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Preparation technology for natural vitamin E

A natural vitamin and preparation technology, applied in the direction of organic chemistry, can solve the problems of low yield, excessive use of organic solvents, and many purification steps, and achieve high yield, qualified optical rotation, and more transparent color.

Active Publication Date: 2014-08-06
JIANGSU XIXIN VITAMIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to provide a purification process for natural vitamin E in view of the problems that there are many purification steps, low yield and many organic solvents used in the current natural vitamin E.

Method used

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  • Preparation technology for natural vitamin E

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Soybean oil fatty acid 1Kg is put into three-necked flask, 95 oC After vacuum degassing in a water bath, the material was cooled to 65 oC Thereafter, concentrated sulfuric acid (20 ml) was added with stirring, and methanol (340 ml) was added. The water bath was added and the temperature was raised to 65 oC , control the temperature in the kettle at 64-78 degrees and stir and reflux for 60min. After reflux, add the material to 90 oC The above hot water 150ml, wash with water, discard the water layer, put the oil layer in 5 oC Cold analysis in the environment, crystallization of phytosterols. Put the material into the filter press tank for press filtration to obtain oily liquid. oily liquid at 120 oC , Distilled at a pressure of 1pa. The residual component after distillation is natural vitamin E crude product with a purity of 48%.

[0025] The above natural vitamin E crude product is carried out column chromatography using a macroporous nonpolar resin, at a f...

Embodiment 2

[0027] Soybean oil fatty acid 1Kg is put into three-necked flask, 95 oC After vacuum degassing in a water bath, the material was cooled to 65 oC Thereafter, concentrated sulfuric acid (20 ml) was added with stirring, and methanol (240 ml) was added. The water bath was added and the temperature was raised to 65 oC , control the temperature in the kettle to 64-78 oC Stir and reflux for 60min. After reflux, add the material to 90 oC The above hot water 220ml, wash with water, discard the water layer, put the oil layer in 10 oC Cold analysis in the environment, crystallization of phytosterols. Put the material into the filter press tank for press filtration to obtain oily liquid. oily liquid at 130 oC , Distilled at a pressure of 5pa. The residual component after distillation is natural vitamin E crude product with a purity of 40%.

[0028] The above-mentioned natural vitamin E crude product is carried out column chromatography using a macroporous non-polar resin, a...

Embodiment 3

[0030] Soybean oil fatty acid 1Kg is put into three-necked flask, 95 oC After vacuum degassing in a water bath, the material was cooled to 65 oC Next, add concentrated sulfuric acid (20ml) and ethanol (440ml) while stirring. The water bath was added and the temperature was raised to 65 oC , control the temperature in the kettle to 64-78 oC Stir and reflux for 60min. After reflux, add the material to 90 oC Wash with 300ml of the above hot water, discard the water layer, place the oil layer in a 10-degree environment for cold analysis, and crystallize phytosterols. Put the material into the filter press tank for press filtration to obtain oily liquid. oily liquid at 120 oC , Distilled at a pressure of 10pa. The residual component after distillation is the natural vitamin E crude product with a purity of 52%.

[0031] The above-mentioned natural vitamin E crude product is carried out column chromatography using non-polar resin, at a flow rate of 5ml / min, the temperat...

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Abstract

The invention discloses a preparation technology for a natural vitamin E. The preparation technology comprises esterification, water washing, cold crystallization, solid-liquid separation, molecular distillation, column chromatography adsorption, and secondary molecular distillation and the like; according to the preparation technology for the natural vitamin E, the molecular distillation technology and the column chromatography technology are combined, so that the higher-purity natural vitamin E is prepared; the adsorption resin is a filling agent and used for purifying the natural vitamin E through column chromatography, the total content of the natural Vitamin E product prepared is 90% above, and the total yield is 80% above. Because the molecular distillation is performed for two times, by-products can be removed to the greatest extent, the natural vitamin E with good quality, more transparent color, qualified optical rotation, and high quality can be prepared; the process route has the characteristics that the steps are less, the yield is high, and the operation condition is mild; meanwhile, the process can be reduced greatly, the high-purity natural vitamin E can be obtained, the yield is higher, and the cost is reduced.

Description

technical field [0001] The invention relates to a preparation process of natural vitamin E, in particular to a preparation and purification process for obtaining high-purity natural vitamin E. Background technique [0002] Natural vitamin E, also known as natural tocopherol, is an antioxidant and nutritional agent with excellent performance. It also has the characteristics of high biological activity and food safety. It is widely used in medicine, health products, food, cosmetics and other fields A hot product that has attracted much attention in recent years. [0003] Natural vitamin E is mainly extracted from the deodorized distillate, a by-product of the vegetable oil refining process. There are foreign mixed vitamin E series products with vitamin E content of 50%, 70%, and 90%. There are already "natural vitamin E concentrated oil" products in China, the content of which is about 50%. Not only the content is low, but also the product has poor transparency and low speci...

Claims

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Application Information

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IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 印建国
Owner JIANGSU XIXIN VITAMIN
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