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

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

Inactive Publication Date: 2014-12-10
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 accuracy is limited by the technical means, its wide pore size distribution, uncontrollable, complex surface functional groups, resulting in the separation efficiency can not be further enhanced

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
Effect test

Embodiment 1

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

[0036] By measuring the breakthrough curve of components i and j in the mixed gas, the adsorption amount of eac...

Embodiment 2

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

[0043] Comparative 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 under stirring at 100°C for 8 hours . The blue precipitate was filtered off and washed with 5 x 120 ml methanol. Dry at 75°C and vacuum...

Embodiment 3

[0049] Weigh 30g of copper acetate, 21g of trimesic acid and dissolve in 500ml of ethanol water (volume ratio 1:1), stir to form a uniform mixture. Transfer the mixed solution into a PTFE-lined 1L reaction kettle, continue the reaction at 110°C for 4h, then gradually cool to room temperature, then gradually cool to room temperature, filter, wash twice with 75ml ethanol, and remove the precipitate at 80°C C dried for 6 hours to obtain blue crystals. After drying, 29 g of the obtained product was pulverized, and 2% graphite and 4% polyvinylpyrrolidone were added to mix evenly. After molding, the adsorbent D was formed after vacuum activation at 130° C. for 4 hours.

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

[0051] The obtained adsorbent D is at 298K, between 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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Patent Type & Authority Patents(China)
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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