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

A metal organic framework, adsorption separation technology, applied in separation methods, dispersed particle separation, chemical instruments and methods, etc., can solve problems such as uncontrollable, complex surface functional groups, and separation efficiency cannot be further enhanced.

Inactive Publication Date: 2013-03-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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Problems solved by technology

Years of research results have shown that super-activated carbon with a super-abundant internal pore structure strengthens the CH 4 -N 2 The adsorption separation efficiency; but its control

Method used

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

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Experimental program
Comparison scheme
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Example Embodiment

[0034] Example 1:

[0035] Weigh 131.4g 2-methylimidazole (2-mIM) and dissolve it in 830ml deionized water to form solution A; 57.5g ZnSO 4 ·7H 2 O was dissolved in 250 ml of deionized water to form solution B. While stirring continuously, add solution B to solution A to form a homogeneous mixture. Add 48 g of triethylamine to 50 ml of methanol and add it to the mixed solution under stirring to form a mixed solution C. Transfer the mixed solution C into a 2L reactor lined with polytetrafluoroethylene, continue the reaction at 100°C for 2h, then gradually cool to room temperature, filter, wash with deionized water 3 times, and dry the precipitate at 105°C Slightly yellow crystals were obtained in 4 hours. After drying, 45 g of the product is added, 1% graphite and 3% polyvinylpyrrolidone are added and mixed uniformly. After molding, it is vacuum activated at 130°C for 4 hours to form adsorbent A.

[0036] By measuring the penetration curves of components i and j in the mixed gas,...

Example Embodiment

[0041] Example 2:

[0042] Weigh 70.2g copper acetate (Cu(CH 3 OO) 2 .H 2 O), 41.2g trimellitic acid is dissolved in 500ml DMF and stirred to form a homogeneous mixture. Under normal pressure and stirring, the reaction was continued for 8 hours at 110°C, then gradually cooled to room temperature, filtered, washed twice with 200ml methanol, and the precipitate was dried at 80°C for 6 hours to obtain dark blue crystals. 60 g of the product obtained after drying, pulverized, 2% graphite and 4% polyvinylpyrrolidone are added and mixed uniformly, and after molding, it is vacuum activated at 180°C for 8 hours to form adsorbent B.

[0043] For comparison test, according to the method described in BASF patent CN101384537A: 12.2g of 1,3,5-BTC and 13.9g of anhydrous copper sulfate were suspended in 275g of ethylene glycol, and kept at 100°C under stirring for 8 hours . The blue precipitate was filtered and washed with 5 x 120 ml methanol. After drying at 75°C and vacuum (0.2bar) for 24 ho...

Example Embodiment

[0048] Example 3:

[0049] Weigh 30 g of copper acetate and 21 g of trimellitic acid in 500 ml of ethanol water (volume ratio 1:1), and stir to form a uniform mixture. The mixed solution was transferred to a 1L reactor lined with polytetrafluoroethylene. The reaction was continued at 110°C for 4h, then gradually cooled to room temperature, then gradually cooled to room temperature, filtered, washed twice with 75ml ethanol, and the precipitate was heated at 80°C. Dry for 6 hours at C to obtain blue crystals. 29 g of the product obtained after drying, pulverized, 2% graphite and 4% polyvinylpyrrolidone were added and mixed uniformly, and after forming, it was vacuum activated at 130°C for 4 hours to form adsorbent D.

[0050] N of the obtained adsorbent D 2 The specific surface area (Langmuir method) is 1982m 2 / g, average pore diameter 0.7nm;

[0051] The obtained adsorbent D is between 298K and 0-1Mpa,

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Abstract

The invention relates to a metal-organic framework material for methane adsorption separation and a preparation method thereof. The metal organic framework material is prepared by reaction of at least a metal compound and at least one organic ligand, wherein the metal is one or more selected from Li, Mg, Al, Fe, Co, Ni, Cu, Zn, Mn, Zr, La and Sm, and the organic ligand is one or more selected from single or multidentate organic compounds containing nitrogen, oxygen or sulfur atom. The material has advantages of simple preparation process, high yield, easily available raw materials, mild reaction conditions; besides, the material has stable self properties and porous structure, and is especially suitable for separation of low-quality methane and purification process of high-concentration methane.

Description

technical field [0001] The invention relates to the design and preparation of novel adsorbents and the technical field of adsorption and separation engineering of mixed gases, in particular to a novel metal-organic framework material for adsorption and separation of methane and a preparation method thereof. Background technique [0002] As a low-carbon, efficient and clean energy and chemical raw material, the global demand for natural gas is expected to continue to rise at a rate of 1.7% in the next ten years, while the growth rate of demand in my country in the next ten years will be far greater than the average level. In 2011, my country's natural gas consumption was 130 billion cubic meters, and its dependence on foreign countries exceeded 20%. It is estimated that by 2015, my country's natural gas consumption will exceed 200 billion cubic meters, which shows that the contradiction between natural gas supply and demand in my country will become increasingly prominent. Se...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D53/02
Inventor 王树东孙天军胡江亮任新宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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