An Experiment to Illustrate the Hazards of Exothermic Reaction Scale-Up

Authors

  • William Clark Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609
  • Melinda Lei Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609
  • Erika Kirichenko Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609
  • Kellie Dickerson Worcester Polytechnic Institute • Worcester, MA 01609
  • Robert Prytko Sunovion Pharmaceuticals • Marlborough, MA 01752

Abstract

 

 Exothermic reactions can present safety hazards and there is a recognized need for reaction safety education at the undergraduate level. We present an experiment that illustrates the pitfall of direct scale-up of an exothermic reaction that can lead to thermal runaway. The iodide-catalyzed hydrogen peroxide decomposition reaction yields dramatically different results when conducted in different sized round-bottom flasks in an ice bath. By combining 1 volume of 30% H2O2 with ½ volume of 0.1M KI solution, the temperature response of the mixture can be followed using different sized reactors being cooled in an ice bath. With similar stirring rates, initial temperatures, and reactant concentrations, the heat removal via an ice bath is sufficient to control the reaction in half-filled flasks less than or equal to 500 ml. Scaling up to 1000 ml results in thermal runaway. Calculations are shown to predict the observed behavior, but direct observation through a laboratory experiment is recommended to ensure that students appreciate the hazards of scaling up exothermic reactions.

Author Biographies

William Clark, Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609

William Clark is an associate professor in the Department of Chemical Engineering at Worcester Polytechnic Institute. He holds a B.S. from Clemson University and a Ph.D. from Rice University, both in chemical engineering. He has taught thermodynamics, separation processes, and unit operations laboratory for 29 years. His current research focuses on using finite element analysis for teaching chemical engineering principles and for analyzing separation processes.

Melinda Lei, Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609

Melinda Lei, Erika Kirichenko, and Kellie Dickerson developed this experiment as part of their Major Qualifying Project (senior thesis) in the Department of Chemical Engineering at Worcester Polytechnic Institute. They have since graduated and begun their careers in the chemical process industry.

Erika Kirichenko, Chemical Engineering Department, Worcester Polytechnic Institute, Worcester, MA 01609

Melinda Lei, Erika Kirichenko, and Kellie Dickerson developed this experiment as part of their Major Qualifying Project (senior thesis) in the Department of Chemical Engineering at Worcester Polytechnic Institute. They have since graduated and begun their careers in the chemical process industry.

Kellie Dickerson, Worcester Polytechnic Institute • Worcester, MA 01609

Melinda Lei, Erika Kirichenko, and Kellie Dickerson developed this experiment as part of their Major Qualifying Project (senior thesis) in the Department of Chemical Engineering at Worcester Polytechnic Institute. They have since graduated and begun their careers in the chemical process industry.

Robert Prytko, Sunovion Pharmaceuticals • Marlborough, MA 01752

Robert Prytko is a research fellow at Sunovion Pharmaceuticals, Inc. He has more than 20 years of experience in small molecule pharmaceutical process development, scale-up, and technology transfer including extensive experience managing and operating a state-of-the-art pharmaceutical kilolab. He holds a B.S. in chemical engineering from Worcester Polytechnic Institute and a Diploma in Brewing and Distilling from Heriot-Watt University.

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Published

2017-01-25

Issue

Vol. 51 No. 1 (2017): Winter 2017

Section

Manuscripts