Preparation of high purity and high optical rotation mixing vitamin E

A technology of mixing vitamins and optical rotation, applied in organic chemistry, etc., can solve problems such as solvent separation difficulties, achieve application safety, improve color, improve fluidity and transparency

Active Publication Date: 2009-07-08
COFCO GROUP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the shortage of difficult solvent separation caused by the use of multiple solvents in the prior art, and to provide a method for preparing mixed vitamin E with high purity and high optical rotation using a single solvent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] A preparation method of high-purity, high optical rotation mixed vitamin E, comprising the following steps:

[0024] (1) Add 150 grams of mixed vitamin E (VE: 47.52% (w / w), sterol: 9.15% (w / w), others: 43.65% (w / w), specific rotation: +17°) In 300ml of 95% ethanol solution by volume, fully dissolve at 35°C;

[0025] (2) The solution obtained in the step (1) with 2 times the volume of the anion exchange resin is subjected to adsorption and separation through the anion exchange resin JK206 (adsorption column: φ20mm*800mm), the adsorption time is 2 hours, and the effluent is removed to reclaim ethanol;

[0026] (3) adding volume percent concentration to the anion exchange resin after adsorption is 95% ethanol aqueous solution, until the effluent is colorless; collect the effluent to concentrate and reclaim ethanol;

[0027] (4) feed carbon dioxide gas and analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.1MPa, and the time is 10 minute...

Embodiment 2

[0035] A preparation method of high-purity, high optical rotation mixed vitamin E, comprising the following steps:

[0036] (1) 1 part by volume of mixed vitamin E with a mass percentage of 10% is added to 0.5 parts by volume of ethanol with a concentration of 100% by volume, and fully dissolved at 25°C;

[0037] (2) The solution obtained in the step (1) of 0.5 times the volume of anion exchange resin is carried out by anion exchange resin (model HZ202) for adsorption separation, the adsorption time is 1 hour, and the effluent is removed to reclaim ethanol;

[0038] (3) adding volume percent concentration to the anion exchange resin after adsorption is 100% ethanol, until the effluent is colorless;

[0039] (4) feed carbon dioxide gas and analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.01MPa, and the time is 2 hours;

[0040] (5) Carry out elution with an ethanol aqueous solution with a concentration of 100% by volume, and collect the el...

Embodiment 3

[0045] A preparation method of high-purity, high optical rotation mixed vitamin E, comprising the following steps:

[0046] (1) 1 volume part of mixed vitamin E with a mass percentage content of 50% is added to 4 volume parts of an ethanol aqueous solution with a volume percentage concentration of 95%, and fully dissolved at 50° C.;

[0047] (2) The solution obtained in step (1) with 3 times the volume of the anion exchange resin is subjected to adsorption and separation through an anion exchange resin (model 201*7), the adsorption time is 6 hours, and the effluent is removed to recover ethanol;

[0048] (3) Adding an aqueous ethanol solution with a concentration of 95% by volume in the anion exchange resin after adsorption, until the effluent is colorless;

[0049](4) feed sulfur dioxide gas and analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.3MPa, and the time is 10 minutes;

[0050] (5) Carry out elution with an ethanol aqueous soluti...

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Abstract

The invention discloses a method for preparing a high-purity and high-optical rotation mixed vitamin E, which comprises the following steps: dissolving a low-content mixed vitamin E into ethanol water; carrying out absorptive separation of anion exchange resin; adding ethanol water into the mixed solution till an effluent is colorless; passing an acidic gas through the mixed solution for analysis; eluting with the ethanol water and concentrating an eluate; adding first-grade edible oil into a concentrate of the eluate with mixing; and subjecting the mixture to three-stage molecular distillation and obtaining the high-purity and high-optical rotation vitamin E. The method overcomes the separation difficulty caused by a plurality of solvents adopted, reduces production cost, simplifies operation, tremendously enhances the color and luster of products, greatly reduces the content of sterol in the raw material, and improves the product purity, optical rotation fluidity and transparency. The products have almost no residual solvent and can be used more safely in food industry and other industries.

Description

technical field [0001] The invention relates to a method for preparing vitamin E, in particular to a method for preparing vitamin E with high purity and high optical rotation. Background technique [0002] Natural vitamin E is an ester-soluble vitamin. It is mainly obtained from the deodorized distillate obtained during the refining process of vegetable oil (referred to as DD oil). Free fatty acids and neutral oils are converted into fatty acid methyl esters through esterification and transesterification, and then crystallized by cold crystallization. Most of the sterols are removed, and then separated by molecular distillation, but the purity is low, generally 30-50%. Natural vitamin E is a mixed type of vitamin E, mainly composed of four isomers α, β, γ, and δ. At present, the purity of natural vitamin E produced by most domestic manufacturers is about 50%, with poor transparency and low optical rotation. The main reason is that the presence of small molecular neutral oi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
Inventor 曹玉平陈学兵倪少利蒋一鸣韩军武文华
Owner COFCO GROUP
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