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Method for quickly synthesizing MOFs nanoparticles

A nano-particle, rapid technology, applied in chemical instruments and methods, alkali metal compounds, zinc organic compounds, etc., can solve the problems of uneven particle size distribution of concentration products, long synthesis cycle, difficult to control the shape, etc., to shorten the synthesis time The effects of time, mild reaction conditions, and narrow particle size distribution

Inactive Publication Date: 2011-11-16
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In traditional scale reactors, not only the synthesis cycle is longer, but also the concentration, pH and temperature of the reactants in the reaction system are not uniform, which easily leads to uneven particle size distribution of the product, and the shape is difficult to control, which affects the physical and chemical properties of the product and application performance
Furthermore, the synthesis process is discontinuous

Method used

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  • Method for quickly synthesizing MOFs nanoparticles
  • Method for quickly synthesizing MOFs nanoparticles
  • Method for quickly synthesizing MOFs nanoparticles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1. Microchannel pretreatment: select a capillary quartz tube with an inner diameter of 0.5mm and a length of 1m as the microchannel, wash the capillary quartz tube with 0.1mol / L nitric acid, 0.1mol / L sodium hydroxide solution and acetone respectively, and finally Rinse with deionized water before use.

[0026] 2. Preparation of precursor solution

[0027] (1) Precursor A: Weigh 5.078g of methylimidazole and dissolve it in 100ml of DMF to prepare a 0.6M methylimidazole DMF solution.

[0028] (2) Precursor solution B: Weigh 5.95g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 100ml DMF to prepare 0.2M Zn(NO 3 ) 2 ·6H 2 O DMF solution.

[0029] 3. The precursor solution is synthesized in the microchannel

[0030] Put the two precursors into two syringes respectively, pump them into the three-way mixer with a syringe pump and mix them completely before entering the capillary quartz tube. The synthesis temperature is controlled at 80 °C, and the residence time of the precursor...

Embodiment 2

[0033] 1. Microchannel pretreatment: select a capillary quartz tube with an inner diameter of 1mm and a length of 2.5m as the microchannel, wash the capillary quartz tube with 0.1mol / L nitric acid, 0.1mol / L sodium hydroxide solution and acetone respectively, and finally Rinse with deionized water before use.

[0034] 2. Preparation of precursor solution

[0035] (1) Precursor A: Weigh 5.078g of methylimidazole and dissolve it in 100ml of DMF to prepare a 0.6M methylimidazole DMF solution.

[0036] (2) Precursor solution B: Weigh 5.95g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 100ml DMF to prepare 0.2M Zn(NO 3 ) 2 ·6H 2 O DMF solution.

[0037] 3. The precursor solution is synthesized in the microchannel

[0038] Put the two precursors into two syringes respectively, pump them into the three-way mixer with a syringe pump and mix them completely before entering the capillary quartz tube. The synthesis temperature is controlled at 100 ° C, and the residence time of the precurs...

Embodiment 3

[0041] 1. Microchannel pretreatment: select a capillary quartz tube with an inner diameter of 0.75mm and a length of 1.5m as the microchannel, wash the capillary quartz tube with 0.1mol / L nitric acid, 0.1mol / L sodium hydroxide solution and acetone respectively, Finally, rinse with deionized water before use.

[0042] 2. Preparation of precursor solution

[0043] (1) Precursor A: Weigh 5.078g of methylimidazole and dissolve it in 100ml of DMF to prepare a 0.6M methylimidazole DMF solution.

[0044] (2) Precursor solution B: Weigh 5.95g Zn(NO 3 ) 2 ·6H 2 O was dissolved in 100ml DMF to prepare 0.2M Zn(NO 3 ) 2 ·6H 2 O DMF solution.

[0045] 3. The precursor solution is synthesized in the microchannel

[0046] Put the two precursors into two syringes respectively, pump them into the three-way mixer with a syringe pump and mix them completely before entering the capillary quartz tube. The synthesis temperature is controlled at 90 ° C, and the residence time of the precurso...

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Abstract

The invention discloses a microchannel flow method for quickly synthesizing uniform ZIF-8 nanoparticles. The method comprises the following steps of: filling 50ml of 0.6M dimethylformamide (DMF) solution of methylimidazole and 50ml of 0.2M DMF solution of Zn(NO3)2.6H2O in two injectors, feeding the two solutions into a tee mixer at a certain speed by using an injection pump at the temperature of 80DEG C, fully mixing the two solutions, introducing into a capillary quartz tube microchannel, and collecting the nano-scale ZIF-8 product at an outlet. Compared with the traditional solvent thermosynthesis method in a reactor, the method has the advantages of greatly shortening reaction time and saving energy. The synthesized ZIF-8 nanoparticles have small average particle size of about 50nm, and have the typical hexagonal structure. Moreover, by controlling reaction temperature, retention time and a reaction material ratio, the ZIF-8 nanoparticles with required size can be easily prepared continuously.

Description

technical field [0001] The invention belongs to the technical field of porous inorganic membranes, and relates to a novel microchannel flow method for rapidly preparing ZIF-8MOFs nanoparticles. Background technique [0002] Metal-organic framework (MOFs) materials have ultra-high specific surface area and huge pore volume, which can realize high-capacity storage of various gases. Efficient separation of gas and liquid, and can greatly improve its material adsorption capacity and dynamic performance. Therefore, applying MOFs materials to CO 2 The field of storage and separation has very attractive application prospects. [0003] ZIFs materials are a class of materials with relatively large specific surface area and pore volume in MOFs materials. Compared with other types of metal-organic framework (MOFs) materials, ZIFs materials have higher thermal stability and chemical corrosion resistance. Therefore, the application of ZIFs materials in gas storage, separation, cataly...

Claims

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Application Information

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IPC IPC(8): C07F3/06B01J20/22B01J20/28B01D69/10B01J31/22
CPCY02P20/10
Inventor 张雄福吕婧张光才刘亚光陈芳邱介山
Owner DALIAN UNIV OF TECH
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