抗溶剂气体重结晶制备聚碳硅烷纳米微粒的溶剂选择

Selection of the Solvent in PCS Nanoparticle Preparation Process by Gas Antisolvent Recrystallization

将理论计算和实验相结合来选择聚碳硅烷(PCS)抗溶剂气体重结晶过程的溶剂。首先,理论计算了聚碳硅烷的溶度参数,并根据极性相似相溶原理筛选出几种待选溶剂;然后,实验比较CO_2对待选溶剂的体积膨胀,待选溶剂与CO_2、PCS 的溶解情况和 PCS在待选溶剂中的析晶率。研究结果表明:在 3种待选溶剂四氢呋喃、对二甲苯和环己烷中,以四氢呋喃的性能最佳。以四氢呋喃作溶剂,采用抗溶剂气体重结晶工艺制备出的 PCS纳米微粒平均粒径为2.2 nm,颗粒粒径分布较为集中。

Based on the combination of theoretical calculation and experimental measurement, the study on the solvent in PCS nanoparticle preparation process by gas antisolvent recrystallization was carried out. The PCS's solvent parameter is calculated with the theoretical method, and some solvents such as cyclohexane, p-dimethyl benzene and tetrahydropyrane, are adopted according to the calculated result. The volume expansion of solvent with the solved CO2, the solubilities of solvent in CO2 and the PCS in solvent are measured for the adopted solvents. The experimental results indicate that the performance of tetrahydropyrane is the best among the three solvents, and the PCS nanoparticle with a average size of 2.2 nm is prepared using the tetrahydropyrane as solvent.