Semibatch reaction crystallization of salicylic acid

• The crystal number mean size increases with decreasing feed rate and feed pipe diameter.
• The crystal number mean size increases with decreasing reactant concentrations.
• The crystal number mean size reach a maximum at intermediate agitation rate.
• Crystallization kinetics are determined by optimization of a population balance model.
• The model cannot fully capture the influence of process conditions.

Reaction crystallization of salicylic acid has been investigated by experiments and modeling. In the experimental work, dilute hydrochloric acid has been added to an agitated aqueous solution of sodium salicylate in 1 L scale, and product crystals have been characterized by image analysis. The results show that the product crystal number mean size at first increases with increasing agitation rate but then gradually decreases again at further increase in stirring rate. At lower stirring rate, larger crystals are obtained when the feeding point is located close to the agitator instead of being located out in the bulk solution. The mean crystal size increases with decreasing feeding rate and with decreasing reactant concentrations. There is a decrease in mean size with increasing feed pipe diameter. These trends in the experimental results show great similarity with previous results on benzoic acid. The experimental results have been examined by a population balance model accounting for meso and micro mixing, and crystal nucleation and growth rate dispersion. It is found that the crystallization kinetic parameter estimation is quite complex, and the objective function hyper surface contains many different minima. Hence, parameter estimation has to rely on a combination of mathematical optimization strategies and a scientific understanding of the physical meaning of the parameters and their relation to current theories. As opposed to our previous work on benzoic acid, it has not been possible to find a set of kinetic parameters that provides for a good description of all experimental data.