A method for preparing furfural after fractional treatment of biomass and adjusting the flow rate for preparing levulinic acid

A technology of levulinic acid and grading treatment, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of being easily affected by acid, increasing reaction paths, obtaining target fuels, etc. The effect of less by-products, less side reactions and low impurity rate

Active Publication Date: 2016-10-12
GUANGZHOU INST OF ENERGY CONVERSION - CHINESE ACAD OF SCI
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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 after fractional treatment of biomass and adjusting the flow rate for preparing levulinic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0021] 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%. The distilled hydrolyzate after removal of FF and a small amount of organic solvent was about 280 mL in total, and still contained a small amount of phosphoric acid. Take 20 mL of the washing liquid after distillation, mix it with washing residue and Amberlyst-70 (accounting for 1% of the total amount of liquid adde...

Embodiment 2

[0027] The method process of this embodiment is as figure 1 shown.

[0028] 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

[0032] The method process of this embodiment is as figure 1 shown.

[0033] 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. Take 20 mL of the distilled washing liquid, mix it with the washing residue and HZSM-5 (1wt%), put it in a preheated high-temperature autoclave, and tighten it quickly...

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Abstract

The invention provides a method for preparing furfural after biomass classification treatment and preparing levulinic acid through adjusting the flow quantity. The method comprises the steps: firstly, carrying out biomass classification pretreatment, separating obtained lignin, hemicellulose and cellulose, converting hemicellulose into xylooligosaccharide, and converting cellulose into amorphous cellulose; then hydrolyzing the xylooligosaccharide into the furfural for recycling; and finally, carrying out acid hydrolysis on the amorphous cellulose in a reaction kettle in a manner of adjusting the adding flow quantity and time of an acid solution, making the amorphous cellulose converted into 5-HMF in the acidic system, and then allowing the 5-HMF to further generate the product LA in the acidic system. The method has the following beneficial effects that sugar, FF and LA with extremely high recovery rate / yield are obtained, a few side reactions exist, the lignin recovery rate is high, the chemical structure change is small, water consumption is less, reactions are quick, requirements on reactors are low, all reagents can be recycled and reused, and the method is green and environmentally friendly.

Description

technical field [0001] The invention relates to the chemical industry field of biomass, in particular to a method for preparing furfural and adjusting flow rate to prepare levulinic acid 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 pla...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/50C07C59/185C07C51/00C08H7/00
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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