Novel technology for extracting vitamin E and squalene by employing multi-stage counter-current liquid-liquid extraction method

A technology of squalene and vitamins, applied in the direction of extraction and purification/separation, purification/separation of hydrocarbons, chemical instruments and methods, etc., can solve problems such as product yields not mentioned

Active Publication Date: 2014-05-21
TIANJIN V HEALTECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Chinese patent with application number 200980126253.0 proposes to extract squalene, natural vitamin E and phytosterol respectively through three vacuum distillations under different conditions after esterification and transesterification of DD oil. This method emphasizes the green characteristics of the process and does not Using white spirit, the product yield is not mentioned

Method used

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  • Novel technology for extracting vitamin E and squalene by employing multi-stage counter-current liquid-liquid extraction method

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Embodiment 1

[0015] Soybean oil deodorized distillate 65g, acid value 69, vitamin E 7.3%, squalene 1.8%, phytosterol 9.5%. (1), add raw material in the flask with condenser tube, add methanol 360ml, concentrated H 2 SO 4 1.0ml, react at reflux temperature for 2 hours. Then add 180ml of deionized water, separate the methanol water phase, wash the oil phase with 30% deionized water containing methanol until neutral; degas at 10mbar and 100°C for 30 minutes to obtain 660g of methyl esterified sample. (2). Add the methyl esterified sample into a flask with a condenser tube, add 25 g of glycerol and 1.5 g of NaOH, and react at 10 mbar and 210° C. for 4 hours to convert the methyl ester into glyceride. (3). Transfer the above sample to a batch-type short-path distillation device. First, under the conditions of 150-180°C and 50-100Pa, distill out 22.6g of the former fraction with a lower boiling point; Continue distillation under the condition, collect main distillate 85.5g, wherein vitamin E...

Embodiment 2

[0017] Rice bran oil deodorized distillate 500g, acid value 110, vitamin E 6.2%, squalene 3.1%, phytosterol 10.5%. (1), add raw material in the flask with condenser tube, add methanol 200ml, concentrated H 2 SO 4 0.75ml, reacted at reflux temperature for 3 hours. Then add 100ml of deionized water, separate the alcoholic water phase, wash the oily phase with deionized water containing 30% methanol until neutral; degas at 20mbar and 100°C for 45 minutes to obtain 510g of methyl esterified sample. (2) Add the raw material for methyl esterification into a flask with a fractionation condenser, add 30 g of glycerol and 1.0 g of NaOH, and react at 10 mbar at 210° C. for 5 hours to convert the methyl ester into glyceride. (3) Transfer the above sample to a batch-type short-path distillation device. First, under the conditions of 150-180°C and 50-100Pa, distill out 25.0g of the previous fraction with a lower boiling point; then under the conditions of 210-250°C and 1030Pa Continue ...

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Abstract

The invention discloses a novel technology for extracting vitamin E and plant squalene from a deodorizer distillate (DD oil) of vegetable oil by employing a multi-stage counter-current liquid-liquid extraction method. The technology comprises the following steps: firstly, converting a free fatty acid in the DD oil into fatty acid methyl ester by a common esterification method, then converting the fatty acid methyl ester into glyceride by glycerolysis reaction; distilling out the vitamin E, squalene and the like with relatively low boiling point by using short-path distillation, and reserving the glyceride, steryl ester and the like with high boiling points at the kettle bottom; and finally, separating out the vitamin E and the squalene by using the multi-stage counter-current liquid-liquid extraction method.

Description

1. Technical field [0001] The invention describes a new process for extracting natural vitamin E and squalene from vegetable oil deodorized distillates, which belongs to the technology of separating oil compounds and trace functional components therein. 2. Background technology [0002] The deodorized distillate (DD for short) during vegetable oil refining is an effective resource for extracting natural substances such as natural vitamin E, plant-derived squalene (squalene) and phytosterols. The research on the process of extracting squalene by using DD oil is later than the research on the process of extracting natural vitamin E, and it has only appeared in the past ten years. The wide application of natural vitamin E in medicine, cosmetics and food industry has become common knowledge, and the special function of squalene has also attracted much attention. Squalene is a triterpenoid highly unsaturated olefin compound, and it is also the earliest hydrocarbon compound disco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72C07C11/21C07C7/10C07C7/148C07J9/00
CPCC07C7/005C07C7/04C07C7/10C07C7/14891C07D311/72C07J9/00C07C11/21
Inventor 孙登文
Owner TIANJIN V HEALTECH CO LTD
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