应用实验设计法包括部分析因设计与中心组合设计,优化自掺杂磺酸化聚苯胺的导电性.部分析因设计发现,需用低温(4℃)、短反应时间(1 h)和少量发烟硫酸(10 mL)等实验条件进行磺酸化反应才能得到好的导电性(ca.127 mS.cm-1);中心组合设计与确认实验表明,其最佳导电性(ca.141 mS/cm)的磺酸化条件是4℃、75 m in反应时间以及8 mL 30%的发烟硫酸.应用傅立叶变换红外光谱(FTIR)、四探针与X光光电子能谱等分析制备的材料.此外,发现磺酸化速率与程度与聚合反应时所使用的酸有关.
The optimal sulfonation condition of self-doped sulfonated polyaniline(prepared from leucoemeraldinebase;denoted as LEB-SPANI) with a high electronic conductivity was obtained by experimental strategies,includingthe fractional factorial design(FFD) and central composite design(CCD).From the FFD experiment,the self-doped LEB-SPANI prepared at a lowtemperature(4oC),a short reaction time(1 h),and a small volume of fumingsulfuric acid(10 mL) showed a better conductivity(ca.127 mS/cm).In the CCD study coupled with a confirmationtest,the highest conductivity(ca.141 mS/cm) of the LEB-SPANI film was obtained under a sulfonation temperatureof 4oC,a sulfonation time of75 minutes,and a volume of8 mLof30% fuming sulfuric acid.The textural cha-racter-istics of self-doped LEB-SPANI were characterized by Fourier transform infrared(FTIR) spectroscopy,four-pointprobe method,and X-ray photoelectron spectroscopy(XPS).The sulfonation rate and degree of LEB-SPANI werefound to be dependent upon the acid used in the polymerization step of PANI.