Environment-friendly d-alpha-tocopherol succinate refining preparation process

A preparation process and tocopherol technology, applied in the field of chemical engineering, can solve the problems of product deterioration, yellowing and agglomeration, high toxicity of organic solvents, high environmental pollution, etc., and achieve improved product safety, low solvent toxicity, and reduced dust hazards. Effect

Pending Publication Date: 2022-03-18
NINGBO DAHONGYING BIO ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. Organic solvents such as n-hexane and petroleum ether are used for crystallization. The organic solvents are highly toxic, and a large amount of organic solvent waste gas is generated during the solid-liquid separation and drying process, causing great environmental pollution; in addition, organic solvent residues in the product are also harmful
[0005] 2. Use oven, boiling drying and other drying methods to dry the product, which will generate organic waste gas. In addition, the dried product will agglomerate and need to be crushed later. The crushing process is easy to generate dust, which is very harmful
[0006] 3. Using conventional oven, boiling drying and other drying methods, the temperature needs to reach 60°C, the melting point of d-α-tocopherol succinate is 73°C, high temperature drying is easy to make the product deteriorate, yellow and agglomerate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Get d-alpha-tocopherol concentrated solution 100g (wherein the mass content of d-alpha-tocopherol is 87%), add 25g succinic anhydride, esterify and obtain d-alpha-tocopherol succinic acid crude product 120.2g (d-alpha-tocopherol The mass content of tocopherol succinate is 89.20%), add 600ml ethanol, heat to 60°C, after completely dissolving, cool to 0°C, slowly add 200ml water, cool for 24 hours, filter the liquid, add 200ml water to the solid, stir Uniform, filtered to obtain a water-containing solid; freeze-drying, at a temperature of -5°C and a vacuum of 1Pa, 102.6g of a powder product was obtained, wherein the content of d-α-tocopherol succinate was 97.85%.

Embodiment 2

[0030] Get d-alpha-tocopherol concentrate 100g (wherein the mass content of d-alpha-tocopherol is 80%), add 25g succinic anhydride, esterify and obtain d-alpha-tocopheryl succinate crude product 118.6g (wherein d-alpha-tocopherol The mass content of tocopherol succinate is 83.14%), add 700ml of ethanol, heat to 50°C, after completely dissolving, cool to -5°C, slowly add 50ml of water, cool for 32 hours, filter the liquid, add 300ml of water to the solid, Stir evenly, filter to obtain a water-containing solid; freeze-dry at a temperature of -8°C and a vacuum of 1Pa to finally obtain a powder product of 92.1g, wherein the content of d-α-tocopherol succinate is 97.62%.

Embodiment 3

[0032] Get d-alpha-tocopherol concentrate 100g (wherein the mass content of d-alpha-tocopherol is 95%), add 25g succinic anhydride, esterify and obtain d-alpha-tocopherol succinate crude product 122.1g (wherein d-alpha-tocopherol The mass content of tocopherol succinate is 95.90%), add 600ml ethanol, heat to 45°C, after completely dissolving, cool to -3°C, slowly add 600ml water, cool for 28 hours, filter the liquid, add 250ml water to the solid, Stir evenly, filter to obtain a water-containing solid; freeze-dry, and finally obtain a powder product 111.2g at a temperature of -6°C and a vacuum of 1Pa, wherein the content of d-α-tocopherol succinate is 98.94%.

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Abstract

The invention discloses an environment-friendly refining preparation process of d-alpha-tocopherol succinate, which comprises the following steps: S1, carrying out esterification reaction on d-alpha-tocopherol and succinic anhydride to obtain d-alpha-tocopherol succinate, heating and dissolving the d-alpha-tocopherol succinate with ethanol, cooling, keeping the temperature below 0 DEG C, adding a proper amount of water, and cooling; s2, carrying out solid-liquid separation, adding a proper amount of water into the separated solid, uniformly mixing, and filtering to obtain water-containing d-alpha-tocopherol succinate; and S3, performing freeze drying to obtain d-alpha-tocopherol succinate powder. According to the method, firstly, ethanol-water is adopted as an organic solvent to crystallize and refine the d-alpha-tocopherol succinate, and the toxicity of the solvent is low; after solid-liquid separation, residual ethanol in the solid is replaced by water, so that only water is discharged in the drying process, and no organic solvent is discharged; and a freeze drying technology is subsequently adopted, so that the product can be in a loose powder shape, a subsequent crushing step is not needed, the generation of dust is reduced, and meanwhile, low-temperature drying is beneficial to reducing oxidative deterioration of the product.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to an environmentally friendly d-alpha-tocopherol succinic acid refining preparation process. Background technique [0002] d-alpha-tocopherol succinate is a crystalline solid powder. At present, the preparation of d-alpha-tocopherol succinate is generally obtained by esterifying d-alpha-tocopherol with succinic anhydride under catalyst conditions. After the reaction is completed, crystallization and refining are carried out by using organic solvents such as n-hexane and petroleum ether. After crystallization, use a plate frame or centrifuge for solid-liquid separation to obtain solvent-containing d-α-tocopherol succinate, and then dry it, and use an oven, boiling drying, etc. to dry the solvent to obtain coarse-grained d-α-succinate The tocopherol is further pulverized to obtain d-α-tocopherol succinate powder. [0003] There is following shortcoming in above-mention...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72
CPCC07D311/72
Inventor 王嘉磊章城亮李泽辉周勇武玉洁汪俊胜姚瑞
Owner NINGBO DAHONGYING BIO ENG
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