Complicated solution environments in oiling-out crystallization can lead to particle
agglomeration with large size distribution and low purity of the products, due to
complex interactions among two liquid phases and one solid phase during the oiling
out crystallization. This research mainly focuses on optimization of size distribution by
control particle agglomeration during the oiling-out crystallization process in model
system of propyl paraben-ethanol-water. Nucleation-control technologies, wet milling,
seeding and ultrasound were investigated to limit the agglomeration. Further
investigations of wet milling was applied before the nucleation or in the crystal growth
process with different geometries, such as the coarse, medium and fine rotor-stator
tooth pairs. An integrated process analytical technology tools (PAT) array, including
focused beam reflectance measurement (FBRM), particle visual monitoring(PVM),
2
and attenuated total reflectance ultraviolet/visible(ATR-UV/vis), was used to observe
the droplet formation of the dispersed phase, size distributions, particle shapes during
the nucleation and crystal growth. The results demonstrate that wet milling, seeding
and ultrasound technologies can help to the control of the particle size distribution in
the complex solution environments with different levels of efficiencies
Funding
China Scholarship Council, National Natural Foundation of China (nos. 21576187 and 21776203)
Tianjin Municipal Natural Science Foundation (no. 18JCYBJC21100)
Regenerative BioCrystallisation
Engineering and Physical Sciences Research Council
This paper was accepted for publication in the journal Industrial & Engineering Chemistry Research and the definitive published version is available at https://doi.org/10.1021/acs.iecr.1c04167