The
reductive amination (RA) of 2-hydroxytetrahydropyran (2-HTHP)
produced from biofurfural-derived dihydropyran provides a new efficient
process for the clean synthesis of valuable 5-amino-1-pentanol (5-AP).
Among various solid catalysts tested, the inexpensive Ni–Mg3AlO
x
catalysts derived from hydrotalcite
precursors were found to be very active and selective, especially
at Ni loadings above 20 wt %. A 85% total yield of 5-AP was obtained
from dihydropyran on 40Ni–Mg3AlO
x
, the catalyst with the highest 2-HTHP RA activity among the
Ni–Mg3AlO
x
catalysts,
under mild conditions of 60 °C and 2 MPa H2. Characterization
results showed that the reducibility of the calcined NiO-Mg3AlO
x
samples increased with increasing
Ni loading from 5 to 50 wt %, while the Ni0 crystallite
sizes exhibited a minimum of 4.8 nm on 40Ni–Mg3AlO
x
after reduction in H2 at 750
°C. The volcanic changes of 5-AP generation rate/yield with increasing
Ni loading of the Ni–Mg3AlO
x
catalysts and with rising prereduction temperature of 30Ni–Mg3AlO
x
catalyst in 2-HTHP RA indicate
that the balance of the reducibility and Ni0 particle size
of the catalysts played an important role in obtaining high 5-AP yields.
The 30Ni–Mg3AlO
x
catalyst
showed a good stability in 2-HTHP RA examined in a continuous flow
reactor over a 90 h time-on stream.