CN107315023A - Exclusive identifications of one porous MOF to iodide ion - Google Patents

Exclusive identifications of one porous MOF to iodide ion Download PDF

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Publication number
CN107315023A
CN107315023A CN201610891905.1A CN201610891905A CN107315023A CN 107315023 A CN107315023 A CN 107315023A CN 201610891905 A CN201610891905 A CN 201610891905A CN 107315023 A CN107315023 A CN 107315023A
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complex
exclusive
iodide ion
identifications
crystal
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CN107315023B (en
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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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Henan University of Technology
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/227—Measuring photoelectric effect, e.g. photoelectron emission microscopy [PEEM]
    • G01N23/2273—Measuring photoelectron spectrum, e.g. electron spectroscopy for chemical analysis [ESCA] or X-ray photoelectron spectroscopy [XPS]
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Health & Medical Sciences (AREA)
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Abstract

The invention belongs to technical field of chemistry and exclusive identifications of the porous MOF to iodide ion is disclosed, identification step is：(1) complex 27 is steeped in KI solution, after 7 hours, crystal becomes blackish green from sky blue, and ClO is found by IR Characterization4 ‑Characteristic peak disappear, XPS results are shown in the presence for having I elements in complex 28；(2) structure of crystal is measured by X ray single crystals.The present invention is simple to operate, be easily achieved, and other anion are not interfered with to the identification process, can be conveniently and quickly used for the detection of iodide ion.

Description

Exclusive identifications of one porous MOF to iodide ion
Technical field
Exclusive identification present invention relates particularly to a porous MOF to iodide ion, belongs to technical field of chemistry.
Background technology
In recent years, in ion detection field, colorimetric method or fluorescence method are because easy to operate, instrument such as is easy to get at the reason and turns into The focus of research.In addition, Ion response type organogel is easily prepared due to its, application method is easy, and becomes ion knowledge The new study hotspot in other field.In view of this, a kind of high selectivity, easily prepared and application I are found-Identification receptor be Highly significant with commercial promise.
The content of the invention
The technical problem to be solved in the present invention overcomes exclusive knowledge of the existing defect there is provided a porous MOF to iodide ion , it is not simple to operate, be easily achieved, and other anion are not interfered with to the identification process, can be conveniently and quickly used for iodine from The detection of son, the problem of effectively can solving in background technology.
In order to solve the above-mentioned technical problem, the invention provides following technical scheme：
The present invention provides exclusive identifications of the porous MOF to iodide ion, and identification step is：(1) by complex 27 steep into In KI solution, after 7 hours, crystal becomes blackish green from sky blue, and ClO is found by IR Characterization4 -Characteristic peak disappear, XPS results are shown in the presence for having I elements in complex 28；(2) structure of crystal is measured by X-ray monocrystalline.
It is preferred that, the molecular formula of the crystal in step (2) is { [Cu6(TTTMB)8(I)11(OH)]·39H2O}n。
It is preferred that, the molecular formula elementary analysis of the crystal is according to C144H247Cu6I11N72O40Calculate：C 32.01%, N 18.66%, H 4.61%.Experiment value：C 33.05%, N 18.95%, H 4.08%.
It is preferred that, the category tetragonal crystal system of the complex 27 in step (1), space group is I4, and Cu1 is in pentacoordinate environment In, tetragonal pyramid configuration is constituted with four N atoms and an O atom coordination respectively, Cu2 is in octahedral configuration, by four Individual N atoms, and two come from ClO4 -O atom coordination with hydrone completes configuration, also has a trip in the cavity of complex From ClO4 -, tttmb takes cis, cis, and trans- configurations are connected to three Cu ions skeleton has been extended into three-dimensional box Frame.
It is preferred that, step (1) and the category heterogeneous isomorphism body of step (2) complex 28 and 27, the Cu1's of the complex 28 matches somebody with somebody Position environment is hexa-coordinate, and respectively with four N1 and two I ion coordinations, Cu-N bond distance isCu-I bond distance ForThe Cu2 of the complex 28 coordination environment is pentacoordinate, and Cu-N bond distance is respectivelyWithCu-O bond distance isThe ClO dissociated in cavity4 -On have two I ions.
The beneficial effect that is reached of the present invention is：Exclusive identifications of one porous MOF to iodide ion, it is simple to operate, be easy to Realize, and other anion are not interfered with to the identification process, can be conveniently and quickly used for the detection of iodide ion.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, the reality with the present invention Applying example is used to explain the present invention together, is not construed as limiting the invention.
In the accompanying drawings：
Fig. 1 is a porous MOF described in the embodiment of the present invention to the asymmetric of the exclusive identification complex 27 of iodide ion Unit figure；
Fig. 2 is the three-dimensional box of a porous MOF described in the embodiment of the present invention to the exclusive identification complex 27 of iodide ion Frame figure；
Fig. 3 is the infrared light of a porous MOF described in the embodiment of the present invention to the exclusive identification complex 27 of iodide ion Spectrogram；
Fig. 4 is a porous MOF described in the embodiment of the present invention to the asymmetric of the exclusive identification complex 28 of iodide ion Unit figure；
Fig. 5 is the XPS results of a porous MOF described in the embodiment of the present invention to the exclusive identification complex 28 of iodide ion Figure；
Embodiment
The preferred embodiments of the present invention are illustrated below in conjunction with accompanying drawing, it will be appreciated that preferred reality described herein Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment：Fig. 1-5, exclusive identifications of the one porous MOF of the present invention to iodide ion are referred to, identification step is：(1) Complex 27 is steeped in KI solution, after 7 hours, crystal becomes blackish green from sky blue, is found by IR Characterization ClO4 -Characteristic peak disappear, XPS results are shown in the presence for having I elements in complex 28；(2) tested and surveyed by X-ray monocrystalline The molecular formula for obtaining the crystal in the structure of crystal, step (2) is { [Cu6(TTTMB)8(I)11(OH)]·39H2O}n, it is described The molecular formula elementary analysis of crystal is according to C144H247Cu6I11N72O40Calculate：C 32.01%, N 18.66%, H 4.61%.It is real Test value：The complex 27 in C 33.05%, N 18.95%, H 4.08%, step (1) belongs to tetragonal crystal system, and space group is I4, Cu1 are in pentacoordinate environment, constitute tetragonal pyramid configuration with four N atoms and an O atom coordination respectively, Cu2 is in In octahedral configuration, by four N atoms, and two come from ClO4 -O atom coordination with hydrone completes configuration, in complex Cavity in also have a free ClO4 -, tttmb takes cis, cis, and trans- configurations are connected to three Cu ions so as to will Skeleton has extended into three-dimensional framework, step (1) and the category heterogeneous isomorphism body of step (2) complex 28 and 27, the complex 28 Cu1 coordination environment is hexa-coordinate, and respectively with four N1 and two I ion coordinations, Cu-N bond distance isCu-I Bond distance beThe Cu2 of the complex 28 coordination environment is pentacoordinate, and Cu-N bond distance is respectivelyWithCu-O bond distance isThe ClO dissociated in cavity4 -On have two I ions.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic. Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., should be included in the present invention's Within protection domain.

Claims (5)

1. exclusive identifications of the porous MOF to iodide ion, it is characterised in that：Identification step is：
(1) complex 27 is steeped in KI solution, after 7 hours, crystal becomes blackish green from sky blue, passes through IR Characterization It was found that ClO4 -Characteristic peak disappear, XPS results are shown in the presence for having I elements in complex 28；
(2) structure of crystal is measured by X-ray monocrystalline.
2. exclusive identifications of the porous MOF according to claim 1 to iodide ion, it is characterised in that：In step (2) The molecular formula of the crystal is { [Cu6(TTTMB)8(I)11(OH)]·39H2O}n。
3. exclusive identifications of the porous MOF according to claim 2 to iodide ion, it is characterised in that：The crystal Molecular formula elementary analysis is according to C144H247Cu6I11N72O40Calculate：C 32.01%, N 18.66%, H 4.61%.Experiment value：C 33.05%, N 18.95%, H 4.08%.
4. exclusive identifications of the porous MOF according to claim 1 to iodide ion, it is characterised in that：In step (1) The complex 27 belongs to tetragonal crystal system, and space group is I4, and Cu1 is in pentacoordinate environment, respectively with four N atoms and an O Atomic coordinate constitutes tetragonal pyramid configuration, and Cu2 is in octahedral configuration, by four N atoms, and two come from ClO4 -And water The O atom coordination of molecule completes configuration, also has a free ClO in the cavity of complex4 -, tttmb takes cis, cis, Trans- configurations are connected to three Cu ions skeleton has been extended into three-dimensional framework.
5. exclusive identifications of the porous MOF according to claim 1 to iodide ion, it is characterised in that：Step (1) and step Suddenly (2) complex 28 and 27 belongs to heterogeneous isomorphism body, and the Cu1 of the complex 28 coordination environment is hexa-coordinate, respectively with four N1 and two I ion coordination, Cu-N bond distance isCu-I bond distance isThe complex 28 Cu2 coordination environment is pentacoordinate, and Cu-N bond distance is respectivelyWithCu-O bond distance is The ClO dissociated in cavity4 -On have two I ions.
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CN112525874A (en) * 2020-11-23 2021-03-19 集美大学 Method for measuring peroxide value of grease
CN114409918A (en) * 2022-01-27 2022-04-29 陕西科技大学 Lead-based microporous adsorption material and preparation method and application thereof
CN114752373A (en) * 2022-03-23 2022-07-15 武汉工程大学 Application of dysprosium metal organic framework material in fluorescence detection of iodide ions in water body

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112525874A (en) * 2020-11-23 2021-03-19 集美大学 Method for measuring peroxide value of grease
CN114409918A (en) * 2022-01-27 2022-04-29 陕西科技大学 Lead-based microporous adsorption material and preparation method and application thereof
CN114752373A (en) * 2022-03-23 2022-07-15 武汉工程大学 Application of dysprosium metal organic framework material in fluorescence detection of iodide ions in water body
CN114752373B (en) * 2022-03-23 2024-01-23 武汉工程大学 Application of dysprosium metal organic framework material in fluorescence detection of iodide ions in water body

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