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Synthesis and refining process of d-alpha-tocopheryl acetate

A technology of tocopherol acetate and tocopherol, which is applied in the field of chemical engineering, can solve the problems of increased cost of raw materials, large amount of solvent used, and large environmental pollution, and achieves the effects of simple operation, small amount of solvent used, and low reaction temperature

Pending Publication Date: 2022-03-18
NINGBO DAHONGYING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. A catalyst is required to participate in the synthesis reaction. The catalyst needs to use organic acid-base or lipase, and the catalyst needs to be removed later, which increases the cost of raw materials; and the organic acid-base as a catalyst has higher requirements on equipment; a large amount of water washing is required in the follow-up Catalyst removal, high processing cost, and large environmental pollution;
[0005] 2. Using silica gel chromatography purification and resin separation and purification as the follow-up purification process, the process is long, the operation is complicated, the amount of solvent is large, more than 20 times, and the cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 100g of d-alpha-tocopherol concentrate (the mass content of d-alpha-tocopherol is 88%), add 50g of acetic anhydride and 300ml of n-hexane, heat it to 68°C after completely dissolving, and keep the n-hexane to continue to distill out during the reaction , After the evaporated solvent is condensed, the acetic acid is removed through the water layer, and the clean n-hexane is refluxed into the reaction system. After reacting for 6 hours, add 5g of hot water (50-60°C) to wash, let the layers stand, and separate the water layer , and then add 3g hot water (50-60°C) to repeat washing twice, evaporate the solvent under reduced pressure, then molecularly distill, vacuum degree 1Pa, collect 180-220°C fractions to obtain 92.1g of the product, d-α-tocopherol The content of acetate is 98.2%.

Embodiment 2

[0031] Take 100g of d-alpha-tocopherol concentrate (the mass content of d-alpha-tocopherol is 67%), add 55g of acetic anhydride and 300ml of petroleum ether, heat it to 70°C after completely dissolving, and keep the petroleum ether continuously distilled out during the reaction After the evaporated solvent is condensed, acetic acid is removed through the water layer, and clean petroleum ether is refluxed into the reaction system. After reacting for 7 hours, add 3g of hot water (50-60°C) to wash, let the layers stand, separate the water layer, and then Add 3g of hot water (50-60°C) to wash repeatedly twice, evaporate the solvent under reduced pressure, then molecularly distill at a vacuum of 1Pa, collect fractions at 180-220°C to obtain 67.8g of the product, d-α-tocopheryl acetate The content of 96.1%.

Embodiment 3

[0033] Take d-alpha-tocopherol concentrated solution 100g (mass content of d-alpha-tocopherol 82%), add 50g acetic anhydride, 300ml toluene, after dissolving completely, heat to 101 ℃, keep the toluene to continuously steam out during the reaction process, steam After the solvent is condensed, the acetic acid is removed through the water layer, and the clean toluene is refluxed into the reaction system. After reacting for 6 hours, add 3g of hot water (50-60°C) to wash, let the layers stand, separate the water layer, and then add 5g of hot water in sequence (50-60 DEG C) repeated washing twice, evaporated the solvent under reduced pressure, then molecular distillation, vacuum degree 1Pa, collected 180-220 DEG C fractions, obtained product 86.2g, the content of d-alpha-tocopheryl acetate was 96.7%.

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Abstract

The invention discloses a synthetic refining process of d-alpha-tocopheryl acetate, which comprises the following steps: mixing a d-alpha-tocopheryl concentrated solution, acetic anhydride and a solvent, carrying out organic synthesis reaction at 67-110 DEG C, and removing acetic acid generated in the reaction process and the solvent through azeotropic distillation; after the reaction is finished, adding a proper amount of water, extracting for at least two times under the condition of 50-60 DEG C, and separating a water layer; evaporating to remove a solvent to obtain a d-alpha-tocopheryl acetate concentrated solution; and carrying out molecular distillation on the d-alpha-tocopheryl acetate concentrated solution, and collecting a fraction at 180-220 DEG C under the vacuum degree of 1pa or below, so as to obtain the d-alpha-tocopheryl acetate. Wherein the solvent is one of normal hexane, petroleum ether and methylbenzene. According to the method, n-hexane / petroleum ether / toluene is introduced as a solvent, and no acid-base catalyst is introduced in the whole process, so that the raw material cost is greatly reduced, the reaction temperature is low, and the conversion rate is high; and a washing extraction purification process is subsequently matched, so that the method is small in solvent consumption, simple to operate and suitable for industrial popularization and application.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a process for synthesizing and refining d-alpha-tocopheryl acetate. Background technique [0002] At present, the preparation of natural d-α-tocopherol acetate is generally obtained by esterifying d-α-tocopherol with acetic anhydride under catalyst conditions. The catalysts used include acid catalysts, alkaline catalysts and lipase, etc.; the preparation methods include solvent method and solvent-free method; and the reaction temperature is either high or low. In the related art, there are many studies on the synthesis process of natural d-α-tocopherol acetate, but there are few studies on the subsequent purification process, mainly focusing on silica gel chromatography purification, resin separation and purification and other methods. [0003] The above-mentioned conventional d-alpha-tocopheryl acetic anhydride preparation process mainly has the following problems:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 王嘉磊章城亮姚瑞周勇李泽辉汪俊胜武玉洁
Owner NINGBO DAHONGYING BIO ENG