Intensified oxalic acid crystallization using ultrasonic reactors: Understanding effect of operating parameters and type of ultrasonic reactor.

The present work reports the comparison of the effectiveness of ultrasonic bath and horn for intensifying the cooling crystallization of oxalic acid for the first time. The effect of various parameters such as temperature, crystallization time, irradiation time, ultrasonic frequency and ultrasonic power on the crystal characteristics has been investigated. The average particle size of oxalic acid crystals reduced with an increase in irradiation time and ultrasonic power dissipation. Comparison of crystal characteristics obtained in ultrasonic bath with that obtained in the ultrasonic horn under optimized parameters revealed that the average size in the case of ultrasonic horn and bath were only marginally different. The studies related to the effect of different cooling modes using ultrasonic horn revealed that a narrow size distribution and lower average size of 357.2µm was obtained for the cooling using ice cold water as compared to air cooling where observed mean size was 439.7µm. A narrow particle size distribution was also obtained in the scale-up studies using ultrasound horn with mean size of 96.70µm, which was significantly lower than 161.1µm obtained under conventional approach. Overall significant process intensification benefits have been established for the ultrasound assisted approach for cooling crystallization of oxalic acid.