Method of preparing vitamin E acetate

A technology for acetate and vitamin, applied in the field of preparation of vitamin E acetate, can solve problems such as difficulty in large-scale industrial production, difficult treatment of process waste liquid, corrosion of catalyst to equipment, etc., and achieves reactivity and product selectivity. The effect of improving, improving product quality, and stabilizing product vitamin E acetate

Active Publication Date: 2017-04-19
WANHUA CHEM GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, as we all know, it is difficult to realize large-scale industrial production of biological esterase in fine chemical production, and the enzymatic hydrolysis process is demanding, which makes the process route more complicated and economical.
[0008] In summary, it can be seen that the current method for preparing vitamin E acetate has the problem of catalyst corrosion to equipment or difficulty in recycling, and the process route is complicated, requiring multi-step reactions to obtain the final product vitamin E acetate, and some process waste liquids are difficult to handle , environmental protection pressure and other issues

Method used

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  • Method of preparing vitamin E acetate
  • Method of preparing vitamin E acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] Cocatalyst 1 preparation method is as follows:

[0058] Preparation of MCM-48 molecular sieve: Add 10g of cetyltrimethylammonium bromide (CTAB) into 100g of pure water, then add 110g of methanol and 20g of concentrated ammonia water respectively, after ultrasonication at room temperature for 30min, add 15g of ethyl orthosilicate dropwise Ester (TEOS), ultrasonicated for 30 minutes at room temperature, filtered with suction and washed with pure water to pH = 7, dried at 120°C for 2 hours and ground into powder, then placed in a muffle furnace and roasted at 800°C for 4 hours to obtain MCM- 48 molecular sieves.

[0059] A 1 Xa / A 2 / MCM-48 molecular sieve preparation: under nitrogen protection conditions, 2.5g FeCl 2 Add 1.0g of nanoscale Fe particles into 400g of pure water, stir and mix fully at room temperature, add 60g of the prepared MCM-48 molecular sieve into it, stir fully at 50°C for 2h, and dry at 120°C for 6h after stirring to obtain FeCl 2 / Fe / MCM-48 molecu...

Embodiment 2-7

[0061] The preparation method of cocatalyst 2-7 is similar to that of cocatalyst 1, and the material ratio and detailed material composition are shown in Table 1 below:

[0062] Table 1 cocatalyst 2-7 preparation raw material formula table

[0063]

[0064]

Embodiment 8

[0066] Add 70.0g of TMHQ-DA, 30.2g of acetic anhydride and 142.3g of glacial acetic acid into a 500mL three-neck flask, heat to 70°C to completely dissolve TMHQ-DA, start stirring, add 1.40g of cocatalyst 1, and pass through at a speed of 7.4mL / min Add hydrogen chloride gas, then start to add IPL (87.9g) dropwise, add dropwise for 120min, continue to react for 60min after the dropwise addition is completed, stop feeding hydrogen chloride gas, sample analysis, the conversion rate of raw material TMHQ-DA is 99.6%, and the product vitamin E acetic acid The ester selectivity is 98.3%. Stirring was stopped, and after standing for 3 minutes, the reaction solution was divided into two layers, the upper layer being the vitamin E acetate product phase, and the lower layer being the cocatalyst and solvent phase.

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Abstract

The invention provides a method of preparing vitamin E acetate. The method includes the steps of: feeding hydrogen halide gas as a catalyst, supporting a metal halide and elementary metal on a molecular sieve to obtain a cocatalyst and a stabilizing agent, and performing a reaction to 2,3,5-trimethylhydroquinone diester (TMHQ-DA) and iso-phytol (IPL) to produce the vitamin E acetate (VEA). The method has high catalyst activity and has low corrosion on equipment, wherein the raw material is converted into the vitamin E acetate directly through one step. The product has good stability and the method is easy to carry out in industrial enlarged production.

Description

technical field [0001] The invention relates to a preparation method of vitamin E acetate, which belongs to the field of fine chemical synthesis. Background technique [0002] Vitamin E (Vitamin E) is a fat-soluble vitamin, and its hydrolyzed product is tocopherol, which is one of the most important antioxidants. Tocopherol can promote the secretion of sex hormones, increase the vitality and quantity of sperm in men; increase the concentration of estrogen in women, improve fertility, prevent miscarriage, and can also be used to prevent and treat male infertility, burns, frostbite, capillary bleeding, menopausal syndrome, Beauty and so on. Vitamin E acetate has broad application prospects and market value in medicine, food, cosmetics, feed and other fields. [0003] German published patent document DE2000111402 discloses a method using zinc halide (Lewis acid) and aqueous protonic acid (Bronsted acid) as a catalyst, through the condensation of trimethylhydroquinone diester ...

Claims

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Application Information

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IPC IPC(8): C07D311/72B01J29/03B01J29/04
CPCC07D311/72B01J29/0333B01J29/044B01J27/08B01J2229/186B01J35/19
Inventor 郭劲资张涛程晓波吕英东张旭王延斌朱龙龙张秀秀于学丽黎源华卫琦
Owner WANHUA CHEM GRP
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