Method for preparing nano-zeolite metal-organic framework compounds by microreactor

A metal-organic framework and micro-reactor technology, applied in the direction of zinc organic compounds, copper organic compounds, etc., can solve the problems of polluted environment particle structure, cumbersome reaction process, harsh reaction conditions, etc. Tuning, crystal structure controllable effect

Inactive Publication Date: 2013-03-27
JIANGNAN UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

[0003] At present, the methods for synthesizing ZIFs are mainly solvothermal method (US2007 / 0202038A, CN102335626A), liquid phase diffusion method (Chem Eur J, 2007, 13, 4146), template method (J Am Chem Soc, 2004, 126, 13218), Dynamic crystallization method (CN102220626A), etc., but these methods have problems such as harsh reaction conditions, cumbersome reaction process, environmental pollution, and difficulty in stabilizing the particle structure.

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  • Method for preparing nano-zeolite metal-organic framework compounds by microreactor

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] (1) Solution configuration: Zinc nitrate and 2-methylimidazole were dissolved in methanol to prepare a metal precursor solution A with a concentration of 0.5 mol / L and an organic ligand solution B with a concentration of 0.5 mol / L.

[0016] (2) Mixing: Place A solution and B solution on both sides of a microfiltration membrane with a pore size of 0.01 microns, and control the pressure difference on both sides of the membrane to 0.02MPa, so that A solution can evenly pass through the membrane and enter B solution. The reaction temperature is 30°C, the type of reactor used is a flat membrane, and the membrane material is polyethersulfone (PES).

[0017] (3) Post-treatment: The white colloidal suspension obtained above was centrifuged at 10,000 r / min, washed twice with methanol, and dried at 80° C. for 10 h to obtain a nano-sized zeolite metal-organic framework compound.

[0018] The measured particle size is 32.44nm and the specific surface area is 980.4332m 2 / g.

Embodiment 2

[0020] (1) Solution configuration: Zinc nitrate and 2-ethylimidazole were dissolved in deionized water to prepare a metal precursor solution A with a concentration of 1mol / L and an organic ligand solution B with a concentration of 4mol / L.

[0021] (2) Mixing: Place A solution and B solution on both sides of the ultrafiltration membrane with a molecular weight cut-off of 50,000, and control the pressure difference on both sides of the membrane to 0.08MPa, so that the A solution can evenly pass through the membrane and enter the B solution. The reaction temperature is 40°C, the type of reactor used is coiled membrane, and the membrane material is polysulfone (PS).

[0022] (3) Post-treatment: centrifuge the white colloidal suspension obtained above at 12,000 r / min, wash with methanol twice, and dry at 100° C. for 12 hours to obtain a nano-sized zeolite metal-organic framework compound.

[0023] The measured particle size is 34.44nm and the specific surface area is 987.5348m 2 / ...

Embodiment 3

[0025] (1) Solution configuration: Dissolve copper nitrate and 2-ethylimidazole in deionized water to prepare metal precursor solution A with a concentration of 1mol / L and organic ligand solution B with a concentration of 1mol / L.

[0026] (2) Mixing: Place A solution and B solution on both sides of a microfiltration membrane with a pore size of 0.08 microns, and control the pressure difference on both sides of the membrane to 0.04MPa, so that A solution can evenly pass through the membrane and enter B solution. The reaction temperature is 35°C, and the type of reactor used is roll-type membrane, and the membrane material is polyvinylidene fluoride (PVDF).

[0027] (3) Post-treatment: centrifuge the white colloidal suspension obtained above at 12,000 r / min, wash with methanol twice, and dry at 90°C for 11 hours to obtain a nano-sized zeolite metal-organic framework compound.

[0028] The measured particle size is 33.56nm and the specific surface area is 1000.2225m 2 / g.

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Abstract

The invention relates to a method for preparing nano-zeolite metal-organic framework compounds by a microreactor, and belongs to the technical field of preparation of nano-particles, which is characterized by comprising the following steps of: constructing a microreactor by a porous film; respectively dissolving a metal precursor and an organic ligand in a solvent to prepare a metal precursor solution A and an organic ligand solution B; respectively arranging the metal precursor solution A and the organic ligand solution B at two sides of the film; by a pressure difference of the two sides of the film, uniformly pressing reactants at one side of the film into reactants at the other side of the film through the pores of the film, to generate nano-particles; and centrifuging, washing and drying to obtain the target product. The method for preparing the nano-zeolite metal-organic framework compounds by the microreactor is simple in operation, strong in controllability of particle structure, and is suitable for preparation and industrial production of various nano-zeolite metal-organic framework compounds.

Description

technical field [0001] The invention relates to a method for preparing nano zeolite-like metal-organic framework compounds with a microreactor, and belongs to the technical field of nano particle preparation. Background technique [0002] Nanomaterials refer to ultrafine particle materials with a particle size of nanometer scale (1-100nm), which have small size effects and surface effects. Nano-type zeolite metal-organic frameworks (ZIFs) are a series of metal-organic compounds (MOFs), which replace Si and Al elements in traditional zeolite molecular sieves with transition metal ions such as Zn / Cu, and imidazole or imidazole derivatives. The bridge oxygen in the traditional zeolite molecular sieve is a kind of zeolite-like material connected by the nitrogen atom on the imidazole ring. Combining the high stability of inorganic zeolites and the porosity of metal-organic complexes, ZIFs have great potential applications in the fields of gas adsorption, catalysis, storage, opti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C07F1/08
Inventor 白云翔董亮亮张春芳顾瑾孙余凭
Owner JIANGNAN UNIV
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