Nitrosation reaction using isothermal power compensation calorimetry

Abstract

Initial plant scale trials of the nitrosation of an amino acid revealed a number of issues: _ Much lower yield compared to laboratory scale _ Considerable loss of mass balance _ Large excess of nitrosating agent required for complete reaction _ Highly reactive off-gases produced causing fires in the carbon absorber _ Reaction sensitive to agitation speed _ The by-product produces an impurity in the next process stage which has high human toxicity A kinetic and mechanistic study of the nitrosation reaction, using isothermal power compensation calorimetry and GC/mass spectrometry, has been undertaken in order to understand the above observations and to produce an improved manufacturing process - more robust, higher yielding, reduced effluent volumes and toxicity.