CN102382145B - Cobalt coordination compound containing 5-(3-pyridyl)-isophthalic acid organic ligands and preparation method for same - Google Patents
Cobalt coordination compound containing 5-(3-pyridyl)-isophthalic acid organic ligands and preparation method for same Download PDFInfo
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- CN102382145B CN102382145B CN 201110248841 CN201110248841A CN102382145B CN 102382145 B CN102382145 B CN 102382145B CN 201110248841 CN201110248841 CN 201110248841 CN 201110248841 A CN201110248841 A CN 201110248841A CN 102382145 B CN102382145 B CN 102382145B
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Abstract
One kind containing the metal cobalt complex and preparation method thereof of 5- (3- pyridine)-M-phthalic acid organic ligand, chemical formula is [Co (C13H9O4N) (2H2O)] n, hexagonal crystal system, space group are P65 (No.170), and cell parameter is
. The invention has the advantages that 1, have good fluorescent characteristic, fluorescence intensity is larger; 2, difference low with the thermal decomposition temperature of most of complexs, the better heat stability of synthesized compound, thermal decomposition temperature are 190 DEG C; 3, synthetic method is simple, and easy to operate, sufficient raw, low production cost, the yield of compound synthesis are higher, and purity is also very high and reproducible, so that it is suitble to the requirement of expanded production.
Description
Technical field
The present invention relates to cobalt metal title complex of a kind of 5-of containing (3-pyridine)-m-phthalic acid organic ligand and preparation method thereof.
Background technology
5-(3-pyridine)-m-phthalic acid, English name 5-(3-Pyridyl)-isophthalic acid, as a kind of multiple tooth, multiple spot coordination organic ligand, can be widely used in the synthetic synthetic and research that spectroscopy, pharmacology and biologic inorganic are learned the novel complex material of researching value that has, it is a flexible and changeable part, have multiple coordination mode, it can form stable title complex with transition metal or rare earth ion.These title complexs are all significant such as scientific domains such as stereochemistry, coordination chemistry, bio-inorganic chemistry, magnetic, spectroscopy research and reaction mechanisms.Therefore research in depth contains structure and the character of the cobalt metal title complex of 5-(3-pyridine)-m-phthalic acid organic ligand, can not only more can play a role in many aspects such as optical element exploitation, bionics techniques, biologic inorganic and drug developments in the coordination chemistry field for we provide more more novel structural modelss.
Summary of the invention
The object of the present invention is to provide cobalt metal title complex of a kind of 5-of containing (3-pyridine)-m-phthalic acid organic ligand and preparation method thereof, synthetic method is simple, the synthetic productive rate of easy to operate, sufficient raw, low production cost, compound is higher, purity is very high and good reproducibility also, makes it be fit to the requirement that extension is produced.
The present invention is achieved like this, and it is characterized in that target compound is the cobalt metal title complex that contains 5-(3-pyridine)-m-phthalic acid organic ligand, and its chemical formula is [Co (C
13H
7O
4N) (2H
2O)]
n, hexagonal system, spacer is P6
5(No. 170), cell parameter is
a=10.1 ~ 10.3
,
b=10.1～10.3
,
c=20.2～20.4
,
=89～91
,
=89～91
,
=119～121
Z=6, the cobalt metal title complex that contains 5-(3-pyridine)-m-phthalic acid organic ligand: with cobalt chloride, 5-(3-pyridine)-m-phthalic acid mixes according to the molar ratio of 2:3, wherein the consumption of cobalt chloride is 0.06 mmole, put into then and fill 8 milliliters of acetonitriles, the volume of 4 ml methanol and 2 ml distilled waters is in 25 milliliters the autoclave, then 150 ℃ of following constant temperature 3 days, in 5 days, temperature is down to room temperature at last, obtain the purple bulk crystals this moment for containing the cobalt metal title complex of 5-(3-pyridine)-m-phthalic acid organic ligand, productive rate is 80-89%.
The cobalt metal title complex of the 5-of containing of the present invention (3-pyridine)-m-phthalic acid organic ligand can be applicable to fluorescent material.
The concrete reaction formula of the present invention is:
N C
13H
9O
4N (5-(3-pyridine)-m-phthalic acid)+n CoCl
2+ 2n H
2O
[Co (C
13H
7O
4N) (2H
2O)]
n+ 2n HCl
Advantage of the present invention is: 1, good fluorescent characteristic is arranged, and its fluorescence intensity is bigger, and its maximum emission peak is at 410 nm, and the maximum excitation peak is at 340 nm; 2, low different with the heat decomposition temperature of most of title complexs, the better heat stability of the compound that is synthesized, its heat decomposition temperature is 190 ℃; 3, synthetic method is simple, and the synthetic productive rate of easy to operate, sufficient raw, low production cost, compound is higher, and purity is very high and good reproducibility also, makes it be fit to requirement that extension is produced.
Description of drawings
(symmetric code among the figure is Fig. 1: A:1+y ,-x+y, 1/6+z for the structure iron of The compounds of this invention molecule; B:1+x, 1+y, z; C:-1+x-y ,-1+x ,-1/6+z; E:-1+x ,-1+y, z).
Fig. 2 is the XRD powder diagram of The compounds of this invention.
Fig. 3 is the fluorescence spectrum figure of The compounds of this invention.
Embodiment
Compound of the present invention [Co (C
13H
7O
4N) (2H
2O)]
nSynthetic:
[Co (C
13H
7O
4N) (2H
2O)]
nAdopt conventional solvent-thermal method to obtain, concrete reaction formula is:
N C
13H
9O
4N (5-(3-pyridine)-m-phthalic acid)+n CoCl
2+ 2n H
2O
[Co (C
13H
7O
4N) (2H
2O)]
n+ 2n HCl
The concrete operations step is: with cobalt chloride, 5-(3-pyridine)-m-phthalic acid mixes according to the molar ratio of 2:3, wherein the consumption of cobalt chloride is 0.06 mmole, put into the volume that fills 8 milliliters of acetonitriles, 4 ml methanol and 2 ml distilled waters then and be 25 milliliters autoclave, then 150 ℃ of following constant temperature 3 days, in 5 days, temperature is down to room temperature at last, obtain the purple bulk crystals this moment for containing the 5-(3-pyridine)-the cobalt metal title complex of m-phthalic acid organic ligand, productive rate is 80-89%.Be target compound through this crystal of single crystal diffractometer test shows, ultimate analysis shows that the mass percent of carbon in this compound, hydrogen and nitrogen element is: H 3.32%, and C 46.46%, and N 4.19%.
Through the single crystal diffractometer test shows, the chemical formula of compound of the present invention is [Co (C
13H
7O
4N) (2H
2O)]
n, hexagonal system, spacer is P6
5(No. 170), unit cell parameters is: a=10.2357
, b=10.2357
, c=20.3953
,
=90
,
=90
,
=120
, Z=6; The molecular structure of compound is seen Fig. 1, and the powdery diffractometry test result of compound is seen Fig. 2.Through fluorescence spectrum test shows (as shown in Figure 3), this compound has good fluorescent characteristic, and its fluorescence intensity is bigger, and its maximum emission peak is at 410nm, and the maximum excitation peak is at 340 nm.The heat decomposition temperature of the compound of thermogravimetric analysis test shows in addition is 190 ℃, and therefore compound of the present invention can be used as good potential fluorescent material.
Claims (2)
1. a cobalt metal title complex that contains 5-(3-pyridine)-m-phthalic acid organic ligand is characterized in that chemical formula is [Co (C
13H
7O
4N) (2H
2O)]
n, hexagonal system, spacer is P6
5, cell parameter is
a=10.1 ~ 10.3
,
b=10.1～10.3
,
c=20.2～20.4
,
=89～91
,
=89～91
,
=119～121
, Z=6.
2. described preparation method who contains the cobalt metal title complex of 5-(3-pyridine)-m-phthalic acid organic ligand of claim 1, it is characterized in that cobalt chloride, 5-(3-pyridine)-m-phthalic acid mixes according to the molar ratio of 2:3, wherein the consumption of cobalt chloride is 0.06 mmole, put into then and fill 8 milliliters of acetonitriles, the volume of 4 ml methanol and 2 ml distilled waters is in 25 milliliters the autoclave, then 150 ℃ of following constant temperature 3 days, in 5 days, temperature is down to room temperature at last, obtains the purple bulk crystals this moment for containing the cobalt metal title complex of 5-(3-pyridine)-m-phthalic acid organic ligand.
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| CN102382145B true CN102382145B (en) | 2013-09-25 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080184883A1 (en) * | 2007-02-02 | 2008-08-07 | Miami University | Mesh-Adjustable Molecular Sieve |
| CN101759723A (en) * | 2009-12-10 | 2010-06-30 | 郑州轻工业学院 | 1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole and 4, 4'-bipyridyl blending cobalt composition and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080184883A1 (en) * | 2007-02-02 | 2008-08-07 | Miami University | Mesh-Adjustable Molecular Sieve |
| CN101759723A (en) * | 2009-12-10 | 2010-06-30 | 郑州轻工业学院 | 1-(4-carboxy phenyl)-5-sulfydryl-1H-tetrazole and 4, 4'-bipyridyl blending cobalt composition and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Nanotubular Metal-Organic Frameworks with High Porosity Based on T-Shaped Pyridyl Dicarboxylate Ligands;Shenglin Xiang等,;《Inorg. Chem.》;20110119;第50卷(第5期);第1743-1748页 * |
| 间苯二甲酸根桥联双核钴(Ⅱ)配合物的合成、表征和磁性;焉翠蔚等,;《曲阜师范大学学报》;19960430;第22卷(第2期);第101-104页 * |
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