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Method for pretreating eucalyptus graded lignin and co-producing furfural based on DES two-phase system

A two-phase system, lignin technology, applied in the direction of lignin derivatives, chemical instruments and methods, organic chemistry, etc., can solve the problems of single type of lignin, long separation time, insufficient utilization of lignocellulose components, etc. Achieve the effects of easy control of reaction, short processing time, designable structure and recyclable utilization

Active Publication Date: 2022-01-21
BEIJING FORESTRY UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the existing deep eutectic solvent pretreatment technology has at least some shortcomings such as long separation time, insufficient utilization of lignocellulose components, and single lignin type.

Method used

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  • Method for pretreating eucalyptus graded lignin and co-producing furfural based on DES two-phase system
  • Method for pretreating eucalyptus graded lignin and co-producing furfural based on DES two-phase system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038](1) Grind Eucalyptus gigantea to 20-100 meshes, extract and dry with benzene alcohol, weigh 3 g of raw materials and DES choline chloride / lactic acid, organic solvent 2-MTHF according to the ratio of 1:5:10 (g :g:mL) ratio blended into the reactor, adding 0.2mol / L of aluminum sulfate and 0.075mol / L of sulfuric acid as a catalyst, rapid heating to 130 ℃ for 30min after the end of the reaction, to obtain a mixed system;

[0039] (2) The mixed system obtained in step (1) is separated to obtain the eutectic reaction mixture and the organic extract phase, and the organic extract phase is filtered through a disposable syringe filter with a pore size of 0.2 μm, and then detected and analyzed by a high performance liquid chromatograph Calculate the furfural content; the eutectic reaction mixture is washed with acetone / water solution (1 / 1, v / v) and centrifuged several times to obtain an eluent containing DES lignin;

[0040] (3) After the organic extract phase and eluent that ste...

Embodiment 2

[0047] (1) Grind Eucalyptus gigantea to 20-100 meshes, extract and dry with benzene alcohol, weigh 3 g of raw materials and DES choline chloride / lactic acid, organic solvent 2-MTHF according to the ratio of 1:5:10 (g :g:mL) was blended into the reactor, adding 0.2mol / L aluminum sulfate and 0.075mol / L sulfuric acid as catalysts, rapidly heating up to 150°C for 30min and then ending the reaction to obtain a mixed system;

[0048] (2) The mixed system obtained in step (1) is separated to obtain the eutectic reaction mixture and the organic extract phase. After the organic extract phase is filtered through a disposable syringe filter with a pore size of 0.2 μm, it is detected by high performance liquid chromatography and Calculate the furfural content; the eutectic reaction mixture is washed with acetone / water (1 / 1, v / v) and centrifuged several times to obtain an eluent containing DES lignin;

[0049] (3) After the organic extract phase and eluent that step (2) obtains are rotary-...

Embodiment 3

[0052] (1) Grind Eucalyptus gigantea to 20-100 meshes, extract and dry with benzene alcohol, weigh 3 g of raw materials and DES choline chloride / lactic acid, organic solvent 2-MTHF according to the ratio of 1:5:10 (g :g:mL) ratio blended into the reactor, adding 0.2mol / L of aluminum sulfate and 0.075mol / L of sulfuric acid as a catalyst, rapid heating to 170 ℃ for 30min after the end of the reaction, to obtain a mixed system;

[0053] (2) The mixed system obtained in step (1) is separated to obtain the eutectic reaction mixture and the organic extract phase. After the organic extract phase is filtered through a disposable syringe filter with a pore size of 0.2 μm, it is detected by high performance liquid chromatography and Calculate the furfural content; the eutectic reaction mixture is washed with acetone / water (1 / 1, v / v) and centrifuged several times to obtain an eluent containing DES lignin;

[0054] (3) After the organic extract phase and eluent that step (2) obtains are r...

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Abstract

The invention aims to provide a method for pretreating eucalyptus graded lignin and co-producing furfural based on a DES two-phase system. The method comprises the following steps of: (1) pretreatment of raw materials: crushing, dewaxing and drying; (2) preparation of DES: mixing a hydrogen bond acceptor and a hydrogen bond donor, performing heating and stirring until the mixture is uniform and transparent; and (3) pre-treating graded lignin and co-producing furfural by using the two-phase system: 1) blending the raw material, DES, an organic solvent and a catalyst, and adding the mixture into a reaction kettle for reaction; 2) performing cooling after the reaction is finished, and separating the mixture to obtain a eutectic reaction mixture and an organic extraction phase; and 3) carrying out rotary evaporation on an eluent obtained by washing the eutectic reaction mixture with an acetone / aqueous solution and the organic extraction phase, and then carrying out acid water precipitation, centrifugation and freeze drying to respectively obtain the DES lignin and the organic solvent lignin. According to the method, lignin with different fractions and high purity and good uniformity is obtained through a one-step method, and furfural is co-produced.

Description

technical field [0001] The invention belongs to the technical field of lignocellulosic biomass utilization, and in particular relates to a method for pretreating eucalyptus graded lignin and co-producing furfural with a DES-based two-phase system. Background technique [0002] At present, the climate and ecological problems brought about by the massive exploitation and use of fossil energy are becoming more and more serious, which seriously restricts the sustainable development of the current social economy. Due to concerns about global energy consumption demands, depletion of natural resources and reserves, and environmental degradation, the development and utilization of biomass resources has received increasing attention. Utilizing renewable lignocellulosic biomass conversion to produce various fuels, high-value chemicals and materials is an effective way to deal with the current resource and energy crisis. The cellulose content in lignocellulosic biomass accounts for on...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07G1/00C08H7/00C07D307/50
CPCC07G1/00C08H6/00C07D307/50
Inventor 孙少妮孙丽丽孙少超曹学飞袁同琦文甲龙
Owner BEIJING FORESTRY UNIVERSITY
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