Journal
CHEMSUSCHEM
Volume 11, Issue 21, Pages 3796-3802Publisher
WILEY-V C H VERLAG GMBH
DOI: 10.1002/cssc.201801624
Keywords
biomass; biofuels; heterogeneous catalysis; palladium; supported catalysts
Funding
- China Ministry of Science and Technology [2016YFA0202804]
- National Natural Science Foundation of China [21773067, 21533002, 21573073]
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The synthesis of biomass-derived ethers to be used as biofuels or biofuel additives has attracted much attention. Following the recently reported synthesis of etherified ester ethyl-4-ethoxy pentanoate (EEP) from gamma-valerolactone (GVL) in ethanol catalyzed by H-beta zeolite, an alternative route to prepare EEP in high yield has been developed by reductive etherification of ethyl levulinate (EL) in ethanol at 140 degrees C under 0.5 MPa H-2 with a silica-modified Pd/C catalyst. The ether production likely follows a tandem acetalization-hydrogenolysis process with ethyl-4,4-diethoxy pentanoate (EDEP) as the intermediate. The acetalization step can be favored by introducing acidic materials, such as SiO2-carbon or beta zeolite, as a cocatalyst. The combination of the Pd/SiO2-C and beta zeolite mixture leads to 100 % EL conversion and 93 % EEP selectivity under optimized reaction conditions. For the first time, the standard molar combustion enthalpy of as-prepared EEP is measured by using a static oxygen bomb, and the value of which is determined to be about -5658 kJ mol(-1), which is much larger than that of GVL (-2650 kJ mol(-1)).
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