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Supertetrahedron metal organic framework material as well as preparation method and application thereof

A metal-organic framework, supertetrahedral technology, used in separation methods, chemical instruments and methods, dispersed particle separation, etc.

Active Publication Date: 2020-12-25
FUJIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The purpose of this material is to provide an efficient and powerful window-space-oriented assembly strategy for the construction of ultra-microporous windows of ultratetrahedral-based mesoporous MOFs, to solve the problem of efficient separation of light hydrocarbon gases, and to design and synthesize functionalities for the future. Paving the way for high-density and high-connectivity materials

Method used

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  • Supertetrahedron metal organic framework material as well as preparation method and application thereof
  • Supertetrahedron metal organic framework material as well as preparation method and application thereof
  • Supertetrahedron metal organic framework material as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The preparation method of ST-sod-Co in ST-sod-MOFs comprises the following steps:

[0048] CoSO 4 ·7H 2 O (0.0633g, 0.225mmol), 2,4,6-tris(4-pyridyl)-1,3,5-triazine (0.0162g, 0.052mmol) and 1,3,5-benzenetricarboxylate (0.0324g, 0.154mmol) into a 20ml glass bottle; then drop into N,N-dimethylformamide (4mL) / methanol (1mL) solution; then add 200uL of HBF 4 (tetrafluoroboric acid, 50 wt% aqueous solution), sonicated for 30 min; finally, the mixture was sealed and heated to 110° C. for 10 days. After collection, DMF washing and vacuum drying, the target product red cubic crystal ST-sod-Co was obtained.

[0049] Refer to attached Figure 4 , ST-sod-Co at 77K for N 2 The results of adsorption measurements indicated that ST-sod-Co exhibited a reversible type I adsorption behavior with a stepwise N 2 Adsorption isotherm, which indicates the presence of mesoporous cages in the framework. The saturated adsorption capacity reaches 400cm 3 g -1 , BET surface area is 1310m ...

Embodiment 2

[0053] The preparation method of ST-sod-Ni in ST-sod-MOFs comprises the following steps:

[0054] First Ni(NO 3 ) 2 ·6H 2 O (0.1308g, 0.45mmol), 2,4,6-tris(4-pyridyl)-1,3,5-triazine (0.0310g, 0.10mmol) and 1,3,5-benzenetricarboxylate (0.0632g, 0.30mmol) into a 20ml glass bottle; then drop N,N-dimethylformamide (3mL) / N,N-dimethylacetamide (3mL) / methanol (1mL) solution; Then add 400uL of HSiF 6 (fluorosilicic acid, 25 wt% aqueous solution), sonicated for 30 min; finally, the mixture was sealed and heated to 125° C. for 7 days. After collection, DMA washing and vacuum drying, the target product green cubic crystal ST-sod-Ni was obtained.

[0055] Refer to attached Figure 4 , ST-sod-Ni at 77K for N 2 The results of adsorption measurements indicated that ST-sod-Ni exhibited a reversible type I adsorption behavior with a stepwise N 2 Adsorption isotherm, which indicates the presence of mesoporous cages in the framework. The saturated adsorption capacity reaches 400cm 3 g ...

Embodiment 3

[0059] The preparation method of ST-sod-Co / Ti in ST-sod-MOFs comprises the following steps:

[0060] CoCl 2 ·6H 2 O (0.0734g, 0.31mmol), titanium dichloride (0.0375g, 0.15mmol), 2,4,6-tris(4-pyridyl)-1,3,5-triazine (0.0310g, 0.10mmol) and 1,3,5-benzenetricarboxylate (0.0632g, 0.30mmol) into a 20ml glass bottle; then drop into N,N-dimethylformamide (3mL) / N,N-dimethyl Acetamide (3mL) / methanol (1mL) solution; then add 400uL of HSiF 6 (fluorosilicic acid, 35 wt% aqueous solution), sonicated for 30 min; finally, the mixture was sealed and heated to 140° C. for 3 days. After collection, DMA washing and vacuum drying, the target product red polyhedral crystal ST-sod-Co / Ti was obtained.

[0061] Refer to attached Figure 4 , ST-sod-Co / Ti at 77K for N 2 The results of adsorption measurements indicated that ST-sod-Co / Ti exhibited a reversible type I adsorption behavior with a stepwise N 2 Adsorption isotherm, which indicates the presence of mesoporous cages in the framework. The...

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Abstract

The invention discloses a supertetrahedron metal organic framework constructed based on a window-space-directed assembly strategy as well as a preparation method and application thereof. The novel window-space-directed assembly strategy is provided, a series of building units based on hypertetrahedron are designed and synthesized to construct a metal organic framework material ST-sod-MOFs with ultra-microporous quadrilateral windows and mesoporous sod cages in an angle sharing mode, and the structural general formula of the metal organic framework material is [M3(OH / O)(H2O / F)(btc)2(tpt)2 / 3], wherein M is a metal ion or a combination of two dissimilar metal ions, and is a single metal ion of magnesium, manganese, iron, cobalt, nickel, zinc, aluminum, scandium, gallium, indium and the like or a binary combination of titanium, vanadium, scandium, gallium and indium with one of iron, cobalt, nickel and magnesium. The metal organic framework material is a three-dimensional sod type networkframework formed by trinuclear metal ion cluster nodes and organic ligands through coordination bonds. ST-sod-Co / Ti not only has good thermal stability and relatively high acid and alkali resistance stability, but also shows good performance in the aspect of C2H2 / CO2 separation.

Description

technical field [0001] The invention belongs to the technical field of porous crystalline material preparation and gas adsorption and separation, and specifically relates to a supertetrahedral metal organic framework material, its preparation method and application. Background technique [0002] Metal-organic frameworks (MOFs) materials, also known as porous coordination polymers (Porous coordination polymers, PCPs), usually refer to the formation of metal ions or metal clusters and organic ligands through a self-assembly process with infinite periodicity. Crystalline materials with a network structure have both the characteristics of organic polymers and inorganic compounds. It has attracted ongoing attention due to its potential applications in gas storage and separation, heterogeneous catalysis, and drug delivery. [0003] The performance of MOFs is highly dependent on the resulting network topology, which is greatly influenced by the coordination geometry of metal nodes...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01D53/02
CPCC08G83/008B01D53/02B01D2253/204Y02C20/40Y02P20/151
Inventor 张磊李芳芳游建钧花能斌王乾廷陈文哲
Owner FUJIAN UNIV OF TECH
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