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An iron-based double-ligand metal-organic framework material that preferentially adsorbs ethane and its preparation method and application

A metal organic framework, preferential adsorption technology, applied in separation methods, chemical instruments and methods, gas treatment, etc., can solve the problems of poor ethane/ethylene adsorption selectivity, easy structure collapse, low ethane ethylene adsorption capacity, etc. Good water vapor stability and efficient separation

Active Publication Date: 2020-05-22
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Choi et al reported an activated carbon that preferentially adsorbs ethane [B.-U. Choi, D.-K. Choi, Y.-W. Lee, B.-K. Lee, S.-H. Kim, Journal of Chemical & Engineering Data 2003, 48 , 603-607.], at 30℃ and 100 kPa, the adsorption capacities for ethylene and ethane are 2.84 and 2.18 mmol / g, respectively, but the material has a low adsorption capacity for ethane and ethylene and for ethane / The problem of poor selectivity of ethylene adsorption
Liang et al found that Ni(bdc)(ted) 0.5 exhibited preferential adsorption of ethane [W. Liang, F.Xu, X. Zhou, J. Xiao, Q. Xia, Y. Li, Z. Li, Chemical Engineering Science 2016, 148 , 275-281.], at 25℃ and 100 kPa, the adsorption capacities for ethylene and ethane are 3.4 and 5.0mmol / g, respectively, and the adsorption selectivity is 1.85, but the structure of this material is easy to collapse when exposed to air

Method used

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  • An iron-based double-ligand metal-organic framework material that preferentially adsorbs ethane and its preparation method and application
  • An iron-based double-ligand metal-organic framework material that preferentially adsorbs ethane and its preparation method and application
  • An iron-based double-ligand metal-organic framework material that preferentially adsorbs ethane and its preparation method and application

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Experimental program
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Effect test

Embodiment 1

[0034] (1) Synthesis of iron clusters: 25.4262 g of anhydrous sodium acetate and 8.08 g of Fe(NO 3 ) 3 9H 2 O was dissolved in 50mL water respectively to obtain sodium acetate solution and ferric nitrate solution; then the sodium acetate solution was dropped dropwise into the ferric nitrate solution, and stirred for 12 hours to form a suspension; then the suspension was suction filtered to obtain a reddish-brown solid, and washed with 50 mL of deionized water and 50 mL of ethanol in turn, and finally put the product in a vacuum oven at 70 °C for 12 h at constant temperature to obtain iron clusters [Fe 3 (CH 3 COO) 6 ].

[0035] (2) Synthesis of iron-based double-ligand metal-organic framework materials: 60 mg terephthalic acid and 33 mg triethylenediamine were dissolved in 5 mL DMF to form a mixed solution; 10 1 mL of DMF solution in which 242 mg of iron clusters were dissolved was added dropwise to 1.525 mg of glacial acetic acid, and stirred for 30 min until the mixture...

Embodiment 2

[0037] (1) Synthesis of iron clusters: 25.4262 g of anhydrous sodium acetate and 8.08 g of Fe(NO 3 ) 3 9H 2 O was dissolved in 50mL water respectively to obtain sodium acetate solution and ferric nitrate solution; then the sodium acetate solution was dropped dropwise into the ferric nitrate solution, and stirred for 12 hours to form a suspension; then the suspension was suction filtered to obtain a reddish-brown solid, and washed with 50 mL of deionized water and 50 mL of ethanol in turn, and finally put the product in a vacuum oven at 70 °C for 12 h at constant temperature to obtain iron clusters [Fe 3 (CH 3 COO) 6 ].

[0038] (2) Synthesis of iron-based double-ligand MOFs: 53.375 mg of terephthalic acid and 27.45 mg of triethylenediamine were dissolved in 5 mL of DMF to form a mixed solution; 10 DMF solution in which 228.75 mg of iron clusters were dissolved was added dropwise to 1.525 mg of glacial acetic acid, and stirred for 30 min until the mixture was uniform; The...

Embodiment 3

[0040] (1) Synthesis of iron clusters: 25.4262 g of anhydrous sodium acetate and 8.08 g of Fe(NO 3 ) 3 9H 2 O was dissolved in 50mL water respectively to obtain sodium acetate solution and ferric nitrate solution; then the sodium acetate solution was dropped dropwise into the ferric nitrate solution, and stirred for 12 hours to form a suspension; then the suspension was suction filtered to obtain a reddish-brown solid, and washed with 50 mL of deionized water and 50 mL of ethanol in turn, and finally put the product in a vacuum oven at 70 °C for 12 h at constant temperature to obtain iron clusters [Fe 3 (CH 3 COO) 6 ].

[0041] (2) Synthesis of iron-based double-ligand metal-organic framework materials: 68.625 mg of terephthalic acid and 36.6 mg of triethylenediamine were dissolved in 5 mL of DMF to form a mixed solution; 10 DMF solution in which 251.625 mg of iron clusters were dissolved was added dropwise to 1.525 mg of glacial acetic acid, and stirred for 30 min until ...

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Abstract

The invention discloses an iron-based double-ligand metal organic framework material capable of preferentially adsorbing ethane as well as a preparation method and application of the iron-based double-ligand metal organic framework material. The method comprises the following steps: (1) dropping a sodium acetate solution into an iron nitrate solution, and carrying out stirring to obtain an iron cluster; and (2) dissolving terephthalic acid and triethylene diamine into N,N-dimethylformamide, then, dropping a DMF solution of the iron cluster, then, dropwise adding glacial acetic acid, and carrying out uniform stirring; and placing a mixed solution into a glass bottle to be sealed, then, carrying out a programmed temperature controlled solvothermal synthesis reaction to obtain the iron-baseddouble-ligand metal organic framework material. The material has the property of preferentially adsorbing ethane, both the ethane adsorption capacity and ethane / ethylene adsorption selectivity are onthe international advanced level, the ethane adsorption capacity of the material is more than 2.5 times as high as that of activated carbon under the same condition, the ethane / ethylene adsorption selectivity is more than 2 times as high as that of activated carbon, and the water vapor stability is good. The material has a good application prospect for industrial ethylene and ethane separation.

Description

technical field [0001] The invention relates to the technical field of adsorption and separation of ethylene and ethane, in particular to an iron-based double-ligand metal-organic framework material that preferentially adsorbs ethane, a preparation method and application thereof. Background technique [0002] Ethylene is an important petrochemical raw material widely used in the preparation of polystyrene, polyethylene, polyester and other chemicals. Industrial ethylene is mostly derived from the cracking of petroleum and the thermal cracking of ethane. When ethylene is produced by thermal cracking, ethane is inevitably produced as a by-product. Separation of ethylene from ethane and ethylene mixtures is extremely challenging due to their similar boiling points and molecular sizes. The traditional industrial separation technology of ethylene and ethane generally adopts the cryogenic separation method, which needs to be operated at low temperature (-25°C) and high pressure (...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G83/00B01J20/22B01J20/30B01D53/02
CPCB01D53/02B01D2257/7022B01J20/226C08G83/008
Inventor 夏启斌吕道飞陈永伟石仁凤吴厚晓奚红霞李忠
Owner SOUTH CHINA UNIV OF TECH
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