Calorimetric Studies in Early Stage of Chemical Process Development


Calorimetric Studies in Early Stage of Chemical Process Development


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White Paper | Procos S.p.A.

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Calorimetric Studies in Early Stage of Chemical Process Development

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ABSTRACT

This White Paper explores the process safety and efficiency implications of different methods of assessing thermodynamic and thermokinetic parameters and investigating thermal stability of all fractions involved before scaling up reactions to industrial quantities. The purpose is to assess whether safety studies can be designed that no longer represent a binary Yes/No determinant of industrial scale-up but can instead integrate calorimetric investigation into deep process optimization.

Approach

The authors investigated R&D structures adapted to available technical skills and readily available calorimetric equipment, including matching reactor size to calorimeter used and uses of automatic reactors (e.g., Mettler-LabMax) to prepare substances, together with DSC or TGA instruments and Systag-RADEX calorimeter for the thermal stability analyses.

Findings

The White Paper includes three representative reaction studies performed in the Procos R&D laboratory:

  1. N-Alkylation Reaction
    Preliminary calorimetric analysis via RC1 prior to scale-up of an N-Alkylation reaction of a secondary amine to produce quaternary ammonium salt revealed a potential thermal problem of the batch system in concentration, indicating need for a semi batch process, optimizing charging ramps for process safety.
  2. Formation of an amidoxyme
    Investigating scale-up of a customer-developed laboratory method of synthesizing amidoxyme through reaction of a Hydroxylamine free base on a substituted benzonitrile integrated calorimetric techniques with risk evaluation applied during the preliminary screening phase. The study highlighted possible criticalities, identifying correct process optimization for time and temperature.
  3. Alkylation of a phenate
    Investigating O–alkylation of sodium phenate by primary Bromo-derivative with a complex structure, developed in a customer laboratory, highlighted how preliminary calorimetric analysis could eliminate wastage of time and resources on optimizing a method with insurmountable safety problems.

Value

Available in English for the first time, this White Paper provides valuable insights from research scientists working with the practicalities of industrial scale-up of reactions. Unlike most previous calorimetric safety studies, prepared by third party safety and academic institutions, this paper has been prepared by a Procos ‘in-house’ R&D team with deep experience in how to make reactions both safe and commercially viable.


Supplier Information
Supplier: Procos S.p.A.
Address: Via G. Matteotti 249, 28062 Cameri, Novara, Italy
Tel: +39 0321 642211
Fax: +39 0321 64219
Website: www.procos.it


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