(437e) Taking the Min to the Max: A Case Study in Small Scale Process Development Using On-Line Reaction Calorimetry and in-Situ Particle Characterization

Authors: 
Teich, C., The Dow Chemical Company
Sarafinas, A., The Dow Chemical Company
Morton, P., The Dow Chemical Company


Many specialty and fine chemicals are produced in batch processes and require fast assessment and development of manufacturing plans to speed time to market and profit. It is unlikely that any one specialty product could justify construction of a dedicated pilot plant, and its construction timeline would further decrease that likelihood. The subject case study demonstrates the breadth, depth, and quality of development and design data that can be obtained for fast, multi-phase chemistry in a small scale reaction calorimeter operated over a range of defined mixing conditions and equipped with in-situ particle characterization.

When a small-volume specialty was transferred to a different plant, the new reactor produced smaller size particles, impacting its downstream processing as well as the Plant's primary operating area. Initial discussions with the Plant centered on ?fixing? the downstream equipment, but the focus moved quickly to the reactor and consideration of the most economical design for the low-volume product. A directed experimental program, incorporating macro, meso, and micro mixing considerations and study of the solid-liquid equilibrium was conducted in a METTLER TOLEDO RC1e? reaction calorimetry equipped with a METTLER TOLEDO FBRM® in-situ particle characterization system. The program results led to an understanding of what ?broke? the process and to a low cost design option, and demonstrate how the lab-scale equipment can be used as an effective pilot plant.