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Method for preparing metal organic framework material

A metal-organic framework and organic solvent technology, which is applied in the field of preparing metal-organic framework materials using microchannel reactors, can solve the problems of affecting the production efficiency and performance of materials, consuming organic solvents, and long processing time, etc., and achieves good activation effects. Effects of shortened reaction time and high material handling efficiency

Active Publication Date: 2016-05-25
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The post-processing method of the above-mentioned patent not only consumes a large amount of organic solvent, but also consumes a long processing time, which seriously affects the production efficiency and performance of the material

Method used

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  • Method for preparing metal organic framework material
  • Method for preparing metal organic framework material

Examples

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Embodiment 1

[0035] Dissolve 12.1 g of copper nitrate trihydrate in 500 ml of ethanol to form liquid A, and dissolve 10.5 g of trimesic acid in 500 ml of ethanol to form liquid B. The flow rate of liquid A is 5 μl / min, which is sent into module I from feed port 1, while the flow rate of liquid B is 5 μl / min, which is injected into module I from feed port 2, wherein the temperature of module I is 40°C and the pressure is 0.1MPa, liquid A and liquid B are uniformly mixed in module I to generate a feed liquid containing Cu-MOFs seed crystals, and the residence time is 180s. The feed liquid containing Cu-MOFs seed crystals is sent into the microchannel reactor module II from the feed port 4 at a flow rate of 10 μl / min, and the remaining B liquid is sent into the microchannel reactor from the feed port 5 at a flow rate of 5 μl / min In module II, the temperature of module II is 80°C, the pressure is 0.1MPa, and the residence time is 200s. After reacting for a certain period of time, the product ...

Embodiment 2

[0037] Dissolve 121g of copper nitrate trihydrate in 500ml of ethanol to form liquid A, and dissolve 210g of trimesic acid in 500ml of ethanol to form liquid B. The flow rate of liquid A is 200 μl / min, which is sent into module I from feed port 1, while the flow rate of liquid B is 200 μl / min, which is injected into module I from feed port 2, where the temperature of module I is 70°C and the pressure 1.0MPa, liquid A and liquid B are uniformly mixed in module I to generate a feed liquid containing Cu-MOFs seed crystals, and the residence time is 30s. The feed liquid containing Cu-MOFs seed crystals is sent into the microchannel reactor module II from the feed port 4 at a flow rate of 400 μl / min, and the remaining liquid B is sent into the microchannel reactor from the feed port 5 at a flow rate of 200 μl / min In module II, the temperature of module II is 150°C, the pressure is 1MPa, and the residence time is 60s. After reacting for a certain period of time, the product feed li...

Embodiment 3

[0039] Dissolve 60.5g of copper nitrate trihydrate in 500ml of ethanol to form liquid A, and dissolve 105g of trimesic acid in 500ml of ethanol to form liquid B. The flow rate of liquid A is 100 μl / min, and it is sent into module I from feed port 1, while the flow rate of liquid B is 100 μl / min, and it is injected into module I from feed port 2, wherein the temperature of module I is 60°C and the pressure is 0.5MPa, liquid A and liquid B are uniformly mixed in module I to generate a feed liquid containing Cu-MOFs seed crystals, and the residence time is 120s. The feed liquid containing Cu-MOFs seed crystals is sent into the microchannel reactor module II from the feed port 4 at a flow rate of 200 μl / min, and the remaining liquid B is sent into the module II from the feed port 5 at a flow rate of 100 μl / min , where the temperature of module II is 120°C, the pressure is 0.5MPa, and the residence time is 150s. After reacting for a certain period of time, the product feed liquid ...

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Abstract

The present invention discloses a method for preparing a metal organic framework material. The method comprises: (1) preparing a metal precursor solution A; (2) preparing an organic ligand solution B; (3) respectively conveying the solutions A and the solution B into a micro-channel reactor module I to carry out in-situ generation of a MOFs crystal seed, carrying out a reaction for a certain time, and conveying the material liquid into a module II; (4) conveying the solution B into the module II when the material liquid enters the module II, carrying out crystal seed induction synthesis, carrying out a reaction for a certain time, and conveying the material liquid into a module III; (5) conveying a solvent C into the module III when the obtained material liquid enters the module III, and carrying out a solvent activation reaction; and (6) carrying out solid-liquid separation on the obtained suspension, washing the solid by using ethanol, and drying to obtain the product. According to the present invention, the multi-module micro-channel reactor is used, the MOFs crystal seed is subjected to in-situ generation in the module I, the crystal seed induction synthesis is performed in the module II, and the solvent activation reaction is completed in the module III, such that the advantages of simple and fast preparation process, narrow product particle size distribution, good dispersion and the like are provided.

Description

technical field [0001] The invention relates to a method for preparing a metal organic framework material, in particular to a method for preparing a metal organic framework material using a microchannel reactor. Background technique [0002] Metal-organic frameworks (MOFs), also known as metal coordination polymers, refer to crystalline materials formed by connecting inorganic metals or metal clusters with nitrogen-oxygen-containing multidentate organic ligands through coordination bonds. Surface area, adjustable pore size, organically functionalized porous material. The commonly used preparation methods include hydrothermal method, solvothermal method, reflux method, microwave method, sonic method, electrochemical method and other methods. [0003] During the synthesis and preparation of MOFs materials, there are a large amount of organic solvents, unreacted metal ions and organic ligands in the material pores, and MOFs materials need to be activated to remove the above im...

Claims

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Application Information

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IPC IPC(8): C07F1/08C07F3/06
Inventor 王海洋马蕊英赵亮张英王刚
Owner CHINA PETROLEUM & CHEM CORP
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