A method for producing furfural by catalyzing xylose extraction with glacial acetic acid under normal pressure

An acetic acid catalyzed xylose extraction technology, which is applied in organic chemistry and other fields, can solve problems such as potential safety hazards, decreased solubility and extraction speed, and reduced furfural yield, so as to ensure smooth production, save production procedures, and reduce side reactions.

Active Publication Date: 2020-08-28
山东乔克环境科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The inventors found that when the reaction system adopts high pressure, a high-pressure container needs to be used, which has certain potential safety hazards. The temperature of the reaction system is too high, the solubility of furfural in the extractant and the extraction speed are significantly reduced, and it is difficult to transfer the furfural in the reaction water phase in time. In the extractant, the furfural in the water phase undergoes side reactions under acidic environment and heating conditions, which significantly reduces the yield of furfural

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A kind of method under normal pressure glacial acetic acid catalysis xylose extraction produces furfural, comprises the steps:

[0031] 1) to 50ml, in the xylose solution that massfraction is 12%, add acetic acid, ferric chloride and dimethyl phthalate, the volumetric concentration of acetic acid is 5%, and the mass percent of ferric chloride is 8%; Dimethyl diformate accounts for 50% of the volume fraction of the entire reaction system; the reaction system is constantly stirred during the reaction; the temperature of the reaction is 145°C, the time is 40min, and the pressure is 1 atmosphere;

[0032] 2) After the reaction is completed, let it stand for 8 minutes to allow the reaction system to stand for stratification, and extract the extractant from the lower outlet; the extractant containing furfural enters the initial distillation tower, the temperature at the bottom of the tower is 200 ° C, and the temperature inside the tower is 180 ° C. °C, the top gas is furfura...

Embodiment 2

[0034] A kind of method under normal pressure glacial acetic acid catalysis xylose extraction produces furfural, comprises the steps:

[0035] 1) to 50ml, in the xylose solution that mass fraction is 20%, add acetic acid, ferric chloride and dimethyl phthalate, the volumetric concentration of acetic acid is 6%, and the mass percentage of ferric chloride is 10%; The added volume of dimethyl diformate accounts for 60% of the total volume of the mixed solution; the reaction system is constantly stirred during the reaction; the temperature of the reaction is 125°C, the time is 45min, and the pressure is 1 atmosphere;

[0036] 2) After the reaction is completed, let it stand for 5-10 minutes to allow the reaction system to stand for stratification, and extract the extractant from the lower outlet; the extractant containing furfural enters the initial distillation tower, the temperature at the bottom of the tower is 180 ° C, and the temperature inside the tower is 180 ° C. The tempe...

Embodiment 3

[0038] A kind of method under normal pressure glacial acetic acid catalysis xylose extraction produces furfural, comprises the steps:

[0039] 1) to 50ml, in the xylose solution that mass fraction is 15%, add acetic acid, ferric chloride and dimethyl phthalate, the volumetric concentration of acetic acid is 3%, and the mass percentage of ferric chloride is 5%; Dimethyl diformate accounts for 70% of the volume fraction of the entire reaction system; the reaction system is constantly stirred during the reaction; the temperature of the reaction is 125°C, the time is 30min, and the pressure is 1 atmosphere;

[0040] 2) After the reaction is completed, let it stand for 5-10 minutes to allow the reaction system to stand for stratification, and extract the extractant from the lower outlet; the extractant containing furfural enters the initial distillation tower, the temperature at the bottom of the tower is 200 ° C, and the temperature inside the tower is 200 ° C. The temperature is ...

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Abstract

The invention discloses a method for extraction production of furfural by adopting glacial acetic acid to catalyze xylose under normal pressure. The method comprises following steps: 1), acetic acid,ferric chloride and dimethyl phthalate are added to a xylose solution, concentration of acetic acid is enabled to be 3%-6% by mass, v / v, and concentration of ferric chloride is enabled to be 5%-10% bymass; adding volume of dimethyl phthalate is 50%-70% of total volume of a mixed solution; a reaction system is continuously stirred in a reaction process; 2), after the reaction is finished, the mixed solution is left to stand for a set period of time, the reaction system is enabled to stand for layering, and a lower extraction phase is conveyed to a distillation column to separate crude furfuraland dimethyl phthalate; 3), dimethyl phthalate obtained after separation is circulated to the step 2) and used as an extraction agent for furfural, crude furfural obtained after separation is distilled, and refined furfural is obtained.

Description

technical field [0001] The invention belongs to the technical field of furfural preparation, in particular to a method for producing furfural by catalyzing xylose extraction with glacial acetic acid under normal pressure. Background technique [0002] The information disclosed in this background section is only intended to increase the understanding of the general background of the present invention, and is not necessarily taken as an acknowledgment or any form of suggestion that the information constitutes the prior art already known to those skilled in the art. [0003] Furfural, also known as furan formaldehyde, has functional groups such as aldehyde groups, dienes, and cyclic ethers in the molecular structure of furfural, so it has the properties of aldehydes, ethers, dienes, and aromatic compounds, and its unique chemical structure can be oxidized and hydrogenated , condensation and other reactions are widely used in many production fields such as medicine, petrochemica...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/50
CPCC07D307/50
Inventor 肖兵董玉平王仲钢
Owner 山东乔克环境科技有限公司
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