Data requirements for reactor selection. Professor John H Atherton
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1 Data requirements for reactor selection Professor John H Atherton
2 What is my best option for manufacturing scale? Microreactor Mesoscale tubular reactor Tubular reactor OBR (oscillatory baffled flow reactor) Spinning disk 1 n CSTRs Recycle flow reactor Bubble column Batch or semi-batch
3 Why PI Most fine chemicals processes can be carried out in batch mode Operating in batch mode often results in serious compromises to performance PI devices can be very efficient but in a narrow operating window
4 So - Realistic choice of PI equipment requires that we define the operating characteristics of equipment To choose equipment need to understand process requirements equipment characteristics
5 What do we need to know about the process? Depends on the process - The more complex the process, the more information is needed
6 Process Complexity Number of phases L-L-S L-G L-S-S L-S L-G-S-S L-S-G L-L liquid Chemical complexity pre-equilibria number of reaction steps number of reagents number of side reactions fast reactions coupling to phase transformation exothermic catalysis length scales heat transfer time mass transfer solubility mixing times density interfacial area rheology energy input Physical and dynamic
7 Phase characteristics fine chemicals manufacture Of 47 processes surveyed: ref ~40% had at least one solid phase present during reaction ~25% had two or more liquid phases present during reaction ~20% involved a gas phase as reactant, product or purge ~ 60% involved feeding a reactant that was insoluble in the reaction mass Ref: JH Atherton JM Double, B Gourlay, paper presented at World Congress of Chemical Engineering, Glasgow 2005.
8 Residence time Mass transfer requirements Heat transfer Unknown, 6% Mass transfer limited, 30% Chemical rate limited, 47% Heat transfer limited, 17% Of the chemical rate limited processes, about 40% had residence times less than 1 hour; 15% less than one minute From: JH Atherton JM Double, B Gourlay, paper presented at World Congress of Chemical Engineering, Glasgow 2005.
9 Overview of data requirements Phase characteristics Kinetics chemical coupled physical processes Physical properties Thermochemistry
10 Phase characteristics - question What are the phase characteristics of your reactants, starting materials and products
11 Chemical reaction scheme A picture of the relevant chemistry with (if relevant) ionic equilibria and competing processes is needed to select the appropriate reactor configuration H 2 H 2 A Int P Solvent P H + pk a? B1 B2 PH + Use to identify branch points in the reaction scheme
12 Reaction picture (p)h 2 H e, k L a H 2 H 2 A Int P k 1 k 2 k solv Solvent P H + k 3 pk a? B1 B2 PH + PH +
13 Some chemistry questions How fast are the main and side reactions What is the required residence time in the absence of heat and mass transfer limitations What are the important side reactions? Are any protonation equilibria involved that influence the rate or selectivity? What is the heat of reaction (highly exothermic reactions are often sensitive to the mixing method) Is the selectivity sensitive to how fast the reactants are mixed? Are there any enforced reagent stoichometries the hydrogenation example
14 Physical properties What are the rheological properties of the reaction mass? pipe pressure drop is viscosity dependent shear thinning fluids can be a big problem in pipes What are the heat transfer requirements? What are the mass transfer requirements?
15 Multiphase reactions The overall rate will be a function of both the chemical reaction rate and the mass transfer rate. The nature of the overall rate function depends on how the two processes are coupled. At the extremes: fast reactions with low solubility reactants have rates proportional to interfacial area (in-film reactions) slow reactions with good co-solubility of reactants have rates proportional to the volume of the phase in which reaction occurs to select a reactor it is necessary to understand these aspects of the process
16 Problems with poorly soluble reactants Reactions where the chemistry is intrinsically fast can be overall very slow if one or more components has low solubility, e.g. Acylation of a poorly soluble amine in an aqueous system Batch process cycle time 5 hours R R + X k 2 =100 M-1 s -1 Product 0.001M 1M Laboratory continuous process, high shear mixer as reactor residence time required was 2 minutes
17 Mass transfer mass transfer requirements need to be defined now becoming recognised as best practice in pharma development can impact on selectivity as well as rate
18 Influence of mass transfer on impurity formation CF 3 CF 3 H 3 C O N hydrogen starved Pd F CF 3 H 2 hydrogen rich H 3 C O N H F desired product CF 3 The process was improved by: reducing the catalyst loading increasing the hydrogen pressure improving the agitation CF 3 CF 3 H 3 C O CF 3 1. Loss of F H 3 C O CF 3 N F Pd 2. H 2 N H H unwanted Merck Research, NJ, OPRD 2006, 10, (10 authors)
19 Overview of data requirements Phase characteristics Physical properties Kinetics chemical coupled physical processes Thermochemistry to permit logical selection of appropriate PI device
20 Some challenges Methodology selection protocol involving identification of process requirements equipment capability Development of techniques for controlled feed of solids to continuous reactors.
21 and finally - IPOS our nascent company at Huddersfield University. Offers expertise in chemical process systems analysis and in chemical and physicochemical data acquisition Please see for further information about the services we offer.
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