CN107586390A - A kind of calcium metal-organic framework materials and preparation method thereof and fluorescence property - Google Patents
A kind of calcium metal-organic framework materials and preparation method thereof and fluorescence property Download PDFInfo
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Abstract
The invention discloses a calcium metal-organic framework materials, its chemical formula is Ca2C28O12H25N2；Part is 3,3 ', 5,5 ' biphenyl tetracids, and solvent is：N, N dimethylformamide, ethanol, water and acetic acid.Crystal parsing shows：Described Ga MOF material crystals belong to anorthic system, P3221 chiral space groups, cell parameter are respectively：α=β=90 °, γ=120 °.Structure is：Contain two Ca (II), 1.5 bptc in minimum asymmetric cell4‑Molecule, contain a chiral metal chain being made up of Ca in structure.Two bptc4‑Molecule is overlapped mutually appearance, metallic bond and double-deck bptc4‑The interconnection of part, form three-dimensional net structure.DMF decomposes generation dimethylamine cation in water and acid in the presence of simultaneously.The porosity of Ga MOF materials is 38.7%.Fluorometric investigation show the material 352nm excite light irradiation under, 430nm bluish violet fluorescence can be launched, there is preferable photoluminescent property, had a good application prospect in optical material scientific domain.
Description
Technical field
The present invention relates to metal-organic framework materials (M-MOF), specially a kind of calcium metal-organic framework materials (Ga-
) and preparation method thereof and fluorescence property MOF.
Background technology
The photoluminescent property of metal-organic framework materials (Metal-Organic Frameworks, MOFs) has in numerous areas
Potential application, such as fluorescence sense, nonlinear optics, photochemical catalyst, opto-electronic conversion, biomedical imaging.Metal is organic
Frame material permanent pore passage structure and its photoluminescent property of uniqueness cause fluorescence MOFs to turn into a kind of and new have potential value
Sensing material.Fluorescence MOFs has preferable effect in terms of regulation white light and near infrared light transmitting, therefore is led in light emitting devices
There is potential using value in domain.The fluorescence MOFs of nano-scale starts to be used to explore to lead in film, bio-imaging, medicament slow release etc.
The application in domain.Metal-organic framework materials are made up of organic component and inorganic component, and MOFs has had concurrently organic as luminescent material
The advantage of component and inorganic component.The luminous of metal-organic framework materials is mainly due to the following aspects：Based on part
Luminous, lighting based on host-guest interaction luminous, based on metal ion or ion cluster.(Zhan S.,Li M.,Seik
W.,et al.Chemistry-A European Journal,2013,19,10217-10225.；Liu T.,Zhang W.,
Sun W.,et al.Inorganic Chemistry,2011,50,5242-5248.；Pu Y.,Takayuki C.,
Kazushige L.,et al.Advanced Materials,2015,27,1327-1332.).Metal-organic framework material
Construct strategy and be broadly divided into two types：Structure directing construct strategy and functional direction constructs strategy.Influence MOFs materials
The factor constructed is divided into internal factor and external factor.Internal factor includes the coordination mode of metal node and part, Yi Jiqi
Coordination ability is strong and weak；External factor has solvent species, pH value, reaction temperature, reaction ratio etc..Traditional, common synthesis gold
The method of category organic framework materials has diffusion method, solwution method, solvent heat and hydro-thermal method, and the selection of wherein organic solvent serves weight
The effect wanted.(Zeng,Y.F.；Hu,X.；Xue,L.；Liu,S.J.；Hu,T.L.；Bu,X.H.Inorg.Chem.2012,51,
9571；Han,S.D.；Song,W.C.；Zhao,J.P.；Yang,Q.；Liu,S.J.；Li,Y.；Bu X.H.Chem.Commun.,
2013,49,871.；Zhang Z.,Michael J.Chemical Society Reviews,2014,43,5444-5455.；
Eddaoudi M.,Kim J.,Rosi N.,et al.Science,2002,295,469-472.；Wang Z.,Victor C.,
Michael J.Angewandte Chemie International Edition,2005,44,2877-2880.；Murat
C.,Gu Z.,Martin N.,et al.Chemical Communications,2015,51,4796-4798.).This kind of material
Synthesis and exploration, first provide reliable experimental basis to constructing for metal-organic framework materials, in addition such compound
Fluorescence property research helps to understand the interaction in complex between metal ion and part.
The content of the invention
In order to overcome above-mentioned deficiency of the prior art, of the invention provides a kind of system of calcium metal-organic framework materials
Preparation Method, the material are a kind of metal organic frame materials with Ga-MOF " calcium -3,3 ', 5,5 '-biphenyl tetracid-dimethylamine "
Material.Ca-MOF material crystallines contain more rare chiral duct in chiral space group, structure；The material has preferably glimmering
Light property, 352nm excite light irradiation under, 430nm fluorescence can be launched.
The object of the present invention is achieved like this：
A kind of calcium metal-organic framework materials, its chemical formula are Ca2C28O12H25N2；Wherein part chooses 3,3 ', 5,5 '-connection
Benzenetetracarboxylic acid, solvent are：N,N-dimethylformamide (DMF), ethanol (EtOH), water and acetic acid (HAC)；
The crystal of described calcium metal-organic framework materials belongs to anorthic system, P3221 chiral space groups, cell parameter point
It is not：α=β=90 °, γ=120 °；
The structure of the calcium metal-organic framework materials is：Contain two Ca (II) in its minimum asymmetric cell, 1.5
bptc4-Molecule, contain a chiral metal chain being made up of Ca in structure.Two bptc4-Molecule is overlapped mutually appearance, metal
Chain and double-deck bptc4-The interconnection of part, form three-dimensional net structure.DMF is decomposed under the conditions of water and acid are simultaneous
Generate dimethylamine cation.The porosity of Ga-MOF materials is 38.7%.
The preparation method of described calcium metal-organic framework materials is：
By calcium nitrate and 3,3 ', 5,5 '-biphenyl tetracid is added to DMF/EtOH/H2In O/HAC mixed solution, by gained
Mixture obtains colourless bulk crystals by solvent thermal reaction, is then washed with ethanol, dries；
Described calcium nitrate and 3,3 ', 5,5 '-biphenyl tetracid mol ratio are 1.5:1~2:1；
Described DMF/EtOH/H2O/HAC solvent ratio is 4:1:1:0.1；
The solvent heat condition of the thermal response naturally cools to room temperature to be reacted 4-6 days at 80~120 DEG C；
The performance of described calcium metal-organic framework materials：Fluorometric investigation shows that the material has preferable photoluminescent property,
352nm excite light irradiation under, 430nm fluorescence can be launched, can apply to optical material field.
Positive beneficial effect：
The invention discloses a kind of Ga-MOF materials, its chemical formula is Ca2C28O12H25N2；Part is 3,3 ', 5,5 '-biphenyl
Tetracid, solvent are：N,N-dimethylformamide, ethanol, water and acetic acid；The crystal yield and purity of gained are higher.Crystal solution
Analysis shows：The Ga-MOF material crystals belong to anorthic system, P3221 chiral space groups, cell parameter are respectively： α=β=90 °, γ=120 °；Structure
For：Contain two Ca (II) in described Ga-MOF material minimum asymmetric cells, 1.5 bptc4- molecules, be connected with Ca
Eight O are both from bptc4-Carboxyl on molecule, contain a chiral metal chain being made up of Ca in structure.Part bptc4-
Take double-deck coordination mode, two bptc4-Molecule is overlapped mutually appearance, metallic bond and double-deck bptc4-The interconnection shape of part
Into three-dimensional net structure.DMF is extremely easy in decomposition generation dimethylamine cation, Ga-MOF materials under the conditions of water and acid are simultaneous
Expect that skeleton is negatively charged, by the dimethylamine cation balancing charge to dissociate in two ducts.Highly unordered solvent molecule in duct
Desolvation processing is carried out by SQUEEZE programs, its porosity is calculated as 38.7% through PLATON.Fluorometric investigation shows the material
Expect 352nm excite light irradiation under, 430nm fluorescence can be launched, there is preferable photoluminescent property, can apply to light
Learn Material Field.
Brief description of the drawings
Fig. 1 is the metal Ca of the present invention2+Coordination mode；
Fig. 2 is the one-dimensional chiral metal chain of the present invention；
Fig. 3 is the Ga-MOF three-dimensional accumulation graphs along c-axis direction of the present invention；
Fig. 4 is the powder xrd pattern of the present invention.
Fig. 5 is the thermogravimetric curve figure of the present invention；
Fig. 6 is the fluorescent exciting spectrogram of the present invention.
Embodiment
Below in conjunction with the accompanying drawings and specific embodiment, the present invention is described further：
A kind of calcium metal-organic framework materials, its chemical formula are Ca2C28O12H25N2；Part is 3,3 ', 5,5 '-biphenyl four
Acid, solvent are：N,N-dimethylformamide, ethanol, water and acetic acid；
Described calcium metal-organic framework materials crystal belongs to anorthic system, P3221 chiral space groups, cell parameter difference
For：α=β=90 °, γ=120 °；
The structure of the calcium metal-organic framework materials is：Contain two Ca (II) in minimum asymmetric cell, 1.5
bptc4-Molecule, contain a chiral metal chain being made up of Ca in structure.Two bptc4-Molecule is overlapped mutually appearance, metal
Chain and double-deck bptc4-The interconnection of part, form three-dimensional net structure.DMF decomposes generation two in water and acid in the presence of simultaneously
Methylamine cation.The porosity of Ga-MOF materials is 38.7%.
The preparation method of described calcium metal-organic framework materials is：
By calcium nitrate and 3,3 ', 5,5 '-biphenyl tetracid is added to DMF/EtOH/H2In O/HAC mixed solution, by gained
Mixture obtains colourless bulk crystals by solvent thermal reaction, is then washed with ethanol, dries；
Described calcium nitrate and 3,3 ', 5,5 '-biphenyl tetracid mol ratio are 1.5:1~2:1；
Described DMF/EtOH/H2O/HAC solvent ratio is 4:1:1:0.1；
The solvent heat condition of the thermal response naturally cools to room temperature to be reacted 4-6 days at 80~120 DEG C；
The fluorometric investigation of described calcium metal-organic framework materials shows that the material has preferable photoluminescent property,
352nm's excites under light irradiation, can launch 430nm fluorescence, can apply to optical material field.
Embodiment 1
The preparation of Ga-MOF materials：
Weigh 40 milligrams of calcium nitrate and 3,3 ', 5,20 milligrams of 5 '-biphenyl tetracid is placed in 20 milliliters of vials, adds 8 millis
Rise DMF, 2 milliliters of ethanol, 2 milliliters of water and 0.2 milliliter of acetic acid, sealing；Reacted 4 days at 85 DEG C, obtain nothing
Color bulk crystals, are then washed with ethanol, are dried.
To the sign of embodiment 1：
(1) crystal structure determination
As Figure 1-3, selection size is suitable under the microscope, and surface is smooth, crackless crystal, passes through X ray list
The point diffraction of brilliant diffractometer scanning crystal, and carry out data parsing.Embodiment 1 is collected on Rigaku SCX-mini monocrystalline instrument
Data.Using the Mo-K alpha rays of graphite monochromator monochromatization It will be selected by the glass fiber in copper target
Single good crystal sticks up, and is placed in collection single crystal diffraction data on monocrystalline instrument.Single crystal data is carried out by SHELX programs direct method
Parsing, and carry out refine with least square method.Non-hydrogen atom coordinate determines by least square method and difference function method, hydrogen atom
Obtained by the method for theory hydrogenation, finally carry out crystal structure refine with least square method again.Solvent molecule in duct, bag
Include DMF, H2O, EtOH etc. can not determine its particular location because it is highly unordered, pass through the SQUEEZE in PLATON softwares
Program carries out solvent and handled.Predominant crystal parameter see the table below：
(2) powder diffraction characterizes phase purity：
Penetrate on instrument and complete in the Rigaku D/Max-2500X- line powder that spreads out as shown in figure 4, powder diffraction data is collected, instrument
Device operating voltage is 40kV, electric current 100mA, uses graphite monochromatised copper target X ray.Scanning constant, it is 1 ° that diverging, which deviates,
Receive a width of 0.3 millimeter of slit.Density data is collected and uses 2 θ/θ scan patterns, the continuous scanning completion in the range of 3 ° to 80 °,
Sweep speed be 8 °/it is per second, span be 0.02 °/every time.Data fitting uses Cerius2 programs, mono-crystalline structures powder diffraction spectrum
Simulation conversion uses Mercury 1.4.2.
(3) to the THERMAL STABILITY of embodiment 1：
The thermal stability data of embodiment 1 is collected by Rigaku standard TG-TDA analyzers, Range of measuring temp：25
~700 DEG C, as a result as shown in Figure 5.
(4) photoluminescent property of embodiment 1 is studied：
The fluorescence property of embodiment 1 is completed by Cary Eclipse types sepectrophotofluorometer, as a result as shown in Figure 6.
The invention discloses a kind of Ga-MOF materials, its chemical formula is Ca2C28O12H25N2；Part is 3,3 ', 5,
5 '-biphenyl tetracid, solvent are：N,N-dimethylformamide, ethanol, water and acetic acid.Crystal parsing shows：Described Ga-
MOF material crystals belong to anorthic system, P3221 chiral space groups, cell parameter are respectively： α=β=90 °, γ=120 °.Structure is：Contain two in minimum asymmetric cell
Individual Ca (II), 1.5 bptc4-Molecule, contain a chiral metal chain being made up of Ca in structure.Two bptc4-Molecule is mutual
Superposition occurs, metallic bond and double-deck bptc4-The interconnection of part, form three-dimensional net structure.DMF exists simultaneously in water and acid
It is lower to decompose generation dimethylamine cation.The porosity of Ga-MOF materials is 38.7%.Fluorometric investigation shows the material 352nm's
Excite under light irradiation, 430nm bluish violet fluorescence can be launched, there is preferable photoluminescent property, can apply to optical material
Field.
Above case study on implementation is merely to illustrate the preferred embodiment of the present invention, but the present invention is not limited to above-mentioned embodiment party
Formula, in the field those of ordinary skill possessed knowledge, that is made within the spirit and principles in the present invention is any
Modification, equivalent substitute and improvement etc., it is regarded as the protection domain of the application.
Claims (8)
1. a kind of calcium metal-organic framework materials, it is characterized in that：Chemical formula is Ca2C28O12H25N2；Part is 3,3 ', 5,
5 '-biphenyl tetracid, solvent are：N,N-dimethylformamide, ethanol, water and acetic acid.
2. calcium metal-organic framework materials according to claim 1, it is characterised in that：Described Ga-MOF material crystals category
In anorthic system, P3221 chiral space groups, cell parameter are respectively： α=β=90 °, γ=120 °.
3. calcium metal-organic framework materials according to claim 1, it is characterised in that：Described its structure of Ga-MOF materials
It is：Contain two Ca (II), 1.5 bptc in minimum asymmetric cell4-Molecule, contain a chirality being made up of Ca in structure
Metallic bond.Two bptc4-Molecule is overlapped mutually appearance, metallic bond and double-deck bptc4-The interconnection of part, form three dimensional network
Network structure.DMF decomposes generation dimethylamine cation in water and acid in the presence of simultaneously；The porosity of calcium metal-organic framework materials is
38.7%.
4. the preparation method of calcium metal-organic framework materials as claimed in claim 1 is：By calcium nitrate and 3,3 ', 5,5 '-connection
Benzenetetracarboxylic acid is added to DMF/EtOH/H2In O/HAC mixed solution, gained mixture is obtained into no color lump by solvent thermal reaction
Shape crystal, is then washed with ethanol, is dried.
A kind of 5. preparation method of calcium metal-organic framework materials according to claim 4, it is characterised in that：Described nitre
Sour calcium and 3,3 ', 5,5 '-biphenyl tetracid mol ratio are 1.5:1~2:1.
A kind of 6. preparation method of calcium metal-organic framework materials according to claim 4, it is characterised in that：Described
DMF/EtOH/H2O/HAC solvent ratio is 4:1:1:0.1.
A kind of 7. preparation method of calcium metal-organic framework materials according to claim 4, it is characterised in that：The heat is anti-
The solvent heat condition answered naturally cools to room temperature to be reacted 4-6 days at 80~120 DEG C.
8. the fluorescence property of calcium metal-organic framework materials as claimed in claim 1, it is characterised in that：Test shows calcium metal
Organic framework material can launch 430nm bluish violet fluorescence under light irradiation in exciting for 352nm, can apply to optical material neck
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| CN114395137A (en) * | 2022-01-25 | 2022-04-26 | 郑州工程技术学院 | MOF material and preparation method and application thereof |
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