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Simulated moving bed chromatography method for separating cresol isomeride mixture

A technology of isomers and simulated moving bed, which is applied in the field of adsorption separation, can solve problems such as the difficulty in separating cresol isomer mixtures, and achieve the effects of reducing energy consumption and energy-saving equipment

Active Publication Date: 2020-12-22
UNIV OF SCI & TECH LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to solve the problem of difficult separation of cresol isomer mixtures by using metal organic framework materials (MOFs) with ultra-high specific surface area and developed pore structure as the stationary phase of SMB, and provide a method for separating cresol isomers. Simulated Moving Bed Chromatography of Construct Mixtures

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Stationary phase: composed of metal ions Fe 3+ With the organic ligand terephthalic acid (H 2 Fe-MOFs formed by BDC) reaction. The reaction conditions are solvothermal synthesis, the solvent is DMF, the reaction temperature is 150°C, and the reaction time is 3 days; the solvothermal synthesis products are washed with DMF and water respectively, and then dried, the drying temperature is 120°C, and the drying time is 12 hours;

[0035] metal ion Fe 3+ specifically FeCl 3 ·6H 2 O;

[0036] Chromatographic column: length 5cm, diameter 1cm;

[0037] SMB working mode: 1 group I with independent three-band SMB, specifically 1-1-2;

[0038] Mobile phase composition: solvent 2, wherein solvent 1 is ethyl acetate, solvent 3 is petroleum ether; mobile phase P: the volume ratio of solvent 3 to solvent 1 is V 石油醚 / V 乙酸乙酯 =1 / 1; mobile phase D: the volume ratio of solvent 3 to solvent 1 is V 石油醚 / V 乙酸乙酯 =7 / 3;

[0039] Mobile phase flow rate: mobile phase D flow rate Q D 1....

Embodiment 2

[0046] Except following condition, other is all with embodiment 1;

[0047] SMB working mode: 1 group I with independent three-band SMB, specifically 2-1-1;

[0048] Mobile phase composition: solvent 2, wherein solvent 1 is ethyl acetate, solvent 3 is petroleum ether; mobile phase P: the volume ratio of solvent 3 to solvent 1 is V 石油醚 / V 乙酸乙酯 =9 / 1; The composition of mobile phase D is the same as that of mobile phase P;

[0049] Mobile phase flow rate: mobile phase D flow rate Q D 1.0mL / min, mobile phase P flow rate Q P 1.5mL / min, flow rate Q of sample solution F F 0.1mL / min;

[0050] Working temperature: room temperature;

[0051] Injection solution: o-cresol 25mg / mL, m-cresol 25mg / mL, medium is mobile phase D;

[0052] Switching cycle: 22min.

[0053] Under the above conditions, the SMB separation result is:

[0054] Obtain o-cresol raffinate from raffinate outlet R, purity: o-cresol 100%, yield: o-cresol 97.4%; Obtain m-cresol extract from extract E outlet, purity:...

Embodiment 3

[0056] Stationary phase: composed of metal ions Al 3+ With the organic ligand terephthalic acid (H 2 Al-MOFs formed by BDC) reaction. The reaction conditions are hydrothermal synthesis, the reaction temperature is 220°C, and the reaction time is 3 days; the hydrothermal synthesis product is washed with water, dried for 12 hours, and then roasted, the roasting temperature is 330°C, and the roasting time is 3 days;

[0057] metal ion Al 3+ Specifically Al(NO 3 ) 3 9H 2 O;

[0058] Chromatographic column: length 5cm, diameter 1cm;

[0059] SMB working mode: 1 group I with independent three-band SMB, specifically 1-1-2;

[0060] Mobile phase composition: solvent 2, wherein solvent 1 is ethyl acetate, solvent 3 is petroleum ether; mobile phase P: the volume ratio of solvent 3 to solvent 1 is V 石油醚 / V 乙酸乙酯 =1 / 1; mobile phase D: the volume ratio of solvent 3 to solvent 1 is V 石油醚 / V 乙酸乙酯 =7 / 3;

[0061] Mobile phase flow rate: mobile phase D flow rate Q D 1.0mL / min, mobil...

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Abstract

The invention aims to solve the problem that a cresol isomeride mixture is difficult to separate by taking MOFs as a stationary phase of SMB, and provides a simulated moving bed chromatography methodfor separating the cresol isomeride mixture. MOFs are high in specific surface area and developed in pore structure, and have excellent adsorption separation performance. According to the method, MOFsformed by Fe<3+> and terephthalic acid (H2BDC) are used as a stationary phase, the mixed xylene isomer is separated by using a simulated moving bed at normal temperature, the purity of the xylene monomer is 95-100%, the yield is 90-100%, especially for the separation of p-cresol and m-cresol, the purity of p-cresol can be purified from 80% to 100%, and the yield is 98.2%. The number of chromatographic columns used in the process is small, efficient separation can be carried out in a 2-1-1 mode (three-zone SMB, I-zone independence and four chromatographic columns), elution is carried out through a low-boiling-point mobile phase, SMB separation is carried out at the normal temperature, energy is saved, and equipment is simple.

Description

technical field [0001] The invention belongs to the technical field of adsorption separation, in particular to a simulated moving bed chromatography for separating cresol mixtures. Background technique [0002] Cresol includes three isomers of p-cresol, m-cresol and o-cresol, all of which are important fine chemical intermediates for the preparation of pesticides, medicines, spices, dyes, antioxidants, synthetic vitamin E, Synthetic resins, coloring materials, developers, fluorescent whitening agents, liquid crystal materials, gasoline additives and edible oil preservatives, etc. In order to meet different purposes, high-purity cresol monomer is required. [0003] Most of the products obtained by natural separation and chemical synthesis are mixtures of cresol isomers, and to obtain cresol monomer needs to be separated from other cresol isomers. The boiling points of o / p / m-cresol are 190.8°C, 202.5°C and 202.8°C, respectively. Ortho-cresol can be separated by rectificatio...

Claims

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Application Information

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IPC IPC(8): C07C37/82C07C39/07
CPCC07C37/82C07C39/07
Inventor 王绍艳李守江吴欣欣陈婧雅彭博张连吉
Owner UNIV OF SCI & TECH LIAONING
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