1-Propanol → Methane

The runs were made without interruption for up to several weeks, and time intervals during steady state operation were selected for analysis, generally of 8 to 24 hours duration. The product composition data generated during steady state operation was averaged to give the average production rates (g/hr) of THF (tetrahydrofuran), BDO (1,4-butanediol), GBL (gammabutyrolactone), PrOH (n-propyl alcohol), BuOH (n-butyl alcohol), and alkanes (primarily butane and methane). The product composition was measured by condensing a portion of the volatilized products and water in the exit gas stream and collecting the liquid product. The volume of liquid product collected each hour was measured, and its composition analyzed using a calibrated gas chromtograph (GC) equipped with a flame ionization detector. The remaining uncondensed products (THF and alkanes) still in the exit gas stream were analyzed by measuring the gas flow rate and then analyzing the composition of the gas stream every two hours using GC procedures similar to those used for liquid analysis. The reactor contents were sampled every four hours and analyzed by GC and titration. Titration with sodium hydroxide was used to monitor the acid concentration in the reactor and the results are reported as percent by weight of succinic acid. The GC analysis was carded out using a Supelcowax 10 capillary column (30 m×0.052 mm) which was maintained at 75° C. for 5 minutes after injection and then heated at 10° C. per minute to a final temperature of 200° C. The combination of these three analyses permits calculation of the catalyst performance in terms of space-time-yield (STY) (calculated as grams of THF produced per kilogram of catalyst per hour), product selectivity and the mass balance for each run.

1. customup to several weeks

ORD record

ord-a4485f3927d64de4a5081c1b4b3aaf12

Source dataset

uspto-grants-1995_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05478952