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Method for extracting vanillic acid by using deep-eutectic solvent/normal propyl alcohol aqueous two-phase system

A low eutectic solvent, two-phase system technology, applied in the separation/purification of carboxylic acid compounds, organic chemistry and other directions, to achieve the effects of fast extraction rate, simple synthesis process, and wide range of synthetic raw materials

Active Publication Date: 2020-05-01
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the extraction of vanillic acid using deep eutectic solvent / n-propanol two-phase system

Method used

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  • Method for extracting vanillic acid by using deep-eutectic solvent/normal propyl alcohol aqueous two-phase system
  • Method for extracting vanillic acid by using deep-eutectic solvent/normal propyl alcohol aqueous two-phase system
  • Method for extracting vanillic acid by using deep-eutectic solvent/normal propyl alcohol aqueous two-phase system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Weigh 7.1724g of betaine and 10.8096g of glucose into a round bottom flask, heat in an 80°C oil bath, and stir with a magnet until a clear and transparent solution is formed, and store for later use. Weigh 0.2g of vanillic acid powder into a 200mL volumetric flask to prepare a 1g / L vanillic acid aqueous solution and store it for future use.

[0033] (2) Weigh 1g of vanillic acid aqueous solution in a 10mL centrifuge tube, add 0.6, 0.8, 1.0, 1.2, 1.4g of betaine-glucose deep eutectic solvent respectively, then add 1g of n-propanol, and vibrate with a vortex shaker to obtain mixture.

[0034] (3) Put the mixed solution in step (2) into a constant temperature shaker to vibrate, set the temperature at 25°C, and shake for 30 minutes. After shaking, place it in a constant temperature water bath at 25°C and let it stand for 4 hours to obtain the above The phase is a n-propanol phase rich in vanillic acid, and the lower phase is a two-phase system of a deep eutectic solven...

Embodiment 2

[0038](1) Weigh 7.1724g of betaine and 22.3078g of sorbitol in a round bottom flask, heat in an 80°C oil bath, and stir with a magnet until a clear and transparent solution is formed, and store for later use. Weigh 0.2g of vanillic acid powder into a 200mL volumetric flask to prepare a 1g / L vanillic acid aqueous solution and store it for future use.

[0039] (2) Weigh 1g of vanillic acid aqueous solution in a 10mL centrifuge tube, add 0.6, 0.8, 1.0, 1.2, 1.4g of betaine-sorbitol deep eutectic solvent, then add 1g of n-propanol, and vibrate with a vortex shaker to obtain mixture.

[0040] (3) Put the mixed solution in step (2) into a constant temperature shaker to vibrate, set the temperature at 25°C, and shake for 30 minutes. After shaking, place it in a constant temperature water bath at 25°C and let it stand for 4 hours to obtain the above The phase is a n-propanol phase rich in vanillic acid, and the lower phase is a two-phase system of a deep eutectic solvent-rich phase. ...

Embodiment 3

[0044] (1) Weigh 7.1724g of betaine and 18.6306g of xylitol in a round bottom flask, heat in an 80°C oil bath, and stir with a magnet until a clear and transparent solution is formed, and store for future use. Weigh 0.2g of vanillic acid powder into a 200mL volumetric flask to prepare a 1g / L vanillic acid aqueous solution and store it for future use.

[0045] (2) Weigh 1g of vanillic acid aqueous solution in a 10mL centrifuge tube, add 0.6, 0.8, 1.0, 1.2, 1.4g of betaine-xylitol deep eutectic solvent, then add 1g of n-propanol, vibrate with a vortex shaker, A mixed solution was obtained.

[0046] (3) Put the mixed solution in step (2) into a constant temperature shaker to vibrate, set the temperature at 25°C, and shake for 30 minutes. After shaking, place it in a constant temperature water bath at 25°C and let it stand for 4 hours to obtain the above The phase is a n-propanol phase rich in vanillic acid, and the lower phase is a two-phase system of a deep eutectic solvent-ric...

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Abstract

The invention discloses a method for extracting vanillic acid by using a deep-eutectic solvent / normal propyl alcohol aqueous two-phase system. According to the method, extraction solvents including adeep-eutectic solvent and normal propyl alcohol are mixed to jointly construct the aqueous two-phase system, salts in a conventional aqueous two-phase system are replaced, and the salting-out problemof a salt-containing system is avoided. According to the method, the deep-eutectic solvent and normal propyl alcohol are added into an aqueous solution of vanillic acid to form the aqueous two-phase extraction system with a lower phase rich in the deep-eutectic solvent and an upper phase rich in the normal propyl alcohol, and vanillic acid is extracted into the upper phase. The purpose of enriching and recovering the vanillic acid from the aqueous solution is achieved by utilizing the deep-eutectic solvent / normal propyl alcohol aqueous two-phase system, the deep-eutectic solvent can be recycled, the process is simple, and cost is low.

Description

technical field [0001] The invention relates to the field of vanillic acid extraction, in particular to a method for extracting vanillic acid using a deep eutectic solvent / n-propanol two-phase system. Background technique [0002] Vanillic acid is a relatively common component of phenolic acids, which has strong antioxidant activity, and also has certain anti-tumor, anti-inflammatory and immune effects. Vanillic acid is widely found in nature, such as in vanilla beans, vanilla pods, Peru balm, benzoin balm, Java balsam and many other plants and essential oils. Claudio et al. explored the extraction ability of ionic liquid two-phase system for vanillic acid, and the results showed that Na 2 SO 4 The two-phase aqueous system based on ionic liquid can effectively extract vanillic acid (Cláudio A.F.M., Marques C.F.C., Boal-Palheiros I., et al.GreenChem., 2014, 16(1):259-268.). Almeida et al. studied in PEG (polyethylene glycol)-Na 2 SO 4 The additive ionic liquid was added ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/48C07C65/21
CPCC07C51/48C07C65/21
Inventor 陈砺邱舜国严宗诚杨婵媛
Owner SOUTH CHINA UNIV OF TECH
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