A method for preparing furfural after fractional treatment of biomass and preparing levulinic acid by rapid temperature change method

A technology of grading treatment and levulinic acid, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc. The effect of less by-products, less side reactions, and less water consumption

Active Publication Date: 2016-10-12
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 after fractional treatment of biomass and preparing levulinic acid by rapid temperature change method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] The method process of this embodiment is as figure 1 shown.

[0021] 10g of corn cobs were treated with 80mL of analytically pure phosphoric acid at 50°C for 60min with stirring and impregnation, added 300mL of pre-cooled acetone, stirred thoroughly, placed in a centrifuge, and centrifuged at 4000rpm for 20min 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%. The distilled hydrolyzate, from which FF and traces of organic solvents were removed, totaled about 280 mL and contained a small amount of acid. The distilled washing liquid and washing residue are mixed, placed in a high-pressure tubular reactor, and then Amberlyst-70 ...

Embodiment 2

[0025] The method process of this embodiment is as figure 1 shown.

[0026] 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

[0028] The method process of this embodiment is as figure 1 shown.

[0029] 10g of corn stalks were soaked with 80mL of trifluoroacetic acid at 50°C for 45min, then added 200mL of pre-cooled isopropanol, stirred thoroughly and then placed in a centrifuge for 1h, then centrifuged at 4000rpm for 20min 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 80 minutes. After the reaction, the hydrolyzate was taken out and distilled. After cooling, it was detected by liquid chromatography that the yield of FF was 61%. After distillation of the hydrolyzate, FF and traces of organic solvent were removed, leaving a small amount of acid. The distilled washing solution and the washing residue are mixed, placed in a high-pressure tubular reactor, and then HZSM-5 (0.7wt%) is added, and the pH of the react...

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Abstract

The invention provides a method for grading biomass, preparing furfural and preparing levulinic acid (LA) through a rapid temperature changing technology. 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 in residues by water, and converting xylooligosaccharide into furfural; and carrying out rapid temperature changing on amorphous cellulose-based residues in acidic environment to make amorphous cellulose converted into 5-HMF (5-hydroxymethylfurfural), and processing the 5-HMF to rapidly and efficiently 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 by fractional treatment of biomass containing hemicellulose and cellulose, and preparing levulinic acid by a variable temperature method. 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 synth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/50C07C59/185C07C51/00
CPCC07C51/00C07D307/50C07C59/185
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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