Preparation method and applications of porous metal organic skeleton material

An organic framework and porous metal technology, applied in the field of preparation of porous metal-organic framework materials, can solve the problems of harsh synthesis conditions, low yield, equipment corrosion and operation hazards.

Active Publication Date: 2015-02-25
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] According to the current patented technology, the MOFs synthesis technology in a weak alkaline environment has disadvantages such as low yield and harsh synthesis conditions; the MOFs synthesis technology in a strong alkaline environment usually uses a large amount of highly corrosive alkali (such as NaOH, US2012 / 0082864) for deprotonation of organic ligands
The use of strong corrosive alkali can realize the synthesis of MOFs materials at low temperature, but it will also cause corrosion of equipment and danger of operation, and will cause difficulties in the subsequent purification of materials, and may also affect some of the porous MOFs materials due to the presence of alkali metal ions. performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Embodiment 1: Synthesis of Zn-dimethylimidazole framework

[0049] 26g of ZnSO 4 ·7H 2 O was dissolved in 150g of water; 16g of urea and 15g of 2-methylimidazole were dissolved in a mixture of 50g of water and 100g of methanol; then zinc sulfate solution and 2-methylimidazole solution were mixed, stirred for 20min until they were evenly mixed, then transferred to In a 500ml autoclave, react at 110°C for 5 hours. Cool down naturally, filter the white precipitate, and then wash twice with 100ml of water. The filter cake was dried at 100°C for 6 hours, then activated by drying at 130°C under vacuum (0.2 bar) for 8 hours to obtain 21 g of product;

[0050] N 2 The specific surface area is 1476m 2 / g (as determined by the Langmuir method).

Embodiment 2

[0051] Embodiment 2: Synthesis of Zn-dimethylimidazole framework

[0052] 26g ZnSO 4 ·7H 2 O, 20g of urea and 15g of 2-methylimidazole were dissolved in 300g of water, and refluxed at 100°C for 7 hours while stirring. A white precipitate formed and was washed once with 100 ml of water and three times with 50 ml of water. The filter cake was dried at 100°C for 6 hours and then activated for 12 hours at 130°C under vacuum (0.2 bar) to obtain 20.2 g of product;

[0053] N 2 The specific surface area is 876m 2 / g (as determined by the Langmuir method).

Embodiment 3

[0054] Embodiment 3: Synthesis of Zn-dimethylimidazole framework

[0055] 27g ZnNO 3 ·6H 2 O, dissolved in 150g of water; 12g of hexamethylenetetramine and 15g of 2-methylimidazole were dissolved in a mixture of 50g of water and 100g of methanol; then the zinc nitrate solution was mixed with the 2-methylimidazole solution and stirred for 20min until After mixing evenly, transfer to a 500ml autoclave and react at 120°C for 6 hours. Cool down naturally, filter the white precipitate, and then wash twice with 100ml of water. The filter cake was dried at 100°C for 6 hours, then activated by drying at 130°C under vacuum (0.2 bar) for 8 hours to obtain 22 g of product;

[0056] N 2 The specific surface area is 1346m 2 / g (as determined by the Langmuir method).

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Abstract

The invention relates to a preparation method of a porous metal organic skeleton material. The porous metal organic skeleton material comprises at least a metal ion and at least an organic compound that can be matched with the metal ion. The material can be prepared by dissolving metal compounds, organic ligand, and sustained-released alkali into a solvent and carrying out direct water (solvent) thermal synthesis at a certain temperature under a certain pressure so as to obtain the porous metal organic skeleton material. The operation of the provided preparation method is simple, the preparation method is suitable for massive industrial production and is suitable for the synthesis of porous metal organic skeleton membrane, and the provided porous metal organic skeleton material is used to absorb, separate, and store gas.

Description

technical field [0001] The invention belongs to the technical field of chemical material synthesis and application engineering, and in particular relates to a preparation method and application of a porous metal organic framework material. Background technique [0002] Porous metal-organic frameworks (Metal-organic Frameworks, MOFs), with specific pore structures, ultra-high specific surface areas, and finely adjustable surface structures, have been a research hotspot in the field of porous materials in the past decade. [0003] The research team represented by Professor Yaghi from the United States has successively published methods for the synthesis, pore size adjustment, and surface performance adjustment of novel structure MOFs in Science in recent years [Science, 2002, 295, 469; 2010, 330, 650; 2012, 336, 1018;]. At the same time, large international chemical companies represented by BASF SE in Germany have also disclosed a large number of preparation technologies for p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/58C07C51/41C07C57/15C07C63/307B01J20/22B01J20/28B01J20/30B01D53/02C10L3/10
CPCB01D53/02B01J20/223C07F1/08C07F3/06C07F5/069C07F15/065C10L3/10
Inventor 王树东孙天军胡江亮任新宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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