CN103337327A - Heterogeneous FeO34/Co metal organic skeleton material as well as preparation method and application thereof - Google Patents

Heterogeneous FeO34/Co metal organic skeleton material as well as preparation method and application thereof Download PDF

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CN103337327A
CN103337327A CN2013102577610A CN201310257761A CN103337327A CN 103337327 A CN103337327 A CN 103337327A CN 2013102577610 A CN2013102577610 A CN 2013102577610A CN 201310257761 A CN201310257761 A CN 201310257761A CN 103337327 A CN103337327 A CN 103337327A
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mof
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郑静
胡莉萍
褚家兴
吴楠
徐菁利
唐博合金
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Beijing Expert Medical Technology Co ltd
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Shanghai University of Engineering Science
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Abstract

The invention relates to the field of materials, in particular to a heterogeneous FeO34/Co metal organic skeleton material as well as a preparation method and application thereof. The heterogeneous FeO34/Co metal organic skeleton material takes metal organic frame compound Co-MOF as a carrier, and FeO34 nano-particles are attached to the face and holes of the heterogeneous FeO34/Co metal organic skeleton material. The preparation method comprises the steps of dissolving the Fe3O4 nano-material, soluble cobalt salt and trimesic acid into deionized water, placing into an airtight reaction kettle, heating to 135-150 DEG C, and maintaining for 20-28 hours; cooing to 118-122 DEG C and maintaining for 4.5-6 hours; cooling to 98-105 DEG C, performing thermal insulation for 4.5-6 hours, and finally naturally cooling to room temperature and standing for 11-14 hours; and washing the sediment, performing suction filtration and naturally drying to finally obtain the Fe3O4/Co-MoF compound material. The obtained material has well thermal stability and chemical stability.

Description

Heterogeneous Fe 3O 4/ Co metal-organic framework materials and its preparation method and application
Technical field
The present invention relates to the synthetic field of a kind of composite material, be specifically related to a kind of heterogeneous Fe 3O 4The preparation method of/Co-MOF and application thereof.
Background technology
Metal-organic framework materials (Metal-Organic-Framework, MOF) be that a class is new, the microporous materials of flexible design, be crystalline material (the J.Rowsell and O.M.Yaghi.Metal-organic frameworks:a new class of porous materials.Microporous Mesoporous Mater. that is constituted by transition metal ions and organic bridge ligand, 2004,73 (1): 3-14.).It combines the characteristics of inorganic compound and organic compound, has one of class system of potential application foreground most owing to the adjustability of the diversity of complexity, metal and the ligand species of its composition, coordination environment becomes in the materials chemistry research.Owing to have good physicochemical characteristics, extraordinary biocompatibility, good electrical conductivity and be easy to functionalization, therefore especially be subjected to researcher's favor (2.G.F é rey.Hybrid porous solids:past, present, future.Chem.Soc.Rev, 2008,37 (1), 191-215.3.Dybtsev, Danil N; Chun, Hyungphil; Kim, Kimoon.Rigid and Flexible.Angewandte Chemie International Edition, 2004,43 (38): 5033-5035.4.Xi Zhu, ab Hanye Zheng, a Xiaofeng Wei, a Zhenyu Lin, a Longhua Guo, a Bin Qiua and Guonan Chen.Chem.Commun, 2013,49 (13): 1276-1278.
5.Tuerk?C,Goldberg?L.Science，1990，249(4968):505-510.）。The MOF material has the topological geometry that can control and adjustable space function, and its cellular structure is the absorption of molecule, enrichment, detecting provides possibility, because the special micro-structural of MOF makes it in absorption, gas storage, the application of catalysis aspect receives researchers' concern gradually.
Magnetic material has many unique effect that are different from conventional material, as quantum size effect, skin effect, small-size effect and macro quanta tunnel effect etc. also have good magnetic conductance tropism, better biocompatibility, because the magnetic-particle stable performance, more easily preparation, can with the compound particle surface functionalization that makes of multiple molecule, magnetic material has become the research focus as a kind of novel compatibility solid phase carrier function nano material.But magnetic nano-particle ubiquity bad dispersibility, shortcomings such as easy reunion.
At present, the preparation of relevant compound MOF material has become the focus of scientific research, but relevant composition metal organic frame (MOF) material and few.The benefit of this material is that wherein a metal ion species makes up stable MOF framework as the node of MOF network, and another kind of metal ion is as the center of active sites.The research of relevant magnetic MOF material still less.The benefit of magnetic MOF material is that the performance that combines the MOF material on the one hand makes up stable MOF framework, and its loose structure is for micromolecular absorption provides possibility; Be the magnetic of tri-iron tetroxide on the one hand in addition, the characteristics of having avoided magnetic nanoparticle in the past to reunite easily, for the separation of molecule and enrichment provide may, and can from reactant and product, separate easily, recycle and reuse.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of simple synthetic method proposed be the synthetic a kind of compound Fe of hydro thermal method 3O 4/ Co-MOF material and preparation method thereof, and this heterogeneous material of utilization is that medium carries out the dyestuff adsorption experiment with water.
Purpose of the present invention is achieved through the following technical solutions:
A kind of heterogeneous Fe 3O 4/ Co-MOF material is carrier with metal organic frame Compound C o-MOF, is attached with ferriferrous oxide nano-particle in its surface and hole.Preferably, Fe 3O 4The diameter of nano particle is 10～40nm, described heterogeneous Fe 3O 4The specific area of/Co metal-organic framework materials is 6～10m 2/ g.
Above-mentioned heterogeneous Fe 3O 4/ Co-MOF preparation methods is:
(1) nanometer Fe 3O 4The material preparation
Solubility trivalent iron salt (as six Ferric Chloride Hydrateds) fully is dissolved in the ethylene glycol, slowly adds anhydrous sodium acetate and polyethylene glycol, fully stir 30min, pour in the reactor, sealing.Be warming up to 200 ℃ and keep 12h, be down to room temperature thereafter, pour into and get precipitation washing three times in the beaker, alcohol is given a baby a bath on the third day after its birth time, 60 ℃ of dryings of baking oven 6 hours, gained Fe 3O 4The particle diameter of nano particle is 10～40nm;
(2) Fe 3O 4/ Co-MOF's is synthetic
Take by weighing the synthetic nanometer Fe of solubility cobalt salt (as the cobalt acetate hydrate), trimesic acid and step (1) respectively 3O 4, place closed reactor, add deionized water, fully stir until dissolving fully.Be heated to 135～150 ℃, kept 20～28 hours; Cool the temperature to 118～122 ℃ then, kept 4.5～6 hours; Be cooled to 98～105 ℃ of insulations 4.5～6 hours afterwards, make it be down to room temperature naturally at last and leave standstill 11～14h.Get precipitation and spend ionized water and ethanol washing respectively, carry out suction filtration then, natural air drying finally obtains Fe 3O 4/ Co-MOF composite material.
Ferro element and the sodium acetate mol ratio of step (1) trivalent iron salt are 1:8～1:10; The amount ratio of ferro element and polyethylene glycol and ethylene glycol is 1mmol:150～240mg:30～50ml.The mol ratio of cobalt element and trimesic acid is 2:1～1:1 in the step (2).
Cobalt element and Fe in the step (2) 3O 4The amount ratio of nano particle is 1mol:10g～1mol:20g.
Above-mentioned synthetic Fe 3O 4The absorption that/Co-MOF composite material can be used for dyestuff with separate, this composite material can be repeatedly used after adsorption reaction was finished.
It is the metal organic frame compound (MOF) of carrier with the metal Co that the present invention has utilized Hydrothermal Preparation, and nano ferriferrous oxide loaded among the Co-MOF, Co-MOF has very high specific area and pore volume, has guaranteed that the even dispersion in adsorption activity site, substrate fully contact with the activated centre; Utilize the method for reduction of ethylene glycol to obtain the be magnetic Co-MOF material of tri-iron tetroxide of load, the magnetic of material can realize to the enrichment of reactive material with separate, this material thermal stability and chemical stability are all fine, and chemical stability shows in the aqueous solution or other organic solvent and can both keep structure not change; This material can effectively prevent the reunion of magnetic material, and therefore, when being the adsorption reaction that medium carries out dyestuff with water, this heterogeneous composite material shows very high activity.
Description of drawings
Fig. 1 is the embodiment of the invention 1 prepared magnetic Fe 3O 4The SEM figure of nano particle
Fig. 2 is Fe in the embodiment of the invention 3O 4The SEM figure of/Co-MOF material.
Fig. 3 is Co-MOF material, magnetic Fe in the embodiment of the invention 3O 4Nano particle, Fe 3O 4The XRD figure of/Co-MOF composite material, wherein (a) MOF material; (b) nanometer Fe 3O 4Material; (c) MOF-Fe 3O 4Composite material.
Fig. 4 is the Fe in the embodiment of the invention 3O 4The thermal weight loss TGA figure of/Co-MOF material.
Fig. 5 is the Fe in the embodiment of the invention 3O 4The BET figure of/Co-MOF material.
Fig. 6 is the Fe in the embodiment of the invention 3O 4/ Co-MOF is used for the lab diagram of dyestuff absorption.
Embodiment
Used Co (Ac) in the present embodiment 24H 2O, 1,3,5-trimesic acid, ethylene glycol, anhydrous sodium acetate, polyethylene glycol, FeCl 36H 2O etc. are that analysis is pure, and institute's water all is deionized water.
Embodiment 1
With six Ferric Chloride Hydrated 0.14g(0.518mmol) fully be dissolved in the 20ml ethylene glycol, slowly add 0.36g(4.4mmol) anhydrous sodium acetate and 0.10g polyethylene glycol, and fully stir 30min, pour in the reactor sealing into.Be warming up to 200 ℃ and keep 12h, be down to room temperature thereafter, go precipitation to pour in the beaker washing into three times, alcohol is given a baby a bath on the third day after its birth time, puts into 60 ℃ of dryings of baking oven 6 hours, and suction filtration or centrifuging and taking precipitation obtain nanometer Fe 3O 4, its particle diameter is 10～40nm, SEM schemes as shown in Figure 1.
Embodiment 2
The Co(Ac that takes by weighing respectively) 24H 2O0.41g(1.65mmol), 1,3,5-trimesic acid 0.20g(0.95mmol), the nanometer Fe of embodiment 1 3O 40.02g, place closed reactor, add the 15ml deionized water, fully stir until Co(Ac) 24H 2O and 1,3,5-trimesic acid dissolve fully, make Fe 3O 4Be uniformly dispersed.
Reactor is placed baking oven, be heated to 140 ℃, kept this temperature 24 hours; Cool the temperature to 120 ℃ then, kept 5 hours; To be cooled to 100 ℃, kept again 5 hours afterwards, make it be down to room temperature naturally at last, leave standstill 12h.Wash 3 times with 10mL deionized water and alcohol respectively, carry out suction filtration then, natural air drying finally obtains Fe 3O 4/ Co-MOF composite material.
Fig. 2 is Fe 3O 4The SEM figure of/Co-MOF material, Fe as can be seen 3O 4The crystal structure of/Co-MOF material.
Fig. 3 is the Co-MOF material, magnetic Fe 3O 4, Fe 3O 4The XRD figure of/Co-MOF material, Fe 3O 4The XRD peak is all corresponding to cubic system inverse spinel Fe 3O 4The standard diffraction spectra (the JCPDS card, No119-0629), as we know from the figure, contrast Co-MOF material is (curve a), by the Fe of Hydrothermal Preparation 3O 4/ Co-MOF composite material (curve c), the two principal character peak is consistent; Contrast Fe 3O 4Material (curve b) has the characteristic peak about 35 ° consistent with it, shows by hydro thermal method successfully to have prepared Fe 3O 4/ Co-MOF composite material.
As shown in Figure 4, Fe of the present invention 3O 4Twice thermogravimetric loss taken place in/Co-MOF in whole temperature range, thermogravimetric takes place between 100 ℃ to 175 ℃ lost the crystallization water and the water of coordination molecule in the compound; Thermogravimetric loss for the second time is the complex coordination bond fission since 385 ℃ at 385 ℃-550 ℃, and skeleton caves in, the process of organic backbone combustion decomposition.Substantially finish to 550 ℃, the thermogravimetric loss is about 63%.
Fig. 5 is Fe 3O 4The BET figure of/Co-MOF material is analyzed as follows.
Table 1BET map analysis
Figure BDA00003407088700051
Specific area refers to the gross area that the unit mass material has, and solid has certain geometric shape, borrows common Instrument measuring numerical value, adopts the BET method to calculate its specific area.
The BET equation at constant temperature is:
1 Q ( p 0 p - 1 ) = 1 V m C + C - 1 V m C × p P 0
In the formula:
P-adsorbate dividing potential drop/Pa;
p 0-adsorbate saturated vapor pressure/Pa;
Q-adsorbance/(cm 2/ g);
V m-monolayer saturated extent of adsorption/(cm 2/ g);
C-BET equation constant;
Can calculate C, V by slope mReach the A by Instrument measuring mCan calculate the BET specific area
Sg = A m × NA × V m 22414 × 10 - 18
In the formula:
A m—0.1620nm 2
NA-Avogadro constant number (6.02 * 10 23)
By above calculating as can be known, MOF-Fe 3O 4Material B ET specific area is 7.7548m 2/ g.
Embodiment 3
Fe 3O 4/ Co-MOF material carries out according to the following step the dyestuff adsorption experiment: get the 4mg/L rhodamine respectively, plain each 5mL of isatin and biological stain adds composite material 0.8g, at room temperature stirs.Behind 300min, above-mentioned solution is also passed through the content of ultraviolet method detecting reactant by centrifugation.
Fig. 6 is the adsorption rate figure of dyestuff, is respectively: 16.8%, 19.3%, 15.3%; Top curve is the preceding absorbance of absorption, and following curve is the absorbance after adsorbing.Remaining heterogeneous composite material can spend deionised water 3 times, and 80 ℃ of following vacuumizes are reused next time, and adsorption effect is constant.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.

Claims (8)

1. heterogeneous Fe 3O 4/ Co metal-organic framework materials is characterized in that, is carrier with metal organic frame Compound C o-MOF, is attached with Fe in its surface and hole 3O 4Nano particle.
2. the described heterogeneous Fe of claim 1 3O 4The preparation method of/Co metal-organic framework materials is characterized in that, Fe 3O 4The diameter of nano particle is 10～40nm, described heterogeneous Fe 3O 4The specific area of/Co metal-organic framework materials is 6～10m 2/ g.
3. claim 1 or 2 described heterogeneous Fe 3O 4The preparation method of/Co metal-organic framework materials is characterized in that, step comprises:
(1) nanometer Fe 3O 4Material preparation: the solubility trivalent iron salt fully is dissolved in the ethylene glycol, slowly adds anhydrous sodium acetate and polyethylene glycol, pour in the reactor after fully stirring, be warming up to 195～205 ℃ and keep 10～15h under the sealing state; Be down to room temperature again and get the washing of precipitate drying, wash three times, alcohol is given a baby a bath on the third day after its birth time, 60 ℃ of dryings of baking oven 6 hours, gained Fe 3O 4The particle diameter of nano particle is 10～40nm
(2) Fe 3O 4/ Co-MOF's is synthetic: the nanometer Fe that solubility cobalt salt, trimesic acid and step (1) is synthetic 3O 4, place closed reactor, add deionized water, fully stir until dissolving fully; Be heated to 135～150 ℃, kept 20～28 hours; Cool the temperature to 118～122 ℃ then, kept 4.5～6 hours; Be cooled to 98～105 ℃ of insulations 4.5～6 hours afterwards again, make it be down to room temperature naturally at last and leave standstill 11～14h; Get the precipitation washing, carry out suction filtration then, natural air drying finally obtains Fe 3O 4/ Co-MOF composite material.
4. the described homogeneous phase Fe of claim 3 3O 4The preparation method of/Co metal-organic framework materials is characterized in that, in the step (1), the ferro element of trivalent iron salt and sodium acetate mol ratio are 1:8～1:10; The amount ratio of ferro element and polyethylene glycol and ethylene glycol is 1mmol:150～240mg:30～50ml.
5. the described homogeneous phase Fe of claim 3 3O 4The preparation method of/Co metal-organic framework materials is characterized in that, in the step (2), the mol ratio of cobalt element and trimesic acid is 2:1～1:1, with Fe 3O 4The amount ratio of nano particle is 1mol:10g～1mol:20g.
6. the described homogeneous phase Fe of claim 3 3O 4The preparation method of/Co metal-organic framework materials is characterized in that, in the step (2), described solubility cobalt salt is cobalt acetate.
7. claim 1 or 2 described heterogeneous Fe 3O 4/ Co metal-organic framework materials is for the preparation of adsorbent.
8. claim 1 or 2 described heterogeneous Fe 3O 4/ Co metal-organic framework materials is for the preparation of absorbing dye.
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CN104492381A (en) * 2014-11-28 2015-04-08 上海工程技术大学 Heterogeneous TiO2/Co-metal organic framework (MOF) material as well as preparation method and application thereof
CN104998688A (en) * 2015-06-17 2015-10-28 北京科技大学 Magnetic composite metal organic framework material of multi-stage structure and manufacturing method thereof
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CN109467714A (en) * 2018-11-14 2019-03-15 江苏师范大学 A kind of magnetic coupling metal-organic framework materials and its application
CN109675640A (en) * 2019-02-12 2019-04-26 济南大学 A kind of preparation method and application of carbon nitrogen base iron cobalt/cobalt oxide nano-cluster MOF catalyst
CN110743502A (en) * 2019-10-24 2020-02-04 莫林祥 Based on Fe3O4-Co-based MOFs magnetic composite adsorption material and preparation method thereof
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CN104492381A (en) * 2014-11-28 2015-04-08 上海工程技术大学 Heterogeneous TiO2/Co-metal organic framework (MOF) material as well as preparation method and application thereof
CN104998688B (en) * 2015-06-17 2017-08-08 北京科技大学 One kind has multilevel hierarchy magnetic coupling metal-organic framework materials and preparation method
CN104998688A (en) * 2015-06-17 2015-10-28 北京科技大学 Magnetic composite metal organic framework material of multi-stage structure and manufacturing method thereof
CN105597685A (en) * 2016-01-12 2016-05-25 郑州轻工业学院 Preparation method and application of Fe3O4@SiO2@Zr-MOF
CN106117593B (en) * 2016-06-16 2019-07-16 南京工业大学 A method of preparing nano material@metal-organic framework materials
CN106117593A (en) * 2016-06-16 2016-11-16 南京工业大学 A kind of method preparing nano material@metal-organic framework materials
CN108102107A (en) * 2017-12-21 2018-06-01 北京化工大学 Integral type two-step hydrothermal route method and its application in POMOF material preparations
CN108102107B (en) * 2017-12-21 2020-05-15 北京化工大学 Integrated two-step hydrothermal synthesis method and application thereof in preparation of POMOF (polyformaldehyde-mof) material
CN109467714A (en) * 2018-11-14 2019-03-15 江苏师范大学 A kind of magnetic coupling metal-organic framework materials and its application
CN109675640A (en) * 2019-02-12 2019-04-26 济南大学 A kind of preparation method and application of carbon nitrogen base iron cobalt/cobalt oxide nano-cluster MOF catalyst
CN110743502A (en) * 2019-10-24 2020-02-04 莫林祥 Based on Fe3O4-Co-based MOFs magnetic composite adsorption material and preparation method thereof
CN113189051A (en) * 2021-05-11 2021-07-30 河南工业大学 Method for preparing magneto-optical glass-based periodic nanopore magnetic plasma sensor
CN113189051B (en) * 2021-05-11 2022-08-02 河南工业大学 Method for preparing magneto-optical glass-based periodic nanopore magnetic plasma sensor
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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