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Synthesis of water soluble sulfonated polyaniline and determination of crystal structure

机译:水溶性磺化聚苯胺的合成及晶体结构的测定

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A polyaniline (PANI) was synthesized by the oxidative polymerization using ammonium persulfate as an oxidizing agent. The PANI was then stirred with excess fuming sulfuric acid at room temperature for 6 h to obtain water soluble sulfonated polyaniline (SPANI). The degree of sulfonation was found to be 93-94% from the Fourier transform infrared (FTIR) and elemental analysis. The solubility of the SPANI in water was 1.25 g/L at room temperature and appeared as a green color solution. Conductivity of the PANI was decreased after sulfonation. A proliferation of hydrophilic nature of the PANI after sulfonation was observed from the water contact angle measurement. From the UV analysis, it was revealed that the energies required for the π-π*and bipolaron/polaron transitions are less and the intensity of these transitions are lower in SPANI compared to those of PANI. A detailed study on the crystal structures of PANI and SPANI were accomplished from the powder X-ray diffraction analysis. The SPANI exhibited a more ordered structure having a higher degree of crystallinity and crystallite sizes with an increased unit cell volume compared to the PANI. After sulfonation the morphology of PANI was transformed from a rod-like shape to a flat-plate shape.
机译:使用过硫酸铵作为氧化剂通过氧化聚合合成聚苯胺(PANI)。然后将PANI与过量的发烟硫酸在室温下搅拌6小时,以获得水溶性磺化聚苯胺(SPANI)。根据傅立叶变换红外光谱(FTIR)和元素分析,发现磺化度为93-94%。 SPANI在室温下在水中的溶解度为1.25 g / L,并显示为绿色溶液。磺化后,PANI的电导率降低。从水接触角测量中观察到磺化后PANI的亲水性的增殖。从紫外线分析中发现,与PANI相比,SPANI中π-π*和双极化子/极化子跃迁所需的能量更少,且这些跃迁的强度更低。通过粉末X射线衍射分析完成了对PANI和SPANI的晶体结构的详细研究。与PANI相比,SPANI表现出更有序的结构,具有更高的结晶度和微晶尺寸,并具有增加的晶胞体积。磺化后,PANI的形态从棒状转变为平板状。

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