CN106046388A - Furan-carboxylic acid rare-earth neodymium metal-organic framework luminescent material and synthesis method therefor - Google Patents
Furan-carboxylic acid rare-earth neodymium metal-organic framework luminescent material and synthesis method therefor Download PDFInfo
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Abstract
The invention belongs to the field of material chemistry and relates to a furan-carboxylic acid rare-earth neodymium metal-organic framework luminescent material and a synthesis method therefor. The compound has near-infrared fluorescent characteristics and ultraviolet-visible luminescent characteristics. The furan-carboxylic acid rare-earth neodymium metal-organic framework luminescent material has the chemical general formula of {[Nd2(H2O)3(FDA)3(CH3OH)].CH3OH}n, wherein FDA is furan-2,5-dicarboxylic acid, CH3OH is methanol, and n is a natural number from 1 to positive infinity. A topological structure is a 3,3,5,6-connected four-node novel topological structure and has the point symbols: (4.5.6)2(4.6<2>)2(4<2>.5<4>.6<2>.7<2>)2(5<2>.6<6>.7<4>.9<2>.10). The synthesis method comprises the steps: mixing neodymium hydroxide and furan dicarboxylic acid according to the mass mole ratio of 1: 2, then, adding 8mL to 10mL of a mixed solvent of methanol and water which are in the volume ratio of 3: 1 into the mixture so as to obtain a mixed solution, and carrying out stirring for 2 minutes at normal temperature; and putting a reactor containing the mixed solution into a baking oven, carrying out constant temperature for 72 hours at the temperature of 120 DEG C, and cooling the reactor to room temperature at the constant speed of 2 degrees centigrade per hour. The furan-carboxylic acid rare-earth neodymium metal-organic framework luminescent material has very good luminescence property and stability, and the preparation process is simple, easy and efficient and is low in cost and good in reproducibility.
Description
Technical field
The present invention relates to a kind of metal-organic framework materials formed with furan dicarboxylic acid as part, with rare earth metal neodymium
And preparation method thereof, and the characteristics of luminescence of this compound.
Background technology
Metal-organic framework materials (Metal-Organic Frameworks, MOFs) is with metal ion or bunch for connecing
Point, with multiple tooth organic ligand as skeleton, has the porous crystalline material of periodic network structure by the class being self-assembly of.
It has, and specific surface area is big, porosity is high, duct type enriches easy tune, framing structure is various, be prone to the characteristics such as functionalization, at gas
The absorption of body with separate, be catalyzed, the aspect such as molecular magnet, fluorescent probe shows the performance of excellence, thus become and grind both at home and abroad
The focus studied carefully.(see: Yaghi O M etc., Nature, 1995,378,703；Zhou H C etc., Chem.Soc.Rev., 2009,
38,1477)。
All the time, compared to main group metal and transition metal M OFs, the research of rare earth MOFs is the most fewer.This is probably
Owing to rare earth element has high ligancy and coordination mode flexibly, therefore its compound is difficult to design synthesis.But, rare earth
MOFs has lot of advantages, if the MOFs generated is through simple process, easily vacates more coordination site, can effectively improve frame
The gas absorption character (seeing: Zhou H C etc., Inorg.Chem.2009,48,2072.) of frame.Meanwhile, rare earth Gd, Dy
There is abundant single electron and big orbital angular momentum, thus magnetic property good (see: Murugesu M etc.,
Angew.Chem.Int.Ed.2009,48,948.).Additionally rare earth element has good photoluminescent property, its rare earth built
MOFs material exist in terms of fluorescent probe and molecule sensor huge application potential (see: Lu T B etc.,
Inorg.Chem.2009,48,6997).Therefore, use rare earth metal to build metal-organic framework, can obtain that there is many merits
The MOFs of energy, this is also one of its reason becoming current Coordinative Chemistry area research focus.But, the rare earth neodymium of report at present
Metal-organic framework less, and its fluorescence Quality Research is the most less.
Additionally, organic ligand is divided three classes, i.e. carboxylic acids, heterocyclic and heterocyclic carboxylic acid class, furan dicarboxylic acid part belongs to
The one of heterocyclic carboxylic acid part, it is advantageous that: (1) coordination mode is various, provides advantage for assembling rare earth metal MOF；
(2) there is higher symmetry and preferable rigidity, be easily formed Stability Analysis of Structures, be difficult to the three-dimensional frame structure interted；(3) easy shape
Become the rare earth MOFs of novel structure diverse in function.Therefore furan diacid causes the attention of vast researcher.Up to now, with furan
Mutter-dicarboxylic acids (H2FDA) it is organic ligand, the metal organic frame crystalline material being metal node with rare earth metal neodymium, have
The metal-organic framework related work report of good fluorescence characteristic is less.
Summary of the invention
The invention provides a kind of metal-organic framework crystalline substance formed using furan dicarboxylic acid as part and rare earth metal neodymium
The method of body material.
A kind of furancarboxylic acid class rare earth metal-organic frame luminescent material, its chemical general formula is: { [Nd2(H2O)3(FDA)3
(CH3OH)]·CH3OH}n, wherein, n is expressed as 1 and arrives the most infinite natural number, and FDA represents furan dicarboxylic acid.
Described rare earth neodymium metal-organic framework exists the Nd of two kinds of coordination environments3+Ion, be labeled as Nd1 and
Nd2；
Wherein, Nd1 is eight-coordinate, respectively with four μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen,
The μ that two monodentates from same FDA part chelate2-η1:η1Carboxyl oxygen, two hydrones constitute double cap Rhizoma Sparganii of eight-coordinate
Post geometric configuration；
Wherein, Nd2 is nine coordinations, respectively with two μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen,
The μ that two monodentates from same FDA part chelate2-η1:η1Carboxyl oxygen, three μ from different FDA parts2-η1:η2Carboxylic
Base oxygen, a methanol molecules and a hydrone constitute the nine three cap triangular prism geometric configurations being coordinated；
By two μ between two Nd12-η1:η1Carboxyl connects into double-core neodymium secondary construction unit (SBU), two Nd2 it
Between by two μ2-η1:η1Carboxyl and two μ2-bridging carboxyl oxygen connects into another double-core neodymium SBU；Two SBU are by (κ2)-
(κ1-κ1)-μ3-FDA2-And (κ2-κ1-μ2)-(κ1-κ1)-μ4-FDA2-The FDA of coordination mode connects formation 3D frame structure；
Described furancarboxylic acid class rare earth metal-organic frame belongs to anorthic system, P-1 space group, and cell parameter is respectively as follows: α=95.606 (7), β=105.399 (6), γ=
100.402(6).Topological structure is one 3,3,5, the 6-four node novel topological structures connected, and its point symbol is (4.5.6)2
(4.62)2(42.54.62.72)2(52.66.74.92.10)。
The synthetic method of a kind of described rare earth neodymium metal-organic framework, with Neodymium hydroxide (Nd (OH)3) it is slaine, with
H2FDA is part, and with the mixing liquid of methanol and water as solvent, synthesis step is as follows:
(1) by Nd (OH) that mol ratio is 1:23And H2FDA mixture puts into the polytetrafluoroethylliner liner of hydrothermal reaction kettle
In, being subsequently adding methanol with water volume ratio is the mixed solvent of 3:1, obtains mixed solution, stirs 2min under room temperature；
(2) reactor that will be equipped with above-mentioned mixed solution is put in baking oven, constant temperature 72h at 120 DEG C, then even with 2 DEG C/h
Solid, to room temperature, is separated after taking out product by prompt drop；
(3) with methanol, above-mentioned solid is washed 3 to 5 times, can be prepared by the grey violet vitta of the metal framework material of neodymium ion
Shape crystal.
In step (1), described Nd (OH)3And H2The mixture of FDA with the amount ratio of mixed solvent is: 0.06～0.1g:8
～10mL.
The present invention relates to the test of X-ray single crystal diffractometer and the data research of metal-organic framework.
The present invention relates to test and the research of metal-organic framework Thermogravimetric Data.
The present invention relates to the research of metal-organic framework fluorometric investigation analytical data.
The present invention relates to metal-organic framework solid uv-vis spectra testing and analysis data research.
The present invention develops a kind of rare earth metal neodymium organic framework materials based on furan dicarboxylic acid, it is demonstrated experimentally that this material
Material has good fluorescent characteristic and heat stability, can be applicable to fluorescent material field.
The present invention further discloses the growing method of this kind of metal organic frame crystal, be to be cultivated by hydro-thermal method to obtain
's.
The invention have the benefit that:
(1) synthetic method is simple, favorable reproducibility, and productivity is high and relatively low to temperature requirement, it is easy to control the temperature of reaction system
Degree；
(2) purposively synthesis possesses the functional material of good luminous performance.
Accompanying drawing explanation
Fig. 1 is { [Nd2(H2O)3(FDA)3(CH3OH)]·CH3OH}nCrystal structure asymmetric cell (a), two kinds of double-core neodymiums
Construction unit figure (b), the edge [1,0,0] (c) of crystal, [0,0,1] (d), the accumulation graph in [0,1,0] (e) direction and crystal knot
The topological diagram (f) of structure；
Fig. 2 is { [Nd2(H2O)3(FDA)3(CH3OH)]·CH3OH}n(in figure, 1 is described chemical combination to the thermogravimetric analysis figure of crystal
Thing)；
Fig. 3 is { [Nd2(H2O)3(FDA)3(CH3OH)]·CH3OH}nCrystallofluorescence spectrogram；
Fig. 4 is { [Nd2(H2O)3(FDA)3(CH3OH)]·CH3OH}n(in figure, 1 is institute to crystalline solids ultraviolet-visible spectrogram
Stating compound, L is H2FDA part).
Detailed description of the invention
Embodiment 1:
A kind of preparation method with characteristics of luminescence rare earth metal-organic frame, with Neodymium hydroxide as slaine, with
H2FDA is part, and the methanol/water mixture with volume ratio as 3:1 is as solvent, and synthesis step is as follows:
1) by the Nd (OH) of 0.1mmol3H with 0.2mmol2In the polytetrafluoroethylliner liner putting into hydrothermal reaction kettle of FDA
Mixing, adds the mixed solvent of 8～10mL, stirs 2min under room temperature；
2) reactor that will be equipped with above-mentioned mixed solution is put in baking oven, bakes 72h, then with 2 DEG C/h at the uniform velocity at 120 DEG C
It is down to room temperature, after taking out product, solid is separated；
3) being washed 3 to 5 times by above-mentioned solid with methanol, can be prepared by chemical formula is C20H18Nd2O20The metal frame of neodymium ion
The light yellow web crystal of frame material, is 58% based on the calculated productivity of neodymium metal.
This multi-function metal is had the-property representation of machine frame material structure:
(1) this metal has-a structure determination of machine frame material:
Use Agilent SuperNova TM type x-ray diffractometer, use through graphite monochromator monochromatization at 293 (2) K
MoKa rayAs incident light source, withScan mode collects point diffraction.Non-hydrogen atom direct method
Solve, and by their coordinate of complete matrix least square refinement and anisotropy thermal parameter thereof, the position of hydrogen atom is by theory
Hydrogenation obtains, and adds fixing isotropism thermal parameter in structure refinement.All of calculate use SHELXS-97 and
SHELXL-97 program bag is carried out.Obtain crystallographic data as follows:
The crystallographic data of table 1 coordination compound
The result of Fig. 1 a shows to exist in described rare earth metal frame structure the Nd of two kinds of coordination environments3+Ion, Nd1 is
Eight-coordinate, respectively with four μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen, two join from same FDA
The μ of the monodentate chelating of body2-η1:η1Carboxyl oxygen, two hydrones constitute double cap triangular prism geometric configurations of eight-coordinate, and Nd2 is nine
Coordination, respectively with two μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen, two from same FDA part
Monodentate chelating μ2-η1:η1Carboxyl oxygen, three μ from different FDA parts2-η1:η2Carboxyl oxygen, a methanol molecules and
One hydrone constitutes three cap triangular prism geometric configurations of nine coordinations, by two μ between two Nd12-η1:η1Carboxyl connects into
Double-core neodymium secondary construction unit (SBU) (Fig. 1 b), by two μ between two Nd22-η1:η1Carboxyl and two μ2-bridging carboxyl
Oxygen connects into another double-core neodymium SBU (Fig. 1 b).Two SBU are by (κ2)-(κ1-κ1)-μ3-FDA2-And (κ2-κ1-μ2)-(κ1-
κ1)-μ4-FDA2-The FDA of coordination mode connects formation 3D frame structure (Fig. 1 c-e), and described rare earth metal-organic frame belongs to
Anorthic system, P-1 space group, cell parameter is respectively as follows: α=95.606 (7), β=105.399 (6), γ=100.402 (6).Topological structure is four joints that a 3,3,5,6-connects
Point novel topological structure (Fig. 1 f), its point symbol is (4.5.6)2(4.62)2(42.54.62.72)2(52.66.74.92.10)。
(2) this metal have-thermostability of machine frame material measures:
It is as follows that the present invention carries out gravitational thermal analysis method to crystal prototype: the TG with 5 DEG C/min heating rate scanning sample is bent
Line, sweep limits temperature range 25～800 DEG C.NETZSCH TG 209 thermogravimetric analyzer is used to be measured.
The first step weightlessness of sample occurs within the temperature range of 25 to 150 DEG C, can be attributed to losing of guest molecule.
Second step is weightless at about 410 DEG C, is mainly due to the decomposition of organic ligand framework.This material visible has good thermally-stabilised
Property (Fig. 2).
(3) photoluminescent property of this frame structure characterizes:
The assay method that the present invention measures fluorescence data is as follows: by metal organic frame crystal { [Nd2(H2O)3(FDA)3
(CH3OH)]·CH3OH}nSolid under the conditions of using Edinburgh FLS920 to measure 310nm excitation wavelength at ambient temperature
Near-infrared fluorescent performance.
The metal-organic framework materials of present invention 310nm ultraviolet excitation at ambient temperature, the characteristic peak of coordination compound is
From Nd3+The series radiation transition of ion4F3/2→4Ij(j=9/2,11/2 and 13/2) this be that part is to Nd3+Having of ion
Usefulness shifts；3 fluorescence spectral characteristic peaks, the most corresponding above three occur at 891nm, 1061nm and 1331nm
Nd3+The radiation transistion of ion.Wherein the intensity at 1061nm is apparently higher than other intensity at two, is applicable to Fluorescence laser and launches
With In vivo detection (see Fig. 3).
(4) the ultraviolet-visible spectrum property representation of this frame structure:
Solid ultraviolet-visible spectrum method for measuring of the present invention is as follows: by { [Nd2(H2O)3(FDA)3(CH3OH)]·
CH3OH}nMaterial measures with barium sulfate mixed grinding laminated flake.By Jasco V-570 type ultraviolet-visible spectrophotometer to it
Carry out ultraviolet-visible spectrum performance test.The wave-length coverage 200～1000nm of ultraviolet-visible spectrometer.
The metal-organic framework material of the present invention at ambient temperature, the absworption peak of coordination compound in λ=450 490,490
At 540,560 600,615 650,670 700,720 770,780 830and 850 890nm, it is from Nd3+Ion be
Row radiation transistion, correspond to respectively4I9/2→2G9/2+2D3/2,4I9/2→4G7/2+4G9/2+2K13/2,4I9/2→4G5/2+2G7/2,4I9/2
→2H11/2,4I9/2→4F9/2,4I9/2→4F7/2+4S3/2,4I9/2→4F5/2+2H9/2And4I9/2→4F3/2, less than the peak at 400nm
It is attributed to H2The absworption peak (Fig. 4) of FDA part.
Claims (6)
1. a furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material, it is characterised in that chemical general formula is: { [Nd2
(H2O)3(FDA)3(CH3OH)]·CH3OH}n, wherein, n is expressed as 1 and arrives the most infinite natural number, and FDA represents furan dicarboxylic acid.
A kind of furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material the most according to claim 1, its feature exists
In, described Nd3+There are two kinds of coordination environments in ion, is labeled as Nd1 and Nd2；
Wherein, Nd1 is eight-coordinate, respectively with four μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen, two
The μ chelated from the monodentate of same FDA part2-η1:η1Double cap triangular prisms that carboxyl oxygen, two hydrones constitute eight-coordinates are several
What configuration；
Wherein, Nd2 is nine coordinations, respectively with two μ from the bidentate bridging of different FDA parts2-η1:η1Carboxyl oxygen, two
The μ chelated from the monodentate of same FDA part2-η1:η1Carboxyl oxygen, three μ from different FDA parts2-η1:η2Carboxyl
Oxygen, a methanol molecules and a hydrone constitute the nine three cap triangular prism geometric configurations being coordinated；
By two μ between two Nd12-η1:η1Carboxyl connects into double-core neodymium secondary and constructs cell S BU, passes through between two Nd2
Two μ2-η1:η1Carboxyl and two μ2-bridging carboxyl oxygen connects into another double-core neodymium SBU；Two SBU are by (κ2)-(κ1-
κ1)-μ3-FDA2-And (κ2-κ1-μ2)-(κ1-κ1)-μ4-FDA2-The FDA of coordination mode connects formation 3D frame structure；
Described furancarboxylic acid class rare earth neodymium metal-organic framework belongs to anorthic system, P-1 space group, and cell parameter is respectively as follows: α=95.606 (7), β=105.399 (6), γ=
100.402(6).Topological structure is one 3,3,5, the 6-four node novel topological structures connected, and its point symbol is (4.5.6)2
(4.62)2(42.54.62.72)2(52.66.74.92.10)。
The synthetic method of a kind of furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material the most according to claim 1,
It is characterized in that, with Neodymium hydroxide as slaine, with H2FDA is part, with the mixing liquid of methanol and water as solvent, including such as
Lower step:
(1) by Nd (OH)3And H2The mixture of FDA is put in the polytetrafluoroethylliner liner of hydrothermal reaction kettle, be subsequently adding methanol with
In the mixed solvent of water, obtain mixed solution, under room temperature, stir 2min；
(2) reactor that will be equipped with step (1) gained mixed solution is put in baking oven, and constant temperature 72h at 120 DEG C, then with 2 DEG C/h
At the uniform velocity it is down to room temperature, after taking out product, solid is separated；
(3) being washed 3 to 5 times by above-mentioned solid with methanol, the lilac strip of the metal framework material that can be prepared by neodymium ion is brilliant
Body.
The synthetic method of a kind of furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material the most according to claim 3,
It is characterized in that, in step (1), in described mixture, Nd (OH)3And H2The mol ratio of FDA is 1:2；In described mixed solvent,
Methanol and water volume ratio are 3:1.
The synthetic method of a kind of furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material the most according to claim 3,
It is characterized in that, described Nd (OH)3And H2The mixture of FDA and the amount ratio of mixed solvent are 0.06～0.1g:8～10mL.
6. an application for furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material as claimed in claim 1, its feature
It is, described furancarboxylic acid class rare earth neodymium metal-organic framework luminescent material is used for fluorescent material field.
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| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
| CN114605656A (en) * | 2022-03-02 | 2022-06-10 | 许昌学院 | Preparation method and application of neodymium-based metal organic framework material Nd-MOF |
| CN115364822A (en) * | 2022-08-22 | 2022-11-22 | 广东美的白色家电技术创新中心有限公司 | Preparation method and application of MOFs material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109142308A (en) * | 2018-10-22 | 2019-01-04 | 河海大学 | A kind of fluorescent test paper and its preparation and detection method for detecting Co (II) |
| CN109142308B (en) * | 2018-10-22 | 2020-05-22 | 河海大学 | Method for detecting Co (II) by using fluorescent test paper |
| CN113563600A (en) * | 2021-08-15 | 2021-10-29 | 福州大学 | Metal organic framework material with single-component white light characteristic |
| CN114605656A (en) * | 2022-03-02 | 2022-06-10 | 许昌学院 | Preparation method and application of neodymium-based metal organic framework material Nd-MOF |
| CN114605656B (en) * | 2022-03-02 | 2023-08-22 | 许昌学院 | Preparation method and application of neodymium-based metal organic framework material Nd-MOF |
| CN115364822A (en) * | 2022-08-22 | 2022-11-22 | 广东美的白色家电技术创新中心有限公司 | Preparation method and application of MOFs material |
| CN115364822B (en) * | 2022-08-22 | 2023-10-27 | 广东美的白色家电技术创新中心有限公司 | Preparation method and application of MOFs material |
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