Method for preparing ethyl acetylpropionate by catalyzing furfural via one-pot method
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A technology of ethyl levulinate and furfural, which is applied in the field of ethyl levulinate, can solve the problems of less research on ethyl levulinate, harsh reaction conditions, and high catalyst cost, and achieve cheap raw materials, simple reaction system, and high preparation process simple effect
Active Publication Date: 2018-10-23
XIAMEN UNIV
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[0007] The purpose of the present invention is to provide a one-pot catalytic method for furfural for the existing research on the preparation of ethyl levulinate from furfural
Method used
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Embodiment 1
[0022] Add 0.2g furfural and 20mL ethanol to a 50mL autoclave, then add 0.1g ZrO 2 / SBA-15(ZrO 2 Loading capacity 40wt%) as a catalyst, seal the reactor, vigorously stir (800rpm), heat to 150 ° C and keep for 5h, finish the reaction and cool at room temperature, centrifuge the reaction mixture and take the supernatant, use GC-MS (Shimadzu) Qualitative and quantitative detection were carried out with GC (Agilent), and the detection results are listed in Table 1, and the serial number is 1.
Embodiment 2～7
[0024] Add 0.2g furfural and 20mL ethanol to a 50mL autoclave, and then add 0.1g SnO 2 -ZrO 2 / SBA-15, MgO-ZrO 2 / SBA-15, Al 2 o 3 -ZrO 2 / SBA-15, CuO-ZrO 2 / SBA-15, ZnO 2 -ZrO 2 / SBA-15, Fe 2 o 3 -ZrO 2 / SBA-15 (the load of metal oxide is 40wt%, the mixing ratio of the two metal oxides is 1:1) as a catalyst, seal the reactor, stir vigorously (800rpm), heat to 150°C and keep it for 5h, to end the reaction Cool at room temperature, centrifuge the reaction mixture and take the supernatant, use GC-MS (Shimadzu) and GC (Agilent) for qualitative and quantitative detection, the detection results of different catalysts are listed in Table 1, numbered 2-7.
Embodiment 8～12
[0026] Add 0.2g of furfural and 20mL of ethanol to a 50mL autoclave, and then add 0.1g of Al 2 o 3 -ZrO 2 / USY, Al 2 o 3 -ZrO 2 / H-β, Al 2 o 3 -ZrO 2 / SBA-15, Al 2 o 3 -ZrO 2 / MCM-41 (the load of metal oxide is 40wt%, the mixing ratio of the two metal oxides is 1:1) as a catalyst, seal the reactor, stir vigorously (800rpm), heat to 150°C and keep it for 5h, to end the reaction Cool at room temperature, centrifuge the reaction mixture and take the supernatant, and use GC-MS (Shimadzu) and GC (Agilent) for qualitative and quantitative detection. The detection results of different catalysts are listed in Table 1, numbered 8-11.
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Abstract
The invention relates to a method for preparing ethyl acetylpropionate by catalyzing furfural via a one-pot method, and relates to ethyl acetylpropionate. The method comprises the following steps of heating furfural, a catalyst and ethyl alcohol in a reaction kettle, cooling to room temperature, centrifuging and decomposing, obtaining a liquid phase, and purifying, so as to obtain ethyl acetylpropionate; using the solid as the recycling catalyst. The method has the advantages that furfural is directly used as the raw material to prepare ethyl acetylpropionate; used ethyl alcohol can be simultaneously used as reaction raw material, solvent and hydrogen donor, the external hydrogen source and other solvents are not needed, and the reaction system is simple, so as to conveniently separate thetarget product and recycle and reutilize the solvent; the preparation procedure of a dual-function molecular sieve-loaded catalyst for simultaneously catalyzing the transfer hydrogenation and alcoholysis reaction is simple, the price of the raw material is low, and ethyl acetylpropionate with higher yield rate can be obtained by catalyzing furfural; the used catalyst can be conveniently recycled,and the activity is still stable after recycling.
Description
technical field [0001] The invention relates to ethyl levulinate, in particular to a method for preparing ethyl levulinate by catalyzing furfural in one pot. Background technique [0002] Ethyl levulinate is a common short-chain fatty acid ester in levulinic acid esters. It is a very potential high value-added new energy chemical, which has attracted more and more attention from academia and industry in recent years. Ethyl levulinate can be used in spices, coatings, adhesives, plasticizers and pharmaceutical industries, and can also be converted into an important downstream bio-based platform compound γ-valerolactone. In addition, its properties are similar to those of biodiesel, so it can be used as a blended fuel for transportation such as petrochemical diesel and biodiesel. After adding it, it can effectively improve combustion cleanliness, and has excellent lubricating ability, flash point stability and low temperature fluidity. [0003] Currently, levulinic acid esters...
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