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A kind of purification method of chromatographically pure hexane

A purification method and n-hexane technology, which is applied in the purification field of chromatographic pure hexane, can solve the problems of many solid particles, high ultraviolet absorption and high water content, and achieve the effects of large specific surface area, developed microporous structure and good oxidation effect.

Active Publication Date: 2022-05-03
天津康科德医药化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the continuous development of science and technology, the application of chromatographic n-hexane is more and more extensive, and the quality requirements are getting higher and higher. In order to meet the needs of scientific research, improve the production process level of chromatographic n-hexane, and change the monopoly of imported reagents, a chromatographic pure The purification method of hexane changes the phenomena existing in the existing technological level such as low content, high ultraviolet absorption, high moisture, many solid particles, low yield, etc., and meets the requirements of users

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  • A kind of purification method of chromatographically pure hexane
  • A kind of purification method of chromatographically pure hexane

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Embodiment 1

[0049] A purification method of chromatographically pure normal hexane: the method steps are:

[0050] 1) Adsorption step 1: Pass the n-hexane raw material through an activated carbon fiber adsorption column to absorb and remove impurities, and the filtration flow rate is 100-300mL / min.

[0051] 2) Oxidation: Put the adsorbed n-hexane raw material into the oxidation reaction kettle, pass in the gas oxidant (pressure: 0.3-0.5MPa, flow rate: 15-30LPM), stir and react at room temperature for 1-3 hours, after the oxidation is completed, pass in Nitrogen, to replace the oxidizing gas in the oxidation tank under stirring conditions. After the replacement is completed, heat the n-hexane sample liquid to 35-45°C with heat transfer oil.

[0052] 3) Adsorption step 2: inject the heated n-hexane sample liquid into the graphene oxide adsorption column, sodium hydroxide alkaline adsorption column and 13X modified molecular sieve adsorption column for adsorption and filtration, and control...

Embodiment 2

[0060] A purification method of chromatographically pure normal hexane: the method steps are:

[0061] 1) Adsorption step 1: Pass the n-hexane raw material through an activated carbon fiber adsorption column to absorb and remove impurities, and the filtration flow rate is 100-150mL / min.

[0062] 2) Oxidation: Put the adsorbed n-hexane raw material into the oxidation reaction kettle, pass in the gas oxidant (pressure: 0.3-0.5MPa, flow rate: 15-30LPM), stir and react at room temperature for 1-3 hours, after the oxidation is completed, pass in Nitrogen, to replace the oxidizing gas in the oxidation tank under stirring conditions. After the replacement is completed, heat the n-hexane sample liquid to 35-45°C with heat transfer oil.

[0063] 3) Adsorption step 2: inject the heated n-hexane sample liquid into the graphene oxide adsorption column, sodium hydroxide alkaline adsorption column and 13X modified molecular sieve adsorption column for adsorption and filtration, and control...

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Abstract

The invention relates to a method for purifying chromatographically pure n-hexane. The steps of the method are as follows: the n-hexane raw material is adsorbed and filtered through a modified activated carbon fiber adsorption column; the filtered n-hexane raw material is oxidized by using ozone as an oxidant; Oxygen adsorption column, sodium hydroxide, modified 13X molecular sieve adsorption and removal of impurities; drying and removal of water through 3A molecular sieve; removal of low-boiling impurities by distillation; removal of impurities by rectification to obtain chromatographic n-hexane. The innovation of the present invention lies in the selection of ozone as the oxidant, which has a good oxidation effect, fast rate and short cycle, and does not introduce new impurities and does not generate solid waste. In addition, the present invention uses graphene oxide and modified activated carbon fibers as impurity adsorption materials, The adsorption effect of the two kinds of adsorption materials on the impurities in the n-hexane raw material is very remarkable, the purity of the n-hexane product obtained through this purification process is ≥99.4%, the moisture content is less than 0.006%, and the yield is ≥92%.

Description

technical field [0001] The invention belongs to the field of chemical reagents and relates to a purification technology, in particular to a purification method of chromatographically pure n-hexane. Background technique [0002] n-Hexane is a colorless liquid with low toxicity and faint special smell. It is one of the solvents widely used in modern industry. Pigment diluent, in addition, n-hexane is widely used in medicine, chemical industry, polymer materials, food analysis and other industries. [0003] Chromatographically pure n-hexane has high requirements on purity, and has strict requirements on moisture, acidity, evaporation residue, ultraviolet absorption, etc., and belongs to the field of high-purity reagents. With the continuous development of science and technology, the application of chromatographic n-hexane is more and more extensive, and the quality requirements are getting higher and higher. In order to meet the needs of scientific research, improve the produc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C7/00C07C7/12C07C7/148C07C7/13C07C9/15B01D15/08
CPCC07C7/005C07C7/12C07C7/148C07C7/13B01D15/08C07C9/15
Inventor 张键鑫宋金链
Owner 天津康科德医药化工有限公司