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Process for purifying special reagent sodium dodecyl sulfonate for ion pair chromatography

The technology of sodium dodecyl sulfonate and ion-pair chromatography is applied in the directions of organic chemistry, chemical instruments and methods, preparation of organic compounds, etc., and can solve the problems of high cost, complicated process, inability to meet the requirements of scientific research and experiments, and the like, To achieve the effect of easy operation, improve dissolution efficiency, and improve dissolution efficiency

Active Publication Date: 2014-09-17
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of commercially available sodium dodecylsulfonate reaches 99%, but there are still trace impurities with high ultraviolet absorption, which cannot meet the requirements of relevant scientific research experiments
[0003] The development of domestic ion-pair chromatography reagents lags behind the needs of current scientific research and development. Although patents CN101693677, CN102351741, and CN102351743 have proposed using 1-bromoalkanes as raw materials to prepare special reagents for ion-pair chromatography by synthetic means, the process 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

[0019] The purification process of ion-pair chromatography special reagent sodium dodecylsulfonate, the steps are as follows:

[0020] (1) Put 250g of raw material sodium dodecylsulfonate into 2000ml of deionized water, and carry out ultrasonic irradiation and vibration. The ultrasonic frequency is set to 35KHz, the temperature is controlled at about 55°C, and the ultrasonic time is 8h.

[0021] (2) The solution obtained in step (1) was naturally cooled to room temperature, a large amount of crystals were precipitated, and filtered under reduced pressure to collect 195 g of crystals.

[0022] (3) The obtained crystals were put into 1800ml of ethanol-water mixed solution, the ethanol used in the ethanol-water mixed solution was absolute ethanol, and the mass ratio of ethanol and water was 50:1, heated under reflux and stirred for 6 hours.

[0023] (4) Cool the solution obtained in step (3) to room temperature, precipitate crystals, filter under reduced pressure, and collect the...

Embodiment 2

[0031] The purification process of ion-pair chromatography special reagent sodium dodecylsulfonate, the steps are as follows:

[0032] (1) Put 200g of raw material sodium dodecylsulfonate into 1200ml of deionized water, and perform ultrasonic irradiation and vibration. The ultrasonic frequency is set to 35KHz, the temperature is controlled at about 50°C, and the ultrasonic time is 6h.

[0033] (2) The solution obtained in step (1) was naturally cooled to room temperature, a large amount of crystals were precipitated, and 164 g of crystals were collected by suction filtration under reduced pressure.

[0034] (3) Put the obtained crystals into 1500ml of 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.

[0035] (4) Cool the solution obtained in step (3) to room temperature, precipitate crystals, filter under reduced pressure, and collect the filtrat...

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Abstract

The invention provides a process for purifying a special reagent sodium dodecyl sulfonate for ion pair chromatography. The process is characterized in that the process concretely comprises the following steps: adding a raw material sodium dodecyl sulfonate to deionized water, carrying out ultrasonic irradiation oscillation, cooling the obtained solution to room temperature to precipitate crystals, and carrying out primary reduced pressure suction filtration, and collecting crystals; adding the obtained crystals to an ethanol-water mixed solution, carrying out heating refluxing stirring for 3-8h, cooling the obtained solution to room temperature to precipitate crystals, carrying out secondary reduced pressure suction filtration, and collecting the obtained filtrate; and carrying out constant low temperature crystallization of the obtained filtrate for 6-12h, carrying out third reduced pressure suction filtration, collecting crystals, and drying to obtain a special reagent sodium dodecyl sulfonate for ion pair chromatography. The purifying process 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 of sodium dodecylsulfonate, a special reagent for ion-pair chromatography, and belongs to the field of chemical reagents. 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 Sodium dodecyl sulfate is an essential special reagent for high performance liquid chromatography. Commercially available sodium dodecyl sulfonate has a content of 99%, but there are still trace impurities with high ultraviolet absorption, which cannot meet the re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/04C07C303/44
Inventor 杨永磊凌青
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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