【摘要】：近年來,聚吡咯因在傳感器、電磁屏蔽材料、電極材料、催化劑、藥物載體以及防腐蝕等領(lǐng)域具有極其廣闊的應(yīng)用前景而引起了人們的廣泛關(guān)注。其中聚吡咯材料的微觀結(jié)構(gòu)形貌與其物性的緊密關(guān)系更是人們研究的重點,但如何實現(xiàn)聚吡咯材料形貌的可控制備卻一直是人們面臨的挑戰(zhàn)性的難題。本文采用雙軟模板法制備聚吡咯納米材料,該部分研究分為兩個體系,以十二烷基苯磺酸鈉(SDBS)和十二烷基硫酸鈉(SDS)為雙模板來制備聚吡咯納米顆粒(球);以十二烷基苯磺酸鈉(SDBS)和十六烷基三甲基溴化銨(CTAB)為雙模板來制備聚吡咯納米纖維。在實驗中,考察了單模板法與雙模板法制備得到的聚吡咯形貌的區(qū)別,探索了摻雜酸的濃度及種類、聚合時間、聚合溫度對聚吡咯形貌的影響。研究表明,在SDBS和SDS聚合體系中,隨著鹽酸濃度的增大,制備得到的聚吡咯納米顆粒尺寸逐漸增大,當(dāng)以檸檬酸為摻雜酸時,聚吡咯呈均一規(guī)整的類球狀。CTAB與SDBS聚合體系,聚合時間越長,聚吡咯納米纖維表面越致密;利用水熱法制備聚吡咯,在相同條件下得到的是納米顆粒而不是納米纖維。在氣液界面處采用界面聚合法制備聚吡咯超薄膜的實驗中,考察了表面活性、氧化劑種類及濃度、單體濃度、摻雜酸、聚合時間、聚合溫度等因素對界面處形成的聚吡咯薄膜形貌的影響。表面活性劑SDBS的加入改變氣液界面處的活性,降低了界面處的表面自由能,從而使得聚吡咯超薄膜更容易形成;隨著聚合時間的增加,聚吡咯薄膜中與液相接觸一側(cè)的表面粗糙度逐漸增大,而與氣相接觸一側(cè)的表面則保持均一光滑的形貌并無明顯的變化;在以鹽酸為摻雜酸的聚合體系中得到厚度達(dá)20 nm的聚吡咯超薄膜,由于鹽酸的摻雜作用,聚吡咯薄膜導(dǎo)電性得到極大的提高。將吡咯單體水溶液進(jìn)行一定程度預(yù)氧化后再進(jìn)行氣液界面聚合,成功制備出聚吡咯超薄多孔膜。研究表明,單體的預(yù)氧化程度以及單體的濃度是決定聚吡咯多孔膜是否出現(xiàn)的關(guān)鍵因素。在添加SDBS的聚合體系中,隨著SDBS濃度的增加,聚吡咯多孔膜的孔洞尺寸逐漸減小且數(shù)量逐漸減少,當(dāng)SDBS濃度達(dá)到1 mM時,多孔膜演變?yōu)闊o孔洞的致密膜。
[Abstract]:In recent years, polypyrrole has attracted wide attention because of its wide application prospects in sensors, electromagnetic shielding materials, electrode materials, catalysts, drug carriers and corrosion protection. Among them, the relationship between microstructure and physical properties of polypyrrole materials is more important, but how to realize the controllable preparation of polypyrrole materials morphology has always been a challenging problem. In this paper, polypyrrole nanoparticles were prepared by double soft template method. This part is divided into two systems: sodium dodecyl benzene sulfonate (SDBS) and sodium dodecyl sulfate (SDS) as double templates to prepare polypyrrole nanoparticles (spheres). Polypyrrole nanofibers were prepared by using sodium dodecylbenzenesulfonate (SDBS) and cetyltrimethylammonium bromide (CTAB) as double templates. In the experiment, the differences of the morphology of polypyrrole prepared by single template method and double template method were investigated, and the effects of the concentration and type of dopant acid, polymerization time and polymerization temperature on the morphology of polypyrrole were investigated. The results show that the size of polypyrrole nanoparticles increases with the increase of hydrochloric acid concentration in the polymerization system of SDBS and SDS. When citric acid is used as dopant acid, polypyrrole exhibits uniform spherical shape. The longer the polymerization time, the denser the surface of polypyrrole nanofibers. Polypyrrole was prepared by hydrothermal method. Under the same conditions, nano-particles were obtained instead of nano-fibers. The surface activity, oxidant type and concentration, monomer concentration, dopant acid and polymerization time of polypyrrole ultrathin films prepared by interfacial polymerization at gas-liquid interface were investigated. The effect of polymerization temperature and other factors on the morphology of polypyrrole films formed at the interface. The addition of surfactant SDBS changes the activity at the gas-liquid interface and reduces the surface free energy at the interface, which makes the polypyrrole ultrathin film easier to form. With the increase of polymerization time, the surface roughness of polypyrrole film on one side of contact with liquid phase increases gradually, but the surface of contact side of polypyrrole film with gas phase has no obvious change of uniform and smooth morphology. Polypyrrole ultrathin films with thickness of 20 nm were prepared in the polymerization system with hydrochloric acid as dopant acid. Due to the doping of hydrochloric acid, the conductivity of polypyrrole films was greatly improved. Polypyrrole ultrathin porous membrane was successfully prepared by pre-oxidation of pyrrole monomer solution and gas-liquid interface polymerization. The results show that the degree of preoxidation and the concentration of monomer are the key factors to determine the appearance of polypyrrole porous membrane. In the polymerization system with the addition of SDBS, with the increase of SDBS concentration, the pore size of polypyrrole porous membrane decreased gradually and the number decreased gradually. When the concentration of SDBS reached 1 mM, the porous membrane evolved into a dense porous membrane.
【學(xué)位授予單位】：天津大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2016
【分類號】：O633.5;TB383

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