Particle agglomeration and close particle size distribution is the main limitation for effective recycling of Si and SiC. In this study, selective comminution was used to liberate fine particles from agglomerated ones before hydrocyclone separation. Furthermore, difference in particle size distribution between Si and SiC was enlarged by milling for 30 min. Compared with other milling time, pre-milling for 30 min showed the best hydrocyclone separation result (from 24 wt% to 8.1 wt%). Silicon with purity of 99.98 wt% was obtained by further treatment. SiC with purity of 99.2 wt% was obtained by washing off the impurities in the underflow.