Porphyrin-based metal organic framework material for CO2 cyclization catalytic reaction and preparation method thereof

A catalytic reaction and organic framework technology, applied in the field of nanomaterials, can solve the problems of loss of activity and agglomeration, and achieve the effects of high reusability, strong stability and high catalytic activity

Active Publication Date: 2019-07-12
DALIAN NATIONALITIES UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the application process of such compounds, there is a problem of agglomeration and loss of activity

Method used

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  • Porphyrin-based metal organic framework material for CO2 cyclization catalytic reaction and preparation method thereof
  • Porphyrin-based metal organic framework material for CO2 cyclization catalytic reaction and preparation method thereof
  • Porphyrin-based metal organic framework material for CO2 cyclization catalytic reaction and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Synthesis of flower-like PCN-222

[0025] Add 20mg ZrCl in 4mL DMF 4 ·6H 2 O, 100 μL triethylamine, 480 μL glacial acetic acid, and 100 μL HO 2 O, after ultrasonic dispersion for 5 min, add 20 mg of Ni-TCPP to the above solution, and stir magnetically for 10 min at room temperature. The resulting homogeneous solution was transferred to a 24 mL Teflon-lined stainless steel autoclave and then heated at 130 °C for 12 h. After cooling to room temperature, it was separated by centrifugation at 8000 rpm for 8 minutes and further purified several times with ethanol.

Embodiment 2

[0033] PCN-222 activation process

[0034] The synthesized sample (~100 mg) and 1.5 mL of 8M HCl were added to 40 mL of DMF, and the DMF suspension was stirred at 120 °C for 12 h to remove unreacted starting ligands, inorganic substances and conditioning reagents. Subsequently, the extract was decanted carefully and the product was dispersed in fresh acetone for 24 hours to exchange and remove DMF. After removing acetone by centrifugation, the samples were activated by vacuum drying at 120 °C for 24 hours. Then the active samples were used for XRD, BET, SEM, TEM characterization and catalytic reaction test.

Embodiment 3

[0036] Cyclization assay

[0037] The PCN-222 with different morphology prepared in Example 1 and Comparative Example 1-2 was selected for CO 2 The cyclization reaction was measured and compared. The flower-shaped PCN-222 was subjected to repeated utilization experiments.

[0038] Dissolve 20mg of rod-shaped PCN-222 and 281mg of TABA in 2ml of styrene oxide, and pass through CO 2, placed in an 80°C oil bath for 20h. Take 50 μL of the reacted solution, dilute it in 1 mL of ethyl acetate, centrifuge, take the supernatant for gas chromatography analysis, and calculate the yield.

[0039] Dissolve 20mg of hexagonal PCN-222 and 281mg of TABA in 2ml of styrene oxide, and pass through CO 2 , placed in an oil bath at 80°C for 20 hours. Take 50 μL of the reacted solution, dilute it in 1 mL of ethyl acetate, centrifuge, take the supernatant for gas chromatography analysis, and calculate the yield.

[0040] Dissolve 20 mg of flower-like PCN-222 and 281 mg of TABA in 2 mL of styrene...

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Abstract

The invention belongs to the technical field of nano materials, and particularly relates to a porphyrin-based metal organic framework material for flower-like morphology of a CO2 cyclization catalyticreaction and a preparation method thereof. The method ultrasonically disperses ZrCl4 6H2O, triethylamine, glacial acetic acid, Ni-TCPP and H2O in DMF, conducts magnetic stirring, conducts heating ina stainless steel high-pressure autoclave at 0-200 DEG C for 1-20 hours, and conducts separating and purifying to obtain a flower-like porphyrin MOF catalyst; the catalyst prepared by the above methodexhibits high catalytic activity and high recyclability on the CO2 cyclization reaction.

Description

technical field [0001] The invention belongs to the technical field of nanomaterials, in particular to a 2 Porphyrin-based metal-organic framework material for cyclization catalytic reaction and preparation method thereof. Background technique [0002] Porphyrin compounds have important application value in the fields of catalysis, sensing and biomedicine. However, during the application process, such compounds have the problem of agglomeration and loss of activity. Metal-organic frameworks (MOFs) use organic ligands as scaffolds, metal ions or metal clusters as nodes, and form a three-dimensional periodic network structure porous material with regular nanopore structure through self-assembly. Compared with other porous materials, MOFs materials have Large specific surface area and high porosity, regular and controllable pore structure, easy functionalization of skeleton metal ions and organic ligands, so it has potential applications in the fields of heterogeneous catalys...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07D317/36
CPCB01J31/1691B01J31/183C07D317/36B01J2531/025B01J2531/48
Inventor 张艳梅张祥
Owner DALIAN NATIONALITIES UNIVERSITY
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