CN103772419A - Preparation method of cadmium metal organic complex - Google Patents
Preparation method of cadmium metal organic complex Download PDFInfo
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- CN103772419A CN103772419A CN201310743310.8A CN201310743310A CN103772419A CN 103772419 A CN103772419 A CN 103772419A CN 201310743310 A CN201310743310 A CN 201310743310A CN 103772419 A CN103772419 A CN 103772419A
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Abstract
The invention discloses a preparation method of a cadmium metal organic complex. The preparation method is characterized by comprising the steps: adding a mixture of 0.2mmol of 6-aminonicotinic acid and 0.1mmol of Cd(NO3)2.4H2O into 10ml of distilled water, adding a NaOH solution dropwise until a pH value is 2-4, fully mixing, putting a mixture into a stainless steel reaction kettle with polytetrafluoroethylene as a liner, carrying out hydrothermal reaction with 2.9-3.2d under the condition of 430-440K, and slowly cooling to the room temperature to obtain a colorless tabular crystal, i.e., the cadmium metal organic complex. The cadmium metal organic complex has the fluorescence and can be applied to fluorescent materials.
Description
Technical field
The present invention relates generally to Material Field, relates in particular to a kind of preparation method of cadmium metal organic coordination compound.
Background technology
Ligand polymer is the compound being formed by coordinate bond by the part of the metal ion as tie point and a bridge linking effect, and 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 separate, have potential application aspect antibacterial and nonlinear optical material and caused that people study interest widely.Nineteen ninety-five, O.M.Yaghi study group has proposed the concept of " metal-organic frameworks " first, and with within 1999, delivered one piece about the synthetic report of MOF-5.In recent ten years, investigators utilize different organic ligands and many kinds of metal ions effect, have prepared the MOFs of many novel structures, character excellence.Research shows, the formation of title complex and structure are subject to the impact of many factors, the structure of part and character are key factors that affects title complex, therefore How to choose is suitable organic ligand and metal ion, control the condition of reaction, directed assemble the key problem that target compound is current research.
The organism that the large more options of part of preparing a metal-organic complex contain the power supply atoms such as O, N, S, for example oxygen containing carboxylic-acid and nitrogenous pyridines, utilize the part of carboxylic-acid and pyridines to synthesize a large amount of a metal-organic complexes.Nicotinic acid is the part that synthetic compound is conventional, has reported many synthetic title complexs of nicotinic acid that utilize in document.As a kind of derivative of nicotinic acid, 6-amino-nicotinic acid contains an amino than nicotinic acid more, can take different coordination modes to form multiple topological framework in the preparation process of title complex, and in addition, amino can be used as the acceptor of hydrogen bond, forms the compound of higher-dimension.On the other hand, 6-amino-nicotinic acid is a chiral material, has increased the possibility of synthesis of chiral title complex.But, utilize so far the synthetic title complex of 6-amino-nicotinic acid 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 Cd (NO of the 6-amino-nicotinic acid of 0.2 mmol and 0.1 mmol
3)
24H
2o mixture is added in the distilled water of 6-10 ml, drip NaOH solution and regulate pH to 2-4, fully stir to be placed on tetrafluoroethylene and do in the stainless steel cauldron of lining, after 430-440 K Water Under thermal response 2.9-3.2d, slowly be cooled to room temperature and obtain colourless tabular 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, the structure iron that Fig. 5 is title complex.
Embodiment
A preparation method for cadmium metal organic coordination compound, comprises the following steps:
By the Cd (NO of the 6-amino-nicotinic acid of 0.2 mmol and 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 10ml, drip NaOH solution and regulate pH to 2 left and right, fully stir to be placed on tetrafluoroethylene and do in the stainless steel cauldron of lining, after 433K Water Under thermal response 3d, slowly be cooled to room temperature and obtain colourless tabular crystal, be described cadmium metal organic coordination compound.
By the Cd (NO of the 6-amino-nicotinic acid of 0.2 mmol and 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 10ml, drips NaOH solution and regulates pH to 3 left and right, fully stirs to be placed on tetrafluoroethylene and does in the stainless steel cauldron of lining, after 433K Water Under thermal response 3d, is slowly cooled to room temperature and obtains target product.
By the Cd (NO of the 6-amino-nicotinic acid of 0.2 mmol and 0.1mmol
3)
24H
2the mixture of O is added in the distilled water of 6ml, drips NaOH solution and regulates pH to 4 left and right, fully stirs to be placed on tetrafluoroethylene and does in the stainless steel cauldron of lining, after 433K Water Under thermal response 3d, is slowly cooled to room temperature and obtains target product.
The crystalline structure test of title complex:
Adopt Bruker Smart Apex CCD single crystal diffractometer to test crystal, result proves that crystal is title complex [Cd (6-Aminonicotinic acid)
2]
n.Crystal belongs to chirality spacer 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=1.821 g/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 Cd half
2+with a 6-amino-nicotinic acid part, Cd
2+what taked at center is the octoploids structure of hexa-coordinate.6-amino-nicotinic acid connects two Cd
2+, form unlimited 1D chiral structure.Adjacent 1D chirality chain is by sharing Cd
2+, form and there is square cancellated 2D plane layer.In 2D structure, there is different chiral structures along different directions.Adjacent 2D reticulated structure, by there is no 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 of two adjacent faces is contrary, and the 3D structure of formation is achiral.
Complex fluorescent test:
At room temperature, utilize the fluorescence of SHIMAZU VF-320 spectrophotofluorometer test 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 Cd (NO of the 6-amino-nicotinic acid of 0.2 mmol and 0.1 mmol
3)
24H
2o mixture is added in the distilled water of 6-10 ml, drip NaOH solution and regulate pH to 2-4, fully stir to be placed on tetrafluoroethylene and do in the stainless steel cauldron of lining, after 430-440 K Water Under thermal response 2.9-3.2d, slowly be cooled to room temperature and obtain colourless tabular crystal, be described cadmium metal organic coordination compound.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237472A (en) * | 2015-10-30 | 2016-01-13 | 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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| CN101429209A (en) * | 2008-12-11 | 2009-05-13 | 重庆大学 | Method for low-temperature atmosphere-pressure hydrothermal synthesis of stephanoporate metal-organic framework |
| CN101948478A (en) * | 2010-09-03 | 2011-01-19 | 天津师范大学 | Cadmium (II) coordination compound including 5-bromoniacin and preparation method thereof |
-
2013
- 2013-12-27 CN CN201310743310.8A patent/CN103772419B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101429209A (en) * | 2008-12-11 | 2009-05-13 | 重庆大学 | Method for low-temperature atmosphere-pressure hydrothermal synthesis of stephanoporate metal-organic framework |
| CN101948478A (en) * | 2010-09-03 | 2011-01-19 | 天津师范大学 | Cadmium (II) coordination compound including 5-bromoniacin and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| NIU S Y. ET AL.,: ""Crystal structure and fluorescence/phosphorescence of two novel Cd(II) coordination polymers"", 《STRUCT CHEM》, vol. 17, 31 December 2006 (2006-12-31), pages 209 - 216 * |
| PAULA C R. ET AL.,: ""Terbium(Ⅲ) complexes of 2-aminonicotinic, thiosalicylic and anthranilic acids: synthesis and photoluminescence properties"", 《JOURNAL OF ALLOYS COMPOUNDS》, vol. 451, 31 December 2008 (2008-12-31), pages 575 - 577, XP022435657, DOI: doi:10.1016/j.jallcom.2007.04.113 * |
| PEI YANG. ET AL.,: ""Structral diversity and solid-state properties of CoⅡ and ZnⅡ coordination complexes with 5-aminonicotinate through metal direction"", 《JOURNAL OF COORDINATION CHEMISTRY》, vol. 66, no. 18, 24 September 2013 (2013-09-24), pages 3305 - 3313 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237472A (en) * | 2015-10-30 | 2016-01-13 | 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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