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A metal-organic framework based on cu(ii) ions and its synthesis method and application

A metal-organic framework and synthesis method technology, which can be applied to 1/11 group organic compounds without C-metal bonds, copper-organic compounds, chemical instruments and methods, etc. Effects of increased thermal stability, short time, mild conditions

Inactive Publication Date: 2018-02-06
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the detection methods of anions mainly include ion selective electrode, ion chromatography, and chemical titration. These methods generally require complex processes or large instruments, and the detection is complicated or costly. Therefore, it is urgent to identify anions simply and quickly. Require

Method used

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  • A metal-organic framework based on cu(ii) ions and its synthesis method and application
  • A metal-organic framework based on cu(ii) ions and its synthesis method and application
  • A metal-organic framework based on cu(ii) ions and its synthesis method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The synthesis route of Cu(II)-MOF-1 synthesized by the present invention is as follows:

[0047] 1. Preparation of Ligand L:

[0048]

[0049]At room temperature, 2,7-dibromofluorene (9.72g, 30mmol), tetrabutylammonium bromide (0.08g, 0.25mmol), 1-bromo-2-methylbutane (10.33g, 90mmol), 50% 10mL of NaOH solution was added to 130mL of DMSO, and ultrasonically reacted (100W) for 5 hours. After the reaction was completed, it was poured into 500mL of water, stirred for 20mins and then allowed to stand for 1 hour. Suction filtration, the filter cake was washed with 1% NaCl aqueous solution, and dried. 11.90 g of purple solid intermediate A was obtained, with a yield of 90.9%.

[0050]

[0051] N 2 Under protection, intermediate A (3.52g, 10mmol) 1,2,4-triazole (1,93g, 28mmol), cesium carbonate (13.03g, 40mmmol, cuprous iodide (0.762g, 4mmol) in 100ml In the there-necked flask, 20mlDMF was used as solvent, heated to 120°C, tracked by TLC, poured into 300ml of water af...

experiment example 2

[0061] Color responsiveness and characterization of experimental example 2 to different anions

[0062] Weigh 50 mg (0.0403 mmol) of each ground Cu(II)-MOF-1 crystal in 5 mL of 0.2 MMX (KF, KCl, KBr, KI, KSCN and NaN 3 ) solution, Cu-MOF-1 will quickly respond to present different colors. The discolored samples were taken out, centrifuged, washed with a solvent, and dried under an infrared lamp to obtain compounds 2, 3, 4, 5, 6, and 7. The reaction time of discoloration is immediately, 5min, 1min, 1min, 3s, immediately. We carried out solid-state ultraviolet, infrared, XPS, and ion chromatography tests on the above five compounds.

[0063] The conclusion of Experimental Example 2 is:

[0064] Figure 6 It shows that, compared with Cu(II)-MOF-1, the colors of compounds 2-7 have changed, which are beige, blue-green, dark green, yellow, grass green, and dark green, respectively. Figure 8 It shows that CF in compound 2-7 3 SO 3 - (1251cm -1 and 1031cm -1 ) peak disappea...

experiment example 3

[0068] Experimental Example 3 Recycling and reuse of anion-sensing materials based on anion exchange

[0069] Weigh 50mg (0.0403mmol) of 6 ground Cu(II)-MOF-1 samples and soak them in 5mL solutions containing different anions (1mmol) with a concentration below 0.2M, and take out the discolored samples and centrifuge them Washing with solvent and drying under infrared lamp gave compounds 2,3,4,5,6,7. Transfer the obtained 2, 3, 4, 5, 6, and 7 to 6 small beakers respectively, with a volume of 5mL and a concentration of 0.2M containing CF 3 SO 3 - The solution of anion (1mmol) was soaked for 12h, during which the solution was replaced every 1-2h. The compounds treated above were centrifuged, washed with solvent and dried under infrared light to obtain compounds 2', 3', 4', 5', 6', 7'. And the colors of compounds 2', 3', 4', 6', 7' are consistent with those of Cu(II)-MOF-1.

[0070] Conclusion of Experimental Example 3:

[0071] Figure 15 and Figure 16 It shows that exce...

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Abstract

The invention discloses a metal organic framework based on a Cu(II) ion, a synthetic method therefor and an application thereof. A structural formula is [Cu(C27H32N6)2(CF3SO3)2]n, wherein n is a nonzero natural number; Cu(II)-MOF-1 is crystallized to an orthorhombic system which belongs to a pbcn space group; a node Cu(II) metal center is positioned in a coordination environment of a deformed octahedron; an octahedron coordination plane is occupied by four triazole N atoms (Cu(1)-N(1)=2.001(3) angstrom and Cu(1)-N(6)=2.011(3) angstrom) from a ligand L; and two trifluorosulfonate radicals take part in coordination in an axial direction: (Cu(1)-O(1)=2.452(2) angstrom. Cu(II)-MOF-1 is applied in ion exchange and regeneration. Cu(II)-MOF-1 is applied in ion selective recognition. Cu(II) ion is highly exposed because of weak coordination properties of an anion CF3SO3-, so that the metal organic framework can display different colors by changing the Cu(II) central coordination environment through exchange of different anions, thereby realizing visual response of anions with different concentrations and different types, and selective recognition on anions with different coordination capacities, and realizing reuse through reversed exchange of anions.

Description

technical field [0001] The invention relates to a metal-organic framework based on Cu(II) ions, a synthesis method and application thereof. Background technique [0002] The application of supramolecular assemblies is the most important research hotspot in current supramolecular chemistry. Discrete or porous supramolecular complexes with balanced anions can undergo anion exchange reactions, thus making MOFs materials derive novel ion recognition properties. Anions are ubiquitous and play an important role in organisms, environmental pollutants, and chemical reaction processes. The simple and rapid identification of anions is of great significance in the fields of biochemistry and environmental protection research. At present, the detection methods of anions mainly include ion selective electrode, ion chromatography, and chemical titration. These methods generally require complex processes or large instruments, and the detection is complicated or costly. Therefore, it is urge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/08C07F1/08C09K11/06G01N21/78
CPCC07D249/08C07F1/005C07F1/08C09K11/06C09K2211/1059C09K2211/188G01N21/78
Inventor 刘启奎王可新曲佩佩董育斌
Owner SHANDONG NORMAL UNIV