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Preparation of mixing vitamin E

A technology of mixing vitamins and anions, applied in organic chemistry and other directions, can solve problems such as difficulty in solvent separation, achieve the effects of application safety, reduce sterol content, and simplify operation

Active Publication Date: 2011-05-04
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 solvent separation difficulties caused by the use of multiple solvents in the prior art, and to provide a method for preparing mixed vitamin E using a single solvent

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] A preparation method of mixed vitamin E, comprising the steps:

[0025] (1) 150 grams of mixed vitamin E (VE: 47.52% (w / w), sterol: 9.15% (w / w), others: 43.65% (w / w), specific optical rotation is +17°) was added In 300ml of 95% ethanol aqueous solution by volume, fully dissolve at 35°C;

[0026] (2) The solution obtained in the step (1) of 2 times the volume of the anion exchange resin is subjected to adsorption separation by anion exchange resin JK206 (adsorption column: φ20mm*800mm), and the adsorption time is 2 hours, and the effluent is recovered ethanol;

[0027] (3) in the anion exchange resin after adsorption, add the ethanol aqueous solution that the volume percent concentration is 95%, wait for the effluent to be colorless; collect the effluent to concentrate and reclaim ethanol;

[0028] (4) feeding carbon dioxide gas to analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.1MPa, and the time is 10 minutes;

[0029] (5) eluti...

Embodiment 2

[0036] A preparation method of mixed vitamin E, comprising the steps:

[0037] (1) adding 1 volume part of the mixed vitamin E with a mass percentage content of 10% to 0.5 volume part of ethanol with a volume percentage concentration of 100%, fully dissolving at 25°C;

[0038] (2) the solution obtained in the described step (1) of 0.5 times the volume of the anion exchange resin is subjected to adsorption separation by anion exchange resin (model HZ202), and the adsorption time is 1 hour, and the effluent goes to recover ethanol;

[0039] (3) adding the ethanol with a volume percentage concentration of 100% to the anion exchange resin after the adsorption, until the effluent is colorless;

[0040] (4) feeding carbon dioxide gas to analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.01MPa, and the time is 2 hours;

[0041] (5) eluting with 100% ethanol aqueous solution by volume percentage, collecting the eluent until the eluent is colorless;...

Embodiment 3

[0046] A preparation method of mixed vitamin E, comprising the steps:

[0047] (1) adding 1 volume part of the mixed vitamin E with a mass percentage of 50% to 4 volume parts of an aqueous ethanol solution with a volume percentage concentration of 95%, fully dissolving at 50°C;

[0048] (2) the solution obtained in the step (1) of 3 times the volume of the anion exchange resin is subjected to adsorption separation by anion exchange resin (model 201*7), and the adsorption time is 6 hours, and the effluent goes to recover ethanol;

[0049] (3) adding an ethanol aqueous solution with a volume percent concentration of 95% to the anion exchange resin after the adsorption, until the effluent is colorless;

[0050] (4) introducing sulfur dioxide gas to analyze the anion exchange resin through step (3), the gas pressure is controlled at 0.3MPa, and the time is 10 minutes;

[0051] (5) eluting with 95% ethanol aqueous solution by volume percentage, collecting the eluent until the eluent...

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PUM

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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 preparation method of vitamin E, in particular to a preparation method of mixed vitamin E. Background technique [0002] Natural vitamin E is an ester-soluble vitamin. It is mainly the deodorized distillate obtained from the refining process of vegetable oil (DD oil for short) through esterification and transesterification. Free fatty acids and neutral oils are converted into fatty acid methyl esters, and then crystallized by cold precipitation. 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 small optical rotation. The main reason for this is that the presence of small molecules of neutral oils and sterols affects its purity, clarity ...

Claims

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Application Information

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Patent Type & Authority Patents(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