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Method for preparing ethyl levulinate based on solid superacid catalysis and furfuryl alcohol alcoholysis

A technology of ethyl levulinate and solid super acid, applied in the field of ethyl levulinate, can solve the problems of non-conformity with green chemistry, difficult separation of products, severe reaction conditions, etc., achieves good application prospects, convenient post-processing, and reaction Simple system effect

Inactive Publication Date: 2013-09-04
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chinese patent CN101709033A discloses a method for preparing methyl levulinate by alcoholysis of hexavalent sugar in near-critical methanol. The method uses biomass sugar as raw material and has the advantages of simple process and low cost, but the reaction conditions are relatively severe and can High consumption
Chinese patent CN102405205A discloses a method for converting furfuryl alcohol into ethyl levulinate in a single-step reaction. The method uses an inorganic liquid acid as a catalyst. As a catalyst, a large amount of waste liquid and residue will be produced, and there are problems such as difficult separation of products and serious corrosion of equipment, which does not conform to the current development direction of green chemistry

Method used

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  • Method for preparing ethyl levulinate based on solid superacid catalysis and furfuryl alcohol alcoholysis
  • Method for preparing ethyl levulinate based on solid superacid catalysis and furfuryl alcohol alcoholysis

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Effect test

Embodiment 1

[0025] 1mL furfuryl alcohol, 0.5g solid superacid SO 4 2– / TiO 2 Add 20mL ethanol into a 50mL reactor, seal it and start the reaction, the stirring speed is 500rpm, start timing when the temperature rises to 125°C, keep the temperature for 2 hours, after the reaction, immediately immerse the reactor in cold water Cool down to room temperature. The reaction solution was centrifuged at 10000rpm, and the supernatant was taken for analysis and detection. After gas chromatography analysis, it was compared with the gas chromatography standard spectrum of furfuryl alcohol and ethyl levulinate (see figure 1 and figure 2 ) After comparison, it is calculated that the yield of the product ethyl levulinate can reach 68.3%.

Embodiment 2

[0027] 1mL furfuryl alcohol, 0.5g solid superacid SO 4 2– / ZrO 2 Add 20mL ethanol into a 50mL reactor, seal it and start the reaction, the stirring speed is 500rpm, start timing when the temperature rises to 125°C, keep the temperature for 2 hours, after the reaction, immediately immerse the reactor in cold water Cool down to room temperature. The reaction solution was centrifuged at 10,000 rpm, and the supernatant was taken for analysis and detection. The yield of ethyl levulinate was calculated by gas chromatography to reach 64.3%.

Embodiment 3

[0029] 1mL furfuryl alcohol, 0.5g solid superacid S 2 o 8 2- / SnO 2 Add 20mL ethanol into a 50mL reactor, seal it and start the reaction, the stirring speed is 500rpm, start timing when the temperature rises to 125°C, keep the temperature for 2 hours, after the reaction, immediately immerse the reactor in cold water Cool down to room temperature. The reaction solution was centrifuged at 10,000 rpm, and the supernatant was taken for analysis and detection. The yield of ethyl levulinate calculated by gas chromatography analysis could reach 65.5%.

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Abstract

The invention discloses a method for preparing ethyl levulinate based on solid superacid catalysis and furfuryl alcohol alcoholysis, and relates to ethyl levulinate. The method comprises the steps of adding furfuryl alcohol, a catalyst and a reaction solvent to a reaction kettle, reacting, and obtaining ethyl levulinate. The catalyst is selected from at least one of solid superacid of SO4<2-> / TiO2, SO4<2-> / ZrO2, SO4<2-> / Fe2O3, SO4<2-> / SnO2, and SO4<2-> / Al2O3, or at least one of solid superacid of S2O8<2-> / TiO2, S2O8<2-> / ZrO2, S2O8<2-> / Fe2O3, S2O8<2-> / SnO2, and S2O8<2-> / Al2O3; the reaction solvent is ethyl alcohol; and reaction conditions are that the temperature is 100-150 DEG C, the rotating speed is 300-500 rpm (revolutions per minute), the time is 0.5-2.5h, a mass ratio of furfuryl alcohol to solid superacid is (1-4):1, and a mass ratio of furfuryl alcohol to ethyl alcohol is (0.01-0.2):1.

Description

technical field [0001] The invention relates to ethyl levulinate, in particular to a method for preparing ethyl levulinate based on solid superacid-catalyzed alcoholysis of furfuryl alcohol. Background technique [0002] With the continuous consumption of coal, oil and other non-renewable resources, human society is facing an unprecedented resource and energy crisis. Biomass is a renewable resource with the advantages of huge quantity, low price, and the realization of carbon cycle. The use of biomass resources to prepare fuels and chemicals has become a research hotspot at home and abroad. A variety of platform compounds can be prepared from biomass resources, and ethyl levulinate is one of them. [0003] Ethyl levulinate contains a carbonyl group and an ester group. The carbon-oxygen double bond on the carbonyl group is a strong polar bond, and the carbon atom is the positive charge center. When the carbonyl group reacts, the electrophilic center of the carbon atom plays ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00
Inventor 曾宪海赵耿孙勇林鹿
Owner XIAMEN UNIV
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