This paper is studied on the efficient purification process of dimethyl carbonate (DMC) from the melt layer crystallization combining crystallization process, sweating process and distillation recovery process. Purity and yield of DMC crystal depended mainly on the crystallization temperature, cooling rate, sweating termperature sweating rate. Through the optimization of crystallization and sweating operation, DMC crystal can be upgraded to very high purity over 99.9% and high yield over 85%.
In T-mixer crystallization, supersaturation is generated by mixing of another solvent or non-solvent in order to reduce the solubility of the compound. Also, T-mixer is a type of continuous crystallization. In order to induce micro-mixing, two solutions were mixed rapidly by T-mixer, which formed high supersaturation. As the results, mean size of HMX crystals decreased with increasing de-supersaturation rate (Rs). Eventually, HMX particles ranging from 0.5 to 5μm can be obtained by T-mixer crystallization. Mixing efficiency in T-mixer increased with increasing Rs values. In T-mixer crystallization without surfactants, homogeneous nucleation was formed when S and Rs was over 54 and 1.6×103/sec. In T-mixer crystallization with surfactants, homogeneous nucleation was formed when S and Rs was over 26 and 7.4/sec.
As an additional high purification method of p-dioxanone monomer for a high molecular weight polymer, the sweating operation of crystalline layer obtained by layered melt crystallization from p-dioxanone-diethylene glycol system was studied. Purity and yield of p-dioxanone crystal depended mainly on the sweating temperature and sweating time. Increasing sweating time and sweating temperature, the purity of p-dioxanone crystal increase, whereas the yield of that decrease, respectively. Through the optimization of sweating operation, p-dioxanone crystal can be upgraded to very high purity over 99.9 % suited to monomer for polymerization.