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Preparation method of MONs (microporous organic networks) quartz capillary column for hexane isomer separation

A quartz capillary and organic network technology, applied in the field of gas chromatography separation, can solve the problem that gas chromatography columns cannot selectively separate hexane isomers, etc., and achieve excellent separation performance, good stability, and good reproducibility

Inactive Publication Date: 2018-11-06
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the existing gas chromatographic column cannot selectively separate hexane isomers, and to provide a preparation method for a microporous organic network quartz capillary column suitable for separating hexane isomers

Method used

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  • Preparation method of MONs (microporous organic networks) quartz capillary column for hexane isomer separation
  • Preparation method of MONs (microporous organic networks) quartz capillary column for hexane isomer separation
  • Preparation method of MONs (microporous organic networks) quartz capillary column for hexane isomer separation

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Effect test

Embodiment 1

[0020] A preparation method for a microporous organic network quartz capillary column for separating hexane isomers, the preparation steps are as follows:

[0021] 1) Quartz capillary pretreatment: Take a 30m long, 0.32mm inner diameter quartz capillary column, inject a sodium hydroxide solution with a concentration of 1.0mol / L and keep it for 2h, then inject pure water to rinse until the eluate is neutral, and then Then inject 0.1mol / L hydrochloric acid solution and keep it for 2 hours, then rinse with pure water until the eluate is neutral, and dry it under nitrogen gas at 120°C for 2 hours before use.

[0022] 2) Preparation of MONs reaction solution: 8.4 mg of bis(triphenylphosphine) palladium dichloride and 2.2 mg of ketone iodide solid powder were added to 30 mL of a mixed solution of toluene and triethylamine with a volume ratio of 1:1, Sonicate under ultrasonic conditions until the solid is completely dissolved, and finally a colorless catalyst solution is obtained. T...

Embodiment 2

[0028] A method for preparing a microporous organic network quartz capillary column for separating hexane isomers, the steps and method are basically the same as in Example 1, except that the halogenated benzene is p-dibromobenzene.

[0029] The separation effect of the prepared MONs quartz chromatographic column on hexane isomers and the scanning electron microscope results are similar to those in Example 1.

Embodiment 3

[0031] A method for rapidly preparing a spherical microporous organic network material at room temperature is prepared by a room temperature method. The steps and method are basically the same as those in Example 1, except that the halogenated benzene is p-dichlorobenzene.

[0032] The separation effect of the prepared MONs quartz chromatographic column on hexane isomers and the scanning electron microscope results are similar to those in Example 1.

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Abstract

The invention provides a preparation method of a MONs (microporous organic networks) quartz capillary column for hexane isomer separation. The MONs quartz capillary column is prepared with an in-situmethod and comprises steps that a quartz capillary is pretreated and a MONs reaction solution is prepared, and the MONs quartz capillary column is prepared in situ. The preparation method has the advantages that: 1), the prepared MONs quartz capillary column shows excellent separation performance on hexane isomer; 2), the separation effect of the MONs quartz capillary column on the hexane isomer is obviously better than that of conventional commodities InertCap-1 and InertCap-5 quartz capillary columns; 3), the MONs quartz chromatographic column is prepared with the in-situ method and has theadvantages of being good in repeatability and stability, capable of being used repeatedly and the like.

Description

【Technical field】 [0001] The invention belongs to the technical field of gas chromatography separation, and relates to a gas chromatography quartz capillary separation column, in particular to a microporous organic network quartz capillary column suitable for separating hexane isomers. 【Background technique】 [0002] Hexane isomers, including five isomers of n-hexane, 2-methylpentane, 3-methylpentane, 2,3-dimethylbutane and 2,2-dimethylbutane , has been widely used in petroleum, chemical industry and other fields, but due to the similarity of physical and chemical properties between hexane isomers, it is very difficult to separate and detect them. Gas chromatography has the advantages of high selectivity and sensitivity, and is very suitable for the separation and detection of hexane isomers. Gas chromatography column is the core of gas chromatography. Although there are many commercial gas chromatography columns on the market, there are not many columns that can selectivel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D15/20C07C7/12C07C9/16
CPCB01D15/20C07C7/12C07C9/16
Inventor 杨成雄王子梦
Owner NANKAI UNIV