Method for preparing high-purity liquid chromatographic grade normal paraffin
A technology of n-alkane and liquid chromatography, which is used in extraction purification/separation, chemical change purification/separation, organic chemistry, etc.
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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 reactants were allowed to stand still to separate into 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 0.02L of 1 / 10 98% concentrated sulfuric acid was reacted at a reaction temperature of 25.0°C for 30 minutes, and the mixture was allowed to stand and separate into layers.
[0027] Repeat the above reaction, and carry ou...
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 reactants are 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 in 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 for a total of 4 sulfonation desul...
Embodiment 3
[0033] In a 2L glass stirred reactor, drop into 0.1L of N-methylsulfonate pyrrolidone bisulfate ionic liquid of 1 / 20 of the raw material volume, and drop into 0.02L of 98% concentrated sulfuric acid of 1 / 5 of the amount of ionic liquid, and pass through 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 reactant 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 times of sulfonation des...
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Abstract
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