This research is to study the green process for the preparation of Y-TiOPc nanoparticles with CF3COOH/1,2-C2H4Cl2 system. The acid-soluble solvent produced in the preparation of Y-TiOPc was recovered by acid-base neutralization followed by strong acid displacement and atmospheric distillation, which could obviously reduce the emissions of both CF3COOH and 1,2-C2H4Cl2, the recovered solvents reach the reuse standards. The crystal stability of the prepared Y-TiOPc nanoparticles was investigated. The results revealed that Y-TiOPc nanoparticles prepared with CF3COOH/1,2-C2H4Cl2 system show much better crystal phase stability than those prepared by traditional concentrated sulfuric acid process. No crystal form transformation from Y-TiOPc to β-TiOPc is observed through the ball-milling or ultrasonic treatment within 4 h, which satisfies the stability requirement in the organic photoconductors (OPC) fabrication process. Finally, the prepared Y-TiOPc nanoparticles were applied in OPCs to evaluate their photoelectric properties. The influence of precipitation temperature of Y-TiOPc nanoparticles for the OPC property was investigated and the optimal precipitation temperature is confirmed as 0 ℃. The property parameter of the OPC fabricated by Y-TiOPc nanoparticles precipitated at 0 ℃ are V0=828.7 V, E1/2=0.09 μJ/cm2, Vr=33.7 V, Rd=20.3 V/s.