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Method for extracting lignins from lignocellulose materials to prepare syringaldehyde by catalytic conversion

A lignocellulose, catalytic conversion technology, applied in the field of biomass extraction and conversion, can solve the problems of easy repolymerization and complexation reaction, complex structure, etc., and achieve the effect of low cost, high catalytic activity and improved conversion rate

Inactive Publication Date: 2016-05-11
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the complex structure of lignin itself and the tendency of repolymerization and complexation reactions during the degradation process, it is extremely important to develop a process route for the efficient catalytic conversion of lignin to prepare syringaldehyde

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Use corn stalks as raw material, use 60% 1,4-butanediol aqueous solution as the solvent, solid-to-liquid ratio 1:8, temperature 220°C, react for 2 hours, cool, filter, and weigh the filter cake; add three times the volume of the filtrate Stand overnight with deionized water, filter, and wash and vacuum-dry the obtained filter residue to obtain lignin extracted from corn stalks. This lignin is used in catalytic conversion system, reaction conditions: lignin concentration 20g / L, LaFe 0.2 Cu 0.8 o 3 Concentration 2g / L, alkali concentration 2mol / L, temperature 180°C, filled with O 2 Pressure 8bar, react for 2h, take it out and centrifuge to get the catalyst, adjust the pH value of the supernatant to 1-2 with concentrated HCl, and precipitate unreacted lignin; filter, wash and weigh the lignin, record the volume of the filtrate, take a sample, and analyze it by HPLC The yield of syringaldehyde was 10.09%.

Embodiment 2

[0024] Use walnut shells as raw materials, use 40% 1,4-butanediol aqueous solution as the solvent, solid-to-liquid ratio 1:8, temperature 220°C, cool after 2 hours of reaction, filter, and weigh the filter cake; add three times the volume of the filtrate deionized water, let stand overnight, filter, and the obtained filter residue is washed and vacuum-dried to obtain lignin extracted from walnut shells. This lignin is used in catalytic conversion system, reaction conditions: lignin concentration 2g / L, LaNi 0.2 Cu 0.8 o 3 Concentration 2g / L, alkali concentration 2mol / L, temperature 100°C, filled with O 2 Pressure 2bar, react for 2h, take it out and centrifuge to get the catalyst, adjust the pH value of the supernatant to 1-2 with concentrated HCl, and precipitate unreacted lignin; filter, wash and weigh the lignin, record the volume of the filtrate, take a sample, and analyze it by HPLC The yield of syringaldehyde was 6.30%.

Embodiment 3

[0026] Coconut shell is used as the raw material, the solvent is 60% 1,4-butanediol aqueous solution, the solid-to-liquid ratio is 1:8, the temperature is 220°C, after 2 hours of reaction, it is cooled, filtered, and the filter cake is recovered and weighed; the filtrate is added with three times the volume of deionized water, let stand overnight, filter, and the obtained filter residue is washed and vacuum-dried to obtain lignin extracted from walnut shells. This lignin is used in catalytic conversion system, reaction conditions: lignin concentration 10g / L, 5% loaded Molecular sieve concentration 2g / L, alkali concentration 2mol / L, temperature 160°C, filled with O 2 Pressure 6 bar, react for 2 hours, take it out and centrifuge to get the catalyst, adjust the pH value of the supernatant to 1-2 with concentrated HCl, and precipitate unreacted lignin; filter, wash and weigh the lignin, record the volume of the filtrate, take a sample, and analyze it by HPLC The yield of syringa...

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Abstract

The invention discloses a method for extracting lignins from lignocellulose materials to prepare syringaldehyde by catalytic conversion. The method mainly includes: 1) using high-boiling solvent for extracting the lignins from the lignocellulose materials of agricultural wastes such as nut shells and straws; 2) preparing perovskite type oxides LaNi1-xCuxO3 and LaFe1-xCuxO3, and loading to carriers such as molecular sieves and MCM-22 type molecular sieves to obtain heterogeneous perovskite type oxide catalysts; 3) applying the prepared catalysts to catalytic oxidation of the lignins for preparation of the syringaldehyde; 4) after reaction is finished, filtering to separate out the heterogeneous catalysts, and recycling after reduction regeneration.

Description

technical field [0001] The invention belongs to the technical field of biomass extraction and conversion, and relates to a method for preparing syringaldehyde by catalytic conversion of lignin extracted from lignocellulosic raw materials, through which the conversion rate of lignin and the yield of syringaldehyde can be significantly improved. The high-value conversion and utilization of lignin provides more possibilities. Background technique [0002] Biomass is a renewable resource that exists widely in nature. As one of the three main components, lignin is composed of three structural monomers, p-hydroxyphenyl, guaiacyl and syringyl, and has a variety of active groups. Groups and complex three-dimensional network structure, in which the main groups are phenolic hydroxyl, alcoholic hydroxyl, active hydrogen, ether bond and carboxyl. These functional group lignins can be used in the preparation and production of soil amendments, adhesives, slow-release nitrogen fertilizers...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/575C07C45/00
CPCC07C45/00C07C47/575
Inventor 徐建曲永水李莉李宏强
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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