CN105175437A - Triazole quinoxaline cadmium complex and preparation method thereof - Google Patents
Triazole quinoxaline cadmium complex and preparation method thereof Download PDFInfo
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- CN105175437A CN105175437A CN201510669436.4A CN201510669436A CN105175437A CN 105175437 A CN105175437 A CN 105175437A CN 201510669436 A CN201510669436 A CN 201510669436A CN 105175437 A CN105175437 A CN 105175437A
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- quinoxaline
- triazole
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Abstract
The invention discloses a triazole quinoxaline cadmium complex, which is a complex of 2,3-di[(2-triazolyl)methyl] quinoxaline, terephthalic acid and cadmium metal, a chemical formula is [(BTQ)(TPA)Cd.2H2O], and the complex has dual functions of adsorption and light emission. The preparation method of the complex comprises the step of standing prepared mixed ligand solution and metal salt solution at room temperature. The preparation method has the advantages of simple process, mild condition, high yield, good repeatability, less used solvent and small environmental pollution.
Description
Technical field
This explanation relates to the title complex of transition metal cadmium, is specifically related to the absorption of a kind of tool, luminous bifunctional triazole quinoxaline cadmium complex and preparation method thereof.
Background technology
Sorbing material has that surface-area is large, porosity is high, pore size distribution is narrow, pore size continuously adjustabe, skeleton structure are stable and internal surface is easy to the features such as modification, can be used as high-efficiency adsorbent.Metal complexes is being subject to the people's attention as the potential application in a kind of novel sorbing material etc., and recently, investigator has prepared a lot of novel functionalization sorbing material, and its widespread use in adsorbing domain illustrates tempting prospect.See: Jozef
valigura, Roman
andJ á n
daltonTrans., 2015,44,12484; Xuan, Z.-H.; Zhang, D.-S.; Chang, Z.; Hu, T.-L.; Bu, X.-H., Inorg.Chem., 2014,53,8985; NicoleKindermann, EckhardBill, SebastianDechert, SerhiyDemeshko, EdwardJ.ReijerseandProf.FrancMeyer, AngewandteChemieInternationalEdition, 2014,54,1738.According to Chinese science report, within 2015, metal complexes is got ready for moving towards commercial applications as sorbing material, and BASF AG represents and prepares to release methane storing system in this year, and it can fill more multi fuel than conventional pressure vessel.Metal complexes is no longer a dream as sorbing material as can be seen here.
Photoluminescence refers to that object relies on external light source and irradiates, thus obtains energy, produces to excite to be directed at luminous phenomenon.Metal complexes is as a kind of novel luminous organic material, be subject to the people's attention due to its potential application in optical pickocff and organic luminescent device etc., cadmium complex wherein in transition metal high-performance of novelty in optics receive people very big concern and by a large amount of synthesis and research, simultaneously one of forward position study hotspot also becoming title complex luminescent chemical.See: JunsangCho, YunKuJungandJin-KyuLee, J.Mater.Chem., 2012,22,10827-10833; BinXing, WanwanLi, XiebingWang, HongjingDou, LuWang, KangSun, XiaotianHe, JunsongHan, HuashengXiao, JinmingMiaoandYueLi, J.Mater.Chem., 2010,20,5664-5674; SungwooKim, SangHyukImandSang-WookKim, Nanoscale, 2013,5,5205-5214.
At present, there is the technological deficiencies such as function singleness, synthesis condition is harsh, building-up process environmental pollution is larger in the metal complexes reported in document.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind ofly has multi-functional, that mild condition, environmental pollution are little triazole quinoxaline cadmium complex, and the present invention also provides the preparation method of this title complex.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of triazole quinoxaline cadmium complex, be 2, the title complex of 3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal, chemical formula is [(BTQ) (TPA) Cd2H
2o], wherein, BTQ is 2,3-bis-[(2-triazolyl) methyl] quinoxaline, and TPA is terephthalic acid; The crystal of this cadmium metal complex belongs to triclinic(crystalline)system, spacer is P-1, unit cell parameters is: a=6.917 (4), b=10.338 (5), c=16.156 (8), α=96.889 (7), β=86.54 (3), γ=96.161 (7)
The preparation method of triazole quinoxaline cadmium complex of the present invention, step is as follows:
(1). by amide solvent and chlorinated paraffin solvent mixing under normal temperature, after stirring, be mixed with mixed solvent;
(2). under normal temperature, 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid are dissolved in the mixed solution of acid amides and chloroparaffin, after stirring, obtain mixed ligand solution;
(3). under normal temperature, by Cd (NO
3)
2be dissolved in alcohol solution, after stirring, obtain Cd (NO
3)
2metal salt solution;
(4). under normal temperature, the mixed ligand solution of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid is added bottom test tube, then adds Cd (NO on test tube top
3)
2metal salt solution;
(5). leaving standstill being placed under reaction solution room temperature condition on stable table face, within 25 days, colourless bulk-shaped monocrystal can be obtained, being the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal.
Described amide solvent is DMF, N,N-dimethylacetamide or N, N-dimethylpropionamide.
Described chlorinated paraffin solvent is methylene dichloride, trichloromethane or tetracol phenixin.
Described alcoholic solvent is methyl alcohol, ethanol or propyl carbinol.
The amount ratio of described part 2,3-bis-[(2-triazolyl) methyl] quinoxaline and mixed solvent is 0.015-0.045mol/L.
The amount ratio of described part terephthalic acid and mixed solvent is 0.015-0.045mol/L.
Described metal-salt Cd (NO
3)
2be 0.03-0.09mol/L with the amount ratio of alcohol solution.
Part 2,3-bis-[(2-triazolyl) methyl] quinoxaline in described reaction solution: terephthalic acid: Cd (NO
3)
2mol ratio be 1:1:2.
The present invention adopts triazole quinoxaline cadmium complex designed by technique scheme and preparation method thereof, this title complex has absorption and luminous two kinds of functions, can be used as while sorbing material uses and also can use as luminescent material, and this complex preparation method technique is simple, mild condition, productive rate is high, and reproducibility is good, and the few environmental pollution of solvent for use amount is little.
Accompanying drawing explanation
Fig. 1 represents the Cd coordination environment figure of cadmium complex of the present invention;
Fig. 2 represents the structural representation of cadmium complex of the present invention.
Embodiment
A kind of triazole quinoxaline of the present invention cadmium complex, be 2, the title complex of 3-bis-[(2-triazolyl) methyl] quinoxaline (BTQ) and terephthalic acid (TPA) and cadmium metal, chemical formula is [(BTQ) (TPA) Cd2H
2o], the crystal of this cadmium metal complex belongs to triclinic(crystalline)system, spacer is P-1, unit cell parameters is: a=6.917 (4), b=10.338 (5), c=16.156 (8), α=96.889 (7), β=86.54 (3), γ=96.161 (7)
Embodiment 1:
The preparation method of a kind of triazole quinoxaline of the present invention cadmium complex, step is as follows:
(1). under normal temperature, DMF and trichloromethane are mixed according to the ratio of volume 1:4, after stirring, be mixed with mixed solvent;
(2). under normal temperature, 2,3-bis-[(2-triazolyl) methyl] quinoxaline 0.2mmoL (0.0584g) and terephthalic acid 0.2mmoL (0.0332g) is dissolved in 8mL mixed solvent, obtains mixed ligand solution after stirring;
(3). under normal temperature, by Cd (NO
3)
24H
2o0.4mmoL (0.1234g) is dissolved in 8mL methyl alcohol, obtains Cd (NO after stirring
3)
2metal salt solution;
. under normal temperature, by 8mL2,3-bis-the mixed ligand solution of [(2-triazolyl) methyl] quinoxaline and terephthalic acid add bottom test tube, then add 8mLCd (NO on test tube top
3)
2metal salt solution;
(5). reaction solution room temperature condition is placed on stable table top and leaves standstill, within about 25 days, colourless bulk-shaped monocrystal can be obtained.Be the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal.
Embodiment 2:
A preparation method for described triazole quinoxaline cadmium metal complex, step is as follows:
(1). under normal temperature, N,N-dimethylacetamide and methylene dichloride are mixed according to the ratio of volume 1:4, after stirring, be mixed with mixed solvent;
(2). under normal temperature, 2,3-bis-[(2-triazolyl) methyl] quinoxaline 0.2mmoL (0.0584g) and terephthalic acid 0.2mmoL (0.0332g) is dissolved in 8mL mixed solvent, obtains mixed ligand solution after stirring;
(3). under normal temperature, by Cd (NO
3)
24H
2o0.4mmoL (0.1234g) is dissolved in 8mL ethanol, obtains Cd (NO after stirring
3)
2metal salt solution;
. under normal temperature, by 8mL2,3-bis-the mixed ligand solution of [(2-triazolyl) methyl] quinoxaline and terephthalic acid add bottom test tube, then add 8mLCd (NO on test tube top
3)
2metal salt solution;
(5). reaction solution room temperature condition is placed on stable table top and leaves standstill, within about 25 days, colourless bulk-shaped monocrystal can be obtained.Be the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal.
Embodiment 3:
A preparation method for described triazole quinoxaline cadmium metal complex, step is as follows:
(1). under normal temperature, N, N-dimethylpropionamide and tetracol phenixin are mixed according to the ratio of volume 1:4, after stirring, be mixed with mixed solvent;
(2). under normal temperature, 2,3-bis-[(2-triazolyl) methyl] quinoxaline 0.2mmoL (0.0584g) and terephthalic acid 0.2mmoL (0.0332g) is dissolved in 8mL mixed solvent, obtains mixed ligand solution after stirring;
(3). under normal temperature, by Cd (NO
3)
24H
2o0.4mmoL (0.1234g) is dissolved in 8mL propyl carbinol, obtains Cd (NO after stirring
3)
2metal salt solution;
. under normal temperature, by 8mL2,3-bis-the mixed ligand solution of [(2-triazolyl) methyl] quinoxaline and terephthalic acid add bottom test tube, then add 8mLCd (NO on test tube top
3)
2metal salt solution;
(5). reaction solution room temperature condition is placed on stable table top and leaves standstill, within about 25 days, colourless bulk-shaped monocrystal can be obtained.Be the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal.
The relevant characterization of title complex and crystal structure determination:
To choose in above-described embodiment obtained monocrystalline under the microscope and at room temperature carry out X – ray diffraction experiments.On RigakuRAXIS-RAPID single crystal diffractometer, with the Mo – K through graphite monochromator monochromatization
aray
yi φ – ω mode collects diffraction data.Reduction of data is carried out by BrukerSAINT program.The diffraction data SADABS program of part-structure carries out absorption correction.Crystalline structure is solved in conjunction with difference Fourier synthesis by direct method.Whole non-hydrogen atom coordinate and anisotropic parameters carry out complete matrix least-squares refinement, and hydrogen atom position is determined by theoretical mode computation.Detailed axonometry data in table 1,
Fig. 1 is the Mn coordination environment figure of manganese complex and the structural representation of title complex.
Table 1: the predominant crystal data of terpyridyl part manganese complex
aR＝Σ(||F
0|-|F
C||)/Σ|F
0|；
bwR＝[Σw(|F
0|
2-|F
C|
2)
2/Σw(F
0 2)]
1/2。
Claims (9)
1. a triazole quinoxaline cadmium complex, it is characterized in that being the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal, chemical formula is [(BTQ) (TPA) Cd2H
2o], wherein, BTQ is 2,3-bis-[(2-triazolyl) methyl] quinoxaline, and TPA is terephthalic acid; The crystal of this cadmium metal complex belongs to triclinic(crystalline)system, spacer is P-1, unit cell parameters is: a=6.917 (4), b=10.338 (5), c=16.156 (8), α=96.889 (7), β=86.54 (3), γ=96.161 (7)
2. a preparation method for triazole quinoxaline cadmium complex, is characterized in that step is as follows:
(1). by amide solvent and chlorinated paraffin solvent mixing under normal temperature, after stirring, be mixed with mixed solvent;
(2). under normal temperature, 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid are dissolved in the mixed solution of acid amides and chloroparaffin, after stirring, obtain mixed ligand solution;
(3). under normal temperature, by Cd (NO
3)
2be dissolved in alcohol solution, after stirring, obtain Cd (NO
3)
2metal salt solution;
(4). under normal temperature, the mixed ligand solution of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid is added bottom test tube, then adds Cd (NO on test tube top
3)
2metal salt solution;
(5). leaving standstill being placed under reaction solution room temperature condition on stable table face, within 25 days, colourless bulk-shaped monocrystal can be obtained, being the title complex of 2,3-bis-[(2-triazolyl) methyl] quinoxaline and terephthalic acid and cadmium metal.
3. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that described amide solvent is DMF, N,N-dimethylacetamide or N, N-dimethylpropionamide.
4. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that described chlorinated paraffin solvent is methylene dichloride, trichloromethane or tetracol phenixin.
5. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that described alcoholic solvent is methyl alcohol, ethanol or propyl carbinol.
6. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that the amount ratio of described part 2,3-bis-[(2-triazolyl) methyl] quinoxaline and mixed solvent is 0.015-0.045mol/L.
7. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that the amount ratio of described part terephthalic acid and mixed solvent is 0.015-0.045mol/L.
8. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2 or 5, is characterized in that described metal-salt Cd (NO
3)
2be 0.03-0.09mol/L with the amount ratio of alcohol solution.
9. the preparation method of a kind of triazole quinoxaline cadmium complex according to claim 2, is characterized in that part 2,3-bis-[(2-triazolyl) methyl] quinoxaline in described reaction solution: terephthalic acid: Cd (NO
3)
2mol ratio be 1:1:2.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503914A (en) * | 2016-01-05 | 2016-04-20 | 天津师范大学 | Triazole isophthalic acid cadmium complex single crystal and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588799A (en) * | 2013-12-05 | 2014-02-19 | 南开大学 | Cadmium coordination polymer and preparation method and application thereof |
| CN103724365A (en) * | 2013-12-18 | 2014-04-16 | 渤海大学 | Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex |
| CN103936773A (en) * | 2014-04-08 | 2014-07-23 | 陕西师范大学 | 1, 4-terephthalic acid-regulated polyazole coordination polymer and preparation method thereof |
| CN104610321A (en) * | 2015-02-26 | 2015-05-13 | 天津师范大学 | Tetraphenyl ethylene four triazole terephthalic acid cadmium complex with potential fluorescent material and preparation method thereof |
| CN104610320A (en) * | 2015-02-26 | 2015-05-13 | 天津师范大学 | Fluorescent material containing tetraphenylethylene-4-triazole three-dimensional cadmium complex and preparation method thereof |
| CN104628752A (en) * | 2015-02-26 | 2015-05-20 | 天津师范大学 | Tetraphenyl ethylene tetratriazole cadmium complex with potential fluorescent material and preparation method thereof |
-
2015
- 2015-10-13 CN CN201510669436.4A patent/CN105175437A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588799A (en) * | 2013-12-05 | 2014-02-19 | 南开大学 | Cadmium coordination polymer and preparation method and application thereof |
| CN103724365A (en) * | 2013-12-18 | 2014-04-16 | 渤海大学 | Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex |
| CN103936773A (en) * | 2014-04-08 | 2014-07-23 | 陕西师范大学 | 1, 4-terephthalic acid-regulated polyazole coordination polymer and preparation method thereof |
| CN104610321A (en) * | 2015-02-26 | 2015-05-13 | 天津师范大学 | Tetraphenyl ethylene four triazole terephthalic acid cadmium complex with potential fluorescent material and preparation method thereof |
| CN104610320A (en) * | 2015-02-26 | 2015-05-13 | 天津师范大学 | Fluorescent material containing tetraphenylethylene-4-triazole three-dimensional cadmium complex and preparation method thereof |
| CN104628752A (en) * | 2015-02-26 | 2015-05-20 | 天津师范大学 | Tetraphenyl ethylene tetratriazole cadmium complex with potential fluorescent material and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| GUO CHANG ET AL.: "Synthesis, Crystal Structure and Luminescent Property of Coordination Polymer [Cd2(BDC)2(obix)2]·H2O", 《CHINESE JOURNAL OF INORGANIC CHEMISTRY》 * |
| JIAN-LONG DU ET AL.: ""Metal Coordination Architectures of 2,3-Bis(triazol-1-ylmethyl)quinoxaline: Effect of Metal Ion and Counterion on Complex Structures"", 《EUR. J. INORG. CHEM.》 * |
| 陈丽华等: "镉( Ⅱ) 与对苯二甲酸和2 ,2′2 联吡啶配合物光谱性质的理论研究", 《分子科学学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105503914A (en) * | 2016-01-05 | 2016-04-20 | 天津师范大学 | Triazole isophthalic acid cadmium complex single crystal and preparation method and application thereof |
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Application publication date: 20151223 |