Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method for high-activity metal organic framework material

A metal organic framework, high activity technology, applied in organic chemistry, copper organic compounds, chemical instruments and methods, etc., can solve the problems of reducing the industrial application value of materials, low metal content in impregnation method, poor thermal stability, etc., and achieve easy scale Expanded production, narrow particle size distribution, and good dispersion

Active Publication Date: 2016-06-01
CHINA PETROLEUM & CHEM CORP +1
View PDF10 Cites 8 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Conventional metal-organic framework materials have poor thermal stability. After the introduction of noble metal ions, metal-organic framework materials with high activity can be obtained through the conventional high-temperature hydrogen reduction reaction. The general processing temperature is 200-800 ° C, which is much higher than most metal-organic framework materials The temperature resistance of framework materials limits the application of metal-organic framework materials to support noble metals to prepare highly active catalysts
[0005] Patents CN103191778 and CN103752276 introduce the method of introducing metal ions on metal organic framework materials to prepare high-activity catalyst / adsorbent by post-synthesis method. The catalyst / adsorbent prepared by this method has good metal dispersion and high activity, which broadens the scope of metal The practical application of organic framework materials, but the impregnation method introduces low metal content and poor stability, which reduces the industrial application value of the material

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method for high-activity metal organic framework material
  • Preparation method for high-activity metal organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Dissolve 2.416g of copper nitrate trihydrate in 100ml of ethanol to form liquid A, dissolve 2.12g of trimesic acid in 100ml of ethanol to form liquid B, and dissolve 5.18g of chloroplatinic acid in 100ml of acetone to form liquid C. The flow rate of liquid A is 5 μl / min, which is sent into module I from feed port 1, and the flow rate of liquid B is 5 μl / min, which is sent into module I from feed port 2, and liquid A and liquid B are in module I The mixed reaction generates the feed liquid of Cu-MOFs seed crystals, in which the temperature of module I is 40°C, the pressure is 0.1MPa, and the residence time is 180s. The feed liquid of the Cu-MOFs seed crystal flows out from the outlet 3 of the module I, and is sent into the module II from the feed port 4, and mixed with the C liquid sent into the module II from the feed port 5, and an in-situ synthesis reaction of metal ions occurs , where the flow rate of liquid C is 5 μl / min, the temperature of module II is 50° C., the ...

Embodiment 2

[0041] Dissolve 24.16g of copper nitrate trihydrate in 100ml of ethanol to form liquid A, dissolve 21.01g of trimesic acid in 100ml of ethanol to form liquid B, and dissolve 51.8g of chloroplatinic acid in 100ml of acetone to form liquid C. The flow rate of liquid A is 20 μl / min, which is sent into module I from feed port 1, while the flow rate of liquid B is 20 μl / min, which is sent into module I from feed port 2, and liquid A and liquid B are in module I The mixed reaction generates the feed liquid of Cu-MOFs seed crystals, in which the temperature of module I is 70°C, the pressure is 1MPa, and the residence time is 30s. The feed liquid of the Cu-MOFs seed crystal is sent into the module II from the feed port 4, mixed with the C liquid sent into the module II from the feed port 5, and the metal ion in-situ synthesis reaction occurs, wherein the flow rate of the C liquid is 20 μl / min, the temperature of module II is 80°C, the pressure is 1MPa, and the residence time is 30s. ...

Embodiment 3

[0043] Dissolve 19.32g of copper nitrate trihydrate in 100ml of ethanol to form liquid A, dissolve 10.51g of trimesic acid in 100ml of ethanol to form liquid B, and dissolve 20.72g of chloroplatinic acid in 100ml of acetone to form liquid C. The flow rate of liquid A is 10 μl / min, which is sent into module I from feed port 1, while the flow rate of liquid B is 10 μl / min, which is sent into module I from feed port 2, and liquid A and liquid B are in module I The mixed reaction generates the feed liquid of Cu-MOFs seed crystals, in which the temperature of module I is 60°C, the pressure is 0.4MPa, and the residence time is 100s. The feed liquid of the Cu-MOFs seed crystal is sent into the module II from the feed port 4, mixed with the C liquid sent into the module II from the feed port 5, and the metal ion in-situ synthesis reaction occurs, and the flow rate of the C liquid is 10 μl / min, the temperature of module II is 70°C, the pressure is 0.5MPa, and the residence time is 100...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
Specific surface areaaaaaaaaaaa
The average particle sizeaaaaaaaaaa
Specific surface areaaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method for a high-activity metal organic framework material. The method includes the steps: (1) preparing a metal 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, and generating an MOFs crystal seed in situ; (4) dissolving a metal in a state of metal powder, nano oxide or metal salt to obtain a solution C, when the material liquid obtained in the step (3) enters a module II, sending the solution C into the module II, and carrying out a metal ion in-situ synthesis reaction; (5) allowing the material liquid of the step (4) to enter a module III, sending the solution B into the module III, and carrying out crystal seed induced synthesis; (6) when the material liquid of the step (5) enters a module IV, sending a light reduction sacrificial agent D into the module IV; (7) when the material liquid obtained in the step (6) enters a module V, carrying out metal reduction reaction by sun illumination; and (8) carrying out solid-liquid separation, washing, and drying to obtain the product. The MOFs material prepared by the multi-module micro channel reactor has the advantages of simple and fast preparation process and good product activity.

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 highly active 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. 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. [0003] However, the metal ions of MOFs pro...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07F19/00C07F15/00C07F1/08
Inventor 王海洋马蕊英赵亮张英王刚
Owner CHINA PETROLEUM & CHEM CORP
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products