Method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in homogeneous system

A technology for composite catalysis of xylose and inorganic salts, which is applied in the field of inorganic salt composite catalysis of xylose to prepare furfural, preparation of xylose, and preparation of furfural by catalysis of xylose, achieving high catalytic efficiency, avoiding equipment corrosion, and high synergistic catalytic efficiency

Inactive Publication Date: 2014-10-08
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are few references on the application of inorganic salts to the hydrolysis of xylose to furfural. In addition, there is no report on the application of water and dimethyl sulfoxide (DMSO) mixed catalytic system to the production of furfural from xylose.

Method used

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  • Method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in homogeneous system
  • Method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in homogeneous system

Examples

Experimental program
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Effect test

Embodiment 1

[0023] (1) Dissolve 1g of xylose in the mixed system of water and dimethyl sulfoxide, where the volumes of water and DMSO are 15mL respectively, and then add SnCl 4 / LiCl compound salt, the molar ratio of compound salt to xylose is 0.5:1, wherein SnCl 4 and LiCl are 0.93g and 0.03g respectively, SnCl 4 The mole fraction of the total amount of inorganic salts is 0.8. React at 130°C for 360min.

[0024] (2) After the reaction, cool naturally, and extract the reaction solution with a large amount of dichloromethane multiple times, and add a small amount of water to wash it several times to remove DMSO in the organic phase. After the organic phase obtained by extraction was washed with saturated brine, dichloromethane was distilled from the organic phase under normal pressure and the temperature was controlled at 40° C. to obtain furfural. figure 1 , 2 The figure obtained by testing the catalytic product with a gas chromatography-mass spectrometer, wherein figure 1 is the mas...

Embodiment 2

[0030] (1) Dissolve 1g of xylose in the mixed system of water and dimethyl sulfoxide (the volume of water is 12.0mL and the volume of DMSO is 8.0mL), and then add the compound inorganic salt AlCl 3 / KCl, the molar ratio of compound salt to xylose is 0.25:1; AlCl 3 The masses of AlCl and KCl are 0.20g and 0.06g respectively, AlCl 3 The mole fraction of the total amount of inorganic salts is 0.5. React at 160°C for 30 minutes.

[0031] (2) After the reaction, cool naturally, and extract the reaction solution with a large amount of dichloromethane multiple times, and add a small amount of water to wash it several times to remove DMSO in the organic phase. After the organic phase obtained by extraction was washed with saturated brine, dichloromethane was distilled from the organic phase under normal pressure and the temperature was controlled at 41° C. to obtain furfural. Judging that reaction product is furfural according to gas chromatography-mass spectrometry measurement res...

Embodiment 3

[0034] (1) Dissolve 1g of xylose in the mixed system of water and dimethyl sulfoxide (the volume of water is 3.33mL and the volume of DMSO is 6.66mL), then add CrCl 3 / NaCl compound salt, the molar ratio of compound salt to xylose is 1:1; CrCl 3 The masses of NaCl and NaCl are 0.36g and 0.31g respectively, CrCl 3 The mole fraction of the total amount of inorganic salts is 0.2. React at 110°C for 600min.

[0035] (2) After the reaction, cool naturally, and extract the reaction solution with a large amount of dichloromethane multiple times, and add a small amount of water to wash it several times to remove DMSO in the organic phase. After the organic phase obtained by extraction was washed with saturated brine, dichloromethane was distilled from the organic phase under normal pressure and controlled at a temperature of 39° C. to obtain furfural. Judging that reaction product is furfural according to gas chromatography-mass spectrometry measurement result, method is with embod...

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Abstract

The invention discloses a method for preparing furfural by inorganic salt-adopted composite catalysis of xylose in a homogeneous system. The method comprises that xylose and a composite inorganic salt are added into a homogeneous reaction system and undergo a reaction at a temperature of 110-160 DEG C for 10-600min, wherein the composite inorganic salt comprises an inorganic salt A selected from SnCl4, AlCl3 and CrCl3 and an inorganic salt B selected from LiCl, KCl and NaCl, the homogeneous reaction system is a mixed solution of water and dimethyl sulfoxide and a volume ratio of water to dimethyl sulfoxide is 0.5-1.5: 1, the reaction solution is naturally cooled and then is subjected to organic solvent-based extraction, and the extract is washed and distilled so that furfural is obtained. The homogeneous catalysis system used by the method has the characteristics of high efficiency, environmental friendliness and cyclic utilization. The composite inorganic salt has the characteristics of good selectivity and high catalytic efficiency. The method has the characteristics of mild technical conditions, operation easiness, high efficiency and good selectivity, is free of inorganic acid used in the reaction process and prevents corrosion on equipment.

Description

technical field [0001] The invention relates to a method for preparing xylose, in particular to a method for preparing furfural by catalyzing xylose, in particular to a method for preparing furfural from xylose in a homogeneous system by composite catalysis of inorganic salts; it belongs to the field of biomass reuse. Background technique [0002] Energy is the premise and foundation for human survival and development. With the reduction of oil and coal reserves, the urgency of developing biomass energy is getting higher and higher. Among them, furfural, also known as furan formaldehyde, is an important heterocyclic organic compound, which can be further converted into plastic or diesel fuel, and is an important chemical platform compound. Furfural can be used to synthesize many organic compounds and new polymer materials through hydrogenation, oxidative dehydrogenation, esterification, halogenation, polymerization, hydrolysis and other chemical reactions. [0003] At pres...

Claims

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Application Information

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IPC IPC(8): C07D307/48
CPCC07D307/48
Inventor 任俊莉王文菊孙润仓李慧玲邓奥杰彭锋
Owner SOUTH CHINA UNIV OF TECH
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