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Method for separating single tocopherol from mixed tocopherol by utilizing polyionic liquid

A technology of polyionic liquid and ionic liquid, applied in the fields of chemical engineering and polymer materials, can solve the problems of low selectivity and high separation cost

Active Publication Date: 2018-12-04
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported adsorbents used for adsorption include silica gel, adsorption resin, such as adsorption (CN11401645A, CN102432584A, etc.), etc., by utilizing four kinds of tocopherol homologues with different adsorption properties on the adsorbent, and selecting an appropriate elution solvent to achieve Separation, but commonly used adsorbents have low selectivity to the four tocopherol monomers, leading to high separation costs

Method used

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  • Method for separating single tocopherol from mixed tocopherol by utilizing polyionic liquid
  • Method for separating single tocopherol from mixed tocopherol by utilizing polyionic liquid
  • Method for separating single tocopherol from mixed tocopherol by utilizing polyionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] First, a porous polyionic liquid was prepared using 1-vinyl-3-ethylimidazolium laurate as a monomer. In a 50mL Schlenk storage bottle, dissolve 1.00g of divinylbenzene, 1.24g of 1-vinyl-3-ethylimidazole laurate and 44.8mg of azobisisobutyronitrile in 20mL of acetonitrile at 100°C , Stir the reaction for 24h. After cooling at room temperature, it was washed with ethanol, dried under vacuum at 60°C for 24 hours, and ground for use. As determined by a nitrogen adsorption instrument, the product exhibits obvious mesoporous characteristics, with a specific surface area of ​​247m 2 g -1 , the pore volume is 0.36cm 3 g -1 , the pore size is 6.1nm. The ionic liquid content in the porous polyionic liquid structure was calculated from the elemental analysis results, and the ionic liquid content was 1.01 mmol / g.

[0072] The polyionic liquid prepared in this example is a carboxylic acid anion functionalized porous polyionic liquid, and its structural formula is as follows: ...

Embodiment 2

[0076] For the fixed-bed separation process, 20 g of the porous polyionic liquid prepared in Example 1 was loaded into a chromatographic column (φ20 mm×500 mm), washed and compacted with absolute ethanol. 5g of mixed tocopherol crude product (content 80%, wherein δ-tocopherol 11.6%, β-tocopherol and γ-tocopherol samples total 55.0%, α-tocopherol 13.4%) was fully dissolved in 20mL absolute ethanol, Prepare a raw material solution with a concentration of 250 mg / mL. At an operating temperature of 15°C, pass the upper column liquid into the chromatography column at 1.5 times the bed volume / hour; wash with n-hexane, control the flow rate at 1.5 times the bed volume / hour, collect the effluent in sections, and use high-efficiency liquid Detected by phase chromatography, merging eluents with the same components, and distilling under reduced pressure, successively obtained 0.59g δ-tocopherol (content 89.4%), 2.78g β-tocopherol and γ-tocopherol mixture (content 90.1%), 0.67 gα-tocopher...

Embodiment 3

[0078] Using 1,6-bis(vinylimidazolium)hexyl bromide as monomer, polyionic liquid gel was prepared. Dissolve 2 g of 1,6-bis(vinylimidazolium) hexyl bromide and 10 mg of azobisisobutylamidine hydrochloride in 2 mL of water, irradiate with light with a wavelength of 365 nm for 20 min, wash with water several times, freeze-dry to remove Grind with water and set aside.

[0079] The polyionic liquid gel structural formula that this embodiment prepares is as follows:

[0080]

[0081] The infrared result picture is as follows Image 6 As shown, 1153cm -1 The peak at the imidazolium cation can replace the characteristic peak of the C-N covalent bond at N, 1620cm -1 、1570cm -1 、1550cm -1 、1455cm -1 The peak at is the characteristic peak of imidazole ring skeleton, 2934cm -1 and 2856cm -1 The peak at is the stretching vibration peak of the alkyl chain saturated C-H group in the porous polyionic liquid structure, 3050cm -1 ~3140cm -1 The peak is the stretching vibration peak...

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Abstract

The invention discloses a method for separating single tocopherol from mixed tocopherol by utilizing a polyionic liquid. The single tocopherol with high purity is separated from a crude product of mixed tocopherol by taking the polyionic liquid as an adsorber. The polyionic liquid has a specific ionic liquid structure and an abundant pore structure so as to have the advantages such as high tocopherol adsorption capacity and high single body selectivity and be capable of realizing selective separation of a tocopherol single body. The tocopherol single body of which the purity is not lower than80% may be obtained under an optimized condition, and the recovery rate is 85% or above. The method is suitable for industrial production.

Description

technical field [0001] The invention relates to the fields of chemical engineering and polymer materials, in particular to a method for adsorbing and separating mixed tocopherols by polyionic liquids. Background technique [0002] Natural Vitamin E (Natural Vitamin E), scientific name Tocopherols (Tocopherols), also known as mixed tocopherols, together with vitamin C and vitamin A, has become the three pillar products of the vitamin series. Large assortment of vital vitamins. Mixed tocopherols have strong anti-oxidation and excellent health care functions, and are widely used in medicine, cosmetics, oil, food, and feed industries. There are four natural vitamin E homologues, which differ only in the number and position of the methyl group on the benzene ring, but they show different characteristics, so they are differentiated in function and application field, and the order of biological activity is α -tocopherol (activity 100)>β-tocopherol (activity 10-50)>γ-tocophe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D311/72C08F226/06C08F212/36C08F220/34C08F230/02C08F126/06B01J20/26B01D15/08B01D15/42
CPCB01D15/08B01D15/424B01J20/264B01J20/28047B01J20/28061B01J20/2808B01J20/28083C07D311/72C08F126/06C08F220/34C08F226/06C08F230/02C08F212/36
Inventor 邢华斌锁显杨启炜杨亦文任其龙鲍宗必
Owner ZHEJIANG UNIV
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