Ammonia → Caprolactam

Participants

Reaction Steps

To a catalyst basket in a 300 milliliter Parr reactor was charged 5.044 grams of a nickel, rhenium, boron catalyst prepared as described in Example 6 of U.S. Pat. No. 4,123,462. The catalyst was activated in 50 milliliters of water for 1 hour at 200° C. under 533 psig hydrogen. The reactor was cooled, vented, and the water discharged. 50 Milliliters of 17% NH3 in water was charged to the reactor and the reactor was heated to 235° C. under 220 psig of 3% hydrogen in nitrogen. A flow of 40 milliliters per minute of 3% hydrogen in nitrogen was maintained through the reactor using a Brooks Mass Flow Meter at a reactor pressure of 725 psig. A solution of 5.00 grams of 6-aminohexanol, 20 grams water and 2.04 grams of tetreglyme as internal standard was prepared and charged to a stainless steel pressure cylinder connected to a metering pump. The 6-aminohexanol in water solution was fed to the reactor at a rate of 1.0 milliliter per minute. The yields of products, i.e., epsilon caprolactam, hexamethyleneimine, and hexamethylenediamine, were determined using gas chromatographic analysis of samples taken over time and were based on the amount of 6-aminohexanol charged. From the time when the 6-aminohexanol feed was completed, the yields of epsilon caprolactam, hexamethyleneimine, and hexamethylenediamine with are shown in the table below.

Provenance & Evidence