Particle engineering of benzoic acid by spherical agglomeration.

The influence of process conditions on the properties of benzoic acid spherical agglomerates, are investigated. Agglomerates are produced in a fed-batch agitated tank process. Benzoic acid is dissolved in ethanol and the solution is mixed with the bridging liquid, before being fed into an agitated aqueous solution. A broader investigation has been performed using heptane as the bridging liquid, and in further experiments different bridging liquids are compared. The results show that the bridging liquid has an influence on the product properties, with diethyl ether and ethyl acetate being at the extreme end with no agglomerates formed at all. Using any of the other five solvents (chloroform, toluene, heptane, pentane, or cyclohexane) spherical agglomerates are formed, as long as a sufficient amount of the bridging liquid is used. The results show that the particle size and strength increase with increasing amount of bridging liquid, and with decreasing temperature. At amount of bridging liquid producing optimum particle shape, the largest agglomerates are produced when using either cyclohexane operating at 5 °C, or using toluene in a process at 20 °C. The highest particle fracture stress is obtained using toluene as the bridging liquid regardless of temperature. The particle shape depends on the bridging liquid, and becomes completely spherical when toluene or pentane is used. For four of the solvents the particle morphology improves with decreasing temperature, but for cyclohexane the result is the opposite. By continued agitation beyond the completion of the feeding, particle size and strength gradually increases and also the shape gradually becomes more spherical. High compressibility and low elastic recovery suggest that the particles are favorable for direct tabletting. The results are analyzed and discussed against capillary theory and granulation mechanisms.

On the mechanisms of formation of spherical agglomerates.

Spherical agglomerates of benzoic acid have been successfully prepared by semi-batch, agitated vessel, drowning-out crystallization in water-ethanol-toluene mixtures. Benzoic acid is dissolved in ethanol, toluene is added and this mixture is fed at constant rate to the agitated crystallizer containing water. The influence of the amount of bridging liquid and the feeding rate on the product particle size distribution, morphology, and mechanical compression characteristics have been investigated. Compression characteristics for single agglomerates are compared with data on bed compression. With increasing amount of bridging liquid the particle size and strength increases and morphology improves. Particle size decreases and the fracture force increases with increasing feeding rate but the morphology remains unchanged. Using toluene as opposed to chloroform as the bridging liquid leads to improved product properties. Experiments have also been performed to reveal the mechanisms of the formation of the agglomerates. The results show that along the course of the process the properties of the particles change gradually but substantially. Particle size and number increases along with increasing feed. The spherical shape does not appear immediately but develops gradually, and is shown to be very much the result of the agitation of the slurry.