《邻苯二胺界面制备空心多角形微米棒》由会员分享，可在线阅读，更多相关《邻苯二胺界面制备空心多角形微米棒（3页珍藏版）》请在金锄头文库上搜索。
1、Synthesis and characterization of poly (o-phenylenediamine) hollow multi-angular microrods by interfacial methodQingli Hao, Baoming Sun, Xujie Yang, Lude Lu, Xin WangKey Laboratory of Soft Chemistry and Functional Materials, Ministry of Education, Nanjing University of Science and Technology, Nanjin
2、g 210094, Chinaa b s t r a c ta r t i c l ei n f oArticle history: Received 18 July 2008 Accepted 22 October 2008 Available online 30 October 2008Keywords: Poly (o-phenylenediamine) Ferric chloride Interfacial polymerization Microstructure Characterization methodsPoly (o-phenylenediamine) (PoPD) hol
3、low multi-angular microrods have been synthesized at 10 C via an interfacial process using ferric chloride and o-phenylenediamine (oPD) as starting materials. The chemical structure of the one dimensional (1D) superstructure is proved to be phenazine-like, and contains the benzenoid and quinoid imin
4、e units doped partly with Cl. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations indicate that the resulting superstructure of PoPD isbuilt from hollow nanofibers aligned parallel to the fiber axis by van der Waals force. The possible formation mechanism of th
5、e structure has been proposed. 2008 Elsevier B.V. All rights reserved.1. IntroductionIn the past decades, poly(o-phenylenediamine) (PoPD) or oPD oligomer (OoPD), a highly aromatic polymer containing 2,3-diamino-phenazine or quinoraline repeating unit 1, has received significantattention because it c
6、an be utilized in many fields, such as sensors 2, catalysts 3, rechargeable cells 4, anticorrosion coatings 5 and electrochromic devices6. Recently, many efforts have been devoted to fabricating one-dimensional (1D) nano- or micro-structures of the material obtained by the polymerization of o-phenyl
7、enediamine (oPD) mainly due to the possibility of enhanced performance in analytical application7,8, or the easy self-assembly of stacking in conducting polymers9. Some template-free chemical methods have been reported to shape the 1D micro- or nanostructure-based PoPD orOoPD. The reported micro- or
8、 nano-fibers or nanobelts are mainly obtained by solution polymerization through mixing 10,11, stirring 9,12,13, or reprecipitation 14 processes. The oxidants concern AgNO3, HAuCl4, FeCl3(FC ) and CuSO415. In the case of AgNO313, HAuCl49,10 used as oxidants, the resulting precipitates are not “pure”
9、, and there are some Au or Ag particle byproducts. Interfacial polymerization is a facile route to obtain the 1D conducting polymers 16. Here, we have successfully obtained a 1D superstructure of PoPD hollow multi-angular microrods on a large scale by the interfacial routeat 10 C, using FC as an oxi
10、dant,without anysurfactants. Such 1D superstructure self-assembled by this method is different from those obtained through other solution routes 914.2. ExperimentalIn a typical procedure, Solution A of 0.1 mol/L oPD (99.5%, Sigma- Aldrich) was prepared by dissolving oPD in chloroform; certain amount
11、 FC was dissolved in water respectively as Solution B with 0.05 and 0.4 mol/L FC. Solution B is transferred carefully upon to A in a breaker at 10 C. A quick color change from light yellow to brown-red was observed within several seconds upon the addition of FC. Soon,red fine fibers of the products
12、formed at the interface and diffused slowly into the aqueous solutions gradually. After 6 h, the aqueousphase was then collected and filtered, and the precipitate were rinsed thoroughly with water, and dried at 30 C for further use. Fourier transform infrared (FT-IR) spectra were recorded with a Bru
13、ker Vector 22 FT-IR spectrometer in the region of 4004000 cm1 using KBr pellets. Raman spectra were performed on a Renishaw Invia spectrometer. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) images were obtained on a JEOL JSM- 6380LV and JEM-2100 electron microscopes,
14、respectively. The X-ray diffraction (XRD) analysis of the samples was carried out on a Bruker D8 advanced X-ray diffractometer.3. Results and discussionThe FT-IR spectrum of the product is given in Fig. 1(A). The single band at around 3301 cm1is due to the NH stretching vibrations of the NH-group. T
15、he two peaks at 3380, 3153 cm1are ascribed to the asymmetrical and symmetrical of NH stretching vibrations of NH2group, respectively. Two strong peaks at 1615 cm1and 1533 cm1are associated with the stretching vibrations of CfC and CfN group in phenazine ring. The peaks at 1367 cm1and 1213 cm1are ass
16、ociated with CNC stretching in the benzenoid and quinoid imine units. Furthermore, the bands at 750 cm1and 610 cm1, which are the characteristic of CH out-of-plane bending vibrations of benzene nuclei in the phenazine skeleton, are also observed.Materials Letters 63 (2009) 334336 Corresponding authors. Tel./fax: +86 25 84315054. E-mail address: (Q. Hao).0167-577X/$ see front matter 2008 Elsevier B.V. All righ
