Hydrothermally stable column cage type metal organic framework material as well as preparation method and application thereof

A metal-organic framework and hydrothermally stable technology, applied in organic chemistry, separation methods, alkali metal compounds, etc., can solve the problems of inability to achieve separation and purification, low adsorption capacity, etc., and achieve good hydrothermal stability and circulation, Ultra-high adsorption capacity, high-efficiency separation effect

Inactive Publication Date: 2022-03-15
ZHEJIANG NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Pillar anions such as polyfluorinated anions can form strong hydrogen bond interactions with alkynes, so that such a structure can obtain high selectivity for the separation of alkynes and alkenes, but the adsorption capacity is often not high, and efficient separation and purification cannot be achieved.

Method used

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  • Hydrothermally stable column cage type metal organic framework material as well as preparation method and application thereof
  • Hydrothermally stable column cage type metal organic framework material as well as preparation method and application thereof
  • Hydrothermally stable column cage type metal organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] In a 50mL round bottom flask, 241.6mg (1mmol) of Cu(NO 3 ) 2 ·3H 2 O and 197.9 mg (1 mmol) of (NH 4 ) 2 TiF 6 Dissolve in 14mL of water. In another 50 mL round bottom flask, 331.05 mg (1.3 mmol) of tris(4-pyridyl)amine (L1) was dissolved in 30 mL of methanol. The methanol solution was added dropwise to the aqueous solution, and stirred at 30° C. for 48 hours to obtain a purple solid precipitate, which was filtered and washed with methanol. Soak the above solid in anhydrous methanol, replace anhydrous methanol every six hours, and replace more than 3 times in total to remove water molecules in the pores of the material, and then vacuum activate at 120°C for 10 hours to obtain a column for gas separation Cage metal-organic frameworks (CuTiF 6 ) 3 (L1) 4 .

[0058] figure 2 Yes (CuTiF 6 ) 3 (L1) 4 Schematic diagram of the crystal structure of , in which copper coordinates to four different pyridine rings in the horizontal direction, and then extends infinite...

Embodiment 2

[0063] In a 50mL round bottom flask, 277.7mg (1mmol) of CuSiF 6 Dissolve in 14mL of water. In another 50 mL round bottom flask, 331.05 mg (1.3 mmol) of tris(4-pyridyl)amine (L1) was dissolved in 30 mL of methanol. The methanol solution was added dropwise to the aqueous solution, and stirred at 30° C. for 48 hours to obtain a purple-red solid precipitate, which was filtered and washed with methanol. Soak the above solid in anhydrous methanol, replace anhydrous methanol every six hours, and replace more than 3 times in total to remove water molecules in the pores of the material, and then vacuum activate at 120°C for 10 hours to obtain a column for gas separation Cage metal-organic frameworks (CuSiF 6 ) 3 (L1) 4 .

[0064] The activated material was measured at 278K, 298K, and 308K for the single-component adsorption curves of acetylene, ethylene, propyne, and propylene, and the results are as follows: Figure 5-8 shown. Then, based on the ideal adsorption solution theory...

Embodiment 3

[0067] In a 50 mL round bottom flask, 339.4 mg (1 mmol) of CuNbOF 5 Dissolve in 14mL of water. In another 50 mL round bottom flask, 331.05 mg (1.3 mmol) of tris(4-pyridyl)amine (L1) was dissolved in 30 mL of methanol. The methanol solution was added dropwise to the aqueous solution, and stirred at 30° C. for 48 hours to obtain a blue solid precipitate, which was filtered and washed with methanol. Soak the above solid in anhydrous methanol, replace anhydrous methanol every six hours, and replace more than 6 times in total to remove water molecules in the pores of the material, and then vacuum activate at 120°C for 24 hours to obtain a column for gas separation Cage metal-organic frameworks (CuNbOF 5 ) 3 (L1) 4 .

[0068] The activated materials were measured at 278K, 298K, and 308K for the single-component adsorption curves of acetylene, ethylene, propyne, and propylene, and then calculated based on the ideal adsorption solution theory (IAST) and adsorption data fitting. ...

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Abstract

The invention discloses a hydro-thermal stable column cage type metal organic framework material, a preparation method thereof and application of the hydro-thermal stable column cage type metal organic framework material in the field of selective adsorption separation of gas. The column cage type metal organic framework material is formed by self-assembly of metal ions M, nonlinear multidentate nitrogen-containing ligands L and high-coordination-number inorganic anions through coordination bonds. The column cage type metal organic framework material disclosed by the invention has good hydrothermal stability and cyclicity, and can be used for high-selectivity adsorption separation of acetylene / ethylene, propyne / propylene and other alkyne olefins.

Description

technical field [0001] The invention relates to the field of synthesis and gas adsorption of porous materials, in particular to a hydrothermally stable column cage metal organic framework material and its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs) are a class of framework materials with a porous structure formed by the assembly of metal ions or clusters and organic ligands through coordination bonds. [0003] Metal-organic framework materials have become the most potential choice in the field of gas storage and separation due to their tunable pore structure and pore surface environment. [0004] Anionic pillared ordered porous materials are a class of metal-organic frameworks assembled by coordination of inorganic anions, metal ions and organic nitrogen-containing ligands. [0005] Anionic pillared ordered porous materials often use linear bidentate nitrogen-containing ligands. The classic structure is: the metal first ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01D53/02B01J20/28B01J20/30C07C7/12C07C11/06C07C11/04
CPCB01J20/226B01J20/28042B01D53/02C07C7/12B01D2256/24C07C11/06C07C11/04
Inventor 张袁斌姜芸佳汪玲瑶
Owner ZHEJIANG NORMAL UNIVERSITY
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