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Ion pair chromatographic-grade reagent sodium 1-octanesulfonate purifying process

The technology of sodium octane sulfonate and ion-pair chromatography is applied in the purification process field of ion-pair chromatography grade reagent 1-octane sulfonate sodium, which can solve the problems of complicated process and high cost, and achieves improved impurity removal efficiency and easy operation. , the effect of reducing the phenomenon of agglomeration

Inactive Publication Date: 2013-06-12
上海晶纯实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The development of domestic ion-pair chromatographic reagents lags behind the needs of current scientific research and development. Although patent CN101693677 and CN102351743 provide 1-bromooctane as raw material, the method for preparing ion-pair chromatographic grade reagent 1-sodium octanesulfonate by synthetic means , but involves chemical reaction, product post-treatment, crude product purification and other process steps, the process is complicated and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The purification process of ion-pair chromatographic grade reagent 1-octane sodium sulfonate, the steps are as follows:

[0022] (1) Put 50g of the raw material 1-octane sodium sulfonate into 400ml of acetone, and perform ultrasonic irradiation and vibration. The ultrasonic frequency is set to 35KHz, the temperature is controlled at about 45°C, and the ultrasonic time is 8h.

[0023] (2) The mixture in step (1) was naturally cooled to room temperature, subjected to vacuum filtration, and the filter cake was pressed dry to obtain 45 g of solid. The mother liquor is distilled under reduced pressure to recover the organic solvent and recycle it.

[0024] (3) Put the obtained solid into 350ml ethanol-water mixed solution, the ethanol used in the ethanol-water mixed solution is absolute ethanol, the mass ratio of ethanol and water is 50:1, heat and reflux and stir for 6h, filter while hot , the filtrate was cooled naturally, and frozen at 5°C to precipitate crystals.

[00...

Embodiment 2

[0033] The purification process of ion-pair chromatographic grade reagent 1-octane sodium sulfonate, the steps are as follows:

[0034] (1) Put 40 g of raw material 1-octane sodium sulfonate into 250 ml of acetone, and carry out ultrasonic irradiation and vibration. The ultrasonic frequency is set to 35 KHz, the temperature is controlled at about 40 ° C, and the ultrasonic time is 3 hours.

[0035] (2) The mixture in step (1) was naturally cooled to room temperature, subjected to vacuum filtration, and the filter cake was pressed dry to obtain 32 g of solid. The mother liquor is distilled under reduced pressure to recover the organic solvent and recycle it.

[0036] (3) Put the obtained solid into 300ml ethanol-water mixed solution, the ethanol used in the ethanol-water mixed solution is absolute ethanol, the mass ratio of ethanol and water is 40:1, heat and reflux and stir for 5h, filter while hot , the filtrate was cooled naturally, and frozen at 5°C to precipitate crystals...

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Abstract

The invention provides an ion pair chromatographic-grade reagent sodium 1-octanesulfonate purifying process. The process is characterized in that the process concretely comprises the following steps: adding a raw material sodium 1-octanesulfonate to acetone, carrying out ultrasonic irradiation vibration, cooling to room temperature, carrying out primary reduced pressure suction filtration of the above obtained mixture, adding the obtained filter cake soild to an ethanol-water mixed solution, carrying out heating refluxing stirring, filtering while hot, naturally cooling the obtained filtrate, freezing at a low temperature to precipitate crystals, carrying out secondary reduced pressure suction filtration, collecting crystals, and drying to obtain an ion pair chromatographic-grade reagent sodium 1-octanesulfonate. The purifying process successfully solves the chromatographic-grade reagent sodium 1-octanesulfonate preparation problem, and has the advantages of novelty, simple operation, fastness, high efficiency, recycle of an organic solvent, economy, environmental protection, and suitableness for the industrialized production.

Description

technical field [0001] The invention relates to a special reagent for high-performance liquid chromatography, in particular to a purification process for ion-pair chromatographic grade reagent 1-octane sodium sulfonate. Background technique [0002] Ion chromatography (Ion Chromatograhpy) is a kind of high performance liquid chromatography (HPLC). Because of its fast analysis speed, high detection sensitivity, good selectivity, simultaneous analysis of multiple ions, and high stability, it is widely used in many fields such as food industry, medicine and health, petrochemical industry, environmental geology, and quality inspection. Ion-pair chromatography reagent 1-octane sodium sulfonate is an essential special reagent for high performance liquid chromatography. The content of commercially available sodium 1-octane sulfonate reaches 98%, but there are still trace impurities with high ultraviolet absorption, which cannot meet the requirements of relevant scientific research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/04C07C303/44
Inventor 凌青杨永磊
Owner 上海晶纯实业有限公司
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