低温液相碳基及聚苯胺基微米纳米材料的制备与性质研究
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摘要
本论文研究和发展了低温液相化学合成方法制备聚苯胺基空心微球以及碳基纳米复合材料的技术,探索了如何通过调整具体实验条件来实现对产物的形貌、组成和结构、性质的可控合成。分别采用氧化—还原驱动法和无机硬模板法制备出近似单分散的聚苯胺和聚邻甲氧基苯胺空心微球,核壳型碳包覆结构纳米复合材料,并提出相应的形成机理。具体内容归纳如下:
1.氧化—还原驱动法聚苯胺微米纳米结构材料的选择性合成
通过选择H_2O_2-Fe~(3+)体系为苯胺聚合的氧化剂,以聚苯胺分子链上还原组分与氧气气泡的氧化—还原反应为驱动在水热条件下一步法制备出近似单分散的聚苯胺空心微球,制得的聚苯胺空心微球的大小、壁厚尺寸、结构组成和电导性质均可控,并且此方法无需借助任何表面活性剂或者有机添加剂。
2.聚苯胺/钯复合结构的制备与应用
以有机聚合物为载体制备的有机无机杂化材料在传感器、有机催化剂等领域有着重要的潜在应用价值。利用合成出的聚苯胺空心微球的还原能力,在温和条件下还原组装上催化贵金属钯纳米颗粒,得到聚苯胺/钯复合结构。
3.氧化—还原驱动法聚邻甲氧基苯胺空心微球的制备及其功能化
一步法合成贵金属@聚邻甲氧基苯胺卵壳(Yolk-Shell)和杂化空心结构,对比实验表明Ag@聚邻甲氧基苯胺卵壳结构的生成是一个非协同生成机理;而对于Pd@聚邻甲氧基苯胺杂化空心结构,大部分Pd元素并未完全还原出来,而是还存在于聚合物壳层中,需要再经过进一步的氧化-还原处理才被大量的还原出来。并且研究了Pd@聚邻甲氧基苯胺杂化空心结构的催化性质。
4.低温液相α-FeOOH/碳复合结构材料的合成研究
设计了一条温和的低温液相路线制备了α-FeOOH/碳纳米复合结构。选择丙酮和水的混合溶液体系有效抑制了环糊精均相碳化形成碳微球的趋势。在溶液体系中引入丙酮,使碳水化合物的分解产物无法达到其临界过饱和度,而选择沉积在α-FeOOH纳米晶上,制备出α-FeOOH/碳纳米复合结构材料。PH值范围对于水溶液中铁的氧化物的物相选择起着至关重要的作用,在所选择的溶液体系中添加的糖类碳水化合物,随着反应的进行,慢慢分解出氢离子保证了反应体系的弱酸性环境,从而有利于形成α-FeOOH物相。
In this dissertation,low-temperature chemical synthesis approaches in liquid phase have been successfully developed to synthesize of polyaniline(PANI), poly(o-anisidine) hollow spheres and carbon-based nanocomposites.Through adjusting the concrete reactive parameters,the morphology,composition/structure, property controllable synthesis is realized.An oxidation-reduction driven approach combined with hydrothermal synthesis has been developed to fabricate well-defined conducting polymer hollow spheres.An inorganic solid template approach has also been developed to synthesis of core-shell goethite@carbon nanocomposites.The details can be summarized as following:
1.We report an oxidation-reduction reaction driven hydrothermal approach that has been developed for synthesis of polyaniline(PANI) hollow spheres by one-pot polymerization of aniline using hydrogen peroxide(H_2O_2) as oxidant and Fe~(3+) as catalyst.The oxidation-reduction reaction between the benzenoid unit in PANI structural chain and O_2 is a driving force for the formation of the hollow spheres. The as-prepared polyaniline hollow spheres have shown the reducing reactivity to be able to spontaneously in-situ reduce palladium metal salts to prepare PANI@Pd hybrid composite materials.These hybrid materials will be used as the heterogeneous catalysis in organic coupling reactions.
2.We report a one-pot self-templated approach for synchronous fabrication-functionalization of the interior space of poly(o-anisidine) hollow structures with noble metal particles.The reduction of metal ions,the encapsulation metal particles and the formation cavity processes are involved in one synchronous core-dissolution and shell-formation processes.The oxidation-reduction reaction between the benzenoid unit in poly(o-anisidine) structural chain and O_2 is the internal driving force for the formation and increase of hollow cavity.Without extra reduction reagent and irradiation technique,Ag,and Pd particles have been encapsulated successfully into polymer shells successfully.
3.A mild solvothermal approach has been designed to synthesize uniform core-shell goethite@carbon nanocomposites with 3D geometrical architectures.We adopt a mixed water/acetone solvent system to effectively restrain the usual homogeneous nucleation of carbon spheres.Meanwhile,iron oxides phase transformation and stability during low-temperature carbonization process is also investigated.With the carbonization process carrying out,there is a mass of hydrogen ions releasing into the solution.The appropriate pH range from the initial to the final is the guarantee of the formation of goethite as a single phase.
1.氧化—还原驱动法聚苯胺微米纳米结构材料的选择性合成
通过选择H_2O_2-Fe~(3+)体系为苯胺聚合的氧化剂,以聚苯胺分子链上还原组分与氧气气泡的氧化—还原反应为驱动在水热条件下一步法制备出近似单分散的聚苯胺空心微球,制得的聚苯胺空心微球的大小、壁厚尺寸、结构组成和电导性质均可控,并且此方法无需借助任何表面活性剂或者有机添加剂。
2.聚苯胺/钯复合结构的制备与应用
以有机聚合物为载体制备的有机无机杂化材料在传感器、有机催化剂等领域有着重要的潜在应用价值。利用合成出的聚苯胺空心微球的还原能力,在温和条件下还原组装上催化贵金属钯纳米颗粒,得到聚苯胺/钯复合结构。
3.氧化—还原驱动法聚邻甲氧基苯胺空心微球的制备及其功能化
一步法合成贵金属@聚邻甲氧基苯胺卵壳(Yolk-Shell)和杂化空心结构,对比实验表明Ag@聚邻甲氧基苯胺卵壳结构的生成是一个非协同生成机理;而对于Pd@聚邻甲氧基苯胺杂化空心结构,大部分Pd元素并未完全还原出来,而是还存在于聚合物壳层中,需要再经过进一步的氧化-还原处理才被大量的还原出来。并且研究了Pd@聚邻甲氧基苯胺杂化空心结构的催化性质。
4.低温液相α-FeOOH/碳复合结构材料的合成研究
设计了一条温和的低温液相路线制备了α-FeOOH/碳纳米复合结构。选择丙酮和水的混合溶液体系有效抑制了环糊精均相碳化形成碳微球的趋势。在溶液体系中引入丙酮,使碳水化合物的分解产物无法达到其临界过饱和度,而选择沉积在α-FeOOH纳米晶上,制备出α-FeOOH/碳纳米复合结构材料。PH值范围对于水溶液中铁的氧化物的物相选择起着至关重要的作用,在所选择的溶液体系中添加的糖类碳水化合物,随着反应的进行,慢慢分解出氢离子保证了反应体系的弱酸性环境,从而有利于形成α-FeOOH物相。
In this dissertation,low-temperature chemical synthesis approaches in liquid phase have been successfully developed to synthesize of polyaniline(PANI), poly(o-anisidine) hollow spheres and carbon-based nanocomposites.Through adjusting the concrete reactive parameters,the morphology,composition/structure, property controllable synthesis is realized.An oxidation-reduction driven approach combined with hydrothermal synthesis has been developed to fabricate well-defined conducting polymer hollow spheres.An inorganic solid template approach has also been developed to synthesis of core-shell goethite@carbon nanocomposites.The details can be summarized as following:
1.We report an oxidation-reduction reaction driven hydrothermal approach that has been developed for synthesis of polyaniline(PANI) hollow spheres by one-pot polymerization of aniline using hydrogen peroxide(H_2O_2) as oxidant and Fe~(3+) as catalyst.The oxidation-reduction reaction between the benzenoid unit in PANI structural chain and O_2 is a driving force for the formation of the hollow spheres. The as-prepared polyaniline hollow spheres have shown the reducing reactivity to be able to spontaneously in-situ reduce palladium metal salts to prepare PANI@Pd hybrid composite materials.These hybrid materials will be used as the heterogeneous catalysis in organic coupling reactions.
2.We report a one-pot self-templated approach for synchronous fabrication-functionalization of the interior space of poly(o-anisidine) hollow structures with noble metal particles.The reduction of metal ions,the encapsulation metal particles and the formation cavity processes are involved in one synchronous core-dissolution and shell-formation processes.The oxidation-reduction reaction between the benzenoid unit in poly(o-anisidine) structural chain and O_2 is the internal driving force for the formation and increase of hollow cavity.Without extra reduction reagent and irradiation technique,Ag,and Pd particles have been encapsulated successfully into polymer shells successfully.
3.A mild solvothermal approach has been designed to synthesize uniform core-shell goethite@carbon nanocomposites with 3D geometrical architectures.We adopt a mixed water/acetone solvent system to effectively restrain the usual homogeneous nucleation of carbon spheres.Meanwhile,iron oxides phase transformation and stability during low-temperature carbonization process is also investigated.With the carbonization process carrying out,there is a mass of hydrogen ions releasing into the solution.The appropriate pH range from the initial to the final is the guarantee of the formation of goethite as a single phase.
引文
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