CN103772419B - A kind of preparation method of cadmium metal organic coordination compound - Google Patents
A kind of preparation method of cadmium metal organic coordination compound Download PDFInfo
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- CN103772419B CN103772419B CN201310743310.8A CN201310743310A CN103772419B CN 103772419 B CN103772419 B CN 103772419B CN 201310743310 A CN201310743310 A CN 201310743310A CN 103772419 B CN103772419 B CN 103772419B
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- nicotinic acid
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Abstract
The invention discloses a kind of preparation method of cadmium metal organic coordination compound, it is characterized in that comprising the following steps: by the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2o mixture is added in the distilled water of 10ml, drip NaOH solution and regulate pH to 2-4, abundant stirring is placed on to be done in the stainless steel cauldron of lining with tetrafluoroethylene, after 430-440K Water Under thermal response 2.9-3.2d, slowly be cooled to room temperature and obtain colorless plate crystal, be described cadmium metal organic coordination compound, title complex of the present invention has fluorescence, can be applied in fluorescent material.
Description
Technical field
The present invention relates generally to Material Field, particularly relates to a kind of preparation method of cadmium metal organic coordination compound.
Background technology
Ligand polymer be by as tie point metal ion and the compound that formed by coordinate bond of the part of bridge linking effect, its dimension has zero dimension, one dimension, two dimension and three-dimensional.Metal organic coordination polymer has the character of inorganic metal ion and organic ligand simultaneously, because of in fluorescence, magneticsubstance, gas adsorption and be separated, have potential application and cause people in antibacterial and nonlinear optical material and study interest widely.Nineteen ninety-five, O.M.Yaghi study group proposes the concept of " metal-organicframeworks " first, and has delivered one section of report synthesized about MOF-5 with 1999.In recent ten years, investigators utilize different organic ligands and many kinds of metal ions effect, have prepared the MOFs of many novel structures, excellent.Research shows, the formation of title complex and structure are subject to the impact of many factors, the structures and characteristics of part is the key factor affecting title complex, therefore suitable organic ligand and metal ion how is selected, control the condition of reaction, directed assembles the key problem that target compound is current research.
The large more options of part preparing a metal-organic complex contain the organism of the donor atoms such as O, N, S, such as oxygen containing carboxylic-acid and nitrogenous pyridines, a large amount of a metal-organic complex that utilized the part of carboxylic-acid and pyridines to synthesize.Nicotinic acid is the part that synthetic compound is conventional, has reported many title complexs utilizing nicotinic acid to synthesize in document.As a kind of derivative of nicotinic acid, 6-amino-nicotinic acid contains an amino than nicotinic acid more, and different coordination modes can be taked in the preparation process of title complex to form multiple topological framework, and in addition, amino as the acceptor of hydrogen bond, can form the compound of higher-dimension.On the other hand, 6-amino-nicotinic acid is a chiral material, adds the possibility of synthesis of chiral title complex.But the title complex utilizing 6-amino-nicotinic acid to synthesize so far have not been reported.
Summary of the invention
The object of the invention is just to provide a kind of preparation method of cadmium metal organic coordination compound.
The present invention is achieved by the following technical solutions:
A preparation method for cadmium metal organic coordination compound, comprises the following steps:
By the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2o mixture is added in the distilled water of 6-10ml, drip NaOH solution and regulate pH to 2-4, abundant stirring is placed on to be done in the stainless steel cauldron of lining with tetrafluoroethylene, after 430-440K Water Under thermal response 2.9-3.2d, slowly be cooled to room temperature and obtain colorless plate crystal, be described cadmium metal organic coordination compound.
Advantage of the present invention is:
Title complex of the present invention has fluorescence, can be applied in fluorescent material.
Accompanying drawing explanation
Fig. 1 is the fluorescence pattern of title complex of the present invention;
Fig. 2 is the thermogravimetric curve of title complex of the present invention;
Fig. 3, Fig. 4, Fig. 5 are the structure iron of title complex.
Embodiment
Embodiment 1
A preparation method for cadmium metal organic coordination compound, comprises the following steps:
By the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 10ml, drip NaOH solution and regulate about pH to 2, abundant stirring is placed on to be done in the stainless steel cauldron of lining with tetrafluoroethylene, after 433K Water Under thermal response 3d, slowly be cooled to room temperature and obtain colorless plate crystal, be described cadmium metal organic coordination compound.
Embodiment 2
By the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 10ml, drips NaOH solution and regulates about pH to 3, fully stirs to be placed on and does in the stainless steel cauldron of lining with tetrafluoroethylene, after 433K Water Under thermal response 3d, be slowly cooled to room temperature and obtain target product.
Embodiment 3
By the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 6ml, drips NaOH solution and regulates about pH to 4, fully stirs to be placed on and does in the stainless steel cauldron of lining with tetrafluoroethylene, after 433K Water Under thermal response 3d, be slowly cooled to room temperature and obtain target product.
The crystalline structure test of title complex:
Adopt BrukerSmartApexCCD single crystal diffractometer to test crystal, result proves that crystal is title complex [Cd (6-Aminonicotinicacid)
2]
n.Crystal belongs to chiral space group P4
12
12, unit cell parameters is: a=8.0200 (12), b=8.0200 (12), c=21.928 (7), β=90.000 °, V=1410.4 (5)
3, Z=4, Dcalc=1.821g/cm
3, μ=0.1.569mm
1, F (000)=760, R
1=0.0233, ω R
2=0.0485.This title complex asymmetric cell comprises half Cd
2+with a 6-amino-nicotinic acid part, Cd
2+the octoploids structure of hexa-coordinate that what center was taked is.6-amino-nicotinic acid connects two Cd
2+, form unlimited 1D chiral structure.Adjacent 1D chirality chain is by sharing Cd
2+, form the 2D plane layer with square meshwork.In 2D structure, along different directions, there is different chiral structures.Adjacent 2D reticulated structure, by not having the Sauerstoffatom of coordination and the hydrogen bond action of nitrogen-atoms in 6-amino-nicotinic acid, is connected to form 3D structure.What is interesting is, the chirality in two adjacent faces is contrary, and the 3D structure of formation is achiral.
Complex fluorescent is tested:
At room temperature, SHIMAZUVF-320 spectrophotofluorometer is utilized to test the fluorescence of title complex.Result shows, the title complex of formation has fluorescence, and pure part does not have fluorescence.
Claims (1)
1. a preparation method for cadmium metal organic coordination compound, is characterized in that comprising the following steps:
By the 6-amino-nicotinic acid of 0.2mmol and the Cd (NO of 0.1mmol
3)
24H
2o mixture is added in the distilled water of 6-10ml, drip NaOH solution and regulate pH to 2-4, abundant stirring is placed on to be done in the stainless steel cauldron of lining with tetrafluoroethylene, after 430-440K Water Under thermal response 2.9-3.2d, slowly be cooled to room temperature and obtain colorless plate crystal, be described cadmium metal organic coordination compound;
Adopt BrukerSmartApexCCD single crystal diffractometer to test crystal, described cadmium metal organic coordination compound is [Cd (6-aminonicotinate)
2]
n, crystal belongs to chiral space group P4
12
12, unit cell parameters is: a=8.0200 (12), b=8.0200 (12), c=21.928 (7), β=90.000 °, V=1410.4 (5)
3, Z=4, Dcalc=1.821g/cm
3, μ=0.1.569mm
1, F (000)=760, R
1=0.0233, ω R
2=0.0485, this title complex asymmetric cell comprises half Cd
2+with a 6-amino-nicotinic acid part, Cd
2+the octoploids structure of hexa-coordinate that what center was taked is; 6-amino-nicotinic acid connects two Cd
2+, form unlimited 1D chiral structure; Adjacent 1D chirality chain is by sharing Cd
2+, form the 2D plane layer with square meshwork, in 2D structure, along different directions, there is different chiral structures; Adjacent 2D reticulated structure, by not having the Sauerstoffatom of coordination and the hydrogen bond action of nitrogen-atoms in 6-amino-nicotinic acid, is connected to form 3D structure, and the chirality in two adjacent faces is contrary, and the 3D structure of formation is achiral.
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| CN103772419B true CN103772419B (en) | 2016-03-30 |
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| CN105237472B (en) * | 2015-10-30 | 2017-02-15 | 淮南师范学院 | Substituted pyridine complex and preparation method therefor as well as application of substituted pyridine complex as nonlinear optical material, ferroelectric material and fluorescent material |
| CN105503915B (en) * | 2015-12-16 | 2017-05-03 | 西北大学 | Europium metal-organic framework compound with fluorescent recognition function and preparation method and application |
| CN109053557A (en) * | 2018-09-18 | 2018-12-21 | 淮南师范学院 | A kind of application of Zn complex and preparation method thereof as well as black light electroluminescent material |
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| CN101948478B (en) * | 2010-09-03 | 2011-12-07 | 天津师范大学 | Cadmium (II) coordination compound including 5-bromoniacin and preparation method thereof |
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