CN104277056A - One-dimensional zinc-containing polymer and preparation method thereof - Google Patents
One-dimensional zinc-containing polymer and preparation method thereof Download PDFInfo
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- CN104277056A CN104277056A CN201410480043.4A CN201410480043A CN104277056A CN 104277056 A CN104277056 A CN 104277056A CN 201410480043 A CN201410480043 A CN 201410480043A CN 104277056 A CN104277056 A CN 104277056A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F3/00—Compounds containing elements of Groups 2 or 12 of the Periodic System
- C07F3/06—Zinc compounds
Abstract
The invention relates to the field of inorganic chemistry and particularly relates to a one-dimensional zinc-containing polymer and a preparation method thereof. The one-dimensional zinc-containing polymer has the chemical formula of C12H16N2O2Cl6Zn2, belongs to an orthorhombic crystal system, has the space group of Pna21 and has the crystal cell parameters that a is equal to 22.8251(4) angstroms, b is equal to 7.7664(1) angstroms, c is equal to 12.3108(1) angstroms, alpha is equal to beta, is equal to gamma and is equal to 90 degrees, and V is equal to 2170.56(4) angstroms<3>. The polymer disclosed by the invention is easy to prepare, and synthesized materials are low in defect and high in crystallinity; N atoms on a pyridine ring of 2-pyridyl methanol do not participate in coordination, so that the synthesized one-dimensional polymer has obvious adsorption to some metal ions; one-dimensional chain structures of polymers are bridged by using halogen elements and are stable in structure, so that the one-dimensional polymer has very good potential application prospects in the fields of catalysis, sensing, molecular recognition, molecular luminescence and the like.
Description
Technical field
The present invention relates to domain of inorganic chemistry, be specifically related to a kind of one dimension containing zinc complex and preparation method thereof.
Background technology
Transition metal polymerization thing has the macroscopic property of clearly orderly one dimension or multidimensional microtexture and uniqueness, chooses the structure of suitable transition metal ion, part and synthetic method controllable ligand polymer, and then regulates and controls its character.Ligand polymer, due to the diversity of structure and the functional performance in catalysis, chemisorption, magnetic and electronic conductor etc., has been subject to the extensive concern of researchist in recent years.In the study on the synthesis of ligand polymer, part is one of deciding factor affecting constitutional features.The factors such as the spacing between the donor groups character of part, the number of teeth of part, part point, the linking group between part and part isomery all may have an impact to the final structure of ligand polymer.But when design and synthetic metals organic backbone, control dimension and remain a significant challenge.
Summary of the invention
Technical problem to be solved by this invention is to provide one dimension containing zinc complex and preparation method thereof.
Another object of the present invention is to provide the above-mentioned preparation method containing zinc complex.
Technical problem to be solved by this invention is achieved by the following technical programs:
A kind of one dimension is containing zinc complex, and chemical formula is C
12h
16n
2o
2cl
6zn
2, this polymkeric substance is rhombic system,
pna21spacer, unit cell parameters is
a=22.8251 (4),
b=7.7664 (1),
c=12.3108 (1),
α=β=γ=90o, V=2170.56 (4)
3.
A kind of one dimension containing the preparation method of zinc complex is: by 2-piconol and ZnCl
2be added in the middle of the methyl alcohol containing hydrochloric acid, at room temperature stir and form mixed solution, at 20 ~ 25 DEG C, then leave standstill volatilization within more than 20 days, obtain described containing zinc complex.
Further, described 2-piconol and ZnCl
2mol ratio be 0.8 ~ 1.2:0.9 ~ 1.2.
Preferred further, described 2-piconol and ZnCl
2mol ratio be preferably 1:1.
Further, the concentration of hydrochloric acid is 0.5 ~ 2mol/L.
Further, described churning time is 3 ~ 6 hours.
The present invention has following beneficial effect:
Polymkeric substance of the present invention is easy to preparation, the fault in material be synthesized is few, degree of crystallinity is high, and the atom N on the pyridine ring of 2-piconol does not participate in coordination, the one-dimensional Polymers synthesized is made to have obvious absorption for some metal ion, and this polymkeric substance utilizes halogens bridging to become the polymkeric substance of one-dimensional catenary structure, Stability Analysis of Structures, this one-dimensional Polymers is made to have extraordinary potential application prospect in fields such as catalysis, sensing, molecular recognition, molecular luminescences.
Accompanying drawing explanation
Fig. 1 is that one dimension of the present invention is containing zinc complex C
12h
16n
2o
2cl
6zn
2with the coordination environment figure of metal center Zn.
Fig. 2 is that one dimension of the present invention is containing zinc complex C
12h
16n
2o
2cl
6zn
2one-dimentional structure schematic diagram.
Embodiment
Below in conjunction with drawings and Examples, the present invention will be described in detail.
embodiment 1
By 1mmol2-piconol and 1mmolZnCl
2be added in the middle of methanol solution that 30mL contains hydrochloric acid (concentration of hydrochloric acid is 1mol/L), at room temperature stir and form mixed solution in 6 hours, at 20 DEG C, then leave standstill volatilization within 40 days, obtain described containing zinc complex, productive rate is 61.8% (based on Zn).
Then by above-mentioned have described carry out structural characterization containing zinc complex
Crystal X-ray diffraction data acquisition Burkcer Smart CCD single crystal diffractometer measures.MoKa radiation (λ=0.71073), graphite monochromator, collects data with ω scan mode, and carries out Lp factor correction and empirical absorption correction.First with direct method determination atoms metal and part other non-hydrogen atoms position, then all the other whole non-hydrogen atom coordinates are obtained by difference functions method and method of least squares, and obtain hydrogen atom position with theoretical hydrogenation method or find from difference Fourier figure, by complete matrix method of least squares, structure is revised.Crystallographic parameter is in table 1, and structure is shown in Fig. 1, Fig. 2.
table 1. contains crystallographic parameter and the structure elucidation of zinc complex
This polymkeric substance belongs to rhombic system,
pna21spacer, it to contain in a crystallography independently Zn atom (as shown in Figure 1), divalence Zn atom adopts the octahedral coordination pattern of distortion, respectively with the O atom (Zn-O bond distance is 2.528(4) on a 2-piconol), five Cl Atomic coordinate (Zn-Cl bond distance is 2.503(2) ~ 2.635(3)) (see figure 1).Wherein, 2-piconol is monodentate ligand, each 2-piconol and a Zn Atomic coordinate, the coordination mode of Cl atom is divided into two classes, and a class and Zn atom adopt double coordination pattern, and a class and Zn atom adopt monodentate ligand pattern, finally, they form one-dimensional catenary structure (see figure 2).
embodiment 2
By 1mmol2-piconol and 1.1mmolZnCl
2be added in the middle of methanol solution that 30mL contains hydrochloric acid (concentration of hydrochloric acid is 1.8mol/L), at room temperature stir and form mixed solution in 4 hours, at 20 DEG C, then leave standstill volatilization within 38 days, obtain described containing zinc complex, productive rate is 51.8% (based on Zn).
embodiment 3
By 0.9mmol2-piconol and 1.2mmolZnCl
2be added in the middle of methanol solution that 30mL contains hydrochloric acid (concentration of hydrochloric acid is 0.5mol/L), at room temperature stir and form mixed solution in 5 hours, at 23 DEG C, then leave standstill volatilization within 30 days, obtain described containing zinc complex, productive rate is 47.5% (based on Zn).
embodiment 4
By 0.9mmol2-piconol and 1mmolZnCl
2be added in the middle of methanol solution that 30mL contains hydrochloric acid (concentration of hydrochloric acid is 1.1mol/L), at room temperature stir and form mixed solution in 3 hours, at 24 DEG C, then leave standstill volatilization within 50 days, obtain described containing zinc complex, productive rate is 56.3% (based on Zn).
The above embodiment only have expressed embodiments of the present invention; it describes comparatively concrete and detailed; but therefore can not be interpreted as the restriction to the scope of the claims of the present invention; in every case the technical scheme adopting the form of equivalent replacement or equivalent transformation to obtain, all should drop within protection scope of the present invention.
Claims (7)
1. one dimension is containing a zinc complex, it is characterized in that: chemical formula is C
12h
16n
2o
2cl
6zn
2.
2. one dimension according to claim 1 is containing zinc complex, it is characterized in that: this polymkeric substance is rhombic system,
pna21spacer, unit cell parameters is
a=22.8251 (4),
b=7.7664 (1),
c=12.3108 (1),
α=β=γ=90o, V=2170.56 (4)
3.
3. a kind of one dimension according to claim 1 is containing the preparation method of zinc complex, it is characterized in that: by 2-piconol and ZnCl
2be added in the middle of the methyl alcohol containing hydrochloric acid, at room temperature stir and form mixed solution, at 20 ~ 25 DEG C, then leave standstill volatilization within more than 20 days, obtain described containing zinc complex.
4. one dimension according to claim 3 is containing the preparation method of zinc complex, it is characterized in that: described 2-piconol and ZnCl
2mol ratio be 0.8 ~ 1.2:0.9 ~ 1.2.
5. one dimension according to claim 4 is containing the preparation method of zinc complex, it is characterized in that: described 2-piconol and ZnCl
2mol ratio be preferably 1:1.
6. one dimension according to claim 4 is containing the preparation method of zinc complex, it is characterized in that: the concentration of hydrochloric acid is 0.5 ~ 2mol/L.
7. one dimension according to claim 3 is containing the preparation method of zinc complex, it is characterized in that: described churning time is 3 ~ 6 hours.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896970A (en) * | 2014-04-11 | 2014-07-02 | 聊城大学 | 2-Pyridinemethanol copper complex as well as preparation method and application |
-
2014
- 2014-09-19 CN CN201410480043.4A patent/CN104277056A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103896970A (en) * | 2014-04-11 | 2014-07-02 | 聊城大学 | 2-Pyridinemethanol copper complex as well as preparation method and application |
Non-Patent Citations (3)
| Title |
|---|
| MARKUS TESMER ET AL.: "Oligonuclear zinc complexes of 2-pyridylmethanol", 《CHEM. COMMUN.》 * |
| NOVAKOVSKII, M. S. ET AL.: "Compounds of zinc nitrate with pyridine derivatives", 《ZHURNAL NEORGANICHESKOI KHIMII》 * |
| SHANE G. TELFER ET AL.: "Helicates, Boxes, and Polymers from Simple Pyridine-Alcohol Ligands: the Impact of the Identity of the Transition Metal Ion", 《INORGANIC CHEMISTRY》 * |
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Application publication date: 20150114 |
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