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A kind of preparation method of metal cluster-based crystalline porous material

A technology of metal clusters and porous materials, applied in chemical instruments and methods, improvement of process efficiency, and other chemical processes, can solve problems such as not being able to greatly improve the performance of COFs, and achieve improved framework stability, high stability, catalytic The effect of excellent performance

Active Publication Date: 2022-04-05
JINAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this inorganic-organic composite material, metal clusters as active sites can be evenly distributed on the framework of porous materials, which solves the difficulty in the current technology of introducing metals into COFs to make the metals evenly distributed in COFs. In the material, the performance of COFs cannot be greatly improved

Method used

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  • A kind of preparation method of metal cluster-based crystalline porous material
  • A kind of preparation method of metal cluster-based crystalline porous material
  • A kind of preparation method of metal cluster-based crystalline porous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) PzPhCHO-Cu 3 preparation of

[0049] Weigh 20 mg (0.1 mmol) of 4-(3,5-dimethyl-1H-pyrazol-4 base) benzaldehyde and 7.2 mg (0.05 mmol) of cuprous oxide into a 10 mL hard glass tube, add 4 mL of Water ethanol and 0.1mL pyridine, sealed tube with hydrogen-oxygen flame machine, put it into a constant temperature oven, raise the temperature from room temperature to 140°C within 10min, keep the temperature constant for 72h, and then drop it to room temperature at a cooling rate of -5°C / h. Get PzPhCHO-Cu 3 Colorless needle-like crystals. PzPhCHO-Cu 3 The yield was 72.3%.

[0050] (2) Preparation of metal cluster-based crystalline porous materials

[0051] 38.45mg PzPhCHO-Cu 3 and 9.75mg of 2,2′,2″-(benzene-1,3,5-triyl)triacetonitrile were added to a Schlenk bottle filled with 2mL of o-dichlorobenzene and n-butanol (volume ratio 1:1) mixed solvent Then add 0.1mL 4M NaOH solution, freeze the solution in the Schlenk bottle with liquid nitrogen, vacuum the gas in the bo...

Embodiment 2

[0053] (1) PzPhCHO-Ag 3 preparation of

[0054] Weigh 100 mg (0.5 mmol) of 4-(3,5-dimethyl-1H-pyrazol-4 base) benzaldehyde and 7.2 mg (0.5 mmol) of silver benzoate into a 50 mL hard glass bottle, add 5 mL of methanol , 12mLTHF and 0.5mL pyridine, stirred at room temperature in the dark for 6h to obtain PzPhCHO-Ag 3 White powder. PzPhCHO-Ag 3 The yield was 82.1%.

[0055] (2) Preparation of metal cluster-based crystalline porous materials

[0056] 46mg PzPhCHO-Ag 3 And 9.75mg 2,2′,2″-(benzene-1,3,5-triyl)triacetonitrile was added into a mixed solvent containing 2mL mesitylene and 1,4-dioxane (volume ratio 1:3) Then add 0.1mL 4M NaOH solution, freeze the solution in the Schlenk bottle with liquid nitrogen, vacuum the gas in the bottle, then seal the Schlenk bottle and thaw it in normal temperature water, repeat this three times , nitrogen protection, nitrogen protection, ultrasonic treatment for 30 minutes; then add a constant temperature oven, the temperature rose from r...

Embodiment 3

[0058] (1) PzPhCHO-Cu 3 preparation of

[0059] Weigh 20 mg (0.1 mmol) of 4-(3,5-dimethyl-1H-pyrazol-4 base) benzaldehyde and 7.2 mg (0.05 mmol) of cuprous oxide into a 10 mL hard glass tube, add 4 mL of Water ethanol and 0.1mL pyridine, sealed tube with hydrogen-oxygen flame machine, put it into a constant temperature oven, raise the temperature from room temperature to 140°C within 10min, keep the temperature constant for 72h, and then drop it to room temperature at a cooling rate of -5°C / h. Get PzPhCHO-Cu 3 Colorless needle-like crystals. PzPhCHO-Cu 3 The yield was 72.3%.

[0060] (2) Preparation of metal cluster-based crystalline porous materials

[0061] 38.45mg PzPhCHO-Cu 3 and 6.15mg of 2,4,6-trimethyl-1,3,5-triazine were added into the Schlenk bottle containing 2mL o-dichlorobenzene and n-butanol (volume ratio 1:1) mixed solvent, and then added 0.1mL 4M NaOH solution, freeze the solution in the Schlenk bottle with liquid nitrogen, vacuum the gas in the bottle, t...

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Abstract

The invention discloses a metal cluster-based crystalline porous material and a preparation method thereof. The metal cluster-based crystalline porous material contains an aldehyde group-containing ring trinuclear metal cluster precursor and an organic ligand. The preparation method is as follows: firstly, the precursor of ring trinuclear metal clusters containing aldehyde groups is prepared by solvothermal synthesis or diffusion method; then, the ring trinuclear metal clusters containing aldehyde groups The cluster precursors are linked with organic ligands to obtain metal cluster-based crystalline porous materials linked by carbon-carbon double bonds. In this inorganic-organic composite material, the metal clusters as active sites can be evenly distributed on the framework of the porous material, which solves the problem that it is difficult to make the metal evenly distributed in the current technology of introducing metal into COFs. In COF materials, it has broad application prospects for the limited performance improvement of COFs.

Description

technical field [0001] The invention belongs to the technical field of inorganic-organic composite materials, and in particular relates to a metal (cuprous or silver) cluster through a Knoevenagel condensation reaction (Knoevenagel Condensation reaction) to form a metal cluster base crystal connected by a carbon-carbon double bond A method for the preparation of porous materials. Background technique [0002] Metal-organic frameworks (MOFs) are a class of crystalline porous materials formed by self-assembly of organic ligands and metal ions (or clusters) through coordination bonds, which have the advantages of diverse structures, strong design, and high specific surface area. After more than 20 years of development, tens of thousands of MOFs have been reported. MOF materials have been widely used in the field of catalysis due to their multi-metal sites, but the problem of poor stability of MOF materials has always been the problem of their application. stumbling block. Cov...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J20/22C22B3/00
CPCC08G83/008C22B11/046B01J20/226Y02P10/20
Inventor 宁国宏李丹罗杰
Owner JINAN UNIVERSITY
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