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Ni (II)-Salen ligand metal organic framework crystal material and preparation method and application thereof

A technology of metal-organic frameworks and crystal materials, applied in the field of gas adsorption and catalysis, and the field of preparation of metal-organic frameworks, achieving good application prospects, no activity loss, and low cost

Active Publication Date: 2020-10-02
ZUNYI MEDICAL UNIVERSITY
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0007] According to literature review, (R,R)-N,N'-bis(3-methyl-5-carboxysalicylidene)-1,2-diphenylethylenediamine nickel (II) is a new type of metal Salen ligand, which coordinates with metal ions to form metal-organic framework materials has not been reported in the literature

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  • Ni (II)-Salen ligand metal organic framework crystal material and preparation method and application thereof
  • Ni (II)-Salen ligand metal organic framework crystal material and preparation method and application thereof
  • Ni (II)-Salen ligand metal organic framework crystal material and preparation method and application thereof

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[0044] {[Zn 4 O(L) 6 ]·DMF·H 2 O} n Synthesis and Characterization of

[0045] The Ni(II)-Salen(L) ligand (10mg, 0.0169mmol, 1.0equiv) was placed in a 10mL threaded transparent high temperature glass vial, followed by zinc nitrate hexahydrate (10mg, 0.0338mmol, 2.0equiv), 2mL DMF, ultrasonically treated for 2 minutes to dissolve, after complete dissolution, tighten the bottle cap, place it in an automatic program-controlled heating box, raise the temperature at a rate of 5°C / h to 80°C, keep warm for 3 days, and then heat at 5°C / h. h cooling rate was reduced to room temperature, filtered to obtain blocky brick red crystals, washed with DMF, and air-dried at room temperature to obtain 8.0 mg with a yield of 80% (calculated by Ni-Salen). Press C 198 H 162 N 14 Ni 6 O 42 Zn 8 Calculated elemental analysis theoretical values ​​(%) are: C, 55.49; N, 4.58; H, 3.81; experimental values: C, 55.38; N, 4.64; H, 3.86. IR(4000-400cm -1 ): 3435(vs), 3059(w), 1660(vs), 1610(vs), ...

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Abstract

The invention discloses a Ni (II)-Salen ligand metal organic framework crystal material and a preparation method and application thereof. The chemical formula of the material is {[Zn4O (L) 6]. DMF.H2O} n, wherein L is a dicarboxylic acid radical divalent anion of (R, R)-N, N '-bis (3-methyl-5-carboxyl salicylidene)-1, 2-diphenylethylenediamine nickel (II), and n is the polymerization degree. The metal organic framework crystal material is synthesized by a solvothermal synthesis method, which 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 high thermal stability (400 DEG C), and the BET specific surface area is 228m <2> / g. And the adsorption quantity of CO2 at 273K and 1atm is 18.8 m<3> / g. In the presence of an oxidizing agent, styrene is catalyzed to be selectively oxidized to generate benzaldehyde in a water phase, the yield reaches 99%, the catalyst is recycled for five times, and the activity loss is small. In the presence of tetrabutylammonium bromide, 1 atm and 50 DEG C solvent-free catalysis is performed on epoxy styrene and CO2 to react to generate styrene carbonate, the yield is 91%, and the catalyst is recycled for five times and still keeps activity. The material is a good heterogeneous catalyst.

Description

technical field [0001] The invention belongs to the field of preparation and application of new MOFs materials, in particular to (R,R)-N,N'-bis(3-methyl-5-carboxysalicylidene)-1,2-diphenylethane A preparation method of a metal-organic framework with diamine nickel (II) as a ligand 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 size, and high metal content that may provide active sites are important features of this class of materials. [0003] MOFs based on metal-Salen complexes are u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01D53/02B01J20/22B01J20/30B01J31/22C07C45/27C07C47/54
CPCC08G83/008B01D53/02B01J20/226B01J31/2243C07C45/27B01J2231/70B01J35/615C07C47/54Y02P20/151
Inventor 史大斌莫双铭
Owner ZUNYI MEDICAL UNIVERSITY
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