Method for preparing vitamin E acetate

A vitamin and acetate technology, which is applied in the field of vitamin E acetate preparation, can solve the problems of catalyst corrosion to equipment, difficult process waste liquid treatment, and increased unit consumption of materials, so as to improve reaction activity and product selectivity , Improve the conversion rate and selectivity, and improve the effect of antioxidant performance

Active Publication Date: 2019-05-03
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, hydrogen halide gas needs to be consumed in each batch of reaction process, the unit consumption of materials increases, and the economy needs to be improved
[0009] 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 for preparing vitamin E acetate
  • Method for preparing vitamin E acetate
  • Method for preparing vitamin E acetate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Catalyst 1 preparation method is as follows:

[0057] In this example, self-made MCM-48 molecular sieves are used, and the preparation process is as follows: Take 10 g of cetyltrimethylammonium bromide (CTAB) and add it to 100 g of pure water, then add 110 g of methanol and 20 g of concentrated ammonia water (with a concentration of 25 wt % ), after ultrasonication at room temperature for 30 minutes, 15 g of tetraethyl orthosilicate (TEOS) was added dropwise, after ultrasonication at room temperature for 30 minutes, filtered by suction and washed with pure water until pH = 7, dried at 120°C for 2 hours and ground into powder, then placed Roast in a muffle furnace at 800°C for 4 hours to obtain MCM-48 molecular sieve.

[0058] Catalyst intermediate preparation: under the condition of nitrogen protection, 1.25g FeCl 2 , Add 1.25g titanocene dichloride and 1.0g nano-scale Fe particles into 400g pure water, stir and mix thoroughly at room temperature, add 60g of the prepar...

Embodiment 2-7

[0062] The preparation method of catalyst 2-7 (CAT-2-7) is basically the same as that of catalyst 1 (CAT-1), the difference lies in the ratio of materials, the ratio of materials and the detailed material composition are shown in Table 1 below:

[0063] MCM-48 molecular sieve preparation raw material formula table in table 1 catalyst 2-7

[0064]

[0065]

[0066] Table 2 Catalyst 2-7 preparation raw material formula table

[0067]

Embodiment 8

[0069] Add 70.0g of TMHQ-DA, 30.2g of acetic anhydride and 142.3g of glacial acetic acid into a 500mL three-necked flask, heat to 70°C to completely dissolve TMHQ-DA, start stirring, add 1.40g of catalyst 1 (CAT-1), and then start to drop IPL (87.9g) was added dropwise for 120 minutes, and the reaction was continued for 60 minutes after the addition was completed. After the reaction was completed, sampling and analysis showed that the conversion rate of raw material TMHQ-DA was 99.8%, and the selectivity of product vitamin E acetate was 98.8%. Stirring was stopped, and after standing for 3 minutes, the reaction liquid was divided into two layers, the upper layer was the vitamin E acetate product phase, and the lower layer was the catalyst and solvent phase.

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Abstract

The invention provides a method for preparing vitamin E acetate. The method has the characteristic of high product selectivity; a catalyst used in the method provided by the invention facilitates recovery and reutilization and has less corrosion to equipment; and a product has good stability. The method for preparing the vitamin E acetate provided by the invention prepares the vitamin E acetate through a reaction of 2,3,5-trimethylhydroquinone diester and isophytol, wherein the reaction is carried out in the presence of the catalyst; and with a molecular sieve as a carrier, the catalyst is prepared by loading Bronsted acid, metal halide, metallocene and a metal element onto the molecular sieve.

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 ( acid) as a catalyst to produce vitamin E acetate by condensation of trimethylhydroqui...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72B01J31/22B01J29/04
Inventor 郭劲资张涛黎源初乃波刘阳乔小飞宋明焱程晓波刘英瑞宋军伟吕英东张旭王延斌朱龙龙林龙李莉华卫琦
Owner WANHUA CHEM GRP CO LTD
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