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Metal-organic framework material for methane adsorption and storage and preparation method thereof

A metal-organic framework, methane technology, applied in chemical instruments and methods, through adsorption, organic chemistry, etc., to achieve the effect of increasing adsorption and storage capacity, high adsorption and storage capacity, and mild reaction conditions

Active Publication Date: 2013-05-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Relatively speaking, there are relatively few reports on the introduction of functional groups that do not participate in coordination when designing organic ligands for MOFs materials that are used to adsorb and store methane gas.

Method used

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  • Metal-organic framework material for methane adsorption and storage and preparation method thereof
  • Metal-organic framework material for methane adsorption and storage and preparation method thereof
  • Metal-organic framework material for methane adsorption and storage and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 15 mg of 5,5'-(pyridine-2,5-diyl)-isophthalic acid and 30 mg of Cu(NO 3 ) 2 (H 2 O) 2.5 dissolved in N,N-dimethylformamide (DMF), acetonitrile, H 2 O (8mL, volume ratio 6:1:1) mixed solvent, then added dropwise 50μL of concentrated hydrochloric acid, placed in a 25ml seed bottle, sealed and placed in an oven at 80°C for 72 hours, taken out and used The DMF was washed repeatedly, and the metal organic framework material was obtained after drying. Its structure was determined by Oxford Xcalibur Gemini Ultra single crystal diffractometer, and the results showed that the structural formula of the metal organic framework material is [Cu 2 (C 21 h 9 NO 8 )(H 2 O) 2 ](DMF) 4 (H 2 O) 6 , the molecular formula is C 33 h 53 N 5 o 20 Cu 2 , belongs to the hexagonal crystal system, the space group is R-3m, the unit cell parameters are a=18.8163?, b=18.8163?, c=38.079?, α=β=90°, γ=120°, and the unit cell volume is 11675.7? 3 , Z=3, D c =0.725g / cm 3 . The single...

Embodiment 2

[0024] 20mg of 5,5'-(4-picoline-2,5-diyl)-isophthalic acid and 40mg of ZnCl 2 (H 2 O) 2 Dissolve it in 8mL of N,N-dimethylacetamide (DMA) solution, put it in a 25ml strain bottle, seal it and place it in an oven at 65°C for 72 hours, take it out, wash it repeatedly with DMA, and dry it Afterwards, metal-organic framework materials are obtained.

[0025] The metal-organic framework material obtained was solvent-exchanged with acetone, and the solvent was exchanged every 15 minutes for ten times, and then activated at 0°C for 36 hours under vacuum conditions, and then activated at 100°C for 12 hours under vacuum conditions to obtain Metal-organic frameworks with unsaturated metal sites and open channels. The gas adsorption data was collected using the Micromeritics ASAP 2020 specific surface area analyzer, whose specific surface area and Langmuir adsorption surface area were over 2200 m 2 g -1 and 3300 m 2 g -1 , the pore volume is greater than 1.300 cm 3 g -1 . Reach...

Embodiment 3

[0027] 25 mg of 5,5'-(3,4,6-trifluoropyridine-2,5-diyl)-isophthalic acid and 50 mg of Cd(ClO 4 ) 2 (H 2 O) 6 Dissolve in a mixed solvent of N,N-diethylacetamide (DEF) and acetonitrile (8mL, volume ratio 6:2), place in a 25ml strain bottle, seal and place in an oven at 90°C for 24 After taking it out, it was washed repeatedly with DEF, and the metal organic framework material was obtained after drying.

[0028] The metal-organic framework material obtained was solvent-exchanged with acetone, and the solvent was exchanged every 15 minutes for ten times, and then activated at 0°C for 36 hours under vacuum conditions, and then activated at 100°C for 12 hours under vacuum conditions to obtain Metal-organic frameworks with unsaturated metal sites and open channels. Gas adsorption data was collected using the Micromeritics ASAP 2020 specific surface area analyzer tester, whose specific surface area and Langmuir adsorption surface area were over 2500m 2 g -1 and 3500 m 2 g -1...

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Abstract

The invention discloses a metal-organic framework material for methane adsorption and storage and a preparation method thereof. The metal-organic framework material is of a three-dimensional network structure formed by transition metal ions, an organic ligand, namely, 5,5'-(pyridine-2,5-diyl)-isophthalic acid, and derivatives of the ligand through coordinate bonds or intermolecular forces. The transition metal ions are preferentially selected from bivalent ions of copper, zinc, cobalt, nickel, cadmium and manganese. The metal-organic framework material is higher in specific surface area and pore volume and good in thermal stability. Pyridine, fluorine, methyl, amino, methoxy, hydroxyl, nitro and other functional groups which do not participate in coordination are introduced into the organic ligand used in the material, can effectively improve the capacity of methane adsorption and storage. The metal-organic framework material is simple in preparation process and low in cost, can be used repeatedly, has high capacity of methane adsorption and storage under variable-temperature and variable-pressure conditions, and is expected to be used as a novel high-efficiency methane adsorption and storage material.

Description

technical field [0001] The invention relates to a metal organic framework material for methane adsorption and storage and a preparation method thereof, belonging to the technical field of metal organic framework materials. Background technique [0002] Methane is a hydrocarbon with the chemical formula CH 4 , which is widely distributed in nature and is the main component of natural gas, biogas, oilfield gas and coal mine tunnel gas. Compared with other petroleum fuel gases, methane gas has a higher H / C ratio, so it is more suitable for use as combustion gas. Clean and reliable. At the same time, methane gas is also an important chemical raw material, which is widely used as a raw material for the production of hydrogen, carbon black, carbon monoxide, acetylene, hydrocyanic acid and formaldehyde. However, the problems of methane gas storage and transportation have become the main obstacles limiting its wide application. There are several ways to store methane gas, such as...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C07D213/55C07D213/73C07D213/61C07D213/68
CPCY02C10/08Y02C20/40
Inventor 钱国栋饶兴堂蔡建锋崔元靖杨雨王智宇
Owner ZHEJIANG UNIV
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