Preparation method of methyl levulinate catalyzed by ionic liquid

A technology for catalyzing methyl levulinate and ionic liquids, applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc., can solve the problem of large equipment loss and unfavorable promotion, high catalyst temperature, and low yield. It is beneficial to the development of large-scale industrialization, the conversion rate of raw materials is high, and the equipment requirements are low.

Active Publication Date: 2021-02-19
YANCHENG TEACHERS UNIV
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  • Abstract
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Problems solved by technology

(Zhang Yangyang, Luo Xuan, Zhuang Xuli, Tong Xinli. Mixed acid catalyzed selective conversion of glucose to methyl levulinate. Acta Chemie Sinica. 2015, 66(9): 3490-3495) The reaction temperature is high; ionic liquids have acidic substances, which are harmful to equipment Large loss is not conducive to promotion
(Zeng Shanshan, Lin Lu, Peng Lincai. Solid acid SO 4 2- / TiO 2 Catalyzing glucose to prepare methyl levulinate. Modern Food Science and Technology. 2011, 27(7): 783-787) The temperature of the preparation catalyst is too high, the yield is not high, and the requirements for equipment are high, which is not conducive to popularization

Method used

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  • Preparation method of methyl levulinate catalyzed by ionic liquid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Preparation of ionic liquid 1-ethyl-3-methylimidazolium bromide bromide: In a 100ml three-necked flask with a condensing reflux device, add 1-methylimidazole (8.2g, 0.1mol), bromoethane (11.99 g, 0.11mol) was stirred at 35°C for 5 hours to obtain a white crystalline powder, which was washed with ethyl acetate to remove ethyl bromide and dried in vacuum at 80°C for 3h. Yield 85%.

Embodiment 2

[0025] In a 50ml reactor, add glucose (0.20g, 1.11mmol), ionic liquid (1-ethyl-3-methylimidazolium bromide bromide) (0.25g, 1.31mmol), SnCl 4 ·5H 2 O (0.039g, 0.11mmol) and methanol (1.6g, about 2ml) were reacted at 100°C for 2 hours, filtered with suction, methanol was distilled off by simple distillation, and then the product was distilled off by vacuum distillation. The yield was 66%.

Embodiment 3

[0027] In a 50ml reactor, add glucose (0.20g, 1.11mmol), ionic liquid (1-ethyl-3-methylimidazolium bromide bromide) (0.25g, 1.31mmol), SnCl 4 ·5H 2 O (0.039g, 0.11mmol) and methanol (1.6g, about 2ml) were reacted at 110°C for 1.5 hours, filtered with suction, methanol was distilled off by simple distillation, and then the product was distilled off by vacuum distillation. The yield was 56%.

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Abstract

The invention discloses a preparation method of methyl levulinate by ion liquid catalysis. The method is characterized in that furfuryl alcohol, glucose, sucrose and the like are used as raw materials; imidazole ion liquid and SnCl4.5H2O are used as catalysts; methanol is used as a raw material and a reaction medium; under the heating condition, a target compound is prepared. The method has the advantages that (1) the used raw materials are renewable resources and conform to the circulation economy development trends; (2) the sources of all raw and auxiliary materials are wide; the preparationis convenient; the cooperated effects of the catalyst are good; the raw material conversion rate is high; the product selectivity is high; (3) the preparation process has low requirements on equipment; the reaction is performed at the normal pressure; the post treatment is convenient; the method is a clean preparation method of the methyl levulinate, and is favorable for scaled industrial development.

Description

[0001] A technical field [0002] The invention relates to a method for preparing methyl levulinate catalyzed by an ionic liquid, and belongs to the technical field of chemical material preparation. This method is suitable for using furfuryl alcohol, glucose, sucrose, etc. as raw materials, imidazole ionic liquid and SnCl 4 ·5H 2 O is used as a catalyst, methanol is used as a raw material and a reaction medium, and the target compound is prepared at a certain temperature. [0003] Two background technology [0004] Due to the gradual depletion of fossil fuels and the increasing severity of environmental problems, it is urgent to find alternative biofuels and chemicals. Among the abundant renewable energy sources, biomass has attracted extensive attention as the only renewable organic carbon resource due to its characteristics of abundant reserves, low price, and the ability to realize carbon cycle. The research results show that ionic liquids have good catalytic properties i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00C07C69/716B01J31/26
CPCB01J31/26C07C67/00C07C69/716
Inventor 刘文雨李佳琪方东颜前
Owner YANCHENG TEACHERS UNIV
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