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Extraction-back extraction system based on alkanol eutectic solvent and application of extraction-back extraction system

A low eutectic solvent and alkanol technology, which is applied in the field of separation and purification of natural products, can solve the problems of complicated heating and reflux extraction technology, loss of activity of target compounds, time-consuming and labor-intensive operation procedures, etc., and achieves low toxicity and purification steps. Less time-consuming effect

Active Publication Date: 2021-10-19
WUHAN UNIV
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Problems solved by technology

However, the traditional methods mostly involve the following problems: ①The use of organic solvents is large, which is against the concept of green chemistry; ②The selectivity of organic solvents is poor for extraction, which increases the workload of subsequent purification; ③The heating and reflux extraction technology is cumbersome and energy-intensive. Cause energy waste, and the high temperature will easily lead to the loss of activity of the target compound
However, they require additional purchase or synthesis of adsorbents in the purification process, the cost is high, the operation process is time-consuming and labor-intensive, and organic solvents are still consumed during elution; the structure of DES is destroyed due to excessive dilution during the recovery process, and it is difficult to recycle. The problem

Method used

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  • Extraction-back extraction system based on alkanol eutectic solvent and application of extraction-back extraction system
  • Extraction-back extraction system based on alkanol eutectic solvent and application of extraction-back extraction system
  • Extraction-back extraction system based on alkanol eutectic solvent and application of extraction-back extraction system

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Embodiment 1: The solid-liquid phase diagram drawing of the deep eutectic solvent based on alkanol

[0040] Accurately weigh 1-dodecanol and menthol in a series of molar ratios respectively (the molar ratios of 1-dodecanol and menthol are successively 9:1, 4:1, 3:1, 2:1, 3: 2, 1:1, 2:3, 1:2, 1:3, 1:4, 1:9) were mixed in a glass vial and heated until a homogeneous liquid was formed. A solid-liquid phase diagram of a deep eutectic solvent is drawn by plotting the melting points corresponding to eutectic mixtures in different molar ratios. Melting point (Tm) is determined by recording the temperature at which the liquid deep eutectic solvent begins to freeze. Such as figure 2 As shown, with the increase of the mole fraction of the hydrogen bond acceptor-menthol, the melting point of the deep eutectic solvent shows a trend of first dropping to a minimum point and then rising, and the lowest point reached is the low eutectic temperature of the deep eutectic solvent. melt...

Embodiment 2

[0041] Example 2: Determination of physicochemical properties of alkanol-based deep eutectic solvents

[0042] 1) 1-dodecanol: menthol molar ratio is the preparation of the deep eutectic solvent of 1:3

[0043] Accurately weigh 1-dodecanol and menthol at the eutectic ratio (the molar ratio of 1-dodecanol and menthol is 1:3) in a glass vial and heat (40-80°C) to form a homogeneous liquid, It is the successfully synthesized 1-dodecanol-menthol deep eutectic solvent.

[0044] 2) Measure the viscosity and density of the above-mentioned alkanol deep eutectic solvent

[0045] Viscosity was measured using a rotational rheometer, and the test conditions were: temperature 25°C, shear rate 0.1-1000s -1 , the distance between parallel plates is 40mm, and the test time is 11min; the determination of density: at room temperature, draw 100μL of eutectic solvent with a pipette gun, and then use an analytical balance to weigh the mass (Δm) added by the tip of the pipette, repeat this proces...

Embodiment 3

[0058] Embodiment 3: The purification method construction based on the deep eutectic solvent of alkanol

[0059] Accurately weigh 5mg of 1,8-dihydroxyanthraquinone and dissolve it in 5mL of a deep eutectic solvent with a molar ratio of 1-dodecanol to menthol of 1:3 to prepare 1,8-dihydroxyanthracene with a concentration of 1mg / mL Quinone solutions in deep eutectic solvents. Accurately measure 500 μL of the above-mentioned deep eutectic solvent solution of 1,8-dihydroxyanthraquinone and 1 mL of 0.1M NaOH solution, mix, vortex for 5 min, centrifuge at 6000 rpm for 5 min, and record it as back extraction once; absorb the NaOH water with a 1 mL syringe After phase, 1 mL of 0.1M NaOH solution was added again, vortexed, centrifuged, and recorded as back-extraction twice; the above operations were repeated for three times and four times for back-extraction respectively. The deep eutectic solvent phase obtained during different times of back extraction (0, 1, 2, 3, 4 times) was respe...

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Abstract

The invention provides an extraction-back extraction system based on an alkanol eutectic solvent. The extraction-back extraction system comprises a liquid-liquid two-phase extraction system and a liquid-liquid back extraction system, wherein the liquid-liquid two-phase extraction system is composed of an alkanol eutectic solvent and water or a first acidic aqueous solution, and the liquid-liquid back extraction system is composed of the alkanol eutectic solvent and an alkaline aqueous solution or a second acidic aqueous solution. The system is more in variety, low in cost, low in toxicity, high in stability, not easy to dissociate, low in melting point and wide in pH tolerance range. The invention also provides application of the extraction-back extraction system based on the alkanol eutectic solvent in extraction and purification of active compounds. The extraction yield is high, the purification effect is good, and the alkanol eutectic solvent can be repeatedly utilized. The invention also provides an extraction and purification method of the active compound. The method is simple to operate, green, less in extraction and purification steps, less in time consumption, free of special equipment and high in recovery rate of active compounds.

Description

technical field [0001] The patent of the present invention relates to the technical field of separation and purification of natural products, especially the extraction-reextraction system based on alkanol deep eutectic solvent and its application. Background technique [0002] Bioactive compounds are usually derived from secondary metabolites in various biological organisms (collectively referred to as biomass) such as plants, fungi, algae, fruits, and microorganisms. They play an irreplaceable role in important mechanisms such as stress response and natural defense. Solid-liquid extraction based on organic solvents (such as heat flow extraction, Soxhlet extraction, etc.) is a traditional method for extracting bioactive compounds from biological matrices. However, the traditional methods mostly involve the following problems: ①The use of organic solvents is large, which is against the concept of green chemistry; ②The selectivity of organic solvents is poor for extraction, w...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/04C07C46/10C07C50/34C07C51/48C07C65/40
CPCB01D11/0492C07C46/10C07C51/48C07C2603/24C07C50/34C07C65/40
Inventor 肖玉秀黄安琪
Owner WUHAN UNIV
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