A method for preparing furfural and two-step preparation of levulinic acid after fractional treatment of biomass

A levulinic acid, graded treatment technology, applied in the direction of chemical instruments and methods, preparation of organic compounds, carboxylate preparation, etc., can solve the problems of being easily affected by acids, increasing reaction paths, and hindering industrial applications, etc., to achieve reaction Less impurities, less by-products, and low cost

Active Publication Date: 2017-01-11
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The difficulty in the implementation of this technology is that the direct depolymerization of solid lignocellulose often requires strong acid high temperature and high pressure conditions, which increases the reaction path and makes it difficult to obtain target fuels and / or chemicals in high yields; / or the necessary purification of the target product, its industrial application is seriously hindered, for example, the high value-added chemical levulinic acid is usually obtained from the degradation of biomass with dilute inorganic acids, and the inorganic acids need to be produced in downstream processes, such as hydrogenation to γ - Before removal of Gamma valerolactone (GVL), if the acid is not removed, the downstream process will be easily affected by the acid, making it difficult to control

Method used

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  • A method for preparing furfural and two-step preparation of levulinic acid after fractional treatment of biomass
  • A method for preparing furfural and two-step preparation of levulinic acid after fractional treatment of biomass

Examples

Experimental program
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Embodiment 1

[0022] The method process of this embodiment is as figure 1 shown.

[0023]10g corncobs were soaked with 80mL phosphoric acid at 50°C for 60 minutes, added 300mL of pre-cooled acetone, stirred thoroughly, placed in a centrifuge, and centrifuged at 4000rpm for 20 minutes to separate the supernatant. Wash the residue after centrifugation with 300mL distilled water and filter. The residue obtained after filtration was used for later use, and the washing solution was hydrolyzed in an autoclave at 120° C. for 2 hours. After the reaction, the hydrolyzate was taken out and distilled. After cooling, it was detected by liquid chromatography that the yield of FF was 63%. 280mL of the hydrolyzed solution after removing FF and a small amount of organic solvent contains a small amount of acid. The distilled hydrolyzate is mixed with the residue after washing, and solid acid Amberlyst-70 (accounting for 1% of the total amount of liquid added in the reaction, ie 1.5wt%) is added, and plac...

Embodiment 2

[0030] The method process of this embodiment is as figure 1 shown.

[0031] Mix 10g of bagasse and 80mL of pre-cooled concentrated hydrochloric acid to form a uniform suspension, then slowly add 20mL of pre-cooled concentrated sulfuric acid in the fume hood several times, seal it and place it on a magnetic stirrer, and stir slowly for 60min. Add 300 mL of pre-cooled dioxane, stir slowly for about 30 min, then place in a centrifuge, centrifuge at 4000 rpm for 10 min, and separate the supernatant. Wash again with 200 mL of pre-cooled dioxane, centrifuge at 4000 rpm for 10 min, and separate the supernatant. The two supernatants can be mixed. Wash the centrifuged residue with 300 mL of distilled water and filter. The residue obtained after filtration was used for later use, and the washing solution was hydrolyzed in an autoclave at 110° C. for 1 hour. After the reaction, the hydrolyzate was taken out and distilled. After cooling, it was detected by liquid chromatography that t...

Embodiment 3

[0033] The method process of this embodiment is as figure 1 shown.

[0034] Mix 10g of bagasse and 80mL of pre-cooled concentrated hydrochloric acid to form a uniform suspension, then slowly add 20mL of pre-cooled concentrated sulfuric acid in the fume hood several times, seal it and place it on a magnetic stirrer, and stir slowly for 60min. Add 300 mL of pre-cooled dioxane, stir slowly for about 30 min, then place in a centrifuge, centrifuge at 4000 rpm for 10 min, and separate the supernatant. Wash again with 200 mL of pre-cooled dioxane, centrifuge at 4000 rpm for 10 min, and separate the supernatant. The two supernatants can be mixed. Wash the centrifuged residue with 300 mL of distilled water and filter. The residue obtained after filtration was used for later use, and the washing solution was hydrolyzed in an autoclave at 110° C. for 1 hour. After the reaction, the hydrolyzate was taken out and distilled. After cooling, it was detected by liquid chromatography that t...

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Abstract

The invention provides a method for grading biomass, preparing furfural and preparing levulinic acid (LA) through two steps. The method comprises the following steps: processing a biomass raw material by using an acid / organic solvent combination system to separate lignose, hemicellulose and cellulose, converting hemicellulose into xylooligosaccharide, and converting cellulose into amorphous cellulose; extracting xylooligosaccharide by water, and converting xylooligosaccharide into furfural; and carrying out two-step acid hydrolysis on amorphous cellulose-based residues to make amorphous cellulose in residues converted into 5-HMF (5-hydroxymethylfurfural), introducing the 5-HMF to a second reactor with acidic environment, and carrying out acid hydrolysis to generate the LA. The method has the advantages of extremely high recovery rate / yield of sugar, FF and LA, few side reactions, high recovery rate and small chemical structure change of lignin, less water consumption, fast reaction, low requirements on a reactor, recycling of all reagents, and environmental protection.

Description

technical field [0001] The invention relates to the chemical industry field of biomass, in particular to a method for preparing furfural and levulinic acid in two steps through fractional treatment of biomass containing hemicellulose and cellulose. Background technique [0002] Biomass contains a large amount of hemicellulose, cellulose and lignin. The traditional biomass conversion method is to depolymerize biomass into sugars, and then ferment to produce ethanol or other energy sources. Now researches at home and abroad have found that biomass Preparation of chemicals based on sugar platforms is more economical and applicable. For example, xylose obtained by depolymerization of hemicellulose can be used to prepare furfural (Furfural, referred to as FF). Furfural has active chemical properties and is an important organic chemical product. Many derivatives can be prepared through oxidation, condensation and other reactions. It is suitable for synthetic plastics, medicine, p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/50C07C59/185C07C51/00
CPCY02P20/582
Inventor 袁振宏王琼庄新姝亓伟谭雪松余强
Owner GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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