Preparation method of high-purity d-alpha-succinate

Abstract

The invention discloses a preparation method of high-purity d-alpha-succinate. The preparation method comprises the following steps of a, esterification reaction: taking d-alpha-tocopherol of more than 95 percent and succinic anhydride as raw materials, wherein the molar ratio of the d-alpha-tocopherol to the succinic anhydride is 1:(1 to1.3); adopting a basic catalyst which can react with hydrochloric acid to generate water-soluble hydrochloride to perform the esterification reaction, wherein the feeding amount mass ratio of the basic catalyst is 3 to 6 percent that of the d-alpha-tocopherol as the raw material; taking petroleum ether as a reaction solvent, wherein the mass ratio of the d-alpha-tocopherol to the petroleum ether is 1:2; controlling the temperature of the esterification reaction to be between 50 and 65DEG C, and performing the esterification reaction for 6 hours; b, water washing; c, decolorization; d, centrifugal filtration; e, crystallizing; f, centrifugal filtration; g, drying; h, granulating; i, drying; j, crushing and sieving. According to the preparation method disclosed by the invention, a higher catalytic effect is realized, and the local overheat problem can be solved; increase of side effects caused by over-high temperature of reaction materials are avoided; a crystallizing effect of the d-alpha-tocopheryl acid succinate can be realized; bulk density of d-alpha-tocopherol powder can be improved.

Description

technical field [0001] The invention relates to the technical field of production of food additive d-alpha-tocopherol succinate, in particular to a preparation method of high-purity d-alpha-tocopherol succinate. Background technique [0002] Tocopherol d-a-succinate is a white powder or granular form. It is an esterified derivative of natural vitamin E. It is often used as a commercial supply form. It is widely used in health food in developed countries such as Europe and the United States, and its application prospect is broad. The preparation of d-α-tocopherol succinate includes esterification, water washing, decolorization, crystallization, separation, drying, granulation and other processes. The d-a-tocopherol succinic acid esterification reaction uses d-a-tocopherol and succinic anhydride as the main raw materials, and the product is produced in the next step of esterification under the action of a catalyst. The catalyst used is generally alkaline, and the acidic catal...

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is to provide a better catalytic effect, which can solve the problem of avoiding local overheating, avoid increasing side reactions due to excessive temperature of the reaction material, and can crystallize d-alpha-tocopherol succinate. Method for preparing high-purity d-alpha-succinate with increased bulk density of d-alpha-tocopherol succinate powder