Method for preparing high-purity liquid chromatographic grade N-alkanes

A technology of normal alkanes and liquid chromatography, applied in the direction of extraction purification/separation, chemical change purification/separation, organic chemistry, etc.

Active Publication Date: 2013-07-03
ANQING FULLTIME CHEM INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The techniques reported in these documents are only limited to the preparation of high-purity n-alkanes, and are not specific techniques for the preparation of n-alkanes by liquid chromatography.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Put 0.2L of N-methylpyrrolidone bisulfate ionic liquid of 1 / 10 of the raw material volume into a 2L glass stirred reactor, and 0.02L of 98% concentrated sulfuric acid of 1 / 10 of the ionic liquid volume, and pass it into the industry while stirring The raw material of n-heptane was 1.03 kg (1.5 L, the absorbance at 220 nm was 0.1832), the temperature was controlled at 25.0° C. for 30 minutes, and the reactant was allowed to stand still to separate layers.

[0026] The alkane is taken out from the upper layer of the stirred reactor to the second 2L sulfonation desulfurization reactor, and 0.2L of N-methylpyrrolidone bisulfate ionic liquid of 1 / 10 of the raw material volume is also put into the second reactor, and the amount of ionic liquid is added 0.02 L of 1 / 10 98% concentrated sulfuric acid was reacted at a reaction temperature of 25.0° C. for 30 minutes, and allowed to stand to separate into layers.

[0027] Repeat the above reaction, and carry out 3 sulfonation desul...

Embodiment 2

[0029] Put 0.3L of N-methylpyrrolidone dihydrogen phosphate ionic liquid of 1 / 5 of the raw material volume into a 2L glass stirred reactor, and 0.03L of 98% concentrated sulfuric acid of 1 / 10 of the ionic liquid volume, and feed it while stirring The raw material of industrial n-pentane is 0.94 kg (1.5 L, the absorbance at 220 nm is 0.1483), the temperature is controlled at 30.0 °C for 100 minutes, and the reactant is allowed to stand still to separate layers.

[0030] Take out the alkane from the upper layer of the stirred reactor to the second 2L sulfonation desulfurization reactor, and put 0.3L of N-methylpyrrolidone dihydrogen phosphate ionic liquid of 1 / 5 of the raw material volume into the second reactor, and put in the ionic liquid 0.03 L of 98% concentrated sulfuric acid with an amount of 1 / 10, reacted at a reaction temperature of 30.0° C. for 100 minutes, and allowed to stand to separate into layers.

[0031] Repeat the above reaction, and carry out 4 sulfonation desu...

Embodiment 3

[0033] In a 2L glass stirred reactor, 0.1L of N-methylsulfonate pyrrolidone bisulfate ionic liquid of 1 / 20 of the raw material volume is dropped into, and 0.02L of 98% concentrated sulfuric acid of 1 / 5 of the ionic liquid amount is dropped into, and the mixture is passed while stirring. Add 1.05 kg (1.5 L, absorbance at 0.2004) of industrial n-octane raw material, control the temperature at 25.0 ° C for 300 minutes, and let the reactants stand still to separate layers.

[0034]The alkane is taken out from the upper layer of the stirred reactor to the second 2L sulfonation desulfurization reactor, and 0.1L of N-methylsulfonate pyrrolidone bisulfate ionic liquid of 1 / 20 of the raw material volume is also put into the second reactor, and the ion 0.02 L of 98% concentrated sulfuric acid with a liquid volume of 1 / 5 was reacted at a reaction temperature of 25.0° C. for 300 minutes, and allowed to stand to separate into layers.

[0035] Repeat the above reaction, and carry out 4 time...

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PUM

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Abstract

The invention discloses a method for preparing high-purity liquid chromatographic grade normal paraffin, in particular to a high-purity liquid chromatographic grade paraffin such as normal pentane, normal hexane, normal heptane, normal octane and the like with low ultraviolet absorption within the range of 195-280nm. The process flow is as follows: utilizing a given amount of ionic liquid and concentrated sulfuric acid to process industrial grade normal paraffin, and rectifying after multi-time sulfonation and desulfuration to obtain the liquid chromatographic grade paraffin. The method has the following advantage that ionic liquid is utilized to selectively extract sulfate and sulfocompound to carry out sulfonation and desulfuration simultaneously, thereby having simple flow, low energy consumption and high product purity.

Description

technical field [0001] The invention relates to a method for preparing high-purity normal alkanes, in particular to a process for preparing high-purity liquid chromatography-grade normal alkanes, which belongs to the field of chemical production. Background technique [0002] High-purity liquid chromatography-grade n-alkanes are mainly used as solvents for normal-phase liquid chromatography, and also as diluents and advanced solvents for pharmaceutical synthesis reactions, such as the preparation of steroids such as acetoxyethyl esters, hormones, etc. Aseptic grade drugs such as cephalosporins and cephalosporins all use n-hexane as co-solvent. With the rapid development of pharmaceutical engineering, biogenetic engineering and related fields at home and abroad, the market demand for high-purity liquid chromatography grade n-alkanes will increase greatly in the next few years, and the market prospect is broad. [0003] The industrial production of n-hexane is mainly separate...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C9/15C07C7/171C07C7/10
Inventor 周沛
Owner ANQING FULLTIME CHEM INDAL
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