Preparation method for nanometer organic metal framework by ultrasonic atomization

An ultrasonic atomization, nano-organic technology, applied in the directions of zinc organic compounds, iron organic compounds, copper organic compounds, etc., can solve the problems of difficulty in large-scale continuous production and cumbersome preparation process.

Inactive Publication Date: 2016-04-27
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current method of preparing NMOF is mainly based on high temperature and high pressure and microwave-assisted solvothermal method, inverse microemulsion method of microreactor, in order to obtain NMOF with controllable shape and size, surfactants are added as template agents to control However, many reaction conditions such as temperature, pH, pressure, heating rate, solvent polarity, metal ions, solubility of ligands and products, microemulsion size, stability and many other factors have an impact on the preparation of NMOF. The preparation process is cumbersome, and it is difficult to achieve large-scale continuous production

Method used

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  • Preparation method for nanometer organic metal framework by ultrasonic atomization
  • Preparation method for nanometer organic metal framework by ultrasonic atomization
  • Preparation method for nanometer organic metal framework by ultrasonic atomization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] 1. Add 577mgFeCl 3 , 354.4 mg of terephthalic acid was dissolved in 50 mL of redistilled N,N-dimethylformamide, and it was fully dissolved by ultrasonication at room temperature for 5 minutes to obtain a uniformly mixed solution.

[0018] 2. Add the homogeneous solution obtained in 1 into the atomizer, and ultrasonically atomize to produce fine droplets with a particle size of 0.5-20 microns. 2 Gas (0.6L / min) was loaded into the tube furnace which had been preheated to 300°C for reaction.

[0019] 3. The obtained solid particles were collected in an ice bath in a buffer bottle filled with ethanol-water mixed solution (volume ratio 2:1), washed with ethanol solvent and dried in vacuum to obtain Fe-1,4-BDCNMOF material.

Embodiment 2

[0021] 1. Add 577mgFeCl 3 , 354.4 mg of terephthalic acid was dissolved in 50 mL of redistilled N,N-dimethylformamide, and it was fully dissolved by ultrasonication at room temperature for 5 minutes to obtain a uniformly mixed solution.

[0022] 2. Add the homogeneous solution obtained in 1 into the atomizer, and ultrasonically atomize to produce fine droplets with a particle size of 0.5-20 microns. 2 Gas (0.6L / min) was loaded into the tube furnace which had been preheated to 400°C for reaction.

[0023] 3. The obtained solid particles were collected in an ice bath in a buffer bottle filled with ethanol-water mixed solution (volume ratio 2:1), washed with ethanol solvent and dried in vacuum to obtain Fe-1,4-BDCNMOF material.

example 3～7

[0025] The difference between embodiment 3-14 and embodiment 1~2 is shown in the table below:

[0026]

[0027] Structural Characterization of Nano Metal Organic Frameworks

[0028] The particle size and morphology of the Fe-MOF prepared by the present invention were characterized by the JEM-2000EX transmission electron microscope produced by Japan JEOL Electronics Co., Ltd. The results are as follows Figure 1~2 shown.

[0029] Figure 1~2 The Fe-MOF materials prepared in Examples 1-2 of the present invention are shown, both of which are similar to the spindle structure, and the sizes are respectively 37-70nm (short end), 130-280nm (long end) and 60-180nm (short end), 60nm ~1.2um (long end), which is consistent with the appearance of Fe-MOF prepared by solvothermal method in the existing literature, which proves the feasibility of this method.

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Abstract

The invention provides a preparation method for a nanometer organic metal framework by ultrasonic atomization. The method comprises the following steps: dissolving a soluble metal salt and an organic ligand in a certain solvent, carrying out ultrasonic atomization so as to produce liquid drops, introducing inert carrier gas so as to bring the liquid drops to a tubular furnace preset with a certain temperature, and carrying out a reaction so as to prepare the nanoscale organic metal framework. The method provided by the invention is simple to operate and can realize continuous reaction to prepare the nanoscale organic metal framework.

Description

technical field [0001] The invention relates to a method for preparing an organic metal frame material, in particular to a preparation method for a nanometer organic metal frame. Background technique [0002] Metal-organic frameworks (MOFs) are a class of three-dimensional space network skeleton compounds formed by the combination of metal ions and organic ligands through coordination chemical bonds. Due to their unique porous structure, high specific surface area, and adjustable morphology, It has attracted extensive attention in the fields of catalysis, gas adsorption, separation, etc. In order to realize the application of MOF materials in the biological field, such as drug carriers, imaging contrast agents, biosensors, etc., it is necessary to reduce their size to the nanoscale to prepare nano-metal organic frameworks (NMOFs). The current method of preparing NMOF is mainly based on high temperature and high pressure and microwave-assisted solvothermal method, inverse mi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/02C07F15/06C07F5/00C07F3/06C07F1/08
Inventor 吴仁安牛欢
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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