Method for preparing ethyl levulinate based on catalysis of alcoholization of furfuryl alcohol with carbon-based solid acid

A technology of ethyl levulinate and carbon-based solid acid, which is applied in the field of ethyl levulinate, can solve problems such as non-compliance with green chemistry, difficult separation of products, severe reaction conditions, etc., and achieve good application prospects, convenient post-processing, The effect of simple reaction system

Active Publication Date: 2013-09-11
XIAMEN UNIV
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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 catalysis of alcoholization of furfuryl alcohol with carbon-based solid acid
  • Method for preparing ethyl levulinate based on catalysis of alcoholization of furfuryl alcohol with carbon-based solid acid

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Embodiment 1

[0019] Add 1mL of furfuryl alcohol, 0.5g of hydrothermal carbon-based solid acid and 20mL of ethanol together into a 50mL reaction kettle, and start the reaction after sealing it. The stirring speed is 500rpm. When the temperature rises to 125°C, start timing. h, after the reaction is over, immediately immerse the reactor in cold water to 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, the calculated yield of ethyl levulinate can reach 63.6%.

Embodiment 2

[0021] Add 1mL of furfuryl alcohol, 0.5g of dry distilled carbon-based solid acid and 20mL of ethanol into a 50mL reaction kettle, and start the reaction after sealing. After the end of the reaction, immediately immerse the reactor in cold water to 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 61.1%.

Embodiment 3

[0023] Add 1mL of furfuryl alcohol, 0.5g of hydrothermal carbon-based solid acid and 20mL of ethanol into a 50mL reaction kettle, and start the reaction after sealing. The stirring speed is 500rpm. When the temperature rises to 100°C, start timing. h, after the reaction is over, immediately immerse the reactor in cold water to 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 39.5%.

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Abstract

The invention relates to a method for preparing ethyl levulinate based on catalysis of alcoholization of furfuryl alcohol with carbon-based solid acid, and relates to ethyl levulinate. The method comprises the following steps: uniformly mixing furfuryl alcohol, anhydrous ethanol and the carbon-based solid acid; adding a mixture obtained from the former step into a stainless steel high pressure reaction kettle; closing the reactor; and catalyzing the alcoholization of the furfuryl alcohol so as to prepare ethyl levulinate. The condition for catalysis of the alcoholization of the furfuryl alcohol is as follows: the reaction temperature is 100-150 DEG C, the stirring rotating speed is 300-500rpm, and the reaction time is 0.5-2.5 hours. The weight ratio of furfuryl alcohol to ethanol is (0.01-0.1):1, and the mass ratio of furfuryl alcohol to carbon-based solid acid is (1-4):1. The carbon-based solid acid can be hydrothermal carbon-based solid acid or carbonized carbon-based solid acid. The carbon-based solid acid is used as a catalyst which is simple to prepare and low in cost, and can be repeatedly used, so that the product yield is high and the byproducts are fewer. The method is simple in reaction system, mild in reaction condition, short in reaction time, environment-friendly, low in cost and convenient to posttreat.

Description

technical field [0001] The invention relates to ethyl levulinate, in particular to a method for preparing ethyl levulinate based on carbon-based solid acid-catalyzed alcoholysis of furfuryl alcohol. Background technique [0002] At present, the vast majority of fuels and chemicals are mainly obtained from resources such as coal and petroleum. With the continuous consumption of such non-renewable resources, human society is facing an unprecedented resource and energy crisis. At the same time, the greenhouse effect and other environmental problems caused by fossil fuels have also attracted people's close attention. Biomass is a renewable resource, which has the advantages of huge quantity, low price, and the realization of carbon cycle. Furthermore, biomass is the only renewable resource capable of carbon fixation, which is important for the production of liquid hydrocarbon fuels and other chemical products. A variety of platform compounds can be prepared from biomass resour...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/716C07C67/00B01J27/02
Inventor 曾宪海赵耿孙勇林鹿
Owner XIAMEN UNIV
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