Patrick Cognet

Precise parameter estimation for chemical batch reactions in heterogeneous medium

Abstract A sequential experimental strategy for precise parameter estimation has been used in the case of liquid–liquid dispersions in batch-stirred tank reactors where slow chemical reactions take place. The mathematical model for a batch reaction in a stirred tank reactor is formulated as a system of non-linear differential equations standing for the mass balance of each component. Physical kinetic parameters and chemical kinetic parameters which arise from this model are estimated simultaneously. The estimation problem is posed as a weighted least squares problem and solved by using a standard Levenberg–Marquardt algorithm. In this work, we intend to show how it is possible to develop efficient experimental design strategies that lead to an accurate estimation of the parameters involved in phenomenological models and most particularly in kinetic models. Three design criteria for designing the experiments have been employed in order to increase the precision on the parameter estimates of the model. A standard non-linear sequential quadratic programming method ensures the determination of the operating conditions which define the experimental design. The well-known alkaline hydrolysis of esters in aqueous phase has been treated as a numerical application example.

Influence of solvent choice on the optimisation of a reaction–separation operation : application to a Beckmann rearrangement reaction

In pharmaceutical syntheses, the solvent choice generally represents a complex design step. Traditionally, this choice is operated according to criteria connected with the reaction step and without any consideration on the following separation steps. The purpose of this study is to highlight the benefits of a global approach of optimisation for the solvent determination. In this way, an optimisation framework dedicated to global synthesis is applied to a simple reaction–separation operation integrating a Beckmann rearrangement reaction, leading to interesting solvent choices.

Intensification of Ester Production in a Continuous Reactor

Numerous continuous intensified reactors are now accessible on the market that offer enhanced thermal performances in a continuous reactor. Such reactors are then particularly suited to fast and highly exothermic reactions. In this paper, the ability to also manage a slow and equilibrated system, the methyl acetate esterification reaction, on condition of intensification in terms of design and operating conditions is presented. To achieve this purpose, a new kinetics model has been developed and validated from experiments carried out in a lab scale batch reactor. Implemented in a simulation framework, this model leads to an intensified design of the reactor and the associated operating conditions. All this intensification methodology has been supported and validated by experimental studies.

MODELING AND OPTIMIZATION OF LACTIC ACID SYNTHESIS BY THE ALKALINE DEGRADATION OF FRUCTOSE IN A BATCH REACTOR

ABSTRACT The present work deals with the determination of the optimal operating conditions of lactic acid synthesis by the alkaline degradation of fructose. It is a complex transformation for which detailed knowledge is not available. It is carried out in a batch or semi-batch reactor. The “Tendency Modeling” approach, which consists of the development of an approximate stoichiometric and kinetic model, has been used. An experimental planning method has been utilized as the database for model development. The application of the experimental planning methodology allows comparison between the experimental and model response. The model is then used in an optimization procedure to compute the optimal process. The optimal control problem is converted into a nonlinear programming problem solved using the sequencial quadratic programming procedure coupled with the golden search method. The strategy developed allows simultaneously optimizing the different variables, which may be constrained. The validity of the methodology is illustrated by the determination of the optimal operating conditions of lactic acid production.

Pre-Design of a Continuous Intensified Reactor Based on Pure Thermo-Chemical Optimisation

A continuous intensified reactor requires precise information to adapt the design to the reaction to be implemented. In this article we present a two step approach to pre-designing such devices. The first step consists of the optimisation of the operating conditions based only on stoichio-chemical schemes and kinetic laws. This is carried out by adjusting the temperature profile and feeding rate strategy in a batch or pseudo-batch operation. The second step departs from the ideal thermo-kinetic path by taking into account heat removal and reagent injection. A simulator is used to evaluate the impact of these constraints on the selectivity and productivity. The approach is applied to the linear alkylbenzene sulfonation which characteristics present most of the challenges encountered in the intensification. Final results give a pre-design in terms of reactor characteristics (size, injections positions) and operating conditions.