摘要
碳纳米材料所具有的多样性结构及各种优异性能，使其在信息、生物、能源、环境保护等各个方面展示了巨大的应用前景。纳米碳材料的结构、维度、形貌、尺寸等因素对它们的性能有着重要影响。因而，碳材料的调控合成是碳纳米科技发展的重要组成部分，也是探索碳材料性能及应用研究的基础。论文借助表面活性剂构筑的限域性微反应器的模板作用可控制备了四种不同的纳米碳材料：碳纳米管、空心碳纳米胶囊、碳包覆铁纳米材料以及纳米碳带，研究了所得碳包覆铁纳米材料用于磁性分离催化剂载体的可行性。具体的研究工作包括以下几个方面：
借助四元微乳体系，即十六烷基三甲基溴化胺(CTAB)／水／环己烷／正戊醇构筑的反相微乳为模板，以间苯二酚和甲醛为聚合单体，在溶剂热条件下通过乳液聚合反应选择性合成了具有不同形貌特征的碳前驱体，后经炭化分别制备了空心碳纳米胶囊、碳纳米管及碳包覆纳米材料。利用TEM、XRD、EDX、Raman、FT-IR及TG等测试手段，对合成样品的形貌、结构及成分进行了分析。考察了水与表面活性剂的摩尔比值、间苯二酚的加入量、甲醛的用量、三氯化铁的添加、CTAB的浓度、溶剂热过程的温度和时间以及炭化温度和升温速率等实验参数对生成产物的影响。结合测试分析结果，对纳米碳管和纳米碳空囊的形成机理进行了初步讨论。采用该制备工艺可实现在合成过程中对碳纳米材料尺寸和形貌等指标的调控。
以CTAB为模板剂，问苯二酚和甲醛为聚合单体，草酸亚铁为金属源，通过乳液聚合法制备了酚醛树脂．铁盐前驱体，将其炭化得到了具有完好壳／核包覆结构的碳包覆铁纳米材料(Fe@C)；考察了金属盐添加量、炭化温度及炭化升温速率等工艺条件对Fe@C形成的影响；磁性能及N_2吸附测试结果表明Fe@C具有超顺磁性及较高的比表面积。以Fe@C为催化剂载体，采用浸渍法制备了Fe@C负载金属Ru催化剂(Ru／Fe@C)，并将其用于苯甲醇选择氧化制备苯甲醛的反应。研究结果表明，反应4.5 h后，苯甲醇的转化率和苯甲醛的选择性均接近100％。利用磁分离技术，Ru／Fe@C可被回收并多次使用，Ru／Fe@C循环使用4次后，苯甲醛的选择性可保持100％，苯甲醇的转化率仍可达80％。
采用水热法，以葡萄糖为聚合单体，借助十二烷基苯磺酸钠(SDBS)的结构导向作用，制备了带状纳米碳材料。EDX、XPS及FT-IR测试结果表明纳米带为富碳高聚物，表面含有羟基、羰基等有机基团。考察了水热反应温度及时间、SDBS的添加及高温炭化处理对产物形貌及组成的影响：随着水热碳化温度的升高或反应时间的延长，所得碳纳米带／片的尺寸增加，产物的结晶度变好。结合测试分析结果，初步探讨了纳米碳带的形成机理。
采用胶溶法获得氢氧化铁水溶胶，加入SDBS将其胶凝后，通过在氢气及氮气气氛下的煅烧处理合成了Fe及Fe_3O_4催化剂，于700℃下气相沉积乙炔，分别制备了竹节状及鱼骨状纳米碳管。运用SEM、TEM、XRD等技术手段对碳材料的形貌、结构及组成进行了分析，讨论了气相沉积的时间及温度对产物形貌的影响。此外，不采用任何催化剂，以氮气／氢气混合气为载气，700℃下直接裂解乙炔，可同时制备空心及实心微米碳球，并可于反应器的不同位置收集产物。考察了沉积温度及载气组成对生成产物形貌的影响，根据不同温度下裂解乙炔所得产物的形貌变化，初步推测了空心及实心碳微球的形成机理。
以十二钨磷酸为氧化剂，在水热条件下对活性炭进行氧化改性，水热氧化改性3天所得改性活性炭的噻吩脱除率为39.6％，远高于初始活性炭的脱硫效果(11.8％)。表面活性剂的加入可以在提高脱硫率的前提下，大大缩短活性炭的水热改性时间。研究结果表明，加入十二烷基苯磺酸钠后，对活性炭的改性时间由3天缩减为1天，所得改性活性炭的脱硫率为50.7％，优于未添加SDBS时，改性3天所得活性炭样品的脱硫效果。考察了SDBS用量及水热反应时间对改性活性炭脱硫性能的影响。结合低温N_2吸附、FT-IR和TPD测试结果，讨论了不同实验条件下，活性炭孔结构及表面化学性质的变化，初步分析了活性炭的自身特性对其吸附转移噻吩的影响。
Recently, carbon nanomaterials attract more and more attention because of their distinctive physical and chemical properties as well as potential applications in many high-tech fields, such as biomedical engineering, catalysis, energy sources, etc. Manipulated synthesis of nanocarbons is one of the most important sections of carbon nanoscience and nanotechnology, and the base to investigate the distinctive properties and applications of carbon nanostructures. In this thesis, carbon nanotubes, hollow carbon nanocapsules, carbon encapsulated iron nanomaterials (Fe@C) and carbon nanobelts are selectively prepared with the assistance of different nano-reactors assembled by surfactants. The possibility of Fe@C as the magnetically separable catalyst support is investigated. The work is now summarized as follow:
A technique combining microemulsion polymerization and the subsequent carbonization process is proposed for the selective synthesis of carbon nanocapsules, carbon nanotubes and carbon encapsulated nanoparticles. A quaternary microemulsion composed of CTAB (cetyltrimethylammonium bromide)/water/cyclohexane/n-pentanol is chosen as the nano-reactor with resorcinol (R) and formaldehyde (F) as the reactant monomers. The morphologies, structures and components of the as-made carbons are investigated by TEM, EDX, XRD, Raman, FT-IR and TG techniques. The experimental parameters such as the molar ratio of water to CTAB, the concentration of CTAB, the feeding amount of R and FeCl_3, and the solvothermal treating time and temperature are addressed. This method may provide an alternative synthetic route for the controllable preparation of carbon nanomaterials with different morphologies that are of great potential in many high-tech fields.
Carbon encapsulated iron nanomaterials have been successfully synthesized by pyrolyzing RF polymer/iron oxalate composite in flowing hydrogen. Microemulsion polymerization of R and F is completed via a micelle-template technique with CTAB as the template agent. The as-made Fe@C exhibits well-constructed metal core/carbon shell structure with high BET surface area and superparamagnetic property. The effect of the experimental conditions on the formation of Fe@C is addressed, including iron salt feeding, carbonization temperature and the heating rate. Moreover, Fe@C supported Ru catalyst (Ru/Fe@C) is prepared through an impregnation process. Ru/Fe@C shows excellent catalytic performance for the oxidation of benzyl alcohol. The conversion of benzyl alcohol is 99.6% and the selectivity to benzaldehyde is 100% at 90°C, oxygen atmosphere with water-toluene biphasic system as the solvent. Ru/Fe@C can be easily separated and recovered by using a foreign magnetic field, and shows no obvious loss in catalytic activity after being reused for 4 times.
Under the mediation of SDBS (sodium dodecyl benzene sulfonate) molecules, carbon-rich nanobelts (CNBs) are formed through carbonization of glucose under hydrothermal condition. The morphology evolution of CNBs has been investigated as the functions of the hydrothermal time and temperature. CNBs grow wider and thicker with the time prolonging and the temperature increasing. The EDX, FT-IR and XPS analysis confirm that there are functional groups abounded in as-made carbon framework. A possible growth model of CNBs is proposed and discussed in terms of the process parameters.
Bamboo-shape and fishbone-like CNTs are selectively prepared by catalytic decomposition of acetylene over Fe-based catalysts that are prepared by SDBS-stabilized colloid chemical method coupled with calcination treatment. XRD analyses and TEM studies indicate that Fe catalysts result in the formation and growth of bamboo-shape CNTs, while Fe_3O_4 catalysts lead to fishbone-like ones. The factors in determining the morphology of the products and the growth mechanism of carbon nanotubes are addressed. Furthermore, simultaneous production of microsize hollow and solid carbon spheres is successfully achieved via non-catalytic chemical vapor deposition of acetylene. The unique feature is that the as-made two ball-like carbons can be collected separately as two individual products. The parameters such as the reaction temperature and the composition of the carrier gas are found to be critical for the formation of microsize hollow and solid carbon spheres.
A polyoxometalates (POMs)-assisted hydrothermal system is developed for the modification of activated carbon (AC). The AC sample (AC-3) modified with hydrothermal treating for 3 days exhibits good adsorption capability, with thiophene removal ratio of 39.6%, much better than that of raw AC sample (11.8%). By adding SDBS, the hydrothermal reaction time can be reduced to 1 day, with the as-modified AC even showing a higher thiophene removal efficiency (50.7%) than that of AC-3. The functional groups and the porous structure are simultaneously responsible for the desulfurization performance of AC.
引文
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