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Preparation method of vitamin E acetate

A technology of acetate and vitamin, applied in the field of preparation of vitamin E acetate, can solve the problems of large energy consumption, influence yield and quality, low conversion rate, etc., to reduce reaction by-products, improve product yield and by-products less effect

Inactive Publication Date: 2014-05-14
ANHUI BBCA FERMENTATION TECH ENG RES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003]The industrialized condensation process of tocopherol is generally under anhydrous conditions, in the catalytic system of zinc halide and hydrogen halide, from 2,3,5-trimethylhydroquinone and Isophytol condensation requires a large amount of zinc halide to be consumed in the reaction process, and it is difficult to reuse and the conversion rate is low. There are by-products 2,3,5-trimethylhydroquinone diacetate, a Byproducts such as acetate and incomplete closure of the color ring seriously affect the yield and quality of the synthesis
There is also the synthesis of vitamin E acetate with 2,3,5-trimethylhydroquinone diacetate under the action of zinc bromide and hydrogen bromide catalysts in industrial production. The reaction system is also an anhydrous environment, and the repeated use of zinc bromide consumes a lot of energy
In addition, polyperfluoroalkene sulfonic acid is used as a catalyst to synthesize tocopherol in benzene or toluene organic solvents. The catalyst is expensive to use, and the solvent is generally poisonous and harmful.
There are also patent reports that the condensation and esterification steps are carried out at the same time, and a small amount of water is introduced, the yield and product quality are improved, but at the same time, there are also problems such as high energy consumption of zinc chloride, and difficult removal of pigments and impurities in the aqueous phase.

Method used

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  • Preparation method of vitamin E acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 600g of n-pentane and 300g of 2,3,5-trimethylhydroquinone to a 2L four-neck flask equipped with a stirrer, thermometer, oil-water separator, condenser tube, nitrogen inlet and isobaric titration funnel , 6g of n-tridecylamine and 200g of zinc chloride, add 5mL of hydrochloric acid with a mass fraction of 31%, stir and heat up to 36°C under nitrogen protection, and drop in 605g of isophytic alcohol at a constant pressure for 2 hours, drop After adding, keep warm for 1 hour, add 100mL of water to wash, add n-butanol to the washing liquid, extract, and then separate the liquid through the oil-water separator. The aqueous phase containing zinc chloride is reserved for the next step, and the organic phase is distilled to remove the solvent. Then add 200g of acetic anhydride, carry out esterification reaction at 140°C for 3 hours under the protection of nitrogen, recover the unreacted acetic anhydride, wash with water and distill at 140°C under normal pressure, the bottom ...

Embodiment 2

[0027] In a 2L four-neck flask equipped with a stirrer, a thermometer, an oil-water separator, a condensing tube and a nitrogen inlet isobaric titration funnel, add 600g of n-hexane, 300g of trimethylhydroquinone, 6g of n-tridecylamine, For the aqueous phase containing zinc chloride in the above example 1, add 40 g of zinc chloride, add 5 mL of hydrobromic acid (mass fraction 30%), stir and heat up to 98 ° C under the protection of nitrogen, and reflux within 2.5 hours. Add 605g of isophytic alcohol dropwise at a constant speed, while adding dropwise, use the oil-water separator to recover the water in the mixed solution. After the dropwise addition is completed, reflux and keep warm for 1 hour, add 100mL of water for washing, and add n-butanol to the washing solution. Extraction, and then liquid separation by oil-water separator, the water phase is a colorless solution, the oil phase is washed with water, and the water phase is combined twice for the next step, the organic pha...

Embodiment 3

[0029] Add 600g of n-heptane, 300g of trimethylhydroquinone, and 6g of n-tridecylamine to a 2L four-neck flask equipped with a stirrer, a thermometer, an oil-water separator, a condenser tube, and an isobaric titration funnel at the nitrogen inlet. Combined with the aqueous phase containing zinc chloride in Example 2 above, add 20g of zinc chloride, add 5mL of hydrobromic acid (mass fraction 30%), stir and heat up to 98°C under nitrogen protection, and reflux at 2.5 Add 605g of isophytic alcohol dropwise at a constant pressure and at a constant speed for 1 hour, and recover water while adding dropwise. Separation device, the aqueous phase containing zinc chloride is reserved for the next step, the organic phase is distilled to remove the solvent, then 200g of acetic anhydride is added, and the esterification reaction is carried out at 140°C for 3 hours under the protection of nitrogen, the unreacted acetic anhydride is recovered, washed with water and Atmospheric pressure dist...

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Abstract

The invention relates to a preparation method of vitamin E acetate. The preparation method comprises the following steps: by taking linear chain type organic amine, zinc halide and hydrogen halide as catalysts, reacting 2,3,5-trimethylhydroquinone with isophytol to generate tocopherol; and taking the tocopherol and acetic anhydride to have an esterification reaction to obtain the vitamin E acetate. The preparation method is simple in steps and moderate in conditions; the catalyst can be repeatedly utilized and few byproducts are generated; the purity and the yield of the product are higher than those of the product obtained by adopting the prior art and the preparation method is suitable for popularization.

Description

technical field [0001] The invention relates to a preparation method of vitamin E acetate, which belongs to the field of organic synthesis. Background technique [0002] The main commercial form of vitamin E is vitamin E acetate and other derivatives, which are mainly produced synthetically from tocopherol. The industrial synthesis of tocopherol is based on the condensation of trimethylhydroquinone and isophytol, phytol or its derivatives. react as figure 1 shown. [0003] The industrial condensation process of tocopherol is generally condensed by 2,3,5-trimethylhydroquinone and isophytic alcohol in a zinc halide and hydrogen halide catalytic system under anhydrous conditions. A large amount of zinc halide is consumed during the reaction process. Moreover, it is difficult to reuse, and the conversion rate is low. There are by-products such as 2,3,5-trimethylhydroquinone diacetate, monoacetate, and incomplete closure of the color ring in the generated vitamin E acetate, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 李荣杰尚海涛杨为华张飞吴鹏举何玉春纪传侠
Owner ANHUI BBCA FERMENTATION TECH ENG RES
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