Method for separating xylene mixture by using metal organic framework material MIL-53 (Cr) and compound as adsorption stationary phase

A metal-organic framework and adsorption immobilization technology, which is applied in the fields of alkali metal compounds, adsorption purification/separation, alkali metal oxides/hydroxides, etc., can solve problems such as unsatisfactory separation factors, and achieve excellent separation ability and good shape The effect of appearance characteristics and fast adsorption rate

Inactive Publication Date: 2019-01-11
TIANJIN UNIV
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Problems solved by technology

[0004] As a new type of porous material, metal-organic frameworks (MOFs) have the characteristics of using metal ions or metal clusters as coordination centers to form a structural framework through coordination with organic ligands containing oxygen or nitrogen. , showing the advantages of high specific surface area, tunable pore structure, structural flexibility, etc., applied to gas storage, drug delivery and imaging, catalysts and separation, and also has some research in the field of xylene isomer separation 16-18 , but the separation factor is not ideal

Method used

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  • Method for separating xylene mixture by using metal organic framework material MIL-53 (Cr) and compound as adsorption stationary phase
  • Method for separating xylene mixture by using metal organic framework material MIL-53 (Cr) and compound as adsorption stationary phase
  • Method for separating xylene mixture by using metal organic framework material MIL-53 (Cr) and compound as adsorption stationary phase

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Experimental program
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Effect test

Embodiment 1

[0026] Mix chromium nitrate nonahydrate, terephthalic acid, water and hydrofluoric acid with a molar ratio of 1:2:280:1, stir and put it into a stainless steel reactor, and react at 220°C for three days. Wash with ethanol and N,N-dimethylformamide three times each, reflux in N,N-dimethylformamide for 25 hours, centrifuge, wash with ethanol, dry, and calcinate at 300°C for 12 hours. Synthesized MIL-53 (Cr) in the present invention has 1550m 2 / g above the specific surface area.

[0027] Weigh 0.1000g metal-organic framework material MIL-53(Cr) and add it to the n-hexane solution of one-component xylene with a total concentration of 0.1mol / L, shake at a constant temperature of 140rpm for 4 hours, filter the supernatant to remove the adsorbent , to obtain the treated solution. The concentration of three xylenes in the treated solution and the concentration of the initial solution were detected by gas chromatography, and the adsorption amount was calculated. The formula for cal...

Embodiment 2

[0034] Selective adsorption of o-xylene and p-xylene:

[0035] Weigh 0.1000g metal-organic framework material MIL-53(Cr) and add it into n-hexane solutions of o-xylene and p-xylene with different concentrations of equimolarity, shake at a constant temperature of 140rpm for 4 hours, filter the supernatant to remove the adsorbent , to obtain the treated solution. The concentration of o-xylene and p-xylene in the treated solution and the concentration of the initial solution were detected by gas chromatography, and the adsorption capacity and selectivity were calculated. selectivity alpha i，j The calculation method is as follows:

[0036]

[0037] Among them, q i and q j (mol / g) is respectively the quality of xylene single-component isomer i and j in the solution that every gram of adsorbent absorbs; c i and c j(mol / L) is the equilibrium concentration of xylene single-component isomers i and j in the solution.

[0038] Depend on Figure 4 It can be seen that in the bin...

Embodiment 3

[0040] Ternary competitive adsorption experiment:

[0041] Weigh 0.1000g metal-organic framework material MIL-53(Cr) and add it to the n-hexane solution of the three xylene isomers with different concentrations of equimolarity. After shaking at a constant temperature of 140rpm for 4 hours, filter the supernatant to remove the adsorbent , to obtain the treated solution. The concentration of three xylene isomers in the treated solution and the initial solution concentration were detected by gas chromatography, and the adsorption capacity and selectivity were calculated. selectivity alpha i，j The calculation method is as follows:

[0042]

[0043] Among them, q i and q j (mol / g) is respectively the quality of xylene single-component isomer i and j in the solution that every gram of adsorbent absorbs; c i and c j (mol / L) is the equilibrium concentration of xylene single-component isomers i and j in the solution.

[0044] Figure 5 The adsorption capacity and selectivity...

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Abstract

The invention discloses a method for separating a xylene mixture by using a metal organic framework material MIL-53 (Cr) and a compound as an adsorption stationary phase. The method comprises the following steps: separating a liquid xylene mixture by using a metal organic framework material MIL-53 (Cr) and a compound as a SMB adsorbent; and then calculating the concentration of the xylene mixturein a solution after gas chromatography detection and the initial solution concentration to obtain the adsorption amount and selectivity. The metal organic framework material MIL-53 (Cr) for separatingan xylene isomer has a high specific surface area (greater than or equal to 1550 m<2> / g) and good morphology features, has excellent separation ability of the xylene mixture, wherein the separation factor reaches 22 and the adsorption capacity reaches 8.2 mol / kg, and has an extremely fast adsorption rate, which can reach a saturated adsorption capacity of 95% or more in half an hour.

Description

technical field [0001] The invention relates to the technical field of adsorption separation, in particular to a metal-organic framework material for separating xylene mixtures and a preparation method thereof. Background technique [0002] Xylene contains three isomers of p-xylene (PX), o-xylene (OX) and m-xylene (MX). The isomer mixture comes from the catalytic reforming of crude oil. Each isomer is a valuable intermediate, so the effective separation of xylene isomers is listed as one of the seven world-changing separations 1 . However, due to the very similar physical and chemical properties of these isomers, it is very difficult to effectively separate them. The traditional distillation separation method is not applicable here, due to the similar boiling points, the number of theoretical plates required for the separation of o-xylene exceeds 150, and the further separation of m-xylene and p-xylene requires up to 360 theoretical plates 2 . An efficient method for the...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/22B01J20/28B01J20/30C07C15/08C07C7/12
CPCB01D15/08B01J20/226B01J20/28066B01J20/3078C07C7/12C07C15/08
Inventor 郭翔海何振江杨玉茜白鹏
Owner TIANJIN UNIV
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