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A kind of extraction-stripping system based on alkanol deep eutectic solvent and its application

A low eutectic solvent and alkanol technology, 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: 2022-07-19
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of extraction-stripping system based on alkanol deep eutectic solvent and its application
  • A kind of extraction-stripping system based on alkanol deep eutectic solvent and its application
  • A kind of extraction-stripping system based on alkanol deep eutectic solvent and its application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Example 1: Solid-liquid phase mapping of alkanol-based deep eutectic solvents

[0040] Precisely weigh 1-dodecanol and menthol in a series of molar ratios respectively (the molar ratio of 1-dodecanol and menthol is 9:1, 4:1, 3:1, 2:1, 3: 2, 1: 1, 2: 3, 1: 2, 1: 3, 1: 4, 1: 9) in a glass vial, and heat until a homogeneous liquid is formed. The solid-liquid phase diagram of a deep eutectic solvent is drawn by plotting the melting points corresponding to different molar ratios of the eutectic mixture. The melting point (Tm) is determined by recording the temperature at which the liquid deep eutectic solvent begins to solidify. like figure 2 As shown, as the mole fraction of hydrogen bond acceptor—menthol increases, the melting point of the deep eutectic solvent first drops to a lowest point and then rises, and the lowest point reached is the deep eutectic solvent of the deep eutectic solvent. melting point. The melting point of 1-dodecanol:menthol deep eutectic solven...

Embodiment 2

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

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

[0043] Precisely weigh 1-dodecanol and menthol in a low eutectic ratio (mol 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 1-dodecanol-menthol eutectic solvent successfully synthesized.

[0044] 2) Determine the viscosity and density of the above alkanol deep eutectic solvent

[0045] Viscosity was measured using a rotational rheometer under the following conditions: temperature 25°C, shear rate 0.1-1000s -1 , The distance between parallel plates is 40mm, and the test time is 11min; Density determination: At room temperature, use a pipette to absorb 100μL of the eutectic solvent, and then use an analytical balance to weigh the increased mass (Δm) of the pipette tip, and repeat the process six times. And calc...

Embodiment 3

[0058] Example 3: Alkanol-based purification method construction of deep eutectic solvents

[0059] Precisely weigh 5mg of 1,8-dihydroxyanthraquinone and dissolve it in 5mL of a deep eutectic solvent with a molar ratio of 1-dodecanol and menthol of 1:3 to prepare 1,8-dihydroxyanthracene with a concentration of 1mg / mL. Quinones in deep eutectic solvent. Precisely measure 500 μL of the above 1,8-dihydroxyanthraquinone solution in deep eutectic solvent and 1 mL of 0.1 M NaOH solution, mix, vortex for 5 min, and centrifuge at 6000 rpm for 5 min, which is recorded as 1 back-extraction; use a 1 mL syringe to remove the NaOH water After the phase, 1 mL of 0.1M NaOH solution was added again, mixed by vortex, centrifuged, and recorded as 2 times of back-extraction; the above operations were repeated for 3 times of back-extraction and 4 times of back-extraction respectively. The deep eutectic solvent phase obtained in different times of back-extraction (0, 1, 2, 3, and 4 times) was tak...

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Abstract

The invention provides an extraction-stripping system based on an alkanol deep eutectic solvent, comprising a liquid-liquid two-phase extraction system composed of an alkanol deep eutectic solvent and water or a first acidic aqueous solution, and an alkanol deep eutectic solvent and a liquid-liquid two-phase extraction system. A liquid-liquid back extraction system composed of an alkaline aqueous solution or a second acidic aqueous solution. The system product is low in price, low in toxicity, strong in stability, not easy to dissociate, low in melting point and wide in pH tolerance; the present invention also provides the above-mentioned extraction-stripping system based on alkanol deep eutectic solvent in the extraction and purification of active compounds applications in . The extraction yield is high, the purification effect is good, and the alkanol low eutectic solvent can be reused for many times. The present invention also provides an extraction and purification method for active compounds. The operation is simple and green, with few extraction and purification steps, less time consumption, no need to use special equipment, and high 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, in particular to an extraction-stripping 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 thermal fluid extraction, Soxhlet extraction, etc.) is a traditional means to extract biologically active compounds from biological matrices. However, the traditional methods mostly involve the following problems: 1) the use of organic solvents is large, which is against the concept of green chemistry; 2) the selectivity of organic solvents for extrac...

Claims

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Application Information

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Patent Type & Authority Patents(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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