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A Ni(ii)-salen ligand metal-organic framework crystal material and its preparation method and application

A metal-organic framework, crystal material technology, applied in separation methods, organic chemistry, chemical instruments and methods, etc., to achieve the effects of good application prospects, high yield and novel structure

Active Publication Date: 2022-05-17
ZUNYI MEDICAL UNIVERSITY
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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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  • A Ni(ii)-salen ligand metal-organic framework crystal material and its preparation method and application
  • A Ni(ii)-salen ligand metal-organic framework crystal material and its preparation method and application
  • A Ni(ii)-salen ligand metal-organic framework crystal material and its preparation method and application

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

[0045] Ni(II)-Salen(L) ligand (10mg, 0.0169mmol, 1.0equiv) was placed in a 10mL transparent high-temperature-resistant glass vial with screw threads, and zinc nitrate hexahydrate (10mg, 0.0338mmol, 2.0equiv) was added successively. 2mL DMF, ultrasonic treatment for 2 minutes to dissolve, after complete dissolution, tighten the bottle cap, place in an automatic program-controlled incubator, heat up to 80°C at a rate of 5°C / h, keep warm for 3 days, and then increase the temperature at 5°C / h h The cooling rate was reduced to room temperature, filtered to obtain blocky brick red crystals, washed with DMF, and 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 The 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(...

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Abstract

Ni(II)-Salen ligand metal-organic framework crystal material and its preparation method and application. The chemical formula of the material: {[Zn 4 O(L) 6 ]·DMF·H 2 O} n , where L is the dicarboxylate dicarboxylate of (R,R)-N,N'-bis(3-methyl-5-carboxysalicylidene)-1,2-diphenylethylenediamine nickel(II) Valence anion, n is the degree of polymerization. The metal organic framework crystal material adopts a solvothermal synthesis method, has simple operation, low cost, high yield, and is easy for large-scale industrial production. The prepared MOF crystalline material has high thermal stability (400°C), and the BET specific surface area is 228m 2 / g. For CO at 273K, 1atm 2 The adsorption capacity is 18.8m 3 / g. In the presence of an oxidizing agent, the selective oxidation of styrene is catalyzed in an aqueous phase to generate benzaldehyde with a yield of 99%. The catalyst is recycled five times with little loss of activity. In the presence of tetrabutylammonium bromide, 1 atm, 50 ℃ solvent-free catalysis of epoxy styrene and CO 2 The reaction produces styrene carbonate with a yield of 91%. The catalyst is recycled five times and still maintains its activity. This 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 Patents(China)
IPC IPC(8): C08G83/00B01D53/02B01J20/22B01J20/30B01J31/22C07C45/27C07C47/54
CPCC08G83/008B01D53/02B01J20/226B01J31/2243B01J35/1019C07C45/27B01J2231/70C07C47/54Y02P20/151
Inventor 史大斌莫双铭
Owner ZUNYI MEDICAL UNIVERSITY
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