Y型酞菁氧钛纳米粒子的绿色制备及晶型稳定性研究

Green Preparation of Y-Type Titanyl Phthalocyanine Nanoparticles and Their Crystal Stability Investigation

研究了采用三氟乙酸/1,2-二氯乙烷(CF3COOH/1,2-C2H4Cl2)体系制备Y型酞菁氧钛(Y-TiOPc)纳米粒子的绿色工艺,采用酸碱中和-强酸置换法和常压蒸馏法对CF3COOH/1,2-C2H4Cl2体系制备Y-TiOPc过程中的酸溶溶剂进行回收,减少了CF3COOH和1,2-C2H4Cl2的排放,回收的试剂达到可再利用标准。研究了采用CF3COOH/1,2-C2H4Cl2体系所制备的Y-TiOPc纳米粒子的晶型稳定性,结果表明,采用该体系制备的Y-TiOPc纳米粒子在超声和球磨中的晶型稳定性均优于传统浓硫酸工艺制备的Y-TiOPc纳米粒子,其晶型经过4h超声和球磨处理不会向最稳定的β-TiOPc转化,完全满足制备有机光导体的电荷产生层时必须的球磨或超声分散工艺要求。最后,将所制备的Y-TiOPc纳米粒子作为电荷产生材料应用于多层有机光导体研究了其光电性能。并研究了析出温度对Y-TiOPc纳米粒子光电性能的影响,在析出温度为0℃时材料性能最优,所制备的有机光导体的性能参数为V0=828.7V、E1/2=0.09μJ/cm^2、Vr=33.7V和Rd=20.3V/s。

This research is to study the green process for the preparation of Y-TiOPc nanoparticles with CF 3 COOH/1, 2- C 2 H 4 Cl 2 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 CF 3 COOH and 1, 2-C 2 H 4 Cl 2 ,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 CF 3 COOH/1, 2-C 2 H 4 Cl 2 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 V 0 =828.7 V, E 1/2 = 0.09 μJ/cm^ 2 , V r =33.7 V, R d =20.3 V/s.