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Method for separating and purifying 2,6-dimethoxy phenol and acetosyringone from biological oil

A technology of dimethoxyphenol and acetosyringone, which is applied in the field of separation and purification of bio-based chemicals, can solve the problems of complex bio-oil components and difficult to obtain pure industrial chemicals, and achieves improved utilization value, low cost and cumbersome process. Effect

Active Publication Date: 2015-11-11
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Due to the complex composition of bio-oil, it is difficult to obtain high-purity industrial chemicals from bio-oil by using a single separation and purification method. Therefore, it is necessary to develop a combination of separation and purification technology to separate bio-oil

Method used

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  • Method for separating and purifying 2,6-dimethoxy phenol and acetosyringone from biological oil
  • Method for separating and purifying 2,6-dimethoxy phenol and acetosyringone from biological oil
  • Method for separating and purifying 2,6-dimethoxy phenol and acetosyringone from biological oil

Examples

Experimental program
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Effect test

Embodiment 1

[0036]Add 1.31g of solid calcium oxide into 10mL of water to react to form a mixed solution of calcium hydroxide. Stir it evenly and add 1.0g of bio-oil produced after hydrothermal liquefaction of rice straw. The shaking reaction temperature is 50°C, and the reaction time is 20min. After the completion, the solid precipitate was separated by suction filtration. After the solid precipitate was subjected to ultrasonic suction filtration with ethanol three times, it was placed in an oven for 4 hours at 105°C, and 0.05 g of the obtained solid precipitate was added to 10 mL of hydrochloric acid with a concentration of 4 mol / L for 20 min. The reaction solution from the previous step was extracted three times with dichloromethane, mixed and shaken, and allowed to stand for 1 h to form a distinct organic phase and an aqueous phase. Take the organic phase from the previous step and remove dichloromethane by rotary evaporation at 50°C, dissolve the sample obtained by rotary evaporation w...

Embodiment 2

[0038] Add 1.56g of solid magnesium hydroxide into 10mL of water to form a mixed solution. Stir it evenly and add 1.0g of bio-oil produced after hydrothermal liquefaction of Salix salix. The shaking reaction temperature is 70°C and the reaction time is 20min. The solid precipitate was separated by filtration. After the solid precipitate was ultrasonically filtered three times with ethanol, it was baked in an oven at 105°C for 4 hours. 0.05 g of the obtained solid precipitate was added to 10 mL of 10 mol / L hydrochloric acid for ultrasonic reaction for 20 min. The reaction solution from the previous step was extracted three times with dichloromethane, mixed and shaken, and allowed to stand for 1 h to form a distinct organic phase and an aqueous phase. Take the organic phase from the previous step and remove dichloromethane by rotary evaporation at 50°C, dissolve the sample obtained by rotary evaporation with 2 mL of ethyl acetate, and add it as the original sample to the top laye...

Embodiment 3

[0040] Add 4.62g of solid barium oxide into 10mL boiling water to react to form barium hydroxide suspension, stir it evenly, add 1.0g of bio-oil produced after hydrothermal liquefaction of water hyacinth, shake the reaction temperature at 60°C, and the reaction time is After 20 minutes, after the reaction was completed, the solid precipitate was separated by suction filtration. After the solid precipitate was ultrasonically filtered three times with ethanol, it was placed in an oven at 105°C for 4 hours, and 0.05 g of the obtained solid precipitate was added to 10 mL of hydrochloric acid with a concentration of 8 mol / L for ultrasonic reaction. 20min. The reaction solution from the previous step was extracted three times with dichloromethane, mixed and shaken, and allowed to stand for 1 h to form a distinct organic phase and an aqueous phase. Take the organic phase from the previous step and remove dichloromethane by rotary evaporation at 50°C, dissolve the sample obtained by r...

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Abstract

The invention belongs to the field of bio-based chemical separation and purification, and relates to a separation and purification process of complex biological oil, particularly to a method for separating and purifying 2,6-dimethoxy phenol and acetosyringone from biological oil. The method comprises: adding a solid alkaline oxide or hydroxide to water so as to form a mixed solution, adding biological oil to the uniformly-stirred mixed solution, carrying out an alkalization reaction, separating to obtain an alkalization precipitate, adding an acid solution to the alkalization precipitate to obtain a phenol mixture and a metal salt solution, carrying out column chromatography separation on the phenol mixture by adopting silica gel or alumina and the like as a carrier, carrying out gradient elution with different proportions of organic solvents so as to respectively obtain different components of phenols and organic carboxylic acids, and concentrating the partial components so as to obtain the high-purity 2,6-dimethoxy phenol and the high-purity acetosyringone. According to the present invention, the high added value chemicals are separated from the complex biological oil through the method, and the method has a certain environmental benefit and a certain economic benefit, and provides the good approach for the resource utilization of the biomass.

Description

technical field [0001] The invention belongs to the field of separation and purification of bio-based chemicals, and relates to a separation and purification process of bio-oil with complex components, in particular to a method for separating and purifying 2,6-dimethoxyphenol and acetosyringone from bio-oil. Background technique [0002] With the growth of population and the improvement of people's living standards, the demand for energy continues to grow, and the traditional energy mainly based on fossil fuels is becoming increasingly scarce. Environmental problems such as the greenhouse effect caused by the use of coal and oil are becoming more and more serious. Facing the dual pressure of energy shortage and environmental protection, the development and utilization of energy such as biomass waste has attracted widespread attention. In addition to direct combustion, thermal cracking, composting and other conversion methods, biomass can also be converted into porous biochar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C41/34C07C43/23C07C45/78C07C49/84
CPCC07C41/34C07C45/78C07C43/23C07C49/84
Inventor 张士成郝诗来陈凯绯曹磊昌吕航陈建民
Owner FUDAN UNIV
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