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High selectivity metal organic skeleton material and preparation method thereof

A metal-organic framework and high-selectivity technology, applied in organic chemistry, separation methods, copper organic compounds, etc., can solve the problems of physical and chemical properties that do not have selective adsorption and separation capabilities, achieve good hydrothermal stability, and shorten processing time , High adsorption effect

Inactive Publication Date: 2016-06-29
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The metal-organic framework material has a certain ability to store methane, but due to the pore size factor, it does not have a good selective adsorption and separation ability for mixed gases with little difference in physical and chemical properties.

Method used

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  • High selectivity metal organic skeleton material and preparation method thereof
  • High selectivity metal organic skeleton material and preparation method thereof
  • High selectivity metal organic skeleton material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1.02 mg of 2,7-bis(3,5-dibenzoic acid)-9-fluorenone, 8 mg of carbon nanotubes and 1.95 mg of Cu(NO 3 ) 2 2.5H 2 O was dissolved in 3 mL of a mixture of N,N'-dimethylformamide and deionized water with a volume ratio of 8:1, and stirred at room temperature for 30 min. Subsequently, 60 μL of nitric acid solution with a mass concentration of 70 wt % was added to the reaction bottle, and after uniform mixing, the airtight container was moved to an oven for crystallization at 60 °C for 72 h. Open the reaction bottle, filter twice with 10 mL of N,N'-dimethylformamide solution at 50°C, and then filter once with 15 mL of methanol solution; the obtained sample is vacuum-dried for 2 hours, and then filter once with the same volume of methanol solution , followed by drying at 80° C. for 2 h; after drying, the sample was transferred to a vacuum drying oven and dried at 100° C. for 2 h to obtain a metal-organic framework material A.

[0038] The determination of the structure of t...

Embodiment 2

[0040] In Example 1, 2,7-bis(3,5-dibenzoic acid)-9-fluorenone was reduced to 0.408 mg, and other reaction conditions and material composition remained unchanged, to obtain pure metal organic framework material B.

Embodiment 3

[0042] In Example 1, the mixed solution of N,N'-dimethylformamide and deionized water with a volume ratio of 8:1 was increased to 6mL, and other reaction conditions and material composition remained unchanged to obtain a pure metal organic framework Material C.

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Abstract

The invention discloses a high selectivity metal organic skeleton material and a preparation method thereof. The preparation method comprises the following steps: adding an organic ligand namely 2,7-bis(3,5-dibenzoic acid)-9-fluorenone, carbon nanotubes, and a copper source into an amine solvent and deionized water, evenly stirring in an enclosed container; then adding a nitric acid solution, evenly mixing, transferring the enclosed container to a baking oven to carry out crystallization; subjecting the obtained blue-green hexagonal crystals to multi-stage solvent extraction and solubilization treatments with N,N'-dimethyl formamide and methanol in sequence, and performing vacuum drying to obtain the pure metal organic skeleton material. The metal organic skeleton material comprises a secondary structural unit, which is formed through coordination between a Cu2(COO)4 structural unit and oxygen atoms of carboxylic acid. The secondary structural units are linked to each other so as to form a three dimensional channel structure. The provided high selectivity metal organic skeleton material is especially suitable for selective adsorption separation of mixed gas (acetylene, ethylene, and ethane), the operation conditions are mild, and the service life is long.

Description

technical field [0001] The invention relates to a metal-organic framework material and a preparation method thereof, in particular to a copper-based metal-organic framework material doped with carbon nanotubes for selective adsorption and separation of methane and a preparation method thereof. Background technique [0002] Methane is the main component of natural gas, coal bed methane, shale gas and biogas, and is a clean, environmentally friendly, economical and affordable energy gas resource. In actual use, it often coexists with acetylene, ethylene, and ethane. Highly selective adsorption and separation of methane helps to increase the storage density and combustion calorific value of fossil gas resources such as natural gas on the one hand, and on the other hand to increase the additional higher value C 2 The utilization rate of gas resources. Therefore, it is of great significance to develop new methane adsorption separation materials with high selectivity and low ope...

Claims

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Application Information

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IPC IPC(8): C07F1/08B01J20/22B01D53/02C07C7/12C07C9/04C07C9/06C07C11/04C07C11/24
CPCY02P20/50
Inventor 赵亮王刚方向晨
Owner CHINA PETROLEUM & CHEM CORP
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