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Lignocellulosic biomass direct pressurized liquefaction and ethyl levulinate directional preparation method

A technology of levulinic acid ester and pressurized liquefaction, which is applied in the field of biomass resource utilization, can solve the problems of large amount of solvent, low product purity, complicated process and the like, achieves easy recovery and reuse, simple method operation, and improved The effect of reaction efficiency

Inactive Publication Date: 2015-11-18
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Technical problem to be solved: In order to solve the shortcomings of traditional separation of bio-oil to obtain chemicals, such as low product purity, low yield, complex process, and large amount of solvent usage, the present invention provides a direct pressurized liquefaction and orientation of lignocellulosic biomass Preparation, extraction and separation of levulinic acid ester method, wide source of raw materials, simple operation process, can obtain high value-added chemicals such as levulinic acid ester, and the product purity is high

Method used

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  • Lignocellulosic biomass direct pressurized liquefaction and ethyl levulinate directional preparation method
  • Lignocellulosic biomass direct pressurized liquefaction and ethyl levulinate directional preparation method
  • Lignocellulosic biomass direct pressurized liquefaction and ethyl levulinate directional preparation method

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Effect test

Embodiment 1

[0025] Weigh 40g of absolute dry weight bamboo, the particle size is 40-60 mesh, add 240g of methanol and 1.0g of sulfuric acid into an autoclave with a volume of 1L, and evacuate the air in the autoclave with nitrogen; at a heating rate of 3°C / min With a stirring speed of 500r / min, the temperature was raised to 200°C, and the pressure of the autoclave was 5MPa. After the reaction was kept for 60 minutes, the heating was turned off, and the cooling water was quickly passed through to cool down to room temperature within 1 to 5 minutes. After the liquefied product was neutralized and filtered, methanol was recovered by rotary evaporation under reduced pressure at 45° C. under a pressure of -0.09 MPa, and 80 g of distilled water was added, resulting in phase separation. 40 g of ethyl acetate was added to the aqueous phase, and after phase separation, the ethyl acetate extract was evaporated to dryness to obtain a part of levulinic acid ester compounds, and the remaining water ph...

Embodiment 2

[0027] Weigh 40g of absolute dry weight bamboo, the particle size is 40-60 mesh, add 400g of methanol and 1.0g of sulfuric acid into an autoclave with a volume of 1L, and empty the air in the autoclave with nitrogen; at a heating rate of 3°C / min With a stirring speed of 500r / min, the temperature was raised to 200°C, and the autoclave pressure was 7MPa. After the reaction was kept for 60 minutes, the heating was turned off, and the cooling water was quickly passed through to cool down to room temperature within 1 to 5 minutes. After the liquefied product was neutralized and filtered, methanol was recovered by rotary evaporation under reduced pressure at 45° C. under a pressure of -0.09 MPa, and 80 g of distilled water was added, resulting in phase separation. 40 g of ethyl acetate was added to the aqueous phase, and after phase separation, the ethyl acetate extract was evaporated to dryness to obtain a part of levulinic acid ester compounds, and the remaining water phase was ev...

Embodiment 3

[0029] Weigh 40g of absolute dry weight bamboo, the particle size is 40-60 mesh, add 240g of methanol and 0.4g of sulfuric acid into an autoclave with a volume of 1L, and empty the air in the autoclave with nitrogen; at a heating rate of 3°C / min With a stirring speed of 500r / min, the temperature was raised to 200°C, and the autoclave pressure was 5MPa. After the reaction was kept for 60 minutes, the heating was turned off, and the cooling water was quickly passed through to cool down to room temperature within 1 to 5 minutes. After the liquefied product was neutralized and filtered, methanol was recovered by rotary evaporation under reduced pressure at 45° C. under a pressure of -0.09 MPa, and 80 g of distilled water was added, resulting in phase separation. 40 g of ethyl acetate was added to the aqueous phase, and after phase separation, the ethyl acetate extract was evaporated to dryness to obtain a part of levulinic acid ester compounds, and the remaining water phase was ev...

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Abstract

A lignocellulosic biomass direct pressurized liquefaction and ethyl levulinate directional preparation method comprises the following steps: firstly, direct pressurized liquefaction reaction: adding biomass raw materials and such low-alcohol acid catalysts as methanol and glycol according to a mass ratio of 1:(6-10):(0.01-0.05) into a 1L autoclave, and performing alcoholysis liquefaction reaction for 60-180 min at 160-240 DEG C, wherein the rotational speed is 500 r / min; secondly, directional preparation: filtering the pressurized liquefaction product, performing neutralization, rotary evaporation and low alcohol recovery on the filtrate, adopting distilled water and an organic solvent extraction agent for directional extraction and separation of levulinic acid ester compounds in the pressurized liquefaction product to obtain ethyl levulinate of which the total content is 78%.

Description

technical field [0001] The invention belongs to the field of biomass resource utilization, and mainly relates to the separation and preparation of levulinic acid ester compounds from biomass pyrolysis liquefied oil. Background technique [0002] Cellulosic biomass is a huge amount of renewable resources. It has a wide range of sources, low prices, and can be regenerated. The rational use of existing biomass energy can not only alleviate the society's consumption of non-renewable energy such as coal, oil, and natural gas. Demand pressure, and can protect the environment, reduce harmful gas emissions. At present, there are many studies on the thermochemical conversion and utilization of fibrous biomass, mainly including rapid pyrolysis liquefaction, indirect liquefaction and solvent liquefaction [Zhang Huiyan. Basic and technological research on the preparation of liquid fuels and chemicals by catalytic pyrolysis of biomass [D]. Nanjing, Southeast University, 2012]. However...

Claims

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Application Information

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IPC IPC(8): C07C69/716C07C67/00C07C67/08C07C67/58
CPCC07C67/00C07C67/08C07C67/58C07C69/716
Inventor 蒋剑春冯君锋徐俊明王奎应浩关倩马艳杨中志
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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