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A microwave-assisted ionic liquid catalyzed method for converting microcrystalline cellulose into 5-hydroxymethylfurfural

A technology of microcrystalline cellulose and hydroxymethyl furfural, applied in organic chemistry and other directions, can solve the problems of difficult industrialization, high cost, expensive ionic liquid, etc., and achieves fast heating rate, improved efficiency, and reduced dosage. Effect

Active Publication Date: 2015-09-30
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the high price of ionic liquids, the cost of preparing 5-HMF as a solvent remains high, and industrial utilization is difficult to achieve

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Microcrystalline cellulose 0.2g, tetramethylguanidine tetrafluoroborate ([TMG]BF 4 ) Catalyst 0.2g, 10% LiCl-DMAc solution 100ml is placed in the microwave reactor, under the protection of nitrogen, stir and reflux reaction, heat up to 100 ℃, microwave output power is 400w, reaction time is 30min, regular sampling analysis, 5-hydroxymethyl The yield of furfural was 19.27%.

Embodiment 2

[0024] Microcrystalline Cellulose 0.5g, tetramethylguanidine lactate ([TMG]L) catalyst 0.1g, 100% LiCl-DMAc solution 100ml are placed in microwave reactor, under the protection of nitrogen, stir reflux reaction, be warming up to 140 ℃, microwave output power is 400w, reaction time is 30min, regular sampling analysis, the yield of 5-hydroxymethylfurfural is 2.34%

Embodiment 3

[0026] Microcrystalline Cellulose 0.5g, tetramethylguanidine acetate ([TMG]OAc) catalyzer 0.3g, 100ml of LiCl-DMAc solution 100ml are placed in the microwave reactor, under the nitrogen protection stirring reflux reaction, be warming up to 140 ℃, microwave output power of 400w, reaction time of 60min, regular sampling and analysis, the yield of 5-hydroxymethylfurfural was 9.72%.

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PUM

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Abstract

The invention discloses a method for converting microcrystalline cellulose into 5-hydroxymethyl furfural through microwave-assisted ionic liquid catalysis. The method comprises the following steps: adding microcrystalline cellulose, an ionic-liquid catalyst and an organic solvent (lithium bromide-N,N-dimethylformamide, lithium chloride-N,N-dimethylacetamide or the like) into a microwave reactor at normal pressure, introducing nitrogen gas for protecting, carrying out magnetic stirring at a constant speed, cooling for refluxing, and carrying out microwave reaction for 1-120 minutes at the power of 400-800w at the constant temperature of 100-160 DEG C. According to the method, ionic liquid is applied to the catalysis of microcrystalline cellulose conversion at normal pressure through microwave-assisted heating for the first time, so as to convert microcrystalline cellulose into 5-hydroxymethyl furfural.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid applied to microcrystalline cellulose directional transformation. The method can significantly reduce the amount of ionic liquid and increase the yield of microcrystalline cellulose converted into 5-hydroxymethylfurfural, thereby helping to improve the use of ionic liquid. Economics of converting microcrystalline cellulose to 5-hydroxymethylfurfural. Background technique [0002] 5-Hydroxymethylfurfural (5-HMF), as a new platform compound, has very broad application prospects and can be used to synthesize a series of precursor compounds for medicine and pesticides; 5-HMF can be used as a biofuel precursor To synthesize 2,5-dimethylfuran (DMF), which can be used as a diesel fuel additive, or even diesel fuel itself, to replace traditional fossil fuels. In addition, 5-HMF can also be used to synthesize macrocyclic compounds with strong coordination ability. [0003] As a new kind of catalyst ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/46
Inventor 徐建曲永水高婧
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI