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A kind of preparation technology of ion-pair chromatographic grade reagent dodecyltrimethylammonium chloride

A technology of dodecyltrimethylammonium chloride and ion-pair chromatography, which is applied in the fields of organic chemistry, purification/separation of amino compounds, etc., can solve the problems that cannot meet the requirements of scientific research and analysis, and the development of ion-pair chromatography grade reagents lags behind scientific research development. and other problems, to achieve the effect of novel technology and easy operation

Active Publication Date: 2017-01-18
SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The content of commercially available dodecyltrimethylammonium chloride reaches 98%, but there are still traces of high-absorbing ultraviolet impurities, which cannot meet the requirements of relevant scientific research analysis
[0003] At present, the use of domestic ion-pair chromatography grade reagent products mainly relies on imports, and the development of domestic ion-pair chromatography grade reagents lags behind the needs of current scientific research and development

Method used

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  • A kind of preparation technology of ion-pair chromatographic grade reagent dodecyltrimethylammonium chloride

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Embodiment 1

[0024] A kind of preparation technology of ion-pair chromatographic grade reagent dodecyltrimethylammonium chloride, concrete steps are:

[0025] (1) Adsorption: the raw material dodecyltrimethylammonium chloride of 98% is dissolved with 2600ml deionized water by 100g purity, and the gained solution is squeezed into the adsorption column, and the length of the column is 300mm, internal diameter 80mm, and 400 mesh activated carbons are installed inside. Flow through the adsorption column at a flow rate of 30ml / min, and evaporate the solution to obtain a solid;

[0026] (2) Ultrasonic crystallization: put the solid obtained in step (1) into 600ml of organic solvent, the organic solvent is a solution prepared by acetone and ethanol at a mass ratio of 60:1, the mixture is subjected to ultrasonic irradiation and vibration, and the ultrasonic frequency is set to 35KHz, the temperature is controlled at 45°C to 65°C, and the ultrasonic time is 2h. The resulting solution was cooled to...

Embodiment 2

[0029] (1) Adsorption: Dissolve 250g of raw material dodecyltrimethylammonium chloride (98%) with a purity of 98% in 6000ml of deionized water, and the resulting solution is put into an adsorption column with a column length of 300mm and an internal diameter of 80mm. Activated carbon flows through the adsorption column with a flow rate of 80ml / min, and the solution evaporates to obtain a solid;

[0030] (2) Ultrasonic crystallization: put the solid obtained in step (1) into 2500ml of organic solvent, the organic solvent is a solution prepared by acetone and isopropanol at a mass ratio of 30:1, the mixture is subjected to ultrasonic irradiation and vibration, and the ultrasonic frequency is set The temperature is 53KHz, the temperature is controlled at 45°C to 65°C, and the ultrasonic time is 4h. The resulting solution was cooled to room temperature, crystals were precipitated, and the first vacuum filtration was performed to collect the crystals;

[0031] (3) Washing and dryi...

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Abstract

The invention provides a preparation process of an ion-pair chromatographic-grade reagent dodecyl trimethyl ammonium chloride. The preparation process is characterized by comprising the following specific steps: dissolving dodecyl trimethyl ammonium chloride as a raw material in deionized water to obtain a solution, pumping the solution into an adsorption column and evaporating the solution to obtain a solid; putting the solid into an organic solvent to obtain a mixture, carrying out ultrasonic irradiation and shaking on the mixture for 2-4 hours at 45 DEG C-65 DEG C to obtain a solution, cooling the solution to room temperature, precipitating crystals, carrying out reduced pressure suction filtration for the first time and collecting the crystals; putting the crystals into an organic solvent to obtain a mixture, carrying out ultrasonic irradiation and shaking on the mixture for 4-8 hours at 30 DEG C-50 DEG C to obtain a solution, cooling the solution to room temperature, carrying out suction filtration and collecting the solid, namely the ion-pair chromatographic-grade reagent dodecyl trimethyl ammonium chloride. Various technical indicators of the product can reach the requirements of ion-pair chromatographic-grade reagent dodecyl trimethyl ammonium chloride.

Description

technical field [0001] The invention belongs to the field of chemical reagents, and relates to special reagents for high-performance liquid chromatography, in particular to a preparation method of ion-pair chromatography grade reagent dodecyltrimethylammonium chloride. Background technique [0002] The methods for preparing ion-pair chromatographic grade dodecyltrimethylammonium chloride are rarely reported in China. Ion-pair chromatographic grade reagents are an essential special reagent for high-performance liquid chromatography, and have particularly high requirements for purity, especially for ultraviolet absorption. The content of commercially available dodecyltrimethylammonium chloride reaches 98%, but there are still traces of high-absorbing ultraviolet impurities, which cannot meet the requirements of relevant scientific research analysis. [0003] At present, the use of domestic ion-pair chromatography grade reagent products mainly relies on imports, and the develo...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/63C07C209/84
Inventor 郝松艳凌青
Owner SHANGHAI JINGCHUN BIOCHEM TECH CO LTD
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