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A kind of preparation method of 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 problems such as unstable product performance, unfavorable scale-up production, and low product yield, and achieve improved reaction efficiency and production efficiency , Good product performance, good dispersion effect

Active Publication Date: 2018-10-12
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned methods for preparing metal-organic framework materials are all batch reaction synthesis methods, which have disadvantages such as long reaction time, low product yield, and unstable product performance during the preparation process, which is not conducive to large-scale industrial scale-up production of products

Method used

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  • A kind of preparation method of metal organic framework material
  • A kind of preparation method of metal organic framework material
  • A kind of preparation method of metal organic framework material

Examples

Experimental program
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Effect test

Embodiment 1

[0033]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 the reaction, the product Cu-MOFs suspension is colle...

Embodiment 2

[0035] 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 the reaction, the product Cu-MOFs suspension is collected a...

Embodiment 3

[0037] 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 B liquid is sent into the microchannel reactor from the feed port 5 at a flow rate of 100 μl / min In module II, the temperature of module II is 120°C, the pressure is 1.0MPa, and the residence time is 150s. After the reaction, the product Cu-MOFs suspension is...

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Abstract

The invention discloses a preparation method for a metal organic framework material. The method includes the steps: (1) adding a metal precursor into an organic solvent, and stirring to dissolve, to obtain a solution A; (2) adding an organic ligand into an organic solvent, and stirring to dissolve, to obtain a solution B; (3) sending the solution A and the solution B into a micro channel reactor module I at a certain flow speed, generating an MOFs crystal seed in situ, and after the reaction is carried out for a certain time, sending the product material liquid into a micro channel reactor module II; (4) when the product material liquid enters the module II, sending the solution B into the module II at a certain flow speed, carrying out crystal seed induction to synthesize an MOFs material; and (5) carrying out solid-liquid separation of the prepared MOFs suspension, washing a solid with ethanol, and drying to obtain the product. The double-module micro channel reactor is adopted, the MOFs crystal seed is generated in the module I in situ, the MOFs material is continuously prepared through crystal seed induction in the module II, and the material has the advantages of simple and fast preparation process, narrow product particle diameter distribution, good dispersion and the like.

Description

technical field [0001] The invention relates to a method for preparing metal organic framework materials, in particular to a method for preparing metal organic framework materials 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. Compared with conventional porous materials, metal organic framework materials have the following advantages: (1) regulate the length and size of organic ligands, and effectively control the texture properties of materials (specific surface area, pore size); Volume; (3) High content of metal ions on the surface of pores or framework, high availability. The commonly used preparation methods include hydrothermal m...

Claims

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Application Information

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