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Purification method of chromatographically pure n-hexane

A purification method and n-hexane technology, 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 effect of enhanced adsorption effect, large specific surface area and good oxidation effect.

Active Publication Date: 2020-01-21
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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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 purification method of chromatographically pure n-hexane. The method comprises the following steps: adsorbing and filtering an n-hexane raw material through a modified activated carbon fiber adsorption column; carrying out oxidation treatment on the filtered n-hexane raw material by taking ozone as an oxidant; adsorbing and removing impurities through a graphene oxide adsorption column, sodium hydroxide and a modified 13X molecular sieve; drying and dewatering through a 3A molecular sieve; removing low-boiling-point impurities by distillation; and rectifying to remove impurities to obtain the chromatographically pure n-hexane. The method is characterized in that the ozone is selected as the oxidant, oxidation effect is good, and a fast rate, a short period, no introduction of new impurities, and no generation of solid waste are achieved; besides, the graphene oxide and the modified activated carbon fiber are used as impurity adsorption materials, the adsorption effects of the two adsorption materials on impurities in the n-hexane raw material are very remarkable, the purity of the n-hexane product obtained through the purification process is larger than or equal to 99.4%, the moisture content is 0.006% or below, and the yield is larger than or equal to 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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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