CN107315023B - Specific identification of iodide ions by a porous MOF - Google Patents

Specific identification of iodide ions by a porous MOF Download PDF

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CN107315023B
CN107315023B CN201610891905.1A CN201610891905A CN107315023B CN 107315023 B CN107315023 B CN 107315023B CN 201610891905 A CN201610891905 A CN 201610891905A CN 107315023 B CN107315023 B CN 107315023B
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iodide ions
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李慧军
徐周庆
王元
徐杲远
徐君
吴伟娜
贾磊
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Henan University of Technology
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Abstract

The invention belongs to the technical field of chemistry and discloses an exclusive identification of iodide ions by porous MOF, which comprises the following steps: (1) will be matched withCompound 27 was soaked in KI solution and after 7 hours, the crystal changed from sky blue to black green and ClO was found by infrared characterization4 ‑The characteristic peak of (a) disappears, and the XPS result shows that the I element exists in the complex 28; (2) the structure of the crystal was determined by X-ray single crystal testing. The method is simple to operate and easy to realize, and other anions do not interfere the identification process, so that the method can be conveniently and quickly used for detecting the iodide ions.

Description

Specific identification of iodide ions by a porous MOF
Technical Field
The invention specifically relates to special identification of iodide ions by porous MOF, and belongs to the technical field of chemistry.
Background
In recent years, in the field of ion detection, colorimetric methods and fluorescent methods have been studied for reasons of simplicity of operation, availability of instruments, and the like. In addition, the ion-responsive organogel is a new research focus in the field of ion recognition because of its easy preparation and simple usage method. In view of this, a highly selective, easily prepared and applied I has been found-Are of great interest and commercial interest.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the existing defects, provide the special identification of the porous MOF to the iodide ions, have simple operation and easy realization, have no interference of other anions to the identification process, can be conveniently and quickly used for detecting the iodide ions, and can effectively solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides a special identification of iodide ions by porous MOF, which comprises the following steps: (1) soaking the complex 27 into KI solution, changing the crystal from sky blue to black green after 7 hours, and finding ClO by infrared characterization4 -The characteristic peak of (A) disappears, and XPS results show the presence of element I in the complex 28(ii) a (2) The structure of the crystal was determined by X-ray single crystal testing.
Preferably, the crystal in step (2) has the formula { [ Cu ]6(TTTMB)8(I)11(OH)]·39H2O}n。
Preferably, the crystals have an elemental analysis of formula C144H247Cu6I11N72O40And (3) calculating: 32.01 percent of C, 18.66 percent of N and 4.61 percent of H. Experimental values: 33.05% of C, 18.95% of N and 4.08% of H.
Preferably, the complex 27 in step (1) is tetragonal, space group is I4, Cu1 is in penta-coordination environment, coordinates with four N atoms and one O atom respectively to form a tetragonal pyramid configuration, and Cu2 is in octahedral configuration, and consists of four N atoms and two from ClO4 -Coordinate with the O atom of water molecule to complete configuration, and have a free ClO in the cavity4 -Tttmb links three Cu ions in a cis, cis, trans-configuration to extend the framework into a three-dimensional framework.
Preferably, the complexes 28 and 27 in the step (1) and the step (2) belong to heteroisomorphs, the coordination environment of Cu1 of the complex 28 is six-coordinate and is respectively coordinated with four N1 ions and two I ions, and the bond length of Cu-N is
Figure BSA0000135218950000021
Bond length of Cu-I of
Figure BSA0000135218950000022
The coordination environment of Cu2 of the complex 28 is penta-coordination, and the bond lengths of Cu-N are respectively
Figure BSA0000135218950000023
And
Figure BSA0000135218950000024
a Cu-O bond length of
Figure BSA0000135218950000025
Free ClO in the cavity4 -There are two I ions.
The invention has the following beneficial effects: the special identification of the porous MOF to the iodide ions is simple to operate and easy to realize, and other anions do not interfere the identification process, so that the detection of the iodide ions can be conveniently and quickly carried out.
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The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention.
In the drawings:
FIG. 1 is a diagram of asymmetric units of a specific recognition complex 27 of a porous MOF for iodide ions according to an embodiment of the present invention;
FIG. 2 is a three-dimensional framework diagram of a specific recognition complex 27 of iodide ions by a porous MOF according to an embodiment of the present invention;
FIG. 3 is a graph of the infrared spectrum of a specific recognition complex 27 of iodide ions by a porous MOF according to an embodiment of the present invention;
FIG. 4 is a diagram of an asymmetric unit of a specific recognition complex 28 of iodide ions by a porous MOF according to an embodiment of the present invention;
FIG. 5 is a graph of XPS results for a specific recognition complex 28 of iodide ions by a porous MOF according to an embodiment of the present invention;
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example (b): referring to FIGS. 1-5, a porous MOF of the present invention provides for the exclusive identification of iodide ions by the following steps: (1) soaking the complex 27 into KI solution, changing the crystal from sky blue to black green after 7 hours, and finding ClO by infrared characterization4 -The characteristic peak of (a) disappears, and the XPS result shows that the I element exists in the complex 28; (2) the structure of the crystal was determined by X-ray single crystal test, and the molecular formula of the crystal in step (2) was { [ Cu { [6(TTTMB)8(I)11(OH)]·39H2O}nThe molecular formula element analysis of the crystal is according to C144H247Cu6I11N72O40And (3) calculating: 32.01 percent of C, 18.66 percent of N and 4.61 percent of H. Experimental values: c33.05%, N18.95% and H4.08%, wherein the complex 27 in the step (1) belongs to a tetragonal system, the space group is I4, Cu1 is in a penta-coordination environment and is respectively coordinated with four N atoms and one O atom to form a tetragonal pyramid configuration, and Cu2 is in an octahedral configuration and is composed of four N atoms and two from ClO4 -Coordinate with the O atom of water molecule to complete configuration, and have a free ClO in the cavity4 -Tttmb connects three Cu ions in cis, cis, trans-configuration to extend the framework into a three-dimensional framework, and step (1) and step (2) complexes 28 and 27 belong to heteroisomorphs, the coordination environment of Cu1 of the complex 28 is hexa-coordinate and coordinates with four N1 ions and two I ions respectively, and the bond length of Cu-N is
Figure BSA0000135218950000041
Bond length of Cu-I of
Figure BSA0000135218950000042
The coordination environment of Cu2 of the complex 28 is penta-coordination, and the bond lengths of Cu-N are respectively
Figure BSA0000135218950000043
And
Figure BSA0000135218950000044
a Cu-O bond length of
Figure BSA0000135218950000045
Free ClO in the cavity4 -There are two I ions.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (2)

1. A method for specifically identifying iodide ions by porous MOF is characterized by comprising the following steps: the identification steps are as follows:
(1) soaking the complex 27 into a KI solution, changing the crystal complex 27 from sky blue to a black green crystal complex 28 after 7 hours, and finding ClO in the crystal complex 27 through infrared characterization4 -The characteristic peak of (a) disappears, and the XPS result shows that the I element exists in the complex 28;
(2) measuring the structure of the crystal through an X-ray single crystal test;
the molecular formula of the crystalline complex 28 in step (2) is { [ Cu ]6(TTTMB)8(I)11(OH)]·39H2O}n；
The complex 27 in the step (1) belongs to a tetragonal system, the space group is I4, the Cu1 is in a five-coordination environment and is respectively coordinated with four N atoms and one O atom to form a tetragonal pyramid configuration, and the Cu2 is in an octahedral configuration and is composed of four N atoms and two ClO atoms4 -Coordinate with the O atom of water molecule to complete configuration, and have a free ClO in the cavity4 -Tttmb connects three Cu ions in cis, cis, trans-configuration to extend the framework into a three-dimensional framework;
in the step (1), the complexes 28 and 27 belong to heteroisomorphs, the coordination environment of Cu1 of the complex 28 is hexa-coordination which is respectively coordinated with four N1 ions and two I ions, and the bond length of Cu-N is
Figure FSB0000191592610000011
Bond length of Cu-I of
Figure FSB0000191592610000012
The coordination environment of Cu2 of the complex 28 isPenta-coordinate, Cu-N bond lengths are respectively
Figure FSB0000191592610000013
And
Figure FSB0000191592610000014
a Cu-O bond length of
Figure FSB0000191592610000015
Free ClO in the cavity4 -There are two I ions.
2. The method for the exclusive identification of iodide ions by porous MOF according to claim 1, wherein: molecular elemental analysis of said crystalline complex 28 according to C144H247Cu6I11N72O40And (3) calculating: 32.01 percent of C, 18.66 percent of N and 4.61 percent of H; experimental values: 33.05% of C, 18.95% of N and 4.08% of H.
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