Continuous synthesis method of metalorganic frame compound with stepped hole structure

Abstract

The invention relates to a continuous synthesis method of a metalorganic frame compound with a stepped hole structure. The continuous synthesis method has the following steps that 1, a continuous reaction device is erected; 2, metal salt is dispersed in a solvent A and is added into an injector of a pump I, anorganic ligand is dispersed in a solvent B and is added into an injector of a pump II, and a continuous phase is added to an injector of a pump III; 3, a heating area is heated to reach set reaction temperature; 4, the flowing speeds of the three pumps are set, and the three pumps are started; 5, a product is collected from the output end of a pipeline, the product is separated out through centrifugation or filtration, and a stepped-hole MOF material is obtained. By adopting a continuous flow s synthesis method, continuous synthesis of the stepped-hole MOF material can be achieved. A template agent and aftertreatment process are not needed in the synthesis process, the stepped-hole MOF prepared by adopting the preparation method can be up to very high space-time yield and conversion rate, straight amplification can be performed in a simple reactor number increasing mode, and the continuous synthesis method is easy to operate and suitable for large-scale continuous production.

Description

technical field [0001] The invention relates to a continuous synthesis method of a metal organic framework compound with a stepped pore structure, and belongs to the field of advanced nanoporous materials and technologies. Background technique [0002] Metal-Organic Framework (MOF) is a kind of crystalline porous material with a repeating network structure formed by the self-assembly of organic ligands and metal ions. Due to its highly ordered structure, a wide variety, With many characteristics such as adjustable structure, it has become one of the most popular research directions in the field of chemistry and materials in recent years. In the synthesis process of MOF, people can construct secondary structural units and select ligands with different structures to realize the artificial design and controllable modification of MOF pore structure, and prepare MOF with various pore structures, high specific surface area and rich surface properties. porous material. These char...

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Problems solved by technology

However, the templating agent added by this method is difficult to remove from MOF materials, which limits the application of this method in MOF materials.

In addition, researchers have also invented a method to prepare step-hole MOFs by introducing defects into the MOF lattice. For example, O.M.Yaghi et al. added a certain proportion of monocarboxylic acid to the synthesis of MOF-5, resulting in MOF-5 The absence of ligands in some channels in the lattice resulted in MOF-5 with both mesopores and micropores (J.Am.Chem.Soc.2011,133(31),11920-11923), Kimoon Kim et al. Utilizing the instability of the coordination bonds in the structure of some MOF materials, point defects are generated in the MOF lattice by solvent corrosion post-processing methods, thereby generating mesoporous pores in microporous MOF materials (Angew.Chem.Int.Ed. 2015,54,13273–13278), however, this method is only effective for some MOF materials with unstable coordination bonds

At the same time, the MOFs prepared by these methods still use the traditional diffusion method, hydrothermal method, solvothermal method, etc. These methods have the disadvantages of long cycle, large crystallization uncertainty, serious influence of external factors, and large preparation scale limitations.

So far, there is no effective continuous production method of step-pore MOF

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