Furfural
(FFR) was selectively hydrogenated in a single pot to
tetrahydrofurfuryl alcohol (THFAL) over a Si–MFI molecular
sieve supported Pd catalyst. Studies on catalyst screening revealed
that both the metal function and the support were critical for directing
the selectivity to the ring-hydrogenated product, THFAL. The structural
feature of MFI as shown by XRD was completely retained in the used
sample of the 3% Pd/MFI catalyst confirming its stability under reaction
conditions. XRD, along with SEM characterization of the used samples,
established retention of morphology of the structured silicate, suggesting
a strong interaction between hexagonal porous silicate and Pd particles.
The complete conversion of FFR with an enhanced selectivity of 95%
to THFAL could be achieved by recycling the crude of the first hydrogenation
experiment over the same 3% Pd/MFI catalyst.
Various noble metal catalysts were screened in a batch operation for a furfural (FFR) single-step decarbonylation and hydrogenation reaction to obtain THF in high selectivity. Among these, the 3% Pd/C showed complete FFR conversion with a total of 80% selectivity to ring hydrogenated products including tetrahydrofuran (THF). The order of activity exhibited by other noble metals was Pt/C > Re/C > Ru/C. Although Pt/C exhibited the highest activity, its decarbonylation and ring hydrogenation ability were the least (24%) with a major product selectivity of 66% to furfuryl alcohol (FAL). Similarly, the Cu catalyst gave almost complete selectivity to FAL. In a continuous operation (23 g catalyst bed), the 3% Pd/C catalyst showed higher selectivity of >40% compared to THF alone with complete FFR conversion and on-stream activity of ∼100 h. The reaction pathway elucidated from some control experiments revealed that the decarbonylation of FFR to furan over the Pd/C catalyst is a prerequisite for THF formation.
The screening of copper chromite catalysts with various promoters such as Al, Zn, and Ba for glycerol hydrogenolysis to 1,2-propanediol (1,2-PDO) in a batch reaction showed that Cu-Cr (Ba) catalyst gave the highest conversion of 34% and selectivity of 84% to 1,2-PDO. In a continuous operation (23 g catalyst bed) the same catalyst showed higher conversion of glycerol and selectivity for 1,2-PDO of 65% and >90%, respectively, with an on-stream activity of ∼800 h. Better performance in a continuous operation could be due to the in situ activation of the catalyst, suppression of glycerol cracking to ethylene glycol, as well as excessive hydrogenation of 1,2-PDO to 2-propanol due to lower contact time of 1.3 h as compared to that in a batch operation (5 h). Effects of various process parameters on conversion and selectivity also have been compared for batch and continuous operations.
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