聚苯胺/纳米氧化物有机—无机杂化材料的制备研究
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摘要
近年来,杂化材料的研究论文快速增长,同时来自行业的关注也不断上升,杂化业已代表着一种设计新型材料的方法。聚合物有机-无机杂化材料以其优异的性能在许多领域得到了广泛的应用,而导电聚苯胺有机-无机纳米杂化材料的研究则引起了强烈持续的研究兴趣,人们用聚苯胺包覆无机纳米粒子期望赋予杂化材料新的功能。
本论文围绕聚苯胺有机-无机纳米杂化材料的制备方法及性能研究,主要开展了以下三方面的研究工作:
1、使用具有高反应活性而价格低廉的甲苯-2、4-二异氰酸酯分别对纳米二氧化钛和二氧化硅表面进行改性,增强了纳米粒子表面的化学反应性,使其表面键接上苯胺结构的官能团。在纳米粒子表面引入了苯胺聚合的反应点后,通过原位氧化接枝聚合技术制备了聚苯胺/二氧化钛纳米杂化材料和聚苯胺/二氧化硅纳米杂化材料。通过扫描电子显微镜、热失重和电导率的研究显示无机纳米粒子完全被聚苯胺包覆,无机粒子的引入提高了杂化材料的热稳定性,杂化材料具有半导体的性质。
2、采用类似于Stober溶胶-凝胶的技术成功构筑了表面氨基化二氧化硅,并通过原位氧化接枝聚合技术制备了聚苯胺/二氧化硅纳米杂化材料。对材料进行了FTIR、TG、Zeta电位和电导性能研究,结果发现氨基化二氧化硅表面带负电,经过和聚苯胺杂化后粒子表面带正电,聚苯胺将氨基化二氧化硅完全包覆,杂化材料依然具有良好的导电性。
3、采用类似于Stober溶胶-凝胶的技术成功构筑了表面乙烯基化二氧化硅,并通过化学氧化法成功实现了二氧化硅表面的羧基化,通过在其表面的静电组装和原位氧化聚合技术成功制备了核壳结构PANI@SiO2纳米杂化微球,对微球的Zeta电位和粒度分析表明,在羧基化二氧化硅表面包覆了一层厚度大约为218nm的聚苯胺。不同pH条件下杂化微球紫外-可见吸收光谱表明,该纳米杂化微球具有一定的pH响应性,可望用于pH传感器。该方法为制备其它聚合物/二氧化硅杂化微球材料提供了一种新途径。
Research in hybrid materials has experienced considerable growth in recent years with increasing interest from a wide range of industries. Hybrid materials have been on behalf of a way to design new materials. Polymer-based organic-inorganic hybrid materials has been widely used in many areas because of its superior properties. In particularly, hybrid materials of polyaniline and inorganic particles have attracted more and more attention. Recently, polyaniline coated inorganic particles has been extensively studied because they frequently exhibit unexpected hybrid properties.
In this thesis, our main aim is to circumfused with the preparation and property of polyaniline-inorganic particles hybrid materials. The research is focused in three aspects:
1. The hybrid materials of polyaniline and TiO2 was prepared by in situ chemical oxidative grafting polymerization. The aniline as initiator site convalent attachment on the surface of TiO2 were obtained utilizing the very cheap toluene diisocyanate as a surface modifying coupling agent. Results from the characterizations of SEM、TG and electrical conductively indicate that grafting PANI from onto the surface of nano TiO2 is successfully achieved. The hybrid materials obtained in this study has a semiconductive property.
2. Amino-functionally modified SiO2 particles were prepared by sol-gel process on the basis of Stober method. The coating of polyaniline onto SiO2 particles was carried out via in situ chemical oxidative covalently graft polymerization from the amino-functionally modified SiO2 particles. Results from the characterizations of FIRT、TG、Zeta potentials and electrical conductively indicate that grafting PANI from onto the surface of SiO2 particles is successfully achieved. The Zeta potentials of the hybrid particles showed a positive indicating that a sufficient number of negatively charged sites on the silica surfaces were neutralized by the PANI.
3. A effective and reproducible method for the preparation of core-shell PANI@SiO2 hybrid nanoparticles was developed successfully. Vinyl-functionally modified SiO2 particles were prepared by sol-gel process on the basis of Stober method. Carboxylic-functionally modified SiO2 particles were obtained via oxidation of vinyl groups to carboxylic groups. The aniline monomers electrostatically assembly to the silica surface were then polymerized by ammonium persulfate as an oxidizing agent. Results from the characterizations of FIRT、TG、Zeta potentials and particle size distributions indicate that preparation of core-shell PANI@SiO2 organic-inorganic hybrid nanoparticles is successfully achieved. The core-shell PANI@SiO2 organic-inorganic hybrid nanoparticles obtained in this study can been used as pH sensors.
本论文围绕聚苯胺有机-无机纳米杂化材料的制备方法及性能研究,主要开展了以下三方面的研究工作:
1、使用具有高反应活性而价格低廉的甲苯-2、4-二异氰酸酯分别对纳米二氧化钛和二氧化硅表面进行改性,增强了纳米粒子表面的化学反应性,使其表面键接上苯胺结构的官能团。在纳米粒子表面引入了苯胺聚合的反应点后,通过原位氧化接枝聚合技术制备了聚苯胺/二氧化钛纳米杂化材料和聚苯胺/二氧化硅纳米杂化材料。通过扫描电子显微镜、热失重和电导率的研究显示无机纳米粒子完全被聚苯胺包覆,无机粒子的引入提高了杂化材料的热稳定性,杂化材料具有半导体的性质。
2、采用类似于Stober溶胶-凝胶的技术成功构筑了表面氨基化二氧化硅,并通过原位氧化接枝聚合技术制备了聚苯胺/二氧化硅纳米杂化材料。对材料进行了FTIR、TG、Zeta电位和电导性能研究,结果发现氨基化二氧化硅表面带负电,经过和聚苯胺杂化后粒子表面带正电,聚苯胺将氨基化二氧化硅完全包覆,杂化材料依然具有良好的导电性。
3、采用类似于Stober溶胶-凝胶的技术成功构筑了表面乙烯基化二氧化硅,并通过化学氧化法成功实现了二氧化硅表面的羧基化,通过在其表面的静电组装和原位氧化聚合技术成功制备了核壳结构PANI@SiO2纳米杂化微球,对微球的Zeta电位和粒度分析表明,在羧基化二氧化硅表面包覆了一层厚度大约为218nm的聚苯胺。不同pH条件下杂化微球紫外-可见吸收光谱表明,该纳米杂化微球具有一定的pH响应性,可望用于pH传感器。该方法为制备其它聚合物/二氧化硅杂化微球材料提供了一种新途径。
Research in hybrid materials has experienced considerable growth in recent years with increasing interest from a wide range of industries. Hybrid materials have been on behalf of a way to design new materials. Polymer-based organic-inorganic hybrid materials has been widely used in many areas because of its superior properties. In particularly, hybrid materials of polyaniline and inorganic particles have attracted more and more attention. Recently, polyaniline coated inorganic particles has been extensively studied because they frequently exhibit unexpected hybrid properties.
In this thesis, our main aim is to circumfused with the preparation and property of polyaniline-inorganic particles hybrid materials. The research is focused in three aspects:
1. The hybrid materials of polyaniline and TiO2 was prepared by in situ chemical oxidative grafting polymerization. The aniline as initiator site convalent attachment on the surface of TiO2 were obtained utilizing the very cheap toluene diisocyanate as a surface modifying coupling agent. Results from the characterizations of SEM、TG and electrical conductively indicate that grafting PANI from onto the surface of nano TiO2 is successfully achieved. The hybrid materials obtained in this study has a semiconductive property.
2. Amino-functionally modified SiO2 particles were prepared by sol-gel process on the basis of Stober method. The coating of polyaniline onto SiO2 particles was carried out via in situ chemical oxidative covalently graft polymerization from the amino-functionally modified SiO2 particles. Results from the characterizations of FIRT、TG、Zeta potentials and electrical conductively indicate that grafting PANI from onto the surface of SiO2 particles is successfully achieved. The Zeta potentials of the hybrid particles showed a positive indicating that a sufficient number of negatively charged sites on the silica surfaces were neutralized by the PANI.
3. A effective and reproducible method for the preparation of core-shell PANI@SiO2 hybrid nanoparticles was developed successfully. Vinyl-functionally modified SiO2 particles were prepared by sol-gel process on the basis of Stober method. Carboxylic-functionally modified SiO2 particles were obtained via oxidation of vinyl groups to carboxylic groups. The aniline monomers electrostatically assembly to the silica surface were then polymerized by ammonium persulfate as an oxidizing agent. Results from the characterizations of FIRT、TG、Zeta potentials and particle size distributions indicate that preparation of core-shell PANI@SiO2 organic-inorganic hybrid nanoparticles is successfully achieved. The core-shell PANI@SiO2 organic-inorganic hybrid nanoparticles obtained in this study can been used as pH sensors.
引文
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[1]Kousik Dutta, S.K. De ,Optical and electrical characterization of polyaniline-silicon dioxide nanocomposite ,Physics Letters A,361, 2007, 141-145.
[2]Li X G,Huang M R,Duan W,Novel Multifunctional Polymers from Aromatic Diamines by Oxidative Polymerizations,Chem. Rev, 102 ,2002, 2925-3030.
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[6]Z. M. Tahir, E. C. Alocilia, D. L. Grooms, Polyaniline synthesis and its biosensor application. Biosens. Bioelectr., 20,2005, 1690-1695.
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[8]J. I. I. Laco, F. C. Villota, F. L. Mestres, Corrosion protection of carbon steel with thermoplastic coatings and alkyd resins containing polyaniline as conductive polymer. Prog. Org. Coat., 52,2005, 151-160.
[9]Arup Choudhury, Polyaniline/silver nanocomposites: Dielectric properties and ethanol vapour sensitivity ,Sensors and Actuators B: Chemical,138, 2009, 318-325.
[10]Shaohuang Weng, Zhonghua Lin, Yan Zhang, Lixian Chen, Jianzhang Zhou ,Facile synthesis of SBA-15/polyaniline nanocomposites with high electrochemical activity under neutral and acidic conditions ,Reactive and Functional Polymers, 69, 2009, 130-136.
[11]Long Zhang, Tingmei Wang, Peng Liu, Polyaniline-coated halloysite nanotubes via in-situ chemical polymerization ,Applied Surface Science,255,2008, 2091-2097 .
[12]Hongfan Guo, Hong Zhu, Haiyan Lin, Jiqiao Zhang, Synthesis of polyaniline/multi-walled carbon nanotube nanocomposites in water/oil microemulsion Materials Letters,62, 2008, 3919-3921.
[13]G.K. Surya Prakash, Palale Suresh, Federico Viva, George A. Olah, Novel single step electrochemical route toγ-MnO2 nanoparticle-coated polyaniline nanofibers: Thermal stability and formic acid oxidation on the resulting nanocomposites, Journal of Power Sources,181, 2008, 79-84.
[14]Liangchao L, Hui Liu, Yuping Wang, Jing Jiang, Feng Xu ,Preparation and magnetic properties of Zn-Cu-Cr-La ferrite and its nanocomposites with polyaniline ,Journal of Colloid and Interface Science,321, 2008, 265-271.
[15]Feng-Yi Chuang, Sze-Ming Yang, Cerium dioxide/polyaniline core–shellnanocomposites, Journal of Colloid and Interface Science,320,2008,194-201.
[16]Nilofar Asim, S. Radiman, M.A.bin Yarmo, Preparation and characterization of core–shell polyaniline/V2O5 nanocomposite via microemulsion method, Materials Letters, 62, 2008, 1044-1047.
[17]P. K. Khanna, Sunil. P. Lonkar, V. V. V. S. Subbarao, Ki-Won Jun,Polyaniline-CdS nanocomposite from organometallic cadmium precursor,Materials Chemistry and Physics,87, 2004, 49-52.
[18]P. S. Khiew, N.M.Huang, S.Radiman,Md. Soot Ahmad ,Synthesis and characterization of conducting polyaniline-coated cadmium sulphide nanocomposites in reverse microemulsion ,Materials Letters,58, 2004, 516-521 .
[19]M. Feng, Y. G. Liu, C. L. Lu, W. H. Hou, J. J. Zhu, One-step synthesis of AgCl/polyaniline core-shell composites with enhanced electroactivity. Nanotechnology, 17,2006, 3578-3583.
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[22]Jing Li,Lihua Zhu,Yinghui Wu,Yutaka Harim,Aiqing Zhang,Heqing Tang, Hybrid composites of conductive polyaniline and nanocrystalline titanium oxide prepared via self-assembling and graft polymerization , Polymer, 47, 2006, 7361-7367 .
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[28] Xueyan Li, Desong Wang,Guoxiang Cheng,Qingzhi Luo,Jing An,Yanhong Wang,Preparation of polyaniline-modified TiO2 nanoparticles and their photocatalytic activity under visible light illumination,Applied Catalysis B: Environmental,81, 2008, 267-273 .
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[1]Kousik Dutta, S.K. De ,Optical and electrical characterization of polyaniline-silicon dioxide nanocomposite ,Physics Letters A,361, 2007, 141-145.
[2]Li X G,Huang M R,Duan W,Novel Multifunctional Polymers from Aromatic Diamines by Oxidative Polymerizations, Chem. Rev, 102 ,2002, 2925-3030.
[3]N. Gospodinova, L. Terlemezyan, Conducting polymers prepared by oxidative polymerization: polyaniline. Prog. Polym. Sci., 23,1998, 1443-1484.
[4]Y. S. Neqi, P. V. Adhyapak, Development in polyaniline conducting polymers. J. Macromol. Sci.-Polym. Rev., 42,2002, 35-53.
[5]T. Nakajima, T. Kawaqoe, Polyaniline: Structural analysis and application for battery. Syn. Metal, 28,1989, 629-638.
[6]Z. M. Tahir, E. C. Alocilia, D. L. Grooms, Polyaniline synthesis and its biosensor application. Biosens. Bioelectr., 20,2005, 1690-1695.
[7]C. H. Yang, Y. K. Chih, W. C. Wu, C. H. Chen, Molecular assembly engineering of self-doped polyaniline film for application in electrochromic devices. Electrochem. Solid-State Lett., 9,2006, 5-8.
[8]J. I. I. Laco, F. C. Villota, F. L. Mestres, Corrosion protection of carbon steel with thermoplastic coatings and alkyd resins containing polyaniline as conductive polymer. Prog. Org. Coat., 52,2005, 151-160.
[9]Arup Choudhury, Polyaniline/silver nanocomposites: Dielectric properties and ethanol vapour sensitivity ,Sensors and Actuators B: Chemical,138, 2009, 318-325.
[10]Shaohuang Weng, Zhonghua Lin, Yan Zhang, Lixian Chen, Jianzhang Zhou ,Facile synthesis of SBA-15/polyaniline nanocomposites with high electrochemical activity under neutral and acidic conditions ,Reactive and Functional Polymers, 69, 2009, 130-136.
[11]Long Zhang, Tingmei Wang, Peng Liu, Polyaniline-coated halloysite nanotubes via in-situ chemical polymerization ,Applied Surface Science,255,2008, 2091-2097 .
[12]Hongfan Guo, Hong Zhu, Haiyan Lin, Jiqiao Zhang, Synthesis of polyaniline/multi-walled carbon nanotube nanocomposites in water/oil microemulsion Materials Letters,62, 2008, 3919-3921.
[13]G.K. Surya Prakash, Palale Suresh, Federico Viva, George A. Olah, Novel single step electrochemical route toγ-MnO2 nanoparticle-coated polyaniline nanofibers: Thermal stability and formic acid oxidation on the resulting nanocomposites, Journalof Power Sources,181, 2008, 79-84.
[14]Liangchao L, Hui Liu, Yuping Wang, Jing Jiang, Feng Xu ,Preparation and magnetic properties of Zn-Cu-Cr-La ferrite and its nanocomposites with polyaniline ,Journal of Colloid and Interface Science,321, 2008, 265-271.
[15]Feng-Yi Chuang, Sze-Ming Yang, Cerium dioxide/polyaniline core–shell nanocomposites, Journal of Colloid and Interface Science, 320, 2008, 194-201.
[16]Nilofar Asim, S. Radiman, M.A.bin Yarmo, Preparation and characterization of core–shell polyaniline/V2O5 nanocomposite via microemulsion method, Materials Letters, 62, 2008, 1044-1047.
[17]P. K. Khanna, Sunil. P. Lonkar, V. V. V. S. Subbarao, Ki-Won Jun,Polyaniline-CdS nanocomposite from organometallic cadmium precursor,Materials Chemistry and Physics, 87, 2004, 49-52.
[18]P. S. Khiew, N.M.Huang, S.Radiman,Md. Soot Ahmad ,Synthesis and characterization of conducting polyaniline-coated cadmium sulphide nanocomposites in reverse microemulsion ,Materials Letters, 58, 2004, 516-521 .
[19]M. Feng, Y. G. Liu, C. L. Lu, W. H. Hou, J. J. Zhu, One-step synthesis of AgCl/polyaniline core-shell composites with enhanced electroactivity. Nanotechnology, 17,2006, 3578-3583.
[20]Peng Liu,Weimin Liu,Qunji Xue,In situ chemical oxidative graft polymerization of anilinefrom silica nanoparticles,Materials Chemistry and Physics,87,2004, 109-113.
[21]Xiping Lei,Zhixing Su,Conducting polyaniline-coated nano silica by in situ chemical oxidative grafting polymerization,Polym. Adv. Technol, 18,2007, 472-476.
[22] Timothy von Werne,Timothy E. Patten,Atom Transfer Radical Polymerization from Nanoparticles: A Tool for the Preparation of Well-Defined Hybrid Nanostructures and for Understanding the Chemistry of Controlled/“Living”Radical Polymerizations from Surfaces,J. Am. Chem. Soc., 123 , 2001, 7497–7505.
[23]H. R. Li, J. Lin, H. J. Zhang, L. S. Fu, Q. G. Meng, S. B. Wang, Preparation and Luminescence Properties of Hybrid Materials Containing Europium(III) Complexes Covalently Bonded to a Silica Matrix , Chem. Mater., 14, 2002, 3651–3655.
[24]井新利,郑茂盛,金志浩,许晓玲,高分子材料科学与工程,14,1998,62-64.
[25]Li H R,Lin J, Zhang H J, Fu L S, Meng Q G, Wang S B.,Preparation and Luminescence Properties of Hybrid Materials Containing Europium(III) Complexes Covalently Bonded to a Silica Matrix ,Chem Mater, 14,2002, 3651-3655.
[26]C. Wu, T.W. Xu, W.H. Yang, Fundamental studies of a new hybrid (inorganic–organic) positively charged membrane: membrane preparation and characterizations,J. Membr. Sci. 216,2003,269-278
[27]Y. Ohnuki,T. Ohsaka,H. Matsuda, N. Oyama, Permselectivity of films prepared by electrochemical oxidation of phenol and amino-aromatic compound, J. Electroanal. Chem.158,1983,55-67
[28]N. Oyama, Y. Ohnuki, K. Chiba, T. Ohsaka, Selectivity of PANI electrode for redox reactions of species in solution.Chem. Lett. 11,1983,1759-1762.
[29]E.T. Kang, K.G. Neho and K.L. Tan, Polyaniline: A polymer with many interesting intrinsic redox states , Prog. Polym. Sci. 23,1998,277-324.
[30]D.C. Schnitzler, M.S. Meruvia, I.A. H¨ummelgen, A.J.G. Zarbin, Preparation and Characterization of Novel Hybrid Materials Formed from (Ti,Sn)O2 Nanoparticles and Polyaniline,Chem. Mater. 15,2003,4658–4665.
[31]Xiping Lei,Zhixing Su,Conducting polyaniline-coated nano silica by in situ chemical oxidative grafting polymerization,Polym. Adv. Technol, 18, 2007, 472-476.
[32]Xiao-Xia Liu, Yu-Qian Dou, Jian Wu, Xu-Yuan Peng,Chemical anchoring of silica nanoparticles onto polyaniline chains via electro-co-polymerization of aniline and N-substituted aniline grafted on surfaces of SiO2 ,Electrochimica Acta 53,2008,4693–4698.
[33]Shuangxi Xing, Chun Zhao, Shengyu Jing , Zichen Wang,Morphology and conductivity of polyaniline nanofibers prepared by‘seeding’polymerization ,Polymer 47,2006,2305–2313.
[34]Shuangxi Xing , Hongwei Zheng, Guoku Zhao,Preparation of polyaniline nanofibers via a novel interfacial polymerization method ,Synthetic Metals 158 ,2008,59–63.
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[16]Y. Ohnuki, T. Ohsaka, H. Matsuda, N. Oyama, Permselectivity of films prepared by electrochemical oxidation of phenol and amino-aromatic compounds,J. Electroanal.Chem.158,1983,55-67.
[17]N. Oyama, Y. Ohnuki, K. Chiba, T. Ohsaka, Permselectivity of films prepared by electrochemical oxidation of phenol and amino-aromatic compound, Chem. Lett. 11 ,1983,1759-1762.
[18]E.T. Kang, K.G. Neho and K.L. Tan, Polyaniline: A polymer with many interesting intrinsic redox states ,Prog. Polym. Sci. 23,1998,277-324.
[19]Xiping Lei,Zhixing Su,Conducting polyaniline-coated nano silica by in situ chemical oxidative grafting polymerization,Polym. Adv. Technol, 18, 2007, 472-476.
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[1]Huan Ma,Lenore L. Dai,Synthesis of polystyrene–silica composite particles via one-step nanoparticle-stabilized emulsion polymerization,Journal of Colloid and Interface Science, 333,2009,807-811.
[2]Asako Narita, Kensuke Naka, Yoshiki ChujoFacile, control of silica shell layerthickness on hydrophilic iron oxide nanoparticles via reverse micelle method, Colliods and Surfaces A: Physicochemical, 336, 2009, 46-48.
[3]Asako Narita, Kensuke Naka, Yoshiki ChujoFacile, control of silica shell layer thickness on hydrophilic iron oxide nanoparticles via reverse micelle method, Colliods and Surfaces A: Physicochemical, 336, 2009, 46-48.
[4]Yi-Hsin Lien, Tzong-Ming Wu, Preparation and characterization of thermosensitive polymers grafted onto silica-coated iron oxide nanoparticles,Journal of Colloid and Interface Science, 326,2008, 517-521.
[5]Ling Li, Eugene Shi Guang Choo, Zhaoyang Liu, Jun Ding, Junmin Xue, Double-layer silica core-shell nanospheres with superparamagnetic and fluorescent functionalities, Chemical Physics Letters, 461, 2008, 114-117.
[6]Dayang Wang , Frank Caruso, Polyelectrolyte-Coated Colloid Spheres as Templates for Sol?Gel Reactions, Chem. Mater., 14, 2002, 1909–1913.
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[10]Yong Wang,Xiaowei Teng,Jin-Shan Wang, Hong Yang, Solvent-Free Atom Transfer Radical Polymerization in the Synthesis of Fe2O3@Polystyrene Core?Shell Nanoparticles,Nano Letters, 3,2003,789-793.
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