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Method for recovery of d-alpha-tocopherol from natural vitamin E leftover material

A technology of natural vitamins and tocopherols, applied in organic chemistry and other directions, can solve the problems of large consumption of fillers and solvents, high separation costs, and complex processes.

Active Publication Date: 2017-01-11
ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Patents CN102382095, CN104130233, CN101220018, etc. use ion exchange chromatography or simulated moving bed chromatography to separate mixed tocopherols to obtain high-purity d-α-tocopherol, d-γ-tocopherol and d-δ-tocopherol, because each tocopherol The structural difference of the homologue is small, it needs to consume a large amount of fillers and solvents, the separation cost is high, and the process is complicated, so it is not easy for industrial application

Method used

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  • Method for recovery of d-alpha-tocopherol from natural vitamin E leftover material
  • Method for recovery of d-alpha-tocopherol from natural vitamin E leftover material
  • Method for recovery of d-alpha-tocopherol from natural vitamin E leftover material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the 1st stage rectification step (1.1) of scrap

[0026] Such as figure 1 As mentioned above, 500 g of scraps (derived from untransformed d-α-tocopherol during the extraction process of amine methylation reaction, specifically refer to Chinese patent CN102633766) were added to a 1L round-bottomed Erlenmeyer flask, wherein the total tocopherol content was 10.2 %, d-alpha-tocopherol relative to 97.5%. A glass rectification tower with an inner diameter of 2.6mm and a height of 700mm is used. The tower is filled with 30mm*30mm stainless steel θ rings. The tower is equipped with a silver-plated jacket and an electric heating jacket for heat preservation. The transformer controls the heating power of the heating jacket and the reflux ratio controller. Carry out rectification under the vacuum degree of 20-40Pa at the top of the tower. The kettle temperature was 200°C, the tower top temperature was 160°C, and the appropriate reflux ratio was adjusted to distill ...

Embodiment 2

[0029] Embodiment 2: the 1st stage rectification step (1.1) of scrap

[0030] Such as figure 1 Said, in a 1L round-bottomed Erlenmeyer flask, add scraps (derived from untransformed d-α-tocopherol in the extraction process of amine methylation reaction, see Chinese patent CN102633766) (500g, wherein the total tocopherol content is 15.8% , d-α-tocopherol is relatively 96.2%.Use a glass rectification tower with an inner diameter of 2.6mm and a height of 500mm. The tower is filled with a 30mm*30mm stainless steel θ ring. The tower is equipped with a silver-plated jacket and an electric heating jacket for heat preservation. Transformer control Heating mantle heating power, reflux ratio controller. Rectification is carried out under the vacuum degree of 20-40Pa at the top of the tower. The temperature of the kettle is 190°C, and the temperature of the top of the tower is 160°C. Adjust the appropriate reflux ratio to distill 286g of light components, and the remaining 207g Heavy compo...

Embodiment 5

[0037] Embodiment 5: the 2nd stage rectification step (1.2) of scrap

[0038] Such as figure 1 As described above, 300g of the heavy component in Example 1 is introduced into the second-stage rectification tower, wherein the inner diameter of the tower is 2.6mm, the height of the tower is 350mm, and the tower is filled with a 30mm*30mm stainless steel θ ring, and the outer belt of the tower is silver-plated. The electric heating jacket is kept warm, the transformer controls the heating power of the heating jacket, and the reflux ratio controller. Under the vacuum condition of 10-20Pa, the kettle temperature is 240°C, and the tower top temperature is 210°C, most of the squalene is distilled out. 128 g of light components were distilled off, 167 g of heavy components remained, 5 g was lost. The total tocopherol content and yield in each component are shown in Table 5 (test results of Example 5);

[0039] table 5

[0040] components mass (g) Total Tocopherol Con...

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Abstract

The invention discloses a method for recovery of d-alpha-tocopherol from natural vitamin E leftover material. The high content d-alpha-tocopherol can be prepared from the natural vitamin E extraction leftover material as a raw material by the technology of a combination of rectification and ion exchange chromatography. Specific steps are as follows: the natural vitamin E extraction leftover material is separated by a two-stage rectifying column, a heavy component after two-stage rectifying is used as a raw material for separation by use of ion exchange chromatography, and after adsorption, replacement, desorption, regeneration and other steps, finally the purely natural high content alpha-tocopherol can be prepared by molecular distillation, wherein the content of total tocopherol in the purely natural high content alpha-tocopherol is greater than or equal to 95.0%, and the relative content of the d-alpha-tocopherol in the pure natural high content alpha-tocopherol is greater than or equal to 96.0%. Compared with the d-alpha-tocopherol produced by a traditional preparation method, the d-alpha-tocopherol prepared by the method is not chemically transformed, the method is safer, green, healthy, simple in process, high in separation efficiency, and easy in industrial production, the obtained d-alpha-tocopherol is high in content and low in cost, and the comprehensive utilization of effective components in the leftover material can be realized.

Description

technical field [0001] The invention relates to a production method of natural vitamin E, in particular to a method for preparing high-content d-alpha-tocopherol monomers from leftovers after extracting natural vitamin E. [0002] technical background [0003] Natural vitamin E (Vitamin E, referred to as VE), also known as anti-sterility vitamin, is a general term for tocopherol, tocotrienol and d-α-tocopherol active derivatives, widely present in animal and vegetable fats, organs, Vegetable oil and chlorophyll. Industrially, natural VE is obtained by using the deodorized distillates of vegetable oils such as soybean oil rich in natural tocopherols as raw materials, and undergoes a series of transformation, separation, distillation and concentration. Natural VE has many functions such as improving fertility rate and anti-oxidation, and is widely used in medicine, food, health food and cosmetics. At present, the annual demand for natural VE series products in the world is ab...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 代志凯赵健李祥清马金萍许新德邵斌
Owner ZHEJIANG MEDICINE CO LTD XINCHANG PHAMACEUTICAL FACTORY
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