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

A technology of sodium decanesulfonate and ion-pair chromatography, which is applied in the field of preparation of ion-pair chromatography reagent sodium decanesulfonate, can solve the problems of low purity, unsatisfactory separation effect and poor solubility of sodium decanesulfonate, 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

Benefits of technology

The technical effect of this patented process involves improving the efficiency and reducing side products while simplifying its production steps through use of specific chemicals like TPA instead of formalin for sulfurization reactions. Additionally, it achieves higher yields without excessive usage of expensive materials such as phenolsulfonic acid (PSA) due to improved reactivity between certain compounds that form part of these molecules.

Problems solved by technology

This patented technical problem addressed in this patents relates to improving the quality and solvability of sodium dodecylsulfanilicate that forms during production without compromising its effectiveness at detecting biological substances like protein molecules.

Method used

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Effect test

Embodiment 1

[0019] A preparation and purification method of ion-pair chromatographic reagent sodium decane 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 decane bromide 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...

Embodiment 2

[0024] A preparation and purification method of ion-pair chromatographic reagent sodium decane 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 bromodecane 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 decane 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 bromodecane 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 decane-1-sulfonate. The method comprises the following steps: adding anhydrous sodium sulfite, water, bromodecane 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 after 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, purifying twice 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 bromodecane in the preparation method, tetrapropylammonium bromide is used as the catalyst, thus the activity of bromodecane 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

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Claims

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Application Information

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Owner TIANJIN CHEM REAGENT RES INST
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