CN101701021B - Rare earth lanthanum chelidonamic acid complex and preparation method thereof - Google Patents
Rare earth lanthanum chelidonamic acid complex and preparation method thereof Download PDFInfo
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- CN101701021B CN101701021B CN2009101864147A CN200910186414A CN101701021B CN 101701021 B CN101701021 B CN 101701021B CN 2009101864147 A CN2009101864147 A CN 2009101864147A CN 200910186414 A CN200910186414 A CN 200910186414A CN 101701021 B CN101701021 B CN 101701021B
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- acid complex
- rare earth
- chelidonamic acid
- chelidonamic
- earth lanthanum
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Abstract
A kind of rare earth lanthanum chelidonamic acid complex, it is characterized in that chemical formula are as follows: [La (C 7H 2NO 5) 4H 2O] n, monoclinic system, space group are P2 (1)/n (No.14), and cell parameter is
α=89~91, β=100~110, γ=89~91 °, Z=4. The invention has the advantages that 1, have good fluorescent characteristic, fluorescence intensity is larger, and peak is wider; 2, difference low with the thermal decomposition temperature of most of complexs, the better heat stability of synthesized compound, thermal decomposition temperature are 180 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 a kind of rare earth lanthanum chelidonamic acid complex and preparation method thereof.
Background technology
Chelidonamic acid, English name 2,6-dicarboxy-4-hydroxypyridine or chelidamic acid, multiple tooth, multiple spot coordination organic ligand as a kind of classics, 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, has multiple coordination mode, and it can form stable title complex with transition metal or rare earth ion.These title complexs are all significant such as the scientific domains such as repercussion study of stereochemistry, coordination chemistry, bio-inorganic chemistry, magnetic, spectroscopy research and reaction mechanism, phenolic group pyridine ligand.Therefore in depth study the structure and the character of metal chelidonamic acid complex, can not only more can play a role in the coordination chemistry field for we provide more more novel structural modelss in many aspects such as optical element exploitation, bionics techniques, biologic inorganic and drug developments.
Summary of the invention
The object of the present invention is to provide a kind of rare earth lanthanum chelidonamic acid complex and preparation method thereof, synthetic method is simple, the synthetic productive rate of easy to operate, sufficient raw, low production cost, compound is higher, the also very high and good reproducibility of purity 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 lanthanoid metal chelidonamic acid complex, and its chemical formula is [La (C
7H
2NO
5) 4H
2O]
n, oblique system, spacer is P2 (1)/n (No.14), cell parameter is a=9.4～10.4
, b=7.0～8.0
, c=15.0～16.0
, α=89～91, β=100～110, γ=89～91 °, Z=4.
The preparation method of lanthanoid metal chelidonamic acid complex is: with Lanthanum trichloride, chelidonamic acid mixes according to 1: 1 molar ratio, put into the volume that fills 10 ml distilled waters then and be 25 milliliters autoclave, constant temperature burnt 3 days at 413K then, in 3 days, temperature is reduced to room temperature at last, obtain yellow styloid this moment is the lanthanoid metal chelidonamic acid complex, and productive rate is 75-85%.
Rare earth lanthanum chelidonamic acid complex of the present invention can be applicable to fluorescent material.
The concrete reaction formula of the present invention is:
NC
7H
5NO
5(chelidonamic acid)+n LaCl
3+ 4.0n H
2O → [La (C
7H
2NO
5) 4H
2O]
n+ 3.0n HCl
Advantage of the present invention is: 1, good fluorescent characteristic is arranged, and its fluorescence intensity is bigger, and the peak is than broad, and the position of its emission peak is at 451nm, and the position of excitation peak is at 318nm; 2, low different with the heat decomposition temperature of most of title complexs, the better heat stability of institute's synthetic compound, its heat decomposition temperature is 180 ℃; 3, synthetic method is simple, and the synthetic productive rate of easy to operate, sufficient raw, low production cost, compound is higher, and the also very high and good reproducibility of purity makes it be fit to requirement that extension is produced.
Description of drawings
Fig. 1 is the structure iron of The compounds of this invention molecule.
Fig. 2 is the fluorescence spectrum figure of The compounds of this invention.
Fig. 3 is the uv drs figure of The compounds of this invention.
Embodiment
Compound of the present invention [La (C
7H
2NO
5) 4H
2O]
nSynthetic:
[La (C
7H
2NO
5) 4H
2O]
nAdopt conventional hydrothermal method to obtain, concrete reaction formula is:
NC
7H
5NO
5(chelidonamic acid)+n LaCl
3+ 4.0n H
2O → [La (C
7H
2NO
5) 4H
2O]
n+ 3.0n HCl
The concrete operations step is: with Lanthanum trichloride, chelidonamic acid mixes according to 1: 1 molar ratio, put into the volume that fills 10 ml distilled waters then and be 25 milliliters autoclave, constant temperature burnt 3 days at 413K then, in 3 days, temperature is reduced to room temperature at last, obtain yellow styloid this moment, and productive rate is about 79%.Through this crystal of single crystal diffractometer test shows is target compound.
As Fig. 1, Fig. 2, shown in Figure 3, crystal parameters of the present invention is: a=9.4～10.4
, b=7.0～8.0
, c=15.0～16.0
, α=89～91, β=100～110, γ=89～91 °, Z=4.Through uv drs and fluorescence spectrum test shows, this compound is a semi-conductor, and it can the band value be 3.58eV, this compound has good fluorescent characteristic, and its fluorescence intensity is bigger, and the peak compares broad, the position of its emission peak is at 451nm, and the position of excitation peak is at 318nm.In addition, the heat stability testing of compound shows that its heat decomposition temperature is 180 ℃, therefore can be used as good potential fluorescent material.
Claims (2)
1. a rare earth lanthanum chelidonamic acid complex is characterized in that chemical formula is [La (C
7H
2NO
5) 4H
2O]
n, oblique system, spacer is P2 (1)/n (No.14), cell parameter is a=9.4～10.4
B=7.0～8.0
C=15.0～16.0
α=89～91, β=100～110, γ=89～91 °, Z=4.
2. the preparation method of the described a kind of rare earth lanthanum chelidonamic acid complex of claim 1, it is characterized in that Lanthanum trichloride, chelidonamic acid mixes according to 1: 1 molar ratio, put into the volume that fills 10 ml distilled waters then and be 25 milliliters autoclave, constant temperature burnt 3 days at 413K then, in 3 days temperature is reduced to room temperature at last, obtain yellow styloid this moment is the lanthanoid metal chelidonamic acid complex.
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|---|---|---|---|
| CN2009101864147A CN101701021B (en) | 2009-11-02 | 2009-11-02 | Rare earth lanthanum chelidonamic acid complex and preparation method thereof |
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|---|---|---|---|
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|---|---|
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| CN101701021B true CN101701021B (en) | 2011-09-14 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102127426A (en) * | 2011-01-11 | 2011-07-20 | 宁波大学 | Fluorescent material with purple luminescence property and preparation method thereof |
| CN102516275B (en) * | 2011-10-26 | 2014-05-07 | 南昌航空大学 | Rare earth metal lanthanum chelidonamic acid complex with asymmetric center and preparation method thereof |
| CN102675195B (en) * | 2012-06-02 | 2013-09-25 | 南昌航空大学 | Chelidamic acid complex of rare-earth metal praseodymium and preparation method for chelidamic acid complex |
| CN108888781B (en) * | 2018-06-27 | 2021-08-06 | 华东理工大学 | Preparation method of supramolecular polyelectrolyte micelle magnetic resonance imaging contrast agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450926A (en) * | 2008-12-01 | 2009-06-10 | 南昌航空大学 | Metal zinc ammonchelidonic acid complexes and preparation method thereof |
| CN101492417A (en) * | 2009-03-10 | 2009-07-29 | 南昌航空大学 | Metallic copper chelidonamic acid complex and method for preparing the same |
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2009
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101450926A (en) * | 2008-12-01 | 2009-06-10 | 南昌航空大学 | Metal zinc ammonchelidonic acid complexes and preparation method thereof |
| CN101492417A (en) * | 2009-03-10 | 2009-07-29 | 南昌航空大学 | Metallic copper chelidonamic acid complex and method for preparing the same |
Non-Patent Citations (1)
| Title |
|---|
| Anne-Sophie Chauvin et al..A Versatile Ditopic Ligand System for Sensitizing the Luminescence of Bimetallic Lanthanide Bio-Imaging Probes.《Chem. Eur. J.》.2007,第14卷1726– 1739. * |
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