Calixarene derivative stationary phase, capillary gas chromatography column and preparation and application of calixarene derivative stationary phase

A gas chromatography column and derivative technology, which is applied in the field of capillary gas chromatography column and calixarene derivative stationary phase, can solve the problems of poor solubility and low column efficiency, and achieves low production cost, simple operation process and rich functional groups. Effect

Active Publication Date: 2019-05-14
SHENYANG POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, as a separation material, calixarene is rarely used in the field of gas chromatography analysis. The main reason is that the solubility is poor and the column efficiency of the prepared chromatographic column is low.
And there is no new calixarene derivative C4A-NO 2 Research Reports Used as Gas Chromatographic Separation Media

Method used

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  • Calixarene derivative stationary phase, capillary gas chromatography column and preparation and application of calixarene derivative stationary phase
  • Calixarene derivative stationary phase, capillary gas chromatography column and preparation and application of calixarene derivative stationary phase
  • Calixarene derivative stationary phase, capillary gas chromatography column and preparation and application of calixarene derivative stationary phase

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Experimental program
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Embodiment 1

[0060]

[0061] Add 10.02g (66.57mmol) of p-tert-butylphenol, 6.2mL (67.30mmol) of 40% formaldehyde solution, and 0.13g (3.13mmol) of NaOH into the round-bottomed flask, then gradually raise the temperature to 115°C, stir and reflux, The reaction solution gradually became turbid and viscous, and a yellow viscous solid appeared after 4 hours of reaction. After adding 50 mL of diphenyl ether, the solid gradually dissolved, and foam was generated and gradually increased. When a large amount of foam is generated, nitrogen is passed into the solution for purging, and after 3 hours, the nitrogen purging is stopped after there are no bubbles in the reaction solution, and the reaction is continued for 2 hours. Add 70mL of ethyl acetate and continue to reflux for 1.5h. Off-white solids are produced. Remove the flask from the oil bath, place it in a cold trap at 0°C, and vacuum filter to obtain a white solid. The filter cake was rinsed with deionized water and dried to obtain 2.42 g ...

Embodiment 2

[0066] Embodiment 2: the difference between this embodiment and embodiment 1 is:

[0067] Add 20.01g (133.22mmol) of p-tert-butylphenol, 12.40mL (134.61mmol) of 40% formaldehyde solution, and 0.25g (6.13mmol) of NaOH into the round-bottomed flask, and gradually raise the temperature from 90°C to 115°C, and stir. Reflux, the reaction solution gradually becomes turbid and viscous, and a yellow viscous solid appears after 4.5 hours of reaction. Add 100mL of diphenyl ether, the solid gradually dissolves, and foams gradually increase. After there were no bubbles in the reaction solution, the nitrogen purging was stopped, and the reaction was continued for 3 h. Add 140mL of ethyl acetate and continue to reflux for 1h. A yellow solid is produced. The flask is removed from the oil bath, placed in a cold trap at 0°C, and vacuum-filtered to obtain a light yellow solid. The filter cake was rinsed with deionized water and dried to obtain 8.22 g of intermediate (I) as a white solid powder...

Embodiment 3

[0070] Embodiment 3: the difference between this embodiment and embodiment 1 is:

[0071]Add 20.08g (133.65mmol) of p-tert-butylphenol, 12.4mL (134.61mmol) of 40% formaldehyde solution, and 0.25g (6.14mmol) of NaOH into the round-bottomed flask, and gradually raise the temperature from 94°C to 115°C, and stir. Reflux, the reaction solution gradually becomes turbid and viscous, and a yellow viscous solid appears after stirring for 4 hours. Add 100mL of diphenyl ether, the solid gradually dissolves, and foams are generated and gradually increase. After there were no bubbles in the reaction solution, the nitrogen purging was stopped, and the reaction was continued for 1 h. Add 140 mL of ethyl acetate and continue to reflux for 2 hours. A large amount of white solids are produced. The flask is removed from the oil bath, placed in a cold trap at 0°C, and vacuum filtered to obtain a light yellow solid. The filter cake was rinsed with 10 mL of deionized water, and dried to obtain 3....

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Abstract

The invention belongs to the field of chromatographic analysis, and particularly relates to a calixarene derivative stationary phase, a capillary gas chromatography column, and a preparation and application of the calixarene derivative stationary phase. According to the calixarene derivative stationary phase, the capillary gas chromatography column, and the preparation and application of the calixarene derivative stationary phase, p-tert-butylphenol is taken as a raw material, an intermediate I is firstly formed through cyclization reaction, an intermediate II is then obtained through reactionof the intermediate I, and the intermediate II is finally nitrated to prepare calixarene derivatives (C4A-NO2), the prepared C4A-NO2 as the stationary phase of the capillary gas chromatography columncan enable the particle size distribution to be uniform, special large holes and rich functional groups are achieved, polar nitro functional groups are arranged at the upper edge of an aromatic ringof the prepared C4A-NO2, and non-polar long alkoxy functional groups are arranged at the lower edge of the aromatic ring of the prepared C4A-NO2. The problems of poor solubility of an existing calixarene derivative and low column efficiency of the prepared chromatographic column are solved, the solubility and film forming property of the calixarene derivative are improved, the chromatographic selectivity of the calixarene derivative is enriched, and the preparation method has the advantages of simplicity, easy availability, low cost and good separation effect.

Description

Technical field: [0001] The invention belongs to the field of chromatographic analysis, and in particular relates to a calixarene derivative stationary phase, a capillary gas chromatography column and its preparation and application. Background technique: [0002] Since its introduction in 1957, capillary gas chromatographic columns have been widely used in separation and analysis science due to their fast, efficient, and sensitive characteristics. Indispensable means of analysis. The chromatographic column is the heart of the gas chromatograph, and the stationary phase is the core of the chromatographic column, so it is very important to choose a suitable stationary phase for separation. At present, the stationary phases of gas chromatography mainly include polysiloxane, liquid crystal, crown ether, cyclodextrin, ionic liquid and fiber filling, etc. However, with the rapid development of the field of chromatographic analysis, in order to meet people's increasing demand fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/60
Inventor 蔡志强帅筱敏付佳赵辰康王庆林丁海关侯英莉谷雨彤李梦瑶
Owner SHENYANG POLYTECHNIC UNIV
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