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A method for preparing high-content mixed tocopherols by extraction and separation of lyotropic liquid crystals

A technology of lyotropic liquid crystals and tocopherols, which is applied in the fields of chemical engineering and natural product separation, can solve problems such as the inability to separate high-content mixed tocopherols with high efficiency and low energy consumption, and achieve good application prospects, environmental friendliness, and high extraction capacity.

Active Publication Date: 2018-07-06
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] The invention provides a method for preparing high-content mixed tocopherols by extraction and separation of lyotropic liquid crystals, which solves the problem in the prior art that high-content mixed tocopherols cannot be separated with high efficiency and low energy consumption, and is environmentally friendly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] The extraction agent is prepared by dissolving choline laurate in DMSO, wherein the molar fraction of choline laurate is 5%; take the deodorized distillate of vegetable oil after esterification (which contains 20% mixed tocopherols), dissolve it in n-hexane , and made into a 150mg / ml raw material solution. Under the condition that the liquid flow ratio of the extractant to the raw material is 1:0.5, after 4 stages of countercurrent extraction at 40°C, the extract phase is collected, 2 times the volume of acetonitrile and water are added thereto, back-extracted with 3 times the volume of n-hexane, and the Evaporation, washing, drying and other post-treatment steps to obtain mixed tocopherol products, the purity of which is 93%, and the yield is 98%.

Embodiment 2

[0049] Dissolve tetraethylquaternary ammonium laurate in DMSO to prepare extractant, wherein the molar fraction of tetraethylquaternary ammonium laurate is 10%; get the vegetable oil deodorization distillate after esterification (which contains mixed tocopherols 75%), dissolved in petroleum ether with a boiling range of 60-90°C, and made into a 100mg / ml raw material solution. Under the condition that the liquid flow ratio of extractant to raw material is 1:10, after 4 stages of countercurrent extraction at 30°C, the extract phase is collected, 3 times the volume of water and acetonitrile are added to it, and the boiling range is 60 Petroleum ether back-extraction at ~90°C, after evaporation, water washing, drying and other post-treatment steps, the mixed tocopherol product is obtained, with a purity of 92% and a yield of 90%.

Embodiment 3

[0051] The extraction agent is prepared by dissolving 1-ethyl-3-methylimidazole laurate in acetonitrile, wherein the molar fraction of 1-ethyl-3-methylimidazole laurate is 15%; take the vegetable oil after esterification The deodorized distillate (which contains 25% mixed tocopherols) is dissolved in petroleum ether with a boiling range of 90-120° C. to prepare a 125 mg / ml raw material solution. Under the condition that the liquid flow ratio of extractant, washing agent and raw material is 1:0.2:0.5, after three-stage fractional distillation extraction operation at 30°C, the extract phase is collected, and a certain amount of DMF and acetonitrile are added to it, and the boiling range is 90~ Back extraction with petroleum ether at 120°C, followed by evaporation, water washing, drying and other post-processing steps to obtain mixed tocopherol products with a purity of 95% and a yield of 99%.

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Abstract

A method for preparing high-content mixed tocopherols through lyotropic liquid crystal extraction and separation, comprising the following steps: dissolving vegetable oil deodorized distillate which is esterified or is subjected to fatty acid removal in a weak-polar organic solvent to prepare a feed solution; mixing ionic liquid or a surfactant with a polar diluent to prepare lyotropic liquid crystals; and separating and purifying the feed solution through countercurrent extraction or fractional extraction by taking the lyotropic liquid crystals as an extraction agent, thus obtaining mixed tocopherols. A lyotropic liquid crystal extraction agent in the present application has high extraction capacity on tocopherols, and the dosage of the extraction agent and the number of theoretical plates required for extraction can be obviously reduced; the lyotropic liquid crystal extraction agent which is adopted still can keep high extraction efficiency and selectivity under a higher feed concentration, the mixed tocopherols of which the purity is larger than 90% can be obtained, and the recovery rate of the mixed tocopherols is more than 90%.

Description

technical field [0001] The invention relates to a method for extracting and separating mixed tocopherols in vegetable oil deodorization distillates, belonging to the fields of chemical engineering and natural product separation. Background technique [0002] Natural Vitamin E, scientific name Tocopherols (Tocopherols), also known as mixed tocopherols, is a commonly used medicine and health care product. Due to its important antioxidant and physiological functions, it has become a widely used product in the international market. , an important vitamin variety with a large production and sales volume, together with vitamin C and vitamin A, it has become the three pillar products of the vitamin series. At the same time, the safety and physiological activity of natural vitamin E are far superior to synthetic vitamin E, so the preparation of high-content natural vitamin E has important economic value. Vegetable oil is the main source of natural vitamin E, but its content is only...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 邢华斌刘献献杨启炜杨亦文任其龙苏宝根鲍宗必张治国苏云
Owner ZHEJIANG UNIV