CN102516275B - Rare earth metal lanthanum chelidonamic acid complex with asymmetric center and preparation method thereof - Google Patents
Rare earth metal lanthanum chelidonamic acid complex with asymmetric center and preparation method thereof Download PDFInfo
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- CN102516275B CN102516275B CN201110329665.3A CN201110329665A CN102516275B CN 102516275 B CN102516275 B CN 102516275B CN 201110329665 A CN201110329665 A CN 201110329665A CN 102516275 B CN102516275 B CN 102516275B
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Abstract
A kind of rare earth lanthanum chelidonamic acid complex and preparation method thereof with center of asymmetry, it is characterized in that chemical formula is
, monoclinic system, space group is Cc (No.9), and cell parameter is
The invention has the advantages that 1,There is good fluorescent characteristic,Its fluorescence intensity is larger,Peak is wider; 2,The complex has center of asymmetry space group,There are preferable Nonlinear Second order Optical Properties; 3,Difference low with the thermal decomposition temperature of most of complexs,The better heat stability of synthesized compound,Its thermal decomposition temperature is 180 DEG C; 4,Synthetic method is simple,Easy to operate,Sufficient raw,Low production cost,The yield of compound synthesis is higher,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 with center of asymmetry and preparation method thereof.
Background technology
Chelidonamic acid, English name 2,6-dicarboxy-4-hydroxypyridine or chelidamic acid, as a kind of multiple tooth, multiple spot coordination organic ligand of classics, be widely used in the synthetic and research of the synthetic novel complex material with spectroscopy, pharmacology and biologic inorganic researching value, 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 in scientific domains such as the repercussion studies such as stereochemistry, coordination chemistry, bio-inorganic chemistry, magnetic, spectroscopy research and reaction mechanism, phenolic group pyridine ligand.Therefore in depth study structure and the character of metal chelidonamic acid complex, can not only, in coordination chemistry field for we provide more more novel structural modelss, more can play a role 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 with center of asymmetry and preparation method thereof, its synthetic method is simple, the productive rate of easy to operate, sufficient raw, low production cost, compou nd synthesis is higher, purity is also very high and reproducible, makes it be applicable 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 with center of asymmetry, and its chemical formula is,
The preparation method of lanthanoid metal chelidonamic acid complex is: chelidonamic acid, zinc nitrate, lanthanum acetate and 4,4-dipyridyl are weighed respectively according to the molar ratio of 4:2:1:2, and wherein the consumption of chelidonamic acid is 20mg; Add 10 ml deionized water in the beaker that fills chelidonamic acid, be then heated to dissolve completely; Again by with 4 after dissolve with ethanol, 4-dipyridyl directly adds and fills in chelidonamic acid clear liquor solution; The last aqueous solution that slowly drips successively zinc nitrate and lanthanum acetate, finally regulating pH is 7, standing after filtering, after about one week, obtaining yellow bulk crystals is lanthanoid metal chelidonamic acid complex.Productive rate is 70-78%.
Rare earth lanthanum chelidonamic acid complex of the present invention is expected to be widely used in fields such as fluorescent material, short-wavelength laser and photomodulators.
The concrete reaction formula of the present invention is:
Advantage of the present invention is: 1, have good fluorescent characteristic, its fluorescence intensity is larger, and peak is wider, and the position of its emission peak is at 476 nm, and the position of excitation peak is at 336 nm; 2, this title complex has center of asymmetry spacer, has good Nonlinear Second order Optical Properties, and its second-harmonic generation is KDP(potassium primary phosphate) 0.3 times; 3, low different from the heat decomposition temperature of most of title complexs, the better heat stability of the compound of synthesized, its heat decomposition temperature is 180 ℃; 4, synthetic method is simple, and the productive rate of easy to operate, sufficient raw, low production cost, compou nd synthesis is higher, and purity is also very high and reproducible, makes it be applicable to the requirement that extension is produced.
Accompanying drawing explanation
Fig. 1 is the structure iron of the compounds of this invention molecule.
Fig. 2 is the powder diagram of the compounds of this invention.
Fig. 3 is the fluorescence spectrum figure of the compounds of this invention.
Fig. 4 is the uv drs figure of the compounds of this invention.
Embodiment
Compound of the present invention
synthetic:
Concrete operation step is: chelidonamic acid, zinc nitrate, lanthanum acetate and 4,4-dipyridyl are weighed respectively according to the molar ratio of 4:2:1:2, and wherein the consumption of chelidonamic acid is 20mg; Add 10 ml deionized water in the beaker that fills chelidonamic acid, be then heated to dissolve completely; Again by with 4 after dissolve with ethanol, 4-dipyridyl directly adds and fills in chelidonamic acid clear liquor solution; The last aqueous solution that slowly drips successively zinc nitrate and lanthanum acetate, finally regulating pH is 7, standing after filtering, after about one week, obtaining yellow bulk crystals is lanthanoid metal chelidonamic acid complex.Productive rate is about 73%.Through single crystal diffractometer test, show that this crystal is target compound.
As shown in Figure 1, Figure 2, Figure 3, Figure 4, crystal parameters of the present invention is:
.Through uv drs and fluorescence spectrum test, show, this compound is semi-conductor, it can band value be 3.45 eV, this compound has good fluorescent characteristic, and its fluorescence intensity is larger, and peak is wider, the position of its emission peak is at 476 nm,, at 336 nm, there is good Nonlinear Second order Optical Properties the position of excitation peak, and its second-harmonic generation is KDP(potassium primary phosphate) 0.3 times.In addition, the heat stability testing of compound shows that its heat decomposition temperature is 180 ℃.Therefore can be used as good potential nonlinear optics or fluorescent material, also can obtain potential application in fields such as short-wavelength laser and photomodulators.
Claims (2)
1. there is a rare earth lanthanum chelidonamic acid complex for center of asymmetry, it is characterized in that
.
2. the preparation method of a rare earth lanthanum chelidonamic acid complex with center of asymmetry claimed in claim 1, it is characterized in that chelidonamic acid, zinc nitrate, lanthanum acetate and 4,4-dipyridyl weighs respectively according to the molar ratio of 4:2:1:2, and wherein the consumption of chelidonamic acid is 20mg; Add 10 ml deionized water in the beaker that fills chelidonamic acid, be then heated to dissolve completely; Again by with 4 after dissolve with ethanol, 4-dipyridyl directly adds and fills in chelidonamic acid clear liquor solution; The last aqueous solution that slowly drips successively zinc nitrate and lanthanum acetate, final pH=7, standing after filtering, after one week, obtaining yellow bulk crystals is lanthanoid metal chelidonamic acid complex.
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| CN101701021A (en) * | 2009-11-02 | 2010-05-05 | 南昌航空大学 | Rare earth lanthanum chelidonamic acid complex and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| Qiu-Ju Xing,et al.."Crystal structure of tetraaqua(4-oxo-pyridine-2,6-dicarboxylato-N,O,Oˊ)lanthanum(III) monohydrate, La(H2O)4(C7H2NO5).H2O".《Zeitschrift fuer Kristallographie- New Crystal Structures》.2010,第225卷(第4期),671-672. * |
| Qiu-JuXing et al.."Crystal structure of tetraaqua(4-oxo-pyridine-2 |
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