CN106518932A - Metal organic framework compound with chemical formula of [CoC17O5H11N2]n, and preparation method and application thereof - Google Patents
Metal organic framework compound with chemical formula of [CoC17O5H11N2]n, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a metal organic framework compound with the chemical formula of [CoC17O5H11N2]n, and a preparation method and an application thereof. The preparation method comprises the following steps: carrying out a reaction on Co(NO3)2.6H2O, 1,2,4,5-pyromellitic acid and 1,10-phenanthroline which are adopted as materials at 100 DEG C for 24 h through using a hydrothermal technology, and slowly cooling the obtained reaction product to room temperature in order to obtain the metal organic framework compound with the chemical formula of [CoC17O5H11N2]n. The compound belongs to a monoclinic system crystal and is characterized by a P 21/n space group, a = 1.01491 nm, b = 0.91436 nm, c = 1.8336 nm, alpha = 90 DEG, beta = 121.073 DEG, gamma = 90 DEG, V = 1.4574 nm<3>, the face-centered unit cell F(000) = 776, Goof = 1.083, and Z = 4. The metal organic framework compound has high fluorescence properties and can be applied to the field of fluorescence analysis used as a fluorescence probe. The preparation method of the metal organic framework compound has the advantages of simplicity in operation, and greenness and environmental protection, and the prepared metal organic framework compound with the chemical formula of [CoC17O5H11N2] n has strong fluorescence properties and wide application prospect.
Description
Technical field
The invention belongs to metal organic framework compound technical field, more particularly to a kind of chemical formula is
[CoC17O5H11N2]nMetal organic framework compound and its preparation method and application.
Background technology
Due to world population sharp increase and the aggravation of energy scarcity situation, people have for feature compound material
Higher demand, in order to alleviate this situation, proposes and has synthesized a kind of new material --- --- --- metal organic frame chemical combination
Thing (MOFs=Metal-Organic Frameworks).Metal organic framework compound is also generally referred to as coordination polymer
(PCOs=Porous Coordination Polymers).MOFs, from structure, is a class by organic ligand and inorganic gold
Category unit is by formation such as covalent bond, hydrogen bonds from one-dimensional to three-dimensional infinite networkss.At present, there is substantial amounts of metal
Organic frame compound is synthesized, mainly based on organic ligand containing carboxyl or common with nitrogen heterocyclic ring organic neutral ligands
Use.In these metal organic framework compounds majority all there is high porosity and larger specific surface area, gas absorption,
The aspects such as biomedicine, photoelectric material, catalyst, proton conduction, ion exchange have with very big application potential.
1999, the Omar M.Yaghi professors in the U.S. synthesized MOF- with p-phthalic acid (Isosorbide-5-Nitrae-H2BDC) as part
5, it is considered to be the same classical architecture of MOFs fields milestone, in subsequent several years he again MOF-5 has been carried out modification and
Processing, has further synthesized IRMOF of new generation (Isoreticular Metal-Organic Framework), in aperture and surely
Qualitative aspect achieves greatly improvement.Solvent (water) full-boiled process is to synthesize one of main method of MOFs.Solvent (water) full-boiled process one
As from the larger organic solvent of water or N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO) isopolarity as reaction
Solvent, is carried out in polytetrafluoroethylkettle kettle or in sample bottle, when being heated to uniform temperature, the high pressure produced in the container of sealing
Raw material is made to melt in supercritical liq while crystallizing during slow cooling.Irena Senkovska seminars with DMF are
Solvent, by Al (NO3)3·9H2O mixes crystallization 24h with 4,4 '-bipyridyl and obtains Al (OH) (bpdc) (DMF) 1.8 at 120 DEG C
(H2O)3.5, Al (OH) (ndc) (DMF) 1.5 (H are obtained when part is replaced by the crystallization of 2,6- naphthalene dicarboxylic acids2O)1.5.By the method
The coordination compound that many other methods can not or be difficult to obtain can be obtained, in contrast to room temperature volatility process, the crystal homogeneity of synthesis
It is few with gross imperfection.2008, Jasmina H.C. et al. were same with DMF as solvent, 1.4- p-phthalic acids (H2BDC) with
ZrCl4Synthesized the Zr-BDC of 24 cores in 0.5～3 ratio, and with 2,2 '-bipyridyl -4,4 '-dioctyl phthalate (BPDC) be with
Heat stability higher Zr-BPDC is then synthesized during body.This application provides one kind is with 1,2,4,5- Pyromellitic Acids, 1,10-
Phen, inorganic metal salt are raw material, and hydro-thermal method synthesis chemical formula is [CoC17O5H11N2]nMetal organic framework compound
(MOFs) method, and propose and can be used as fluorescent probe using its stronger photoluminescent property.
The content of the invention
It is an object of the invention to provide a kind of chemical formula is [CoC17O5H11N2]nMetal organic framework compound and its system
Preparation Method and application.
The chemical formula of the present invention is [CoC17O5H11N2]nMetal organic framework compound belong to monoclinic system crystal, its
Crystallographic parameter is shown in Table 1, and part bond distance and bond angle are shown in Table 2.
1 chemical formula of table is [CoC17O5H11N2]nMetal organic framework compound crystallographic parameter
2 chemical formula of table is [CoC17O5H11N2]nMetal organic framework compound part bond distanceWith bond angle (°)
A)1-x,y+1/2,-z-1/2；B)-x+1,y-1/2,-z-1/2；C)-x+1,-y,-z-1.
Above-mentioned chemical formula is prepared for [CoC17O5H11N2]nMetal organic framework compound concretely comprise the following steps：
(1) by 0.3mmol (0.0873g) Co (NO3)2·6H2The equal benzene tetramethyls of O, 0.25mmol (0.0572g) 1,2,4,5-
Acid (H4BETA) add equipped with 10mL water and 4mL N, N- with 0.3mmol (0.0595g) 1,10- Phens (1,10-phen)
In the beaker of dimethylformamide (DMF), magnetic agitation 1h under room temperature is obtained uniform mixed solution.
(2) mixed solution obtained in step (1) is transferred in hydrothermal reaction kettles of the 25mL with polytetrafluoroethylsubstrate substrate,
Hydrothermal reaction kettle is put in baking oven and is heated to 100 DEG C of crystallization 24h, turn off baking oven and room temperature is cooled in its natural state by which,
Hydrothermal reaction kettle is taken out, there are rufous bulk crystals to generate, is filtered, after drying naturally, collect sample, that is, chemical formula is obtained is
[CoC17O5H11N2]nMetal organic framework compound.
The chemical formula of the present invention is [CoC17O5H11N2]nMetal organic framework compound have stronger photoluminescent property,
Fluorescence analysiss field can be applied to as fluorescent probe.
The preparation method of the present invention is simple to operate, environmental protection, and obtained chemical formula is [CoC17O5H11N2]nMetal
Organic frame compound has stronger photoluminescent property, has a extensive future.
Description of the drawings
It is [CoC that Fig. 1 is chemical formula of the present invention17O5H11N2]nMetal organic framework compound crystal structure figure.
It is [CoC that Fig. 2 is chemical formula of the present invention17O5H11N2]nMetal organic framework compound coordination polyhedrom figure.
It is [CoC that Fig. 3 is chemical formula of the present invention17O5H11N2]nMetal organic framework compound crystal two dimension accumulation graph
(b directions).
It is [CoC that Fig. 4 is chemical formula of the present invention17O5H11N2]nMetal organic framework compound DMF solution fluorescence spectrum
Figure.
Specific embodiment
Embodiment：
(1) by 0.3mmol (0.0873g) Co (NO3)2·6H2The equal benzene tetramethyls of O, 0.25mmol (0.0572g) 1,2,4,5-
Acid (H4BETA) add equipped with 10mL water and 4mL N, N- with 0.3mmol (0.0595g) 1,10- Phens (1,10-phen)
In the beaker of dimethylformamide (DMF), magnetic agitation 1h under room temperature is obtained uniform mixed solution.
(2) mixed solution obtained in step (1) is transferred in hydrothermal reaction kettles of the 25mL with polytetrafluoroethylsubstrate substrate,
Hydrothermal reaction kettle is put in baking oven and is heated to 100 DEG C of crystallization 24h, turn off baking oven and room temperature is cooled in its natural state by which,
Hydrothermal reaction kettle is taken out, there are rufous bulk crystals to generate, is filtered, after drying naturally, collect sample, that is, chemical formula is obtained is
[CoC17O5H11N2]nMetal organic framework compound, its crystallographic parameter is shown in Table 1, and part bond distance and bond angle are shown in Table 2, crystal
Structure chart is shown in Fig. 1, and coordination polyhedrom figure is shown in Fig. 2, and b directions accumulation graph is shown in Fig. 3.
Chemical formula obtained in the present embodiment is [CoC17O5H11N2]nMetal organic framework compound fluorescent emission (Em)
With excite (Ex) spectrum as shown in figure 4, the compound maximum emission wavelength, λ Em=320nm, compared with part H4BETA there occurs
The blue shift of 41nm, it may be possible to because after part is bonded with metal ion, its configuration for reversing limits relaxation transition, the compound
Photoluminescent property is shown, fluorescence analysiss field can be applied to as fluorescent probe.
Claims (3)
1. a kind of chemical formula is [CoC17O5H11N2]nMetal organic framework compound, it is characterised in that the metal organic frame
Compound belongs to monoclinic system crystal, and its crystallographic parameter is shown in Table 1, and bond distance and bond angle are shown in Table 2：
1 chemical formula of table is [CoC17O5H11N2]nMetal organic framework compound crystallographic parameter
2 chemical formula of table is [CoC17O5H11N2]nMetal organic framework compound bond distanceWith bond angle (°)
A)1-x,y+1/2,-z-1/2；B)-x+1,y-1/2,-z-1/2；C)-x+1,-y,-z-1.
2. one kind prepares chemical formula as claimed in claim 1 for [CoC17O5H11N2]nMetal organic framework compound side
Method, it is characterised in that concretely comprise the following steps：
(1) by 0.3mmol Co (NO3)2·6H2O, 0.25mmol 1,2,4,5- Pyromellitic Acids and 0.3mmol1,10- are adjacent luxuriant and rich with fragrance
During sieve quinoline adds the beaker equipped with 10mL water and 4mL DMFs, magnetic agitation 1h under room temperature is obtained uniform
Mixed solution；
(2) mixed solution obtained in step (1) is transferred in hydrothermal reaction kettles of the 25mL with polytetrafluoroethylsubstrate substrate, by water
Thermal response kettle is heated to 100 DEG C of crystallization 24h in being put into baking oven, turn off baking oven and be cooled to room temperature in its natural state by which, takes out
Hydrothermal reaction kettle, has rufous bulk crystals to generate, filters, sample is collected after drying naturally, that is, chemical formula is obtained and is
[CoC17O5H11N2]nMetal organic framework compound.
3. chemical formula obtained in method according to claim 2 is [CoC17O5H11N2]nMetal organic framework compound
Using, it is characterised in that the chemical formula is [CoC17O5H11N2]nMetal organic framework compound be applied to as fluorescent probe
Fluorescence analysiss field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440766A (en) * | 2018-04-17 | 2018-08-24 | 山西大学 | A kind of cobalt metal-organic framework materials and its preparation method and application |
| CN109384818A (en) * | 2018-11-25 | 2019-02-26 | 南京科技职业学院 | A kind of cobalt metal organic supermolecular compound and its synthetic method |
| CN112552527A (en) * | 2020-12-25 | 2021-03-26 | 山西大学 | One-dimensional Ni functional complex and preparation method and application thereof |
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| CN105237582A (en) * | 2015-10-22 | 2016-01-13 | 桂林理工大学 | Method for compounding metal-organic framework with chemical formula [C20H4Co5O32]n |
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| DE-QING CHU等: "The synthesis and structural characterization of a two-dimensional coordination polymer [Co(H2O)(phen)(μ4-bta)1/2]n (H4bta = benzenetetracarboxylic acid)", 《COLLECTION OF CZECHOSLOVAK CHEMICAL COMMUNICATIONS》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108440766A (en) * | 2018-04-17 | 2018-08-24 | 山西大学 | A kind of cobalt metal-organic framework materials and its preparation method and application |
| CN109384818A (en) * | 2018-11-25 | 2019-02-26 | 南京科技职业学院 | A kind of cobalt metal organic supermolecular compound and its synthetic method |
| CN112552527A (en) * | 2020-12-25 | 2021-03-26 | 山西大学 | One-dimensional Ni functional complex and preparation method and application thereof |
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