Pyridine type chiral Cu(II)-Salen ligand metal organic framework crystal material as well as preparation method and application thereof

A technology of metal-organic frameworks and crystalline materials, applied in organic chemistry, separation methods, alkali metal compounds, etc., to achieve the effects of high yield, high specific surface area, and novel structure

Active Publication Date: 2020-09-22
ZUNYI MEDICAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the known literature reports, 4,4'-biphenyl dicarboxylic acid is a commonly used ligand, (R,R)-N,N'-bis(5-(4-pyridyl)-2- Hydroxyacetophenonyl)-1,2-diphenylethylenediamine copper (II) is a new type of Salen ligand, and the combination of the two and the coordination of metal ions to form a metal-organic framework material has not been reported in the literature.

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  • Pyridine type chiral Cu(II)-Salen ligand metal organic framework crystal material as well as preparation method and application thereof
  • Pyridine type chiral Cu(II)-Salen ligand metal organic framework crystal material as well as preparation method and application thereof
  • Pyridine type chiral Cu(II)-Salen ligand metal organic framework crystal material as well as preparation method and application thereof

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preparation example Construction

[0040]The pyridine-type chiral Cu(II)-Salen ligand metal-organic framework crystal material of the present invention and its preparation method and application, the synthesis and characterization steps are as follows:

[0041] Divalent zinc salt compound, (R,R)-N,N'-bis(5-(4-pyridyl)ylidene-2-hydroxyacetophenonyl)-1,2-diphenylethylenediamine copper (II) Dissolve 4,4'-biphenyldicarboxylic acid in a solvent, stir evenly, then add it into a threaded high-temperature-resistant glass vial, heat up slowly, and after reacting at a certain temperature for a period of time, gradually lower the temperature, Cool to room temperature, filter, wash with solvent, dry to give {[Zn 2 (L)(BPDC) 2 ]·DMF·5H 2 O} n crystal material. Then use the Rigaku RAXIS~RAPID IPX-ray diffractometer to measure the single crystal structure of the compound, Nicolet Nexus 470FTIR infrared spectrometer to measure the compound infrared spectrum, and the thermogravimetric / differential thermal analysis of the sa...

specific Embodiment

[0043] {[Zn 2 (L)(BPDC) 2 ]·DMF·5H 2 O} n Synthesis and characterization of

[0044] Pyridine Cu(II)-Salen(L) ligand (10mg, 0.015mmol, 1.0equiv) was placed in a 10mL screw-threaded transparent high-temperature-resistant glass vial, and zinc nitrate hexahydrate (9mg, 0.030mmol, 2.0equiv ), 4,4'-biphenyldicarboxylic acid (7.3mg, 0.030mmol, 2.0equiv), 2mL DMF, ultrasonic treatment for 2 minutes to dissolve, after complete dissolution, stir for 5 minutes, then tighten the bottle cap, place in In an automatic program-controlled heating box, raise the temperature to 80°C at a heating rate of 5°C / h, keep it warm for 3 days, then cool down to room temperature at a cooling rate of 5°C / h, filter to obtain strip-shaped dark green crystals, wash with DMF, and dry at room temperature After drying, 14 mg was obtained, and the yield was 65% (calculated as Cu-Salen). Press C 71 h 65 CuN 5 o 17 The theoretical value (%) of elemental analysis calculated by Zn is: C, 60.16; N, 4.87; H, ...

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Abstract

The invention relates to a pyridine type chiral Cu(II)-Salen ligand metal organic framework crystal material as well as a preparation method and application thereof. The material has the following chemical formula: {[Zn2(L)(BPDC)2].DMF.5H2O}n, wherein L is (R,R)-N,N'-bis(5-(4-pyridyl) diyl-2-hydroxyacetophenone)-1,2-diphenylethylenediamine copper (II), BPDC is a 4,4'-biphenyl dicarboxylate divalent anion, and n is the degree of polymerization. The metal organic framework crystal material provided by the invention adopts a solvothermal synthesis method, and is simple to operate, low in cost, high in yield and easy for large-scale industrial production. The prepared metal organic framework crystal material has a relatively high specific surface area (BET specific surface area is 752 m<2> / g),and the adsorption capacities of CO2 and N2 under 1atm and 273 K are 3.47 mmol / g and 0.57 mmol / g respectively. TEMPO is used as an additive, selective oxidation of benzyl alcohol is catalyzed in a water phase to generate benzaldehyde, the yield reaches 99%, the catalyst is recycled for five times with almost no activity loss, and the catalyst is a good heterogeneous catalyst.

Description

technical field [0001] The invention belongs to the field of preparation and application of new metal-organic framework (MOFs) materials, and specifically relates to pyridine-type chiral Cu(II)-Salen ligand metal-organic framework crystal materials with (R,R)-N,N'-bis( Preparation method of metal-organic framework of 5-(4-pyridyl)ylidene-2-hydroxyacetophenonyl)-1,2-diphenylethylenediamine copper (II) and 4,4'-biphenyldicarboxylic acid And its application in the fields of gas adsorption and catalysis. Background technique [0002] Metal-organic frameworks (MOFs) represent a class of hybrid organic-inorganic ordered network supramolecular materials, which are ordered network structures formed by the combination of organic bridging ligands and inorganic metal ions, including one-dimensional chains, two-dimensional layered and three-dimensional network structures. These materials consist of rigid multi-tooth bridge struts and metal nodes. High micropore volume, large pore siz...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/28B01J20/30B01D53/02B01J31/22B01J35/10C07C45/29C07C47/54
CPCC08G83/008B01J20/226B01J20/28064B01J20/28014B01J20/28011B01D53/02B01J31/1691B01J35/1023C07C45/29B01J2531/26B01J2531/16B01J2531/0252B01J2531/0261B01J2231/763C07C47/54Y02P20/151Y02P20/584
Inventor 史大斌莫双铭
Owner ZUNYI MEDICAL UNIVERSITY
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