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Method for preparing nanoscale Cu-based metal organic framework material

An organic framework and metal-based technology, which is applied in the field of preparing nano-scale Cu-based metal-organic framework materials using microchannel reactors, can solve the problems of increasing the post-processing cost of organic liquids, reducing raw material utilization efficiency, and unstable product performance. Good prospects for large-scale industrial production, improved reaction efficiency and production efficiency, and good product performance

Active Publication Date: 2016-06-01
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 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
In addition, a large amount of organic solvent is consumed in the above preparation process, and a large amount of organic liquid is produced after the preparation, including unreacted metal precursors, organic ligands, and organic solvents, which not only reduces the utilization efficiency of raw materials, but also increases the waste of organic liquid. processing cost

Method used

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  • Method for preparing nanoscale Cu-based metal organic framework material
  • Method for preparing nanoscale Cu-based metal organic framework material
  • Method for preparing nanoscale Cu-based metal organic framework material

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Dissolve 12.1 g of copper nitrate trihydrate in 500 ml of ethanol to form liquid A, and dissolve 10.5 g of trimellitic acid in 500 ml of ethanol to form liquid B. The flow rate of A liquid is 5μl / min, and it is fed into module I from feed port 1, while the flow rate of B liquid is 5μl / min, and it is injected into module I from feed port 2. The temperature of module I is 40°C and the pressure At 0.1MPa, the A liquid and the B liquid are uniformly mixed in the module I to produce a liquid containing Cu-MOFs seed crystals, and the residence time is 180s. The feed liquid containing Cu-MOFs seed crystals is fed into the microchannel reactor module II from the feed port 4, and the flow rate is 10μl / min. The remaining liquid B is fed into the microchannel reactor from the feed port 5 at a flow rate of 5μl / min In module II, the temperature of module II is 50°C, the pressure is 0.1MPa, and the residence time is 240s. After reacting for a certain period of time, the product liqui...

Embodiment 2

[0039] Dissolve 121 g of copper nitrate trihydrate in 500 ml of ethanol to form liquid A, and dissolve 210 g of trimellitic acid in 500 ml of ethanol to form liquid B. The flow rate of A liquid is 200μl / min, which is fed into module I from the feed port 1, while the flow rate of B liquid is 200μl / min, which is injected into module I from the feed port 2. The temperature of module I is 70°C, and the pressure At 1.0MPa, the A liquid and the B liquid are uniformly mixed in the module I to produce a liquid containing Cu-MOFs seed crystals, and the residence time is 30s. The feed liquid containing Cu-MOFs seed crystals is sent to module II from the feed port 4, and the flow rate is 400μl / min. The remaining B liquid is sent to the module II from the feed port 5 at a flow rate of 200μl / min. -The initial crystallization reaction of MOFs material, where the temperature of module II is 100°C, the pressure is 1.0MPa, and the residence time is 60s. After reacting for a certain period of t...

Embodiment 3

[0041] 60.5 g of copper nitrate trihydrate was dissolved in 500 ml of ethanol to form liquid A, and 105 g of trimellitic acid was dissolved in 500 ml of ethanol to form liquid B. The flow rate of A liquid is 100μl / min, and it is fed into module I from the feed port 1, while the flow rate of B liquid is 100μl / min, and it is injected into the module I from the feed port 2. The temperature of module I is 60℃ and the pressure At 0.5MPa, the A liquid and the B liquid are uniformly mixed in the module I to generate a liquid containing Cu-MOFs seed crystals, and the residence time is 60s. The feed liquid containing Cu-MOFs seed crystals is fed into module II from the feed port 4 with a flow rate of 100μl / min. The remaining liquid B is fed into module II from the feed port 5 at a flow rate of 100μl / min, and Cu is generated. -The initial crystallization reaction of MOFs material, where the temperature of module II is 60°C, the pressure is 0.5MPa, and the residence time is 120s. After a...

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Abstract

The invention discloses a method for preparing a nanoscale Cu-based metal organic framework material. The method includes the steps: (1) preparing a copper precursor solution A; (2) preparing an organic ligand solution B; (3) sending the solution A and the solution B into a micro channel reactor module I at a certain flow speed, generating a Cu-MOFs crystal seed in situ, and after the reaction is carried out for a certain time, sending the product material liquid into a 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 induced synthesis reaction, and after the reaction is carried out for a certain period of time, sending the product material liquid into a module III; (5) allowing the material liquid prepared in the step (4) to enter the micro channel reactor module III, and carrying out secondary crystallization reaction to synthesize a Cu-MOFs material; and (6) carrying out solid-liquid separation of the Cu-MOFs suspension prepared in the step (5), and allowing the filtrate to return to the micro channel reactor module II at a certain flow speed to participate in secondary crystallization reaction; and washing the solid with ethanol, and drying to obtain the product. The Cu-MOFs material is prepared by a multi-module micro channel reactor, and the method has the advantages of simple and fast preparation process, good product performance and the like.

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 nano-scale Cu-based metal organic framework material by using a microchannel reactor. Background technique [0002] Metal organic framework materials (MOFs), also known as metal coordination polymers, refer to crystalline materials formed by connecting inorganic metals or metal clusters with nitrogen and oxygen-containing multidentate organic ligands through coordination bonds. Surface area, adjustable pore size, organic functionalized porous material. Cu-based metal organic framework (Cu-MOFs) materials are a type of MOFs with a hole-cage structure. In 1999, Chui et al. used a solvothermal method to synthesize Cu-MOFs. Later, researchers used different preparation methods to synthesize Cu-MOFs with different physical and chemical properties. The preparation methods include hydrothermal, microwave, sonic, and Methods such as electr...

Claims

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Application Information

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