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Method for purifying tocotrienol by use of chromatographic column

A technology of trienol and chromatography column, applied in the field of chemical engineering, can solve the problems of difficult environmental protection treatment, unfavorable environmental protection, environmental pollution and the like, and achieves the effects of low production cost, small environmental impact and high economic benefit

Inactive Publication Date: 2018-11-16
浙江伊宝馨生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The core process of this method is to use ion column or chromatographic column to purify the crude product of trienol, and after the trienol is freed, the used ion column and chromatographic column must be regenerated before they can be recycled, and a large amount of The mixed wastewater of waste alkaline water and waste oil is very difficult to follow-up environmental protection treatment, and the investment is large, which will still pollute the environment, which is neither economical nor environmentally friendly.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] The diameter of the chromatography column is 1m, the height is 9m, and the volume of the chromatography column is 7.065m 3 , the chromatographic column is filled with stationary phase adsorbent silica gel 3.5m 3, with a quality of 1500 kg, and immersed in the initial solvent petroleum ether; take 50 kg of the crude product of trienol obtained after molecular distillation (wherein the content of trienol is 35%), mix it with 25 kg of petroleum ether, and heat at 35 °C The temperature and the speed of 7 kg per hour are added from the upper end of the chromatography column; the eluent petroleum ether and ethanol are used for gradient elution of the chromatography column at a speed of 400 kg per hour, and the elution time is maintained for 4 hours, with 1200 kg as a point The elution material is collected in sections according to the number of sections; the product collected in each section is distilled under reduced pressure, and the trienol components are combined to obtai...

Embodiment 2

[0047] The diameter of the chromatography column is 1m, the height is 9m, and the volume of the chromatography column is 7.065m 3 , the chromatographic column is packed with stationary phase adsorbent alumina 3.5m 3 , with a quality of 3000 kg, and immersed in the initial solvent petroleum ether; take 100 kg of the crude product of trienol obtained after molecular distillation (wherein the content of trienol is 40%), mix it with 50 kg of petroleum ether, and heat The temperature and the speed of 10 kg per hour are added from the upper end of the chromatography column; the eluent petroleum ether and acetone are used for gradient elution of the chromatography column at a speed of 700 kg per hour, and the elution time is maintained for 5 hours, divided into 2500 kg The number of sections collects the eluting material in sections; the product collected in each section is distilled under reduced pressure, and the trienol components are combined to obtain trienol with a purity of 95...

Embodiment 3

[0049] The diameter of the chromatography column is 1m, the height is 9m, and the volume of the chromatography column is 7.065m 3 , the chromatographic column is packed with stationary phase adsorbent quartz 3.5m 3 , with a quality of 5600 kg, and immersed in the initial solvent petroleum ether; take 200 kg of the crude product of trienol obtained after molecular distillation (wherein the content of trienol is 45%), mix it with 100 kg of petroleum ether, and heat it at 45°C The temperature and the speed of 20 kg per hour are added from the upper end of the chromatography column; the eluent petroleum ether and n-butanol are used for gradient elution of the chromatography column at a speed of 1400 kg per hour, and the elution time is maintained for 5 hours. The eluting material is collected in sections for the number of sections; the product collected in each section is distilled under reduced pressure, and the trienol components are combined to obtain trienol with a purity of 9...

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Abstract

The invention provides a method for purifying tocotrienol by use of a chromatographic column. The method comprises steps as follows: (1) a tocotrienol crude product obtained after molecular distillation is selected, wherein the content of tocotrienol is 30%-70%; (2) packing: the chromatographic column is packed with a stationary phase adsorbent, and the stationary phase adsorbent is soaked in an initial solvent; (3) a raw material and the initial solvent are mixed, and the mixture is added to the upper end of the chromatographic column at the temperature of 30-50 DEG C at the speed of 5%-10% of the total quantity of packing materials each hour; (4) gradient elution is performed on the chromatographic column; (5) the eluted materials are collected section by section; (6) products collectedin each subsection are subjected to reduced pressure distillation, tocotrienol components are combined, and purified tocotrienol is obtained. The provided method is efficient, convenient and high in economic benefits, the purity of purified tocotrienol is high, completely no wastewater or waste residues are produced in the whole process, almost no waste gas is produced through matching of an efficient solvent recovery device, and almost no environmental protection facilities are required for treatment.

Description

technical field [0001] The invention belongs to the field of chemical engineering, and in particular relates to a method for purifying trienol by using a chromatographic column. Background technique [0002] Vitamin E (tocopherol) plays an important role in different growth stages of various animals, and is essential for the functional development of reproductive, muscle, nervous and immune systems. The most effective ingredient in vitamin E is d-alpha tocopherol, which is representative of its high activity and wide distribution, while trienol has stronger efficacy than d-alpha tocopherol, and is effective in anti-oxidation, anti-cancer, lowering cholesterol, etc. All aspects are stronger than d-alpha tocopherol. This is because trienols contain unsaturated side chains, which can more effectively penetrate into tissues containing saturated fatty acid layers, thus having very good antioxidant and free radical scavenging effects. In addition, it has good biocompatibility and...

Claims

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Application Information

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IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 黄茂清陆定贤金琦王忠军应卫民郭秦恺伍钟健
Owner 浙江伊宝馨生物科技股份有限公司
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