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Method for separating D-alpha-tocofecol from mixed tocofecol

A technology of tocopherol and binary mixing, which is applied in the field of chemical engineering, can solve the problems of consuming large resins and solvents, cannot realize industrialization, and is difficult for industrial application, etc., and achieves easy recycling and utilization, high selective separation ability, and low consumption Effect

Inactive Publication Date: 2009-05-27
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] U.S. patents US 3122565, US 3402183, and US 2005 / 131240 all use ion exchange resins to separate tocopherols, and obtain high-purity D-α-tocopherols, D-γ-tocopherols, and D-δ-tocopherols. Phenol homologues have very little structural difference, consume a large amount of resin and solvent, and the separation cost is too high to realize industrialization; U.S. Patents US 4480108, US 4602098, US 4607111, etc. are based on D-α-tocopherol, D-β-tocopherol , D-γ-tocopherol and D-δ-tocopherol ester derivatives have different degrees of difficulty in the deacylation reaction, and the deacylation reaction is combined with chromatographic separation or distillation to achieve the separation of each tocopherol homolog
This type of method does not directly use tocopherol as the raw material for separation, and the process is relatively complicated, so it is not easy for industrial application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Raw material mixed tocopherol (wherein the total content of D-α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol is 98%) is dissolved in n-hexane to prepare D- The total concentration of α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol was 15.3 g / L of the raw material solution. With 1-butyl-3-methylimidazolium trifluoromethanesulfonate ([bmim]CF 3 SO 3 ) as the extractant, with n-hexane as the detergent, the flow ratio of the extractant, the detergent, and the raw material liquid is 2:1:1.5, fractional distillation extraction is carried out at 35°C, the raffinate is collected, washed with water and concentrated in vacuo Finally, the D-α-tocopherol product is obtained with a purity of 97% and a yield of 99%.

Embodiment 2

[0027]Mixed raw material tocopherol (wherein the total content of D-α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol is 96%) is dissolved in n-heptane to prepare D - A stock solution in which the total concentration of α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol is 2.2 g / l. With 1-ethyl-3-methylimidazolium tetrafluoroborate ([emim]BF 4 )—acetonitrile mixed solvent is the extractant ([emim]BF 4 Mole fraction 90%), with n-heptane as detergent, the flow ratio of extractant, detergent, raw material liquid three is 2: 2: 1, fractional extraction is carried out at 30 ℃, raffinate is collected, washed with water and The D-α-tocopherol product was obtained after vacuum concentration with a purity of 97% and a yield of 98%.

Embodiment 3

[0029] Raw material mixed tocopherols (wherein the total content of D-α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol is 97%) are dissolved in ethyl acetate and formulated into D - A stock solution in which the total concentration of α-tocopherol, D-β-tocopherol, D-γ-tocopherol and D-δ-tocopherol is 4.8 g / l. With 1-butyl-3-methylimidazolium tetrafluoroborate ([bmim]BF 4 )—dimethylformamide mixed solvent is the extractant ([bmim]BF 4 Mole fraction 80%), with ethyl acetate as detergent, the flow ratio of extractant, detergent, raw material liquid three is 3: 2: 2, carry out fractional distillation extraction at 20 ℃, collect raffinate, wash with water and The D-α-tocopherol product was obtained after vacuum concentration with a purity of 96% and a yield of 98%.

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Abstract

The invention discloses a method for separating D-alpha-tocopherol from mixed tocopherol, which comprises the following steps: an ionic liquid or a binary mixed solvent consisting of the ionic liquid and a polar solvent are taken as an extracting agent, and a fractional extraction method is adopted to efficiently separate the D-alpha-tocopherol from the mixed tocopherol containing the D-alpha-tocopherol, D-beta-tocopherol, D-gamma-tocopherol and D-delta-tocopherol. The method has the advantages of high separation efficiency, less solvent consumption, low production cost, safety, environmental protection, easy for industrialized production and so on.

Description

technical field [0001] The invention relates to a method for separating D-alpha-tocopherol from mixed tocopherols, in particular to a method for selectively separating D-alpha-tocopherol from mixed tocopherols by using ionic liquid or a composite solvent composed of ionic liquid and polar solvent as a medium. The method for α-tocopherol belongs to the technical field of chemical engineering. Background technique [0002] Natural vitamin E (Natural Vitamin E) is a commonly used medicine and health care product. It has become an important vitamin variety with a wide range of uses and a large production and sales volume in the international market. Together with vitamin C and vitamin A, it has become the three pillars of the vitamin series. product. Natural vitamin E is a mixture mainly composed of four tocopherol homologues derived from tocol, including: D-α-tocopherol, D-β-tocopherol, D-γ-tocopherol phenol and D-delta-tocopherol, both with saturated C 16 The side chains di...

Claims

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Application Information

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IPC IPC(8): C07D311/72
Inventor 任其龙杨启炜邢华斌苏宝根杨亦文曹义风倪晓蕾
Owner ZHEJIANG UNIV
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