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Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof

A technology of organic framework and catalytic performance, which is applied in the field of trinuclear cadmium fluoride cluster-based metal-organic framework compounds, and can solve problems such as poor selectivity

Inactive Publication Date: 2012-06-27
FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Oxygen is the most ideal oxygen source for the oxidation reaction. According to our investigation, the selectivity of the oxidation reaction of cyclohexene directly using oxygen is relatively poor. No report

Method used

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  • Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof
  • Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof
  • Cadmium metal organic frame compound with catalytic performance and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Trinuclear cadmium fluoride cluster metal organic framework compound 1 - 4 preparation of

[0029] [Cd 3 F(ina) 4 (4-pic) 3 ] . BF 4 ( 1 ): Cd(NO 3 ) 2 4H 2 O (1.5 mmol), 4-methylpyridine (4-methylpyridine) (0.4 mmol) and 1.0 g of BmimBF 4 Add it into a 20 mL stainless steel reactor lined with polytetrafluoroethylene, react at a constant temperature of 160 °C for 6 days, then cool down to room temperature naturally, filter and wash thoroughly with distilled water and ethanol to obtain yellow blocky crystals (target product) , the yield of crystal product can reach 75%.

[0030] [Cd 3 F(ina) 3 (4,4'-bpy) 2 (4-pic) 2 ]·(4,4’-bpy).2BF 4 .2H 2 O ( 2 ): Cd(NO 3 ) 2 4H 2 O (1.5 mmol), 4,4'-bipyridine (4,4'-bipyridine) (1.0 mmol), 4-methylpyridine (4-methylpyridine) (0.4 mmol) and 1.0 g of BmimBF 4 Add it into a 20 mL stainless steel reactor lined with polytetrafluoroethylene, react at a constant temperature of 160 °C for 6 days, then cool...

Embodiment 2

[0033] Example 2: Catalytic Experiments and Analytical Procedures

[0034] The compound obtained by the above reaction 1 and 2 As catalysts, the oxidation of cyclohexene was carried out in a 40 mL stainless steel reactor lined with polytetrafluoroethylene, with acetonitrile (8 mL) as solvent, cyclohexene (0.80 mL), catalyst (0.05 g), O 2 The pressure is 1 MPa, and the temperature of the reactants is raised to 100 within 30 minutes after stirring and mixing. o C, then at 100 o C for 4 or 6 hours. The product was analyzed by GC-MS gas phase and mass spectrometry (instrument: GC6890N, MS5970).

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PUM

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Abstract

The invention provides a cadmium metal organic frame compound with catalytic performance and a preparation method and use thereof. A type of rarely-reported metal organic frame compound built by a three-core metal cluster formed by taking F as a central bridging cadmium ion and a carboxylic acid ligand generated through an in-situ reaction is synthesized thermally by using an ionic liquid. The ionic liquid plays multiple roles of a solvent, a soft template, an effective oxidation reaction accelerate and a ligand precursor in an ionic thermal synthesis process. The type of metal organic frame compound can be used for catalyzing a tetrahydrobenzene oxidation reaction, and the selectivity of a tetrahydrobenzene peroxide can be about 96 percent. Moreover, a catalyst is very easy to separate from a reaction system in a simple filtering way, the catalytic activity is kept, and the catalyst can be recycled repeatedly.

Description

[0001] technical field [0002] The invention relates to a class of trinuclear cadmium fluoride cluster-based metal organic framework compound (MOF) with catalytic performance synthesized under ionic liquid thermal conditions. Ionic liquids play multiple roles in the synthesis process: solvents, soft templates, effective accelerators for oxidation reactions, and ligand precursors. The structural characteristics of this type of compound are rarely reported MOF compounds constructed by trinuclear metal clusters formed by bridging cadmium ions with F as the center and carboxylic acid ligands generated by the in-situ reaction. Cyclohexene oxidation reaction, and the selectivity of cyclohexene peroxide can reach about 96%. Moreover, the catalyst is easily separated from the reaction system by simple filtration, and the catalytic activity is maintained, so it can be recycled for many times. Background technique [0003] Metal-organic frameworks (MOFs) have attracted extensive at...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/08B01J31/22C07C27/12C07C49/603C07C45/34C07C409/14C07C407/00
CPCY02P20/54Y02P20/584
Inventor 黄小荥谢在来冯美玲
Owner FUJIAN INST OF RES ON THE STRUCTURE OF MATTER CHINESE ACAD OF SCI
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