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Magnesium-based metal organic framework material for methane-nitrogen adsorption separation and preparation

A metal organic framework, nitrogen adsorption technology, applied in adsorption purification/separation, nitrogen purification/separation, separation methods, etc., can solve problems such as high cost and blockage

Inactive Publication Date: 2015-03-18
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Kuznicki et al. (Nature, 2001, 412 (6848), 720) described that ETS-4 can achieve methane molecular sieve through cation exchange and heat treatment. It is the most promising adjustable molecular sieve, but the cost is high. It is used in methane gas It is easy to be blocked by C2 and other substances during separation and concentration, and requires frequent activation

Method used

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  • Magnesium-based metal organic framework material for methane-nitrogen adsorption separation and preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] (1) Weigh 36.9g MgSO 4 ·7H 2 O and 15ml (99% formic acid) were dissolved in 850ml of DMF, slowly added 2.8g of ammonium fluoride while stirring continuously, and stirred for 20min until uniform to obtain a mixed solution; the mixed solution was transferred to a 1L Teflon liner The autoclave was tightly sealed, placed in an oven at 120°C for 12 hours, and cooled down to room temperature naturally. The precipitate was separated by centrifugation (10000rpm, 5min), washed three times with 80ml of ethanol, and then dried at 100°C for 6 hours to obtain a white powder.

[0049] (2) The white powder was impregnated with 100 ml of acetone for 12 hours, filtered, and activated at 170° C. under a vacuum of 100 mbar for 12 hours to form adsorbent A, which weighed 14.3 g.

[0050] For comparative experiments, adsorbent B was prepared according to the method described in BASF patent US2011178335A1.

[0051] The specific surface area determined by the Langmuir method of gained adso...

Embodiment 2

[0058] (1) Weigh 49.3g MgSO 4 ·7H 2 O was dissolved in 720ml DMF to form solution A; 11.2g triethylenediamine was dissolved in 50ml deionized water to form solution B; solution B was slowly added to solution A while stirring continuously to form a uniform mixed solution. Add 82ml (98% methyl formate) dropwise to the mixed solution at a constant speed, stir for 20 minutes until uniform, and obtain mixed solution C; transfer the mixed solution to a 1L autoclave with a Teflon liner and seal it tightly, place it at 100 ℃ oven reaction for 24 hours, naturally cooled to room temperature. The precipitate was separated by centrifugation (10000rpm, 5min), washed three times with 80ml of methanol, and then dried at 100°C for 6 hours to obtain a white powder.

[0059] (2) The white powder was impregnated with 100 ml of acetone for 12 hours, filtered, and activated at 160° C. under a vacuum of 100 mbar for 12 hours to form adsorbent C, which weighed 16.1 g.

[0060] The specific surfac...

Embodiment 3

[0064] (1) Weigh 36.9g MgSO 4 ·7H 2O, 22.5g D-tartaric acid is dissolved in 607.6ml methanol (98%), slowly adds 2.8g ammonium fluoride while stirring constantly, stirs 30min until uniform, obtains mixed solution; Seal tightly in a ethylene-lined 1L autoclave, place in an oven at 120°C for 36 hours, and cool down to room temperature naturally. The precipitate was filtered out, washed three times with 300 ml of deionized water, and then the filter cake was dried at 60° C. for 10 hours to obtain a milky white lump.

[0065] (2) The product was activated at 130° C. for 6 hours under a vacuum of 100 mbar to form adsorbent D, which weighed 23.6 g.

[0066] The specific surface area determined by the Langmuir method of the obtained adsorbent D is 208m 2 / g, the average pore diameter is 2.4nm;

[0067] The obtained adsorbent D is at 298K, between 0-1MPa (absolute atmospheric pressure), αCH 4 / N 2 =2.6-4.4;

[0068] CH of the obtained adsorbent D 4 The dynamic adsorption capaci...

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Abstract

The invention relates to a magnesium-based metal organic framework material for methane-nitrogen adsorption separation and a preparation method. The metal organic framework material is formed by coordination of at least one metal compound with at least one organic ligand to generate a framework material; the metal ions in the metal compound comprise one or more than one of Mg (II), Ni (II), Cu (II), Zn (II), Co (II), and Ca (II), and at least one metal ion is Mg (II); the organic ligand is a monodentate or polydentate organic compound of carboxylic acid or its derivatives. The invention also relates to an application of the porous magnesium-based organic framework material in methane-nitrogen adsorption separation.

Description

technical field [0001] The invention belongs to the design and preparation of novel adsorbents and the technical field of adsorption and separation of mixed gases, and in particular relates to a magnesium-based metal-organic framework material and its preparation for methane-nitrogen adsorption and separation. Background technique [0002] Energy and environmental issues are two basic issues closely related to sustainable development today. After entering the 21st century, the excessive dependence of the economy on energy has led to prominent environmental problems. The rapid growth of my country's economy has put forward a strong rigid demand for energy consumption. However, the current energy consumption pattern dominated by coal and oil has made my country's fragile natural environment overwhelmed. Methane is a high-quality fuel with large reserves in nature, high calorific value, and the highest H / C ratio. It is a cleaner energy source than coal and oil. In 2010, natura...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D53/02C01B21/04C07C7/12C07C9/04
CPCB01J20/226B01D53/047B01D2253/204B01D2256/245C01B21/0405C07C7/12C07C9/04
Inventor 王树东胡江亮孙天军任新宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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