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A metal-organic framework material based on low-symmetry tetradentate pyrazole ligand Ni and its preparation method

A technology of organic framework and tetradentate pyrazole, which is applied in the field of metal-organic framework and its preparation based on the new low-symmetry tetradentate pyrazole ligand Ni, and metal-organic coordination polymer materials, achieving the effect of novel structure

Inactive Publication Date: 2018-07-31
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, most of the pyrazole ligands used for the synthesis of metal-organic frameworks are highly symmetrical dipyrazole or tripyrazole ligands, and there are relatively few studies on the synthesis of metal-organic frameworks using asymmetric tetrapyrazole ligands.

Method used

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  • A metal-organic framework material based on low-symmetry tetradentate pyrazole ligand Ni and its preparation method
  • A metal-organic framework material based on low-symmetry tetradentate pyrazole ligand Ni and its preparation method
  • A metal-organic framework material based on low-symmetry tetradentate pyrazole ligand Ni and its preparation method

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Experimental program
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Effect test

Embodiment 1

[0029] First, carbazole reacts with halogen Br to obtain 1,3,6,8-tetrabromo-9H-carbazole; 5.00g (10.36mmol) 1,3,6,8-tetrabromo-9H-carbazole, g (82.85mmol) 1-(4-methoxybenzyl)-pyrazole borate, 12.59g (82.85mmol) cesium fluoride, 0.60g (0.517mmol) tetrakistriphenylphosphine palladium, 320mL ethylene glycol di Methyl ether was added into a 500 mL three-necked bottle, sealed, vacuumed, protected by nitrogen, and reacted at 100°C for 24 hours. After the reaction stopped, it was extracted with dichloromethane, washed with water, dried over anhydrous sodium sulfate, filtered, distilled under reduced pressure, separated and purified by silica gel column chromatography to obtain 1,3,6,8-tetra(1-(4- Methoxybenzyl)-1H-pyrazol-4-yl)-9H-carbazole 6.85g, yield 72%. 1H NMR (400MHz, DMSO-d 6 )δ3.94(s,12H),5.56(s,8H),6.89(d,8H),7.15(d,8H),7.88(d,2H),8.18(m,2H),8.32(m,6H ), 8.57(s,2H), 9.77(s,1H).

Embodiment 2

[0031] Add 6.85g 1,3,6,8-tetrakis(1-(4-methoxybenzyl)-1H-pyrazol-4-yl)-9H-carbazole and 200mL trifluoroacetic acid into a 500mL three-necked flask , after 24 hours of reaction under reflux conditions. After the reaction stopped, add 100mL deionized water after vacuum distillation, add ammonia water drop by drop until there is no precipitation at the bottom, and suction filter to obtain 1,3,6,8-tetrakis(1H-pyrazol-4-yl)-9H-carba azole. 1 HNMR (400MHz, DMSO-d 6 )δ7.89(d,2H)8.14(d,2H)8.36(m,6H)8.56(s,2H)9.77(s,1H)12.97(s,2H)13.19(s,2H)

Embodiment 3

[0033] The organic ligand CTP (0.01 mmol) and nickel chloride (0.03 mmol) were mixed uniformly in a mixed solution of 1 mL of N,N-dimethylformamide, 1 mL of acetonitrile and 0.4 mL of deionized water, and sealed into a vial. Crystals of the metal-organic framework were obtained via thermal reaction at 65°C for 48 hours.

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Abstract

The invention belongs to the technical field of crystalline materials and discloses a low-symmetry tetradentate pyrazole ligand Ni based metal-organic framework material and a preparation method thereof.A chemical formula of the low-symmetry tetradentate pyrazole ligand Ni based metal-organic framework material is [Ni(CTP)], and CTP refers to an organic ligand 1,3,6,8-tetra(-1H-pyrazolyl-4-yl)-9H-pyrazole.The metal-organic framework material is synthesized by that under closed conditions, the 1,3,6,8-tetra(-1H-pyrazolyl-4-yl)-9H-pyrazole is in thermal reaction with nickel chloride in a mixed solution of N,N-dimethylformamide, acetonitrile and water to obtain metal-organic framework crystals.The low-symmetry tetradentate pyrazole ligand Ni based metal-organic framework material has an application potential in gas adsorption and storage.

Description

technical field [0001] The invention belongs to the technical field of crystalline materials, and the technology relates to metal-organic coordination polymer materials, in particular to a metal-organic framework based on novel low-symmetry tetradentate pyrazole ligand Ni and a preparation method thereof. Background technique [0002] Metal-organic frameworks (MOFs) have been widely studied by researchers because of their potential applications in gas adsorption and storage, catalysis, fluorescence, electrochemistry, etc., as well as their fascinating structures and diverse topological configurations. s concern. Metal-organic frameworks are constructed by metal ions or metal clusters and organic ligands through coordination bonds. The complex and diverse framework structures of MOFs are mainly due to the diverse structures of organic ligands, rich coordination modes and metal Various coordination geometries of ions. However, when the coordination numbers and geometric conf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D403/14C07F15/04C08G83/00
CPCC07D403/14C07F15/045C08G83/00
Inventor 李建荣张永正谢亚勃何涛
Owner BEIJING UNIV OF TECH
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