmission electron microscope picture.As shown in Fig. 2 a and d, most of Fe3O4Particle is spherical in shape, particle diameter 367~504nm it
Between.Fig. 2 b and c show, in Fe3O4Particle shows after growth in situ MIL-101 (Fe) that total particle diameter increase is 472~654nm.
From Fig. 2 e and f can with it is further seen that, the composite has uneven electron density, shows the deeper core of color and face
The shallower shell of color, the thickness of shell is about 73.5nm.
Fig. 3 provides Fe of the present invention3O4The X ray diffracting spectrum of@MIL-101 (Fe) core-shell material and pass through crystallography number
According to MIL-101 (Fe) X ray diffracting spectrum of simulation.From figure 3, it can be seen that belonging to Fe3O4Characteristic diffraction peak have 30.2 °
(220), 35.6 ° (311), 43.3 ° (400), 57.3 ° (511) and 63 ° (440) (JCPDS file 89-4319).In addition,
2.1 ° (111), 3.4 ° (022), 3.9 ° (113), 5.4 ° (333), 11.1 ° (428), 13.8 ° (088) and 20.1 ° (4814) go out
Existing diffraction maximum is also consistent with MIL-101 (Fe) simulation collection of illustrative plates, and the above results illustrate Fe3O4Coexisted with MIL-101 (Fe)
In the product of synthesis.The electronic microscope photos result of complex chart 2, the product for illustrating synthesis is Fe3O4@MIL-101 (Fe) core-shell material.
Fig. 4 provides the reaction time for (a) 12；(b)16；(c) Fe of the present invention prepared by 18h3O4@MIL-101 (Fe) nucleocapsid material
The transmission electron microscope picture of material.As shown in Figure 4, with the extension in reaction time, the thickness of shell increases to 148nm by 73.5nm, the knot
Fruit explanation can control the thickness of MIL-101 (Fe) shell by controlling the reaction time.
Fig. 5 and 6 provides Fe of the present invention3O4And Fe3O4@MIL-101 (Fe) N2Adsorption-desorption isothermal curve and pore-size distribution
Figure.Fig. 5 shows Fe3O4Adsorption/desorption curve belongs to IV type thermoisopleths, and result of calculation shows that its specific surface area and pore volume are only
26m2g-1, pore volume is 0.048cm3g-1, its aperture focuses primarily upon 2~4nm macropore range (Fig. 6).Fe3O4@MIL-101
(Fe) adsorption/desorption curve illustrates that it has typical I types thermoisopleth, without hysteresis loop, belongs to pure pore type and returns stagnant ring, its
Specific surface area is up to 730m2g-1, pore volume is 0.4526cm3g-1.Fig. 6 further demonstrate that its aperture focus primarily upon 1.24nm and
1.75nm micropore.The above results illustrate the Fe of synthesis3O4@MIL-101 (Fe) have larger specific surface area and pore volume, have
Beneficial to its application in terms of absorption and separation.
Fig. 7 is given by oscillating magnetic field sample meter to Fe of the present invention3O4@MIL-101 (Fe) saturation magnetization analysis
Figure.Fig. 7 shows, two kinds of materials under external magnetic field, generate with the equidirectional intensity of magnetization in magnetic field, and without coercivity and
Remanent magnetism, with obvious superparamagnetism, wherein Fe3O4And Fe3O4@MIL-101 (Fe) saturation magnetization is respectively 66.5 Hes
46.6emu g-1.Insertion figure further demonstrates that, the Fe of synthesis3O4@MIL-101 (Fe) (left side bottles well dispersed in the solution
Son), in the presence of magnet, only need 5s, you can separation and recovery (the right bottle) is realized to it, the feature is beneficial to sample
Quickly collect and recycle.
The Fe prepared below in conjunction with specific embodiment to this method3O4The absorption and recycling of@MIL-101 (Fe) material
Performance carries out detailed investigation.
Embodiment 1：Fe prepared by the present invention given below3O4Absorption of@MIL-101 (Fe) materials to 7 kinds of organic dyestuff
Efficiency chart.As can be known from Fig. 8, the material has adsorption effect to 7 kinds of dyestuffs, and adsorption efficiency order is：Methylene blue>Alkali blue
6B>Rhodamine B>Acid chromium blue k>Eriochrome black T>It is indigo>Acid fuchsin, adsorbance 42.0-221mg g between-1Between, the knot
Fruit explanation Fe3O4@MIL-101 (Fe) material can be used for the removal of dyestuff in water, available for improvement water quality.
Embodiment 2：Fe prepared by the present invention given below3O4Absorption behavior of@MIL-101 (Fe) materials to methylene blue
Research.Its absorption behavior is studied by two kinds of isotherm adsorption models of Langmuir and Freundlich.Under different temperatures
Fe3O4@MIL-101 (Fe), referring to table 1, are shown methylene blue isothermal adsorption parameter by table 1, are inhaled using Freundlich isothermals
Attached model carries out linear fit to its absorption behavior, and its linear regression coeffficient is only 0.895, and with Langmuir models fittings
Linear regression coeffficient illustrates that its absorption behavior meets Langmuir isotherm adsorption models up to 0.9976.
Table 1
Embodiment 3：Fe prepared by the present invention given below3O4@MIL-101 (Fe) material after recycling for several times
The changing value of its adsorption efficiency.Fig. 9 shows, after 4 times recycle, Fe3O4@MIL-101 (Fe) material adsorbs methylene blue
Adsorption efficiency still has 154.7mg g-1, original efficient 70% is kept, the result illustrates that it has good recycling effect
Rate.
Claims (10)
1. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material, it is characterised in that it includes following step
Suddenly：
1) Fe is prepared3O4Micron ball；
2) magnetic metal organic framework core-shell material, i.e. Fe are prepared3O4@MIL-101 (Fe) core-shell material.
2. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 1, its feature exists
In in step 1) in, the preparation Fe3O4The specific method of micron ball is：FeCl is sequentially added into container3·6H2It is O, anhydrous
Sodium acetate and ethylene glycol, after mixing, are transferred in reactor, and heating response is cooled to after room temperature, and gained black product is used
Ethanol is washed, and after drying, produces Fe3O4Micron ball.
3. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 2, its feature exists
In the FeCl3·6H2O, ethylene glycol, the proportioning of sodium acetate are 1.6g: 60mL: 4.3g, wherein FeCl3·6H2O and sodium acetate
Calculated by mass, ethylene glycol is in terms of volume.
4. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 2, its feature exists
It it is 200 DEG C in the temperature of the heating response, the time of heating response is 8h.
5. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 2, its feature exists
In the washing number of times be 6~8 times.
6. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 2, its feature exists
It is dried in vacuo in dry use, the temperature of the drying is 60 DEG C, and the dry time is 8h.
7. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 1, its feature exists
In in step 2) in, it is described to prepare concretely comprising the following steps for magnetic metal organic framework core-shell material：
Successively by step 1) obtained Fe3O4Micron ball, trimesic acid, water add reactor, mix, and after heating response, obtain
Brown solid sample, is cooled to after room temperature, dries under nitrogen atmosphere, and gained sample is magnetic metal organic framework nucleocapsid material
Material, i.e. Fe3O4@MIL-101 (Fe) core-shell material.
8. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 7, its feature exists
In the Fe3O4Micron ball, trimesic acid, the proportioning of water are 0.2g: 0.3g: 4.28mL, wherein Fe3O4Micron ball, equal benzene three
Formic acid is calculated by mass, and water is in terms of volume；The water can use ultra-pure water.
9. a kind of method that Situ Hydrothermal prepares magnetic metal organic framework core-shell material as claimed in claim 7, its feature exists
It it is 150~180 DEG C in the temperature of the heating response, time of heating response is and 12~18h；The temperature of the drying can be
60 DEG C, the dry time can be 8h.
10. a kind of Situ Hydrothermal as described in claim 1~9 prepares the method preparation of magnetic metal organic framework core-shell material
Magnetic metal organic framework core-shell material, it is characterised in that the magnetic metal organic framework core-shell material is with core-shell structure copolymer knot
The spherical micro particles of structure, Fe3O4Micron ball is core, a diameter of 200~400nm, MIL-101 (Fe) be shell, thickness be 40~
100nm, the particle diameter of magnetic metal organic framework core-shell material is 240~500nm.
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Cited By (11)
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| CN109647364A (en) * | 2019-02-03 | 2019-04-19 | 重庆音波科技有限责任公司 | A kind of preparation method of the recyclable magnetic adsorptive material for heavy metal processing |
| CN110252415A (en) * | 2019-07-11 | 2019-09-20 | 佛山科学技术学院 | For eliminating the preparation method of the amino functional MOFs of indoor formaldehyde |
| CN110668504A (en) * | 2019-09-25 | 2020-01-10 | 安徽工程大学 | Mesoporous Fe3O4Granules and process for their preparation |
| CN112979985A (en) * | 2021-03-19 | 2021-06-18 | 宁波浙铁江宁化工有限公司 | Composite metal organic framework material and preparation method thereof |
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| CN115382512A (en) * | 2021-05-24 | 2022-11-25 | 中国水产科学研究院 | Magnetic metal organic framework composite material, preparation method and application thereof |
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| CN113832479A (en) * | 2021-10-13 | 2021-12-24 | 石家庄铁道大学 | Fe2O3(Ti)@NH2-MIL-101(Fe) composite photoelectric catalyst and preparation method thereof |
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| CN117089082A (en) * | 2023-08-15 | 2023-11-21 | 北京建筑大学 | Preparation method of iron-based metal organic framework material |
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