Organic metal framework supported palladium, preparation method and application thereof

Abstract

The invention discloses an organic metal framework supported palladium in the technical field of chemical industry, a preparation method and application thereof. The organic metal framework supported palladium is prepared by the method comprising the steps of: dissolving terephthalic acid and zinc nitrate hexahydrate into N, N-dimethylformamide, dripping triethylamine with the stirring, continuing stirring the obtained solution, filtering the obtained solution, and washing a precipitate to obtain a solid, namely MOF-5; and dissolving Na2PdC14 into the N, N-dimethylformamide to obtain solution, adding the MOF-5 into the solution, and then dripping hydrazine hydrate to obtain Pd@MOF-5 through stirring, filtration, washing and vacuum drying. The invention also relates to the method for preparing the organic metal framework supported palladium, application thereof taken as a catalyst in a Sonogashira reaction, and the method for preparing diaryl acetylene. The organic metal framework supported palladium in the invention has good stability, can catalyze the reaction with high selectivity and high efficiency under rather low loading of the catalyst, and can be repeatedly used.

Description

technical field The invention relates to an organometallic framework in the technical field of chemical industry and its preparation method and use, in particular to an organometallic framework supporting palladium and its preparation method and use. Background technique Metal-organic frameworks (MOFs), which are porous materials containing transition metal centers and organic linkers, have been widely used in gas adsorption, catalysis, and separation. MOF-5 (chemical formula: Zn 4 O(BDC) 3 ·(DMF) 8 , (wherein BDC=1,4-dicarboxylate benzene, DMF=N, N-dimethylformamide)) is one of them typical representative, it is by [Zn 4 O] 6+ The inorganic groups and [OOC-C 6 h 4 -COO] 2- As an organic linker to form a three-dimensional skeleton structure, according to "Nature", 1999, Volume 402, page 276, MOF-5 synthesized by Li, H. and Yaghi, O.M. et al. has a specific surface area of ​​up to 2900m 2 / g, much larger than common activated carbon and zeolite. And solid supports wi...

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Problems solved by technology

After searching the literature of the prior art, it was found that Shigeki Mori et al. used Pd / C to catalyze the Sonogashira reaction (Chem. Eur. J. 2008, 14, 6994-6999), in a mixed solvent of isopropanol and water at 80°C The reaction of synthesizing diaryl acetylene, but the selectivity of the catalyst in this reaction is not good, the yield of various products is not very high, the scope of application of the substrate has certain limitations, and the loading of Pd is large, and the recycling rate is low. loss of precious metals