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Method for recovering high-content natural d-alpha-tocopherol succinate from leftovers

A tocopherol succinate, high-content technology, applied in organic chemistry, fermentation and other directions, can solve the waste of resources, the inability to propose α-tocopherol succinate crystallization methods, and limit the crystallization yield of crystalline tocopherol succinate, etc. problems, to achieve the effect of good industrialization feasibility, strong operability, and simple process

Active Publication Date: 2021-06-04
山东新元素生物科技有限公司
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

And the drawback of this method is that because the solvent has a certain solubility to the substance, so the crystallization yield of the solvent method crystallization tocopheryl succinate is limited, so that part of the tocopheryl succinate remains in the crystallization mother liquor
[0004] Generally, the crystallization yield of α-tocopherol succinate in an organic solvent can reach about 85%, and the remaining about 15% is in the mother liquor. - The content of tocopheryl succinate is generally below 35%, so the α-tocopheryl succinate retained in the waste cannot be proposed by simple crystallization methods, and there is no relevant information about extracting and recovering α-tocopherol from the waste. The report of phenolsuccinate
[0005] Affected by the current extraction process, low-content d-α-tocopheryl succinate residues have not been valued and utilized, resulting in a large amount of low-content d-α-tocopheryl succinate residues being stockpiled or used as cheap dregs Oil treatment, resulting in a huge waste of resources

Method used

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  • Method for recovering high-content natural d-alpha-tocopherol succinate from leftovers

Examples

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Effect test

Embodiment 1

[0034] A method of recovering high content natural D-α-gyphenol succinate from the foot, comprising the step of: taking 1.5 kg of foot (D-α-tocapol succinate content of 28.5%), Heat 42 ° C, after filtration of 200 macotte filtration, 7.5 kg of methanol was added to the esterifying kettle, and the heat was stirred to dissolve the feet, and 30 g of concentrated sulfuric acid was added dropwise, and the dropwax time was 40 min, and the temperature was 40 min. The reaction was reacted at 68 ° C for 3.5 h. The reaction was completed, and the methanol was evaporated under reduced pressure at 75 ° C, and the methanol was used to the temporary tank for use, and the water was washed with a hot water at 70 ° C after steaming until there was no methanol. Wash to wash to pH> 6. After washing, the water was washed into the molecular distillation system, first performed the first stage film distillation, dehydration treatment at 140 ° C, continuously carrying the second stage short range distil...

Embodiment 2

[0037] A method of recovering high content natural D-α-gyphenol succinate from the foot, comprising the step of: taking 1.5 kg of foot (D-α-tocapol succinate content is 22.7%), Heat 45 ° C, after filtration of 200 martial filters, 9 kg of methanol was added to the esterification, and the heat was stirred to dissolve the foot, and 45 g of concentrated sulfuric acid was added dropwise, and the dropwise time was 50 min, and the temperature was 10,000. ° C reaction for 4 h. The reaction was completed, and the methanol was evaporated under reduced pressure at 73 ° C, and the methanol was used to the temporary tank for use, and the water was washed with 65 ° C for methanol. Wash to wash to pH> 6. The water was washed into the molecular distillation system, first performed the first grade film distillation, dehydration treatment at 150 ° C, continuously carrying the second stage short range distillation, distilled at 175 ° C to the resulting methyl ester product, weight 353.2g.

[0038]T...

Embodiment 3

[0040] The present invention recovered a method of recovering high content natural D-α-tocobquinate from the foot, including the steps of: taking 1.5 kg foot (D-α-tocophenous succinate content of 34.2%), Heat 44 ° C, after filtration of 200 macotte filtration, 10.5 kg of methanol was added to the esterifying kettle, and the heat was stirred to dissolve the foot, and 60 g of concentrated sulfuric acid was added dropwise, and the dropwax time was 60 min, and the temperature was heated. The reaction was reacted at 690 ° C for 4 h. The reaction was completed, and the methanol was evaporated under reduced pressure at 78 ° C, and methanol was hit to the temporary tank for use, and the water was washed with 73 ° C after stirring, water was washed to pH> 6. The water was washed into the molecular distillation system, first performed the first stage film distillation, dehydrated at 145 ° C, continuously subjected to the second stage short range distillation, distilled at 165 ° C to the obt...

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Abstract

The invention belongs to the field of natural tocopherol succinate preparation, and particularly relates to a method for recovering high-content natural d-alpha-tocopherol succinate from leftovers. The method comprises the following steps of adding 2-10 times by weight of methanol into the pretreated leftovers, adding 0.5-5% of acid catalyst, carrying out esterification reaction at 60-70 DEG C to obtain a corresponding methyl ester product, carrying out reduced pressure distillation to recover methanol, washing with water until the methanol is neutral, carrying out secondary molecular distillation to obtain a secondary light phase which is a methyl ester product, hydrolyzing the methyl ester product in a water-organic solvent system under the catalysis of lipase, and carrying out post-treatment to obtain the high-content natural d-alpha-tocopherol succinate. The method is simple in process, environmentally friendly and high in operability, has very good industrial feasibility, can recover the natural alpha-tocopherol succinate from the leftovers, is used for recycling waste resources, and has important economic value and social value.

Description

Technical field [0001] The present invention belongs to the preparation of natural plastic phenol succinate, and in particular, a method of recovering high content natural D-α-gyphenol succinate from the foot. Background technique [0002] The D-α-tocobquinate is one of the D-α-tochenol-derived products, and since the action of the succinate group is introduced on the original basis, it is made in addition to the function of continuing D-α-tocopherol. It also has some unique pharmacological functions, such as anti-cancer effects, is a very effective anionic anti-cancer drug. In addition, it is still a good promoter in which the prolaptic hormone and growth hormone are secreted. Therefore, the price of D-α-tempered phenol succinate is much higher than that of the general hophenol, and the D-α-tocopherol is converted into succinate is an effective way to increase the added value of the gyl. [0003] At present, there is a chemical method and biochenol succinate process at home and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P17/06C07D311/72
CPCC12P17/06C07D311/72Y02P20/584
Inventor 庞宗梅李若坤张伟张心月
Owner 山东新元素生物科技有限公司
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