Method for preparing levulinic acid and furfural by hydrolyzing biomass

A technology of levulinic acid and biomass, applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylate, etc., can solve the problems of many by-products, low yield, long reaction time, etc.

Inactive Publication Date: 2016-06-15
ENERGY RES INST CO LTD HENAN ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] In the research on the preparation of levulinic acid by direct hydrolysis of biomass, furfural residue, xylose residue, cottonseed hull, starch, etc. are mostly used as r

Method used

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  • Method for preparing levulinic acid and furfural by hydrolyzing biomass

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Embodiment 1

[0032] A method for preparing levulinic acid and furfural by hydrolysis of biomass, comprising the following steps:

[0033] 1) After crushing 230kg of corn stalks with a moisture content of 11% (the main components are: 25% hemicellulose, 33% cellulose, and 16% lignin) into 15mm, fill it into the reactor, and add 170kg of catalyst (concentration 5% dilute sulfuric acid and 0.5% FeCl 3 ), at a speed of 0.6t / h, 170°C, 0.6MPa water vapor is introduced to undergo primary hydrolysis. When the temperature of the biomass and catalyst reaches 160°C, the gas phase of the primary hydrolysis is discharged until the primary hydrolysis is completed, and the gas phase of the primary hydrolysis passes through Condensation to obtain an aqueous solution containing furfural, the reaction time for a hydrolysis is 1h;

[0034] 2) Introduce steam at 210°C and 2.0MPa at a rate of 0.5t / h into the reactor after the primary hydrolysis in step 1) for secondary hydrolysis. When the biomass temperature...

Embodiment 2

[0043] A method for preparing levulinic acid and furfural by hydrolysis of biomass, comprising the following steps:

[0044] 1) After crushing 280kg corncobs with a moisture content of 7% (the main components are: 36% hemicellulose, 32% cellulose, and 15% lignin) into 20mm, fill it into the reactor, and add 190kg of catalyst (concentration: 3% dilute sulfuric acid and 0.3% FeCl 3 ), at a speed of 0.7t / h, 170°C, 0.6MPa water vapor is introduced to undergo primary hydrolysis. When the temperature of the biomass and catalyst reaches 160°C, the gas phase of the primary hydrolysis is discharged until the primary hydrolysis is completed, and the gas phase of the primary hydrolysis passes through Condensation to obtain an aqueous solution containing furfural, the reaction time for a hydrolysis is 1h;

[0045] 2) Introduce steam at 210°C and 2.0MPa at a rate of 0.56t / h into the reaction kettle after the primary hydrolysis in step 1) for secondary hydrolysis. When the biomass temperat...

Embodiment 3

[0052] A method for preparing levulinic acid and furfural by hydrolysis of biomass, comprising the following steps:

[0053] 1) After crushing 300kg of wood chips with a moisture content of 11% (the main components are: 50% hemicellulose, 30% cellulose, and 25% lignin) into 10mm, fill it into the reactor, and add 300kg of catalyst (concentration: 5% dilute sulfuric acid and 0.5% FeCl 3 ), at a speed of 0.8t / h, 180°C, 1MPa water vapor is introduced to undergo primary hydrolysis. When the temperature of the biomass and catalyst reaches 170°C, the gas phase of the primary hydrolysis is discharged until the primary hydrolysis is completed, and the gas phase of the primary hydrolysis is condensed To obtain an aqueous solution containing furfural, the reaction time for one hydrolysis is 1.1h;

[0054] 2) Introduce steam at 223°C and 2.5MPa at a rate of 0.6t / h into the reactor after the primary hydrolysis in step 1) for secondary hydrolysis. When the biomass temperature reaches 200°...

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Abstract

The invention discloses a method for preparing levulinic acid and furfural by hydrolyzing biomass. The method comprises the following steps of firstly, mixing the biomass with a catalyst, introducing water vapor to generate primary hydrolysis, discharging a gaseous phase of the primary hydrolysis and condensing to obtain an aqueous solution containing the furfural; secondly, introducing water vapor into the biomass subjected to primary hydrolysis to perform secondary hydrolysis, and discharging a gaseous phase of the secondary hydrolysis; thirdly, performing temperature and pressure reduction on the gaseous phase subjected to the secondary hydrolysis, enabling the gaseous phase to enter into a reaction kettle filled with the biomass, generating primary hydrolysis, discharging the gaseous phase of the primary hydrolysis, and condensing the gaseous phase to obtain an aqueous solution containing the furfural and the levulinic acid; fourthly, supplementing the catalyst into the reaction still in the third step, introducing water vapor for secondary hydrolysis, and discharging a gaseous phase of the secondary hydrolysis; fifthly, repeating the third step and the fourth step; sixthly, purifying and separating the aqueous solution in the first step from the aqueous solution in the third step to obtain the levulinic acid and the furfural. According to the method disclosed by the invention, the yields of the levulinic acid and the furfural are increased; the yield of the furfural reaches 60 percent or above 60 percent, and the yield of the levulinic acid reaches 50 percent or above 50 percent.

Description

technical field [0001] The invention belongs to the technical field of biomass chemical industry, and in particular relates to a method for preparing levulinic acid and furfural by hydrolyzing biomass. Background technique [0002] Levulinic acid (Levulinic Acid, LA), also known as 4-oxovaleric acid, levulonic acid or valeric acid, its appearance is white flake or needle crystal, it is flammable, low toxicity, hygroscopic, when heated No carbon dioxide is released, and distillation under normal pressure hardly decomposes. Since the molecular structure of levulinic acid contains multiple functional groups such as carbonyl, carboxyl, methyl and methylene, it has both the properties of carboxylic acid and the properties of ketone, and has good chemical reactivity, and can undergo esterification and substitution. , condensation and neutralization reactions, etc., and products such as resins, medicines, pesticides, spices, solvents, paints, inks, rubber, plastic additives, lubri...

Claims

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Application Information

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IPC IPC(8): C07C51/00C07C59/185C07D307/50
CPCC07C51/00C07D307/50C07C59/185
Inventor 雷廷宙李在峰林鹿李顺清徐海燕杨延涛任素霞何晓峰杨树华朱金陵
Owner ENERGY RES INST CO LTD HENAN ACADEMY OF SCI
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