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Preparation method of ion-pair chromatography reagent sodium octane-1-sulfonate

A technology of sodium octane sulfonate and ion-pair chromatography, which is applied to the preparation of sulfonate, preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of low purity of sodium octane sulfonate, unsatisfactory separation effect and poor solubility. To achieve the effect of stable and reliable quality, low cost and short response time

Inactive Publication Date: 2012-02-15
TIANJIN CHEM REAGENT RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the sodium octane sulfonate produced by existing manufacturers has low purity and poor solubility, resulting in unsatisfactory separation effects and failing to achieve the purpose of detection

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A preparation and purification method of ion-pair chromatographic reagent sodium octane sulfonate, comprising the following steps:

[0020] (1) Sulfonation: Add 126 grams of anhydrous sodium sulfite and 450 ml of water into a 1000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, then add 125 grams of bromooctane and 1.2 grams of tetrapropylammonium bromide, and heat to reflux 16 hours until the reaction solution was clear and separated.

[0021] (2) Purification: evaporate the moisture in the reaction mixture under reduced pressure at 85° C. / 20 mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 1300 ml of absolute ethanol to obtain 162 grams of crude product. Then use 2600ml of absolute ethanol to recrystallize, and obtain the pure product after filtration.

[0022] (2) Drying: the purified product was placed in a vacuum oven and dried for 2 hours at 80° C. / 100 mmHg to obtain 132 grams of...

Embodiment 2

[0024] A preparation and purification method of ion-pair chromatographic reagent sodium octane sulfonate, comprising the following steps:

[0025] (1) Sulfonation: In a 5000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, add 378g of anhydrous sodium sulfite and 1350ml of water, then add 376g of bromooctane and 5g of tetrapropylammonium bromide, and heat to reflux for 20 hours, until the reaction solution is clear and does not separate into layers.

[0026] (2) Purification: steam the moisture in the reaction mixture under reduced pressure at 85°C / 20mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 4100ml of absolute ethanol to obtain 508 grams of crude product. Then recrystallize with 8200ml of absolute ethanol, and obtain the pure product after filtration.

[0027] (3) Drying: the purified product was placed in a vacuum oven and dried for 3 hours at 80° C. / 100 mmHg to obtain 415 grams of fin...

Embodiment 3

[0029] A preparation and purification method of ion-pair chromatographic reagent sodium octane sulfonate, comprising the following steps:

[0030] (1) Sulfonation: Add 630g of anhydrous sodium sulfite and 2250ml of water to a 10,000ml three-necked flask equipped with a cooling reflux device and mechanical stirring, then add 627g of bromooctane and 8g of tetrapropylammonium bromide, and heat to reflux for 24 hours, until the reaction solution is clear and does not separate into layers.

[0031] (2) Purification: evaporate the moisture in the reaction mixture under reduced pressure at 85° C. / 20 mmHg, dry the remaining solid and pulverize it, put it into a Soxhlet extractor, and extract with 7000 ml of absolute ethanol to obtain 870 grams of crude product. Then recrystallize with 14000ml of absolute ethanol, and obtain the pure product after filtration.

[0032] (3) Drying: the purified product was placed in a vacuum oven and dried for 4 hours at 80°C / 100mmHg to obtain 713 grams...

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Abstract

The invention relates to a preparation method of an ion-pair chromatography reagent sodium octane-1-sulfonate. The method comprises the following steps: adding anhydrous sodium sulfite, water, bromooctane and tetrapropylammonium bromide in a reaction container, which is provided with a cooling backflow device and adopts mechanical agitation, in turn to sulfonate for 16-24 hours, then reducing the pressure to evaporate the water in the mixture subjected to the sulfonation reaction, drying and grinding the residual solid, placing the obtained powder in a Soxhlet extractor, extracting with absolute alcohol to obtain a crude product, recrystallizing the crude product with absolute alcohol, filtering twice, purifying to obtain a pure product, and finally drying the pure product for 2-4 hours to obtain the finished product. During the sulfonation reaction process of sodium sulfite and bromooctane in the preparation method, tetrapropylammonium bromide is used as the catalyst, thus the activity of bromooctane can be increased, the sulfonation reaction can be performed successfully, by-products can be reduced, the reaction time can be significantly shortened and the yield can reach 66%.

Description

Technical field: [0001] The invention belongs to the field of chromatographic reagents, and relates to special reagents for high-performance liquid chromatography, in particular to a preparation method of sodium octanesulfonate, an ion-pair chromatographic reagent. Background technique: [0002] High performance liquid chromatography (HPLC) is widely used in bioengineering, food industry, pharmaceutical industry, petrochemical industry, environmental Supervision, commodity inspection, legal inspection and other disciplines. Sodium octane sulfonate, an ion-pair chromatography reagent, is an indispensable special reagent for high-performance liquid chromatography. The aqueous buffer system (mobile phase) composed of phosphate or acetate and organic modifier (methanol or acetonitrile) can be used in a certain A neutral association is formed in an equilibrium state, and an ion pair with an analyte of opposite charge is retained on the reversed-phase column to achieve the purpos...

Claims

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Application Information

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IPC IPC(8): C07C309/04C07C303/32C07C303/44
Inventor 何金
Owner TIANJIN CHEM REAGENT RES INST