Porous metal organic framework material based on transition metal cobalt and preparation method thereof

A technology of porous metals and organic frameworks, applied in separation methods, chemical instruments and methods, fuels, etc., can solve problems such as lack of research on MOFs materials, and achieve good application effects

Inactive Publication Date: 2013-03-13
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

[0011] So far, for CH 4 /N 2 Research on

Method used

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  • Porous metal organic framework material based on transition metal cobalt and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Embodiment 1: Synthesis of Co at high pressure 3 (BTC) 2

[0063] (1) Weigh 1.64g cobalt acetate (Co(CH 3 COO) 2 4H 2 O) and 0.80g trimesic acid (H 3 BTC) was dissolved in 60ml of absolute ethanol, and stirred for 30min until uniform to obtain a mixed solution;

[0064] (2) Transfer the mixed solution to a 150ml autoclave with a polytetrafluoroethylene liner, seal it tightly, place it in an oven at 150°C for 120h (5 days), and cool down naturally.

[0065] (3) Centrifuge (10000rpm, 5min) to separate the obtained solid;

[0066] (4) Wash the solid with water (4×25ml) and ethanol (2×25ml) respectively.

[0067] (5) The solid powder was dried at 110°C overnight to obtain 0.73 g of purple lumps.

[0068] N 2 The specific surface area is 109.04m 2 / g (determined by Langmuir method);

[0069] The obtained adsorbent is at 298K, between 0-1Mpa, CH 4 / N 2 The equilibrium adsorption separation factor is between 3.5-6, CO 2 / CH 4 The equilibrium adsorption separatio...

Embodiment 2

[0070] Example 2: Synthesis of CoBDC at high pressure

[0071] (1) Weigh 2.70g of cobalt acetate (Co(CH 3 COO) 2 4H 2 O) and 1.50g terephthalic acid (H 2 BDC) was dissolved in 60ml of DMF, stirred for 30min until uniform, to obtain a mixed solution;

[0072] (2) Transfer the mixed solution to a 150ml autoclave with a polytetrafluoroethylene liner, seal it tightly, place it in an oven at 140°C for 72h (3 days), and cool down naturally.

[0073] (3) Centrifuge (10000rpm, 5min) to separate the obtained solid;

[0074] (4) Wash the solid with water (2×50ml) and ethanol (50ml) respectively.

[0075] (5) The solid powder was dried at 110° C. for 12 hours to obtain 1.33 g of the product.

[0076] N 2 The specific surface area is 31.54m 2 / g (as determined by the Langmuir method).

[0077] The obtained adsorbent is at 298K, between 0-1Mpa, CH 4 / N 2 The equilibrium adsorption separation factor is between 3.5-5.5, CO 2 / CH 4 The equilibrium adsorption separation factor is ...

Embodiment 3

[0078] Embodiment 3: high pressure synthesis Co (bdc) (dabco) 0.5

[0079] (1) Weigh 1.25g cobalt acetate (Co(CH 3 COO)2 4H 2 O), 0.84g terephthalic acid (H 2 BDC) and 0.56g of triethylenediamine (DABCO) were dissolved in 60ml of DMF, stirred for 30min until uniform, and a mixed solution was obtained;

[0080] (2) Transfer the mixed solution to a 150ml autoclave lined with polytetrafluoroethylene, seal it tightly, place it in an oven at 120°C for 48 hours, and then cool down naturally.

[0081] (3) Centrifuge (10000rpm, 5min) to separate the obtained solid;

[0082] (4) The solid was washed with DMF (2×50ml) and methanol (2×50ml) respectively.

[0083] (5) The solid was dried overnight at 110°C to obtain 1.14 g of purple lumps.

[0084] N 2 The specific surface area is 830.12m 2 / g (as determined by the Langmuir method).

[0085] The obtained adsorbent is at 298K, between 0-1Mpa, CH 4 / N 2 The equilibrium adsorption separation factor is between 4-7, CO 2 / CH 4 The...

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Abstract

The invention relates to a porous metal organic framework material based on transition metal cobalt and a preparation method thereof. The metal organic framework material is a compound with supramolecular porous network structure and formed by self-assembly of metal ions and organic ligands through coordination complexation. The porous cobalt-based metal organic framework material contains one or more metal ions, and one or more organic ligands; and at least one of the metal ions is Co (II). The porous cobalt-based organic framework material has excellent selective adsorption on CH4 in a separation process of CH4 and N2; and the advantage of adsorption selectivity on CH4 is particularly evident under low pressure. The material is particularly suitable for development and recovery of oil field gas, coal bed methane and biogas.

Description

technical field [0001] The invention relates to the technical field of chemical material synthesis and mixed gas adsorption and separation engineering, in particular to a porous metal organic framework material based on transition metal cobalt and a preparation method thereof. Background technique [0002] The current energy and environmental problems are becoming more and more prominent. With the sharp increase in the world's energy consumption dominated by fossil fuels such as coal, oil and natural gas, serious environmental problems have been brought about, which have seriously affected the survival and development of all human beings. develop. As the cleanest fossil energy recognized in the world, natural gas is playing an increasingly important role in the energy consumption structure of various countries. With the depletion of conventional natural gas resources and the increasing difficulty of development, unconventional natural gas, mainly coalbed methane, shale gas,...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30B01D53/02C10L3/10
Inventor 王树东任新宇孙天军胡江亮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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