Method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin

A technology for lignin and vanillin, which is applied in the field of catalytic oxygenolysis of lignin to prepare extracts containing vanillin and syringaldehyde, can solve the problems of harsh reaction conditions of strong acid and strong alkali, low yield of target products, corrosive environment of equipment and the like, Achieve the effect of low price, stable hydrothermal performance and easy oxidative depolymerization

Active Publication Date: 2019-06-28
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But there are still obvious deficiencies: one is that the reaction conditions of strong acid and strong alkali are relatively harsh, which is easy to cause corrosion of equipment and is not friendly to the environment; the other is that the yield of target product is low

Method used

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  • Method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin
  • Method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin
  • Method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin

Examples

Experimental program
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Effect test

example 1

[0045] Example 1: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 , CeCuO 3 , CeFeO 3 , CeNiO 3 One of them is placed in a reaction kettle, and 20ml of ethanol / water mixed solvent is added, and the volume ratio of ethanol and water in the mixed solvent is 1:1; the reaction kettle is filled with nitrogen to 1MPa, and then exhausted, and repeated three times Complete the purging process; then feed oxygen into the reactor to 0.6MPa; set the reaction temperature to 180°C and the reaction time to 60 minutes. After the reaction is over, place the reactor in an ice-water mixture to cool to normal temperature and discharge, filter Oxidation residue was obtained; the obtained filtrate was rotary evaporated until the solvent was evaporated to dryness, and ethyl acetate was added for extraction, and the organic phase was combined and fixed to 10ml for GC-MS detection; 3 When used as a catalyst, the yields of vanillin and syringaldehyde in the extract all reached th...

example 2

[0046] Example 2: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 Placed in the reaction kettle, the volume ratio of ethanol and water in the mixed solvent is 1:1; fill the reaction kettle with nitrogen to 1MPa, then exhaust, repeat three times to complete the purging process; then pass into the reaction kettle Oxygen to 0.6MPa; set the reaction temperature to 120°C, and the reaction time to 60min; after the reaction, place the reaction kettle in an ice-water mixture to cool to room temperature and discharge the material, and filter to obtain the oxidation residue; the obtained filtrate is rotary evaporated until the solvent is evaporated to dryness, and added Extract with ethyl acetate, combine the organic phases and settle to 10ml, and carry out GC-MS detection; at this moment, vanillin and syringaldehyde are not detected in the extract, as image 3 , 4 shown.

example 3

[0047] Example 3: 0.2g of corn stover lignin and 0.02g of perovskite catalyst CeCoO 3 Put it in the reaction kettle, add 20ml of ethanol / water mixed solvent, the volume ratio of ethanol and water in the mixed solvent is 1:1; fill the reaction kettle with nitrogen to 1MPa, then exhaust, repeat three times to complete the purging process ; Immediately after, feed oxygen into the reactor to 0.6MPa; set the reaction temperature to 150°C and the reaction time to 60min, place the reactor in an ice-water mixture to cool to normal temperature and discharge the material after the reaction, and filter to obtain the oxidation residue; The filtrate was rotary evaporated until the solvent was evaporated to dryness, and ethyl acetate was added for extraction, the organic phases were combined and fixed to 10ml, and then detected by GC-MS; the yields of vanillin and syringaldehyde in the extract were 0.8%, 0.4% respectively. %,Such as image 3 , 4 shown.

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Abstract

The invention relates to a method for preparing extracting liquid containing vanillic aldehyde and syringaldehyde through catalytic oxygen decomposition of lignin. The method comprises the following steps: (1) preprocessing corn straw lignin in a NaHCO3 water solution; (2) putting the corn straw lignin preprocessed in the step (1) and a perovskite type catalyst into a closed reaction kettle, introducing O2 for reacting by taking an ethanol / water mixed solution as a solvent, after the reaction is finished, cooling the reaction liquid to the normal temperature, and carrying out discharging; and(3) sequentially carrying out filtration, rotary evaporation and ethyl acetate extraction on the discharged product in the step (2), so as to obtain the extracting liquid containing vanillic aldehydeand syringaldehyde. The method is mild in reaction condition and environment-friendly, the high-valued utilization of biomass can be realized, and the method has important significance to the protection of the ecological environment.

Description

technical field [0001] The invention relates to the technical field of lignin utilization, in particular to a method for preparing an extract containing vanillin and syringaldehyde by catalyzing oxygen decomposition of lignin. Background technique [0002] With the depletion of fossil energy, it is imminent to find new renewable alternatives to fossil energy. Biomass energy reserves are huge, clean and harmless, and have great potential to replace fossil energy. Biomass is mainly divided into three categories: cellulose, hemicellulose, and lignin. Among them, although lignin has a complex structure and is amorphous, it is the only renewable source of benzene rings in nature. In my country, a huge amount of lignin is produced in the papermaking and wood hydrolysis industries. Due to the complex physical and chemical characteristics of lignin, about 95% of lignin cannot be used for high-value utilization, but is directly discharged into rivers, resulting in Huge environmental ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/58C07C47/575C07C45/51C07C45/80B01J23/83
Inventor 沈德魁王瑾芝程崇博迂文兵
Owner SOUTHEAST UNIV
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