Gamma-Butyrolactone → Gamma-Butyrolactone

Participants

Reaction Conditions

Reaction Steps

A stainless steel tubular reaction with an O.D. of 1 inch and I.D. 0.93 inches was packed with 70 ml (27 g.) of the catalyst from Example 1 to provide a 7 inch bed length. The catalyst was reduced over a six hour period at 150°-300° C. using hydrogen in nitrogen in increasing concentration of from about 3% to about 10% H2. The hydrogen mixture was introduced intermittently until there was little exotherm, after which the hydrogen concentration was increased to 100%. A feed of γ-Butyrolactone was pumped to a vaporizer from which the vapor was carried by a hydrogen stream to the reaction. The ratio of hydrogen to butyrolactone feed (99% pure) was 150:1. The reactor was maintained at 160° C. temperature, 600 psig. pressure and an LHSV of 0.05 (g. of feed/hour/volume of catalyst). The product vapors were collected and condensed. A conversion of 90% butyrolactone with 95% selectivity to butanediol was obtained.

Provenance & Evidence