Conceptual design, steady state economic optimization, and decentralized plantwide control of a conventional reaction followed by separation process for continuous manufacture of monoisopropyl amine (MIPA) via the catalytic amination of isopropyl alcohol (IPA) is studied. A unique feature of the design is the recycle to extinction of the diisopropyl amine (DIPA) side product for a sustainable zero DIPA discharge process. The reactor effluent mixture separation is complicated by the presence of DIPA-water, IPA-water, and IPA-DIPA minimum boiling binary azeotropes. Using the residue curve map tool, two alternative designs, without a decanter (FS1) and with a decanter (FS2), are devised and optimized with respect to the dominant design variables. A high single-pass reactor conversion is necessary so that the reactor effluent composition is in the appropriate distillation region to guarantee feasibility of the separation scheme. Also, reactor oversizing is needed to ensure operability for a moderately large throughput increase. FS2 is finally recommended as it consumes similar to 8% less energy than FS1 and its total annualized cost (TAC) is approximately the same as that of FS1 post reactor oversizing. Effective rejection of large throughput and feed composition changes using decentralized plantwide control is demonstrated for FS2. In particular, the organic layer material balance control on the decanter is shown to significantly affect the overall plantwide response time. The case study is a categorical pitch for simultaneous design and operability studies.