CN101250264A - High nuclear zinc coordination polymer as well as preparation method and uses thereof - Google Patents
High nuclear zinc coordination polymer as well as preparation method and uses thereof Download PDFInfo
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- CN101250264A CN101250264A CNA2008100525184A CN200810052518A CN101250264A CN 101250264 A CN101250264 A CN 101250264A CN A2008100525184 A CNA2008100525184 A CN A2008100525184A CN 200810052518 A CN200810052518 A CN 200810052518A CN 101250264 A CN101250264 A CN 101250264A
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Abstract
The invention relates to a high nuclear zinc coordination polymer, and a coordination preparation process and the application thereof. The coordination polymer has the following chemical formula that {Zn14 (trz) 12 (nip) 8 (H2O) 4 .7.5 H2O} n, wherein trz is 1, 2, 4-triazole univalence anion, and nip is 5-nitroisophthalate acid dianion. The preparation of high nuclear zinc coordination polymer is different from the common synthesis process of d10 metal mixed ligand complex which is reported in current documents, which synthesizes fourteen nuclear zinc coordination polymers which have excellent heat stability and is dissolved with common organic solvent through replacing metal salt with metallic oxide as the source of complex metal center. The fluorescence spectrum data of the crystal sample of the high nuclear zinc coordination polymer shows that the coordination polymer can be used as fluorescent material, and can be applied in the material science field.
Description
Technical field
The invention belongs to transition metal complex material technology field, relate to high nuclear zinc coordination polymer and preparation method thereof, especially a kind of 1,2,4-triazole and 5-nitroisophthalic acid be mixed 14 nuclear zinc coordination polymers and application thereof, described polymkeric substance has Zn-trz bunch of secondary building unit of 14 nuclears and contains the three-dimensional net structure in two-dimentional duct, and its photoluminescent property makes it can be used as fluorescent material and is applied.
Technical background
In recent years with d
10Metal coordinating polymer as fluorescent material be subjected to people very big concern and by a large amount of synthetic and researchs, because they have higher stability than pure organic ligand, moreover because the coordination of metal, the emission wavelength and the intensity of organic ligand obviously are affected.By generating ligand polymer and then combination organic spacer base and transition metal center, be regarded as obtaining the effective way of novel materials for electroluminescence, this material has potential to use in light emitting diode.(V.W.W.Yam，K.K.-W.Lo，W.K.-M.Fung，C.-R.Wang，Coord.Chem.Rev.1998，171，17-41；S.Leininger，B.Olenyuk，P.J.Stang，Chem.Rev.2000，100，853-908；S.Wang，Coord.Chem.Rev.2001，215，79-98；O.R.Evans，W.Lin，Acc.Chem.Res.2005，38，243-250)。
Have the carboxylic acid part that enriches coordination mode, the many carboxyls part that particularly contains phenyl ring is by the extensive and a large amount of research of people (E.-C.Yang, H.-K.Zhao, B.Ding, X.-G.Wang, X.-J.Zhao, Cryst.Growth Des.2007,7,2009-2015; D.-R.Xiao, E.-B.Wang, H.-Y.An, Y.-G.Li.L.Xu, Cryst.Growth Des.2007,7,506-512; J.-H.He, J.-H.Yu, Y.-T.Zhang, Q.-H.Pan, R.-R.Xu.Inorg.Chem.2005,44,9279-9282; M.D, X.-J.Jiang, X.-J.Zhao, Chem.Commun.2005,44,5521-5523; N.L.Ros i, J.Kim, M.Eddaoudi, B.Chen, O.M.Yaghi, J.Am.Chem.Soc.2005,127,1504-1518).
1,2, the 4-triazole is considered to the desirable part of a kind of structure multi-nuclear metal ligand polymer with its multiple coordination mode.Compare multinuclear d with common ligand polymer with fluorescence
10Ligand polymer has various topological framework and good fluorescence property and higher thermostability, and the existence of coenocytism also makes it be difficult for being dissolved in the general organic solvent.(Q.-G.Zhai，C.-Z.Lu，S.-M.Chen，X.-J.Xu，W.-B.Yang，Crystal?Growth&Design，2006，6，1393-1398；Q.-G.Zhai，X.-Y.Wu，S.-M.Chen，C.-Z.Lu，W.-B.Yang，2006，6，2126-2135；Q.-G.Zhai，X.-Y.Wu，S.-M.Chen，Z.-G.Zhao，C.-Z.Lu，Inorg.Chem.2007，46，5046-5058；Q.-G.Zhai，C.-Z.Lu，X.-Y.Wu，S.R.Battern，Cryst.Growth&Design，2007，6，2332-2342；B.Ding，L.Yi，P.Cheng，D.-Z.Liao，Shi-Ping?Yan，Inorg.Chem.2006，45，5799-5803；J.-R.Li，Q.Yu，E.C.
，b?Y.Tao，X.-H.Bu，Chem.Commun.，2007，2602?2604；J.-P.Zhang，Y.-Y.Lin，X.-C.Huang，X.-M.Chen，J.Am.Chem.Soc.，2005，127，5495-5506；W.Ouellette，B.S.Hudson，J.Zubieta?Inorg.Chem.2007，46，4887-4904；W.Ouellette，A.V.Prosvirin，V.Chieffo，K.R.Dunbar，B.S.Hudson，J.Zubieta，Inorg.Chem.2006，45，9346-9366；J.Tao，M.-L.Tong，J.-X.Shi，X.-M.Chen，S.W.Ng，Chem?Commun.2000，2043-2044；J.Tao，J.-X.Shi，M.-L.Tong，X.-M.Chen，Inorg.Chem.2001，40，6328-6330)。Therefore, this type of title complex has wide space aspect the further research and development of structural research and performance.
Summary of the invention
One object of the present invention is to provide a kind of high nuclear zinc coordination polymer, and it is the ligand polymer that contains Zn-trz bunch of secondary building unit of 14 nuclears and contain the three-dimensional net structure in two-dimentional duct.
Another object of the present invention is to provide a kind of preparation method of zinc coordination polymer.
A further object of the present invention be to provide a kind of high nuclear zinc coordination polymer in preparation as the application aspect the fluorescent material.The fluorescence data of crystal sample shows that this ligand polymer has good fluorescence property.
Technical scheme of the present invention is as follows: the high nuclear zinc coordination polymer with following chemical general formula:
{[Zn
14(trz)
12(nip)
8(H
2O)
4]·7.5H
2O}
n
Wherein trz is 1,2,4-triazole univalent anion; Nip is a 5-nitroisophthalic acid dianion; Its molecular formula is as follows:
N repeateding unit wherein, n of the present invention＞10.
The secondary building unit of high nuclear zinc coordination polymer of the present invention is Zn-trz bunch of 14 nuclear, and crystal belongs to triclinic(crystalline)system, and spacer is P-1, and unit cell parameters is a=12.3739 (17), b=14.4950 (19),
α=78.997 (2), β=78.968 (2), γ=82.590 (2) °,
Contain two-dimentional duct in the three-dimensional structure of polymkeric substance, channel diameter is
High nuclear zinc coordination polymer of the present invention, its main infrared absorption peak are 3414 (m), 3145 (m), 3090 (m), 1629 (s), 1567 (ms), 1529 (s), 1462 (m), 1374 (s), 1349 (s), 1299 (m), 1202 (w), 1163 (m), 1084 (m), 1039 (w), 1001 (m), 925 (w), 892 (w), 787 (m), 732 (s), 664 (m), 561 (w), 466 (w); Decomposition temperature is 320 ℃ of (see figure 1)s.
The preparation method of high nuclear zinc coordination polymer of the present invention, comprise the steps: that with organic ligand 1,2 4-triazole, 5-nitroisophthalic acid and zinc oxide obtain bulk-shaped monocrystal through hydro-thermal reaction in water solvent, then successively with distilled water, ethanol and ether washing, drying.
Preparation method of the present invention, wherein 1,2, the mol ratio of 4-triazole, 5-nitroisophthalic acid and zinc oxide is 1.5-2.5: 1: 0.85-1.1 preferred 2: 1: 1, is more preferably 2: 1: 0.92.
Heating condition of the present invention is 170-220 ℃, preferred 180-200 ℃, be more preferably 200 ℃, be incubated 3-5 days, preferably be incubated three days after, reduce to room temperature with 5 ℃/h speed.
Aqueous solvent consumption of the present invention is 8-15ml, preferred 10ml.
The distinguishing feature of high nuclear zinc coordination polymer of the present invention is:
(1) preparation of high nuclear zinc coordination polymer of the present invention is different from the d commonly used that reports in the present document
10The synthetic method of metal mixed ligand coordination compound replaces metal-salt to synthesize 14 nuclear zinc coordination polymers that have good thermostability and be not soluble in general organic solvent as the source of title complex metal center with metal oxide.
(2) adopt 14 nuclear zinc coordination polymers of the present invention to make fluorescent material, its luminous efficiency height, brightness is big.
(3) contain two-dimentional duct in the high nuclear of the present invention Zn complex three-dimensional structure, channel diameter is
Can be used for making molecular screen material, separate the particular chemical composition.The different guest molecules of introducing, ion (as contain the phenyl ring organism in this external two-dimentional duct, halide anion) can change the interior π of complexes system ... pi accumulation and C-H ... π interacts, thereby change the fluorescence intensity and the emission wavelength of title complex, be expected to make advanced fluorescence tunable radiation emitting material.
The present invention further discloses high nuclear zinc coordination polymer application as fluorescent material aspect the preparation material.Preferred polymers of the present invention is that 14 nuclear zinc coordination polymers have the good fluorescence performance aspect material, the fluorescence data of this high nuclear zinc coordination polymer crystal prototype shows that this ligand polymer can be used as fluorescent material, be applied to the materialogy field, have good potential application foreground.
Description of drawings
Fig. 1 { [Zn
14(trz)
12(nip)
8(H
2O)
4] 7.5H
2O}
n14 nuclear Zn-trz bunch of secondary building unit figure;
Fig. 2 { [Zn
14(trz)
12(nip)
8(H
2O)
4] 7.5H
2O}
nThree-dimensional net structure figure;
Fig. 3 { [Zn
14(trz)
12(nip)
8(H
2O)
4] 7.5H
2O}
nThermogram;
Fig. 4 { [Zn
14(trz)
12(nip)
8(H
2O)
4] 7.5H
2O}
nFluorescence spectrum figure.
Embodiment
For simple and purpose clearly, hereinafter appropriate omission the description of known technology, in order to avoid those unnecessary details influences are to the description of the technical program.Below in conjunction with preferred embodiment, the present invention will be further described, and what be illustrated especially is, the initial substance 1,2 of preparation The compounds of this invention, and the 4-triazole, the 5-nitroisophthalic acid all can have been bought or easily made by known method from the market.
Embodiment 1
Synthesizing of 14 nuclear zinc coordination polymers:
With organic ligand, 1,2,4-triazole (0.2 mmole, 14 milligrams), 5-nitroisophthalic acid (0.1 mmole, 21 milligrams) and zinc oxide (0.092 mmole, 7.5 milligrams) is dissolved in to stir after 15 minutes in the redistilled water (10ml) and adds in the water heating kettle.Reduce to room temperature with 5 ℃/h and obtain bulk-shaped monocrystal after 3 days in insulation under 200 ℃, then successively with distilled water, ethanol and ether washing, drying.
Main infrared absorption peak is: 3414 (m), 3145 (m), 3090 (m), 1629 (s), 1567 (ms), 1529 (s), 1462 (m), 1374 (s), 1349 (s), 1299 (m), 1202 (w), 1163 (m), 1084 (m), 1039 (w), 1001 (m), 925 (w), 892 (w), 787 (m), 732 (s), 664 (m), 561 (w), 466 (w).
Embodiment 2
Synthesizing of 14 nuclear zinc coordination polymers:
With organic ligand, 1,2,4-triazole (0.25 mmole, 17.5 milligrams), 5-nitroisophthalic acid (0.1 mmole, 21 milligrams) are dissolved in the middle stirring of redistilled water (15ml) after 15 minutes with zinc oxide (0.11 mmole, 9 milligrams), add in the water heating kettle.Reduce to room temperature with 5 ℃/h and obtain bulk-shaped monocrystal after 4 days in insulation under 220 ℃, then successively with distilled water, ethanol and ether washing, drying.
Main infrared absorption peak is: 3414 (m), 3145 (m), 3090 (m), 1629 (s), 1567 (ms), 1529 (s), 1462 (m), 1374 (s), 1349 (s), 1299 (m), 1202 (w), 1163 (m), 1084 (m), 1039 (w), 1001 (m), 925 (w), 892 (w), 787 (m), 732 (s), 664 (m), 561 (w), 466 (w).
Embodiment 3
Synthesizing of 14 nuclear zinc coordination polymers:
With organic ligand, 1,2,4-triazole (0.2 mmole, 14 milligrams), 5-nitroisophthalic acid (0.1 mmole, 21 milligrams) and zinc oxide (0.85 mmole, 6.8 milligrams) are dissolved in the second distillation and stir in (8ml) after 15 minutes, add in the water heating kettle.Reduce to room temperature with 5 ℃/h and obtain bulk-shaped monocrystal after 3 days in insulation under 170 ℃, then successively with distilled water, ethanol and ether washing, drying.
Main infrared absorption peak is: 3414 (m), 3145 (m), 3090 (m), 1629 (s), 1567 (ms), 1529 (s), 1462 (m), 1374 (s), 1349 (s), 1299 (m), 1202 (w), 1163 (m), 1084 (m), 1039 (w), 1001 (m), 925 (w), 892 (w), 787 (m), 732 (s), 664 (m), 561 (w), 466 (w).
Embodiment 4
The relevant characterization of 14 nuclear zinc coordination polymers:
(1) crystal structure determination (Fig. 1,2)
Choose the monocrystalline (seeing embodiment 1) of suitable size at microscopically, at room temperature, use through the Mo of graphite monochromatization K alpha-ray (
) the X-ray diffraction structure (the results are shown in Table 1) of mensuration monocrystalline on Bruker Apex II CCD diffractometer.It is rotten not occur crystalline in the data-gathering process.Carry out the semiempirical absorption correction with the SADABS method.Unit cell parameters is determined with method of least squares.Reduction of data and structure elucidation use SAINT and SHELXL routine package to finish respectively.All non-hydrogen atoms carry out the anisotropy refine with the complete matrix method of least squares.Structure is seen Fig. 1: Zn-trz bunch of secondary building unit figure of 14 nuclears of ligand polymer; Fig. 2: the three-dimensional net structure figure of ligand polymer.
The solid fluorescence character of (2) ten four nuclear zinc coordination polymers
Ligand polymer crystal prototype (seeing embodiment 1) after enrichment is handled is through further milled processed, and carry out the test of solid fluorescence: ligand polymer excites at the 374nm place, obtains maximum emission peak at the 423nm place, sees Fig. 4.(instrument model: Varian Caryeclipse).
Embodiment 5
The polymethyl methacrylate of 4 grams is dissolved in the dichloromethane solution, is decided to be solution A; Getting high nuclear Zn complex 0.00021 gram again is dissolved in the 100ml dimethyl sulfoxide solution and is decided to be solution B; Get A10ml, solution B 10ml stirs in a container, is coated in the transparent fluorescence membrane that gets controllable thickness on the colourless egative film after the drying, shows bright purple light under the 200nm-450nm rayed.The purple light of angle emitting bright under daylight tilts.This solution is coated on the colour picture because the background color difference can obtain tenebrescents such as livid purple look, red-purple.
The main crystallographic data of table 1 14 nuclear zinc coordination polymers
Claims (8)
1. the high nuclear zinc coordination polymer that has following chemical general formula:
{[Zn
14(trz)
12(nip)
8(H
2O)
4]·7.5H
2O}
n
Wherein trz is 1,2,4-triazole univalent anion; Nip is a 5-nitroisophthalic acid dianion; N＞10; Its molecular formula is as follows:
2. the described high nuclear zinc coordination polymer of claim 1, the secondary building unit that it is characterized in that described polymkeric substance are Zn-trz bunch of 14 nuclear, and crystal belongs to triclinic(crystalline)system, and spacer is P-1, and unit cell parameters is a=12.3739 (17), b=14.4950 (19),
α=78.997 (2), β=78.968 (2), γ=82.590 (2) °,
Contain two-dimentional duct in the three-dimensional structure of polymkeric substance, channel diameter is
3. the described high nuclear zinc coordination polymer of claim 1, its main infrared absorption peak is 3414 (m), 3145 (m), 3090 (m), 1629 (s), 1567 (ms), 1529 (s), 1462 (m), 1374 (s), 1349 (s), 1299 (m), 1202 (w), 1163 (m), 1084 (m), 1039 (w), 1001 (m), 925 (w), 892 (w), 787 (m), 732 (s), 664 (m), 561 (w), 466 (w); Decomposition temperature is 320 ℃.
4. the preparation method of the described high nuclear zinc coordination polymer of claim 1, it is characterized in that it comprises the steps: organic ligand 1,2,4-triazole, 5-nitroisophthalic acid and zinc oxide obtain bulk-shaped monocrystal through hydro-thermal reaction in water solvent, then successively with distilled water, ethanol and ether washing, drying.
5. the described preparation method of claim 4, wherein 1,2, the mol ratio of 4-triazole, 5-nitroisophthalic acid and zinc oxide is 1.5-2.5: 1: 0.85-1.1.
6. the described preparation method of claim 4 is characterized in that described water consumption is 8-15ml.
7. the described preparation method of claim 4, the temperature that it is characterized in that described thermal response is 170-220 ℃, is incubated 3-5 days, drops to room temperature with 5 ℃/h.
8. the application of each described high nuclear zinc coordination polymer of claim 1-3 aspect the preparation fluorescent material.
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