中间相沥青基泡沫炭的可控制备及若干应用探索
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摘要
泡沫炭具有独特的三维网状内部结构,呈现出密度小、孔隙率高、耐高温、耐腐蚀、易加工等突出性能,是近年来隔热、导热、吸波、导电、传质材料等领域的研究热点。本论文针对泡沫炭的结构控制、复合增强以及应用方面存在的共性科学难题或研究空白点,以中间相沥青为原料,采用自发泡法和超临界发泡法制得不同孔结构的泡沫炭,系统归纳了中间相沥青的物化性质、自发泡条件、超临界发泡条件与孔结构(孔形、孔径、韧带结构、开/闭孔)及材料力学性能之间的内在关系,分别阐明了自发泡机理和超临界发泡机理,揭示了石墨化泡沫炭微裂纹的产生共性机制,并探讨了泡沫炭在气-固催化反应以及生物污水处理中等新型领域的应用可能。
本论文针对泡沫炭的孔结构控制和自发泡、超临界发泡机理以及石墨化泡沫炭微裂纹的产生机制,形成了较具特色的研究,并得出如下主要结论：
1)以中间相沥青为原料,采用自发泡技术,制得结构可控的中大孔泡沫炭,系统考察了中间相沥青的性质、自发泡条件、炭化、石墨化工艺对泡沫炭孔结构的影响。通过对中间相沥青进行预氧化,结合沥青的簇组成及其粘-温特性,推断自发泡机理如下：在发泡温度下,中间相沥青中的轻组分或裂解气将优先在喹啉不溶物(QI组分)处成核、聚集和膨胀,然后形成泡孔；在升温至发泡温度的过程中,当沥青内部由裂解产生气体的压力高于外界压力时,部分气体在内外压差的作用下从沥青内部逸出,导致泡沫炭的开孔率较高。
2)以甲苯为发泡剂,采用超临界发泡制得孔径为100-200μm的泡沫炭,并结合不同工艺条件对泡沫炭的结构进行了有效调控,推断发泡机理如下：在超临界条件下,当甲苯和中间相沥青形成均相体系后,在快速卸压过程中,溶解在中间相沥青中的甲苯处于过饱和状态,进而与熔融沥青分相：由于轻组分/QI界面处的Gibbs自由能比沥青主体相要低,于是甲苯则优先在轻组分/QI界面处成核,并逐渐扩散、聚集和膨胀,最终形成泡孔。
3)通过调控不同程度萃取的中间相沥青的簇组成,考察不同石墨化泡沫炭微裂纹结构,推断其产生机制如下：泡沫炭在石墨化过程中,由于孔壁及韧带处存在热应力梯度分布,导致热应力的释放速度不同,进而产生微裂纹。其中,微裂纹的产生及其形状与石墨化过程中产生的热应力、热应力的释放速度和碳基体的物理性质有关。通过调节中间相沥青的族组成可以有效控制石墨化泡沫炭微裂纹的产生。
4)协同超声和磁力搅拌分散功效,实现了CNTs在中间相沥青中的均匀分散,并成功自发泡制备出CNT增强的泡沫炭。当CNTs分散量为3.5wt.%时,所制泡沫炭孔结构的均一性最好,压缩强度达4.7MPa。
5)泡沫炭经HNO3适当氧化后,孔壁表面形成新的中孔、大孔,并有效的改进了其界面的亲水性,从而有利于金属催化剂的均匀分散；通过化学气相沉积法,可以在改性泡沫炭表面均匀生长一层致密的纳米碳纤维,在不影响泡沫炭的孔结构和强度的同时,大大增强了材料的有效界面,从而有利于MnOx-CeO2纳米催化剂在泡沫炭界面的高度分散。MnOx-CeO2/CNFs-泡沫炭催化剂具有极高的NO的催化脱除能力,在180-220℃范围内,对NO的脱硝效率可以达到90%以上。
6)泡沫炭经过HNO3氧化、水洗、生物接种、生物驯化之后,成功的在其表面生长出致密的高活性生物膜。生物菌种类和数量较多,对多种污水成分具有一定的普适性降解效果。其中,生物泡沫炭对COD、BOD和NH3-N等典型污染物降解率分别高达81%、81%和75%,明显优越于生物陶瓷颗粒,揭示了泡沫炭良好的生物相容性和作为微生物固定化载体的应用前景。
Carbon foams, which exhibit an interconnected structure and a large porosity made up of macrospores, are important in many areas of modern science and technology, including aerospace, heat exchanger, catalyst support and electrode material due to their remarkable properties, such as low density, high open-cell ratio, low coefficient of thermal expansion, resistance to corrosion, easy machining and other superior performances. However, the tailor of pore architecture and enforcement of mechanical performance of carbon foams for some special application were still a challenging task. This therefore, calls for research into more economic and effecitive ways to prepare high qulitiy carbon foams with controlled structure and porperties. In this thesis, we focused on these issues and developed two methods (self-foaming and supercritical foaming) to foam mesophase pitch. The pore texture (pore shape, pore size, ligament structure, and opening/closing pore) and mechanical properties have been systematically investigated by adjusting the physical chemistry parameters of mesophase pitch, self-foaming and supercritical foaming conditions. The mechanisms of self-foaming and supercritical foaming were clarified and the occurrence of micro-cracks in graphitized carbon foams was explained. Meanwhile, the applications of carbon foams in gas-solid catalysis and the water treatment were also preliminarily studied.
The major innovations of the thesis were from three aspects:tailoring of pore structure (especially pore range from10to200μm), the mechanism of self-foaming and supercritical foaming and the foming mechanism for the micro-crack in the matrix. The main research contents are summaried as follows.
1) Carbon foams with pore size of100to600μm were prepred by self-foaming approach, using mesophase pitches as precusors. The pore control has been systematically studied. The mechanisms of self-foaming have been revealed. Under the foaming temperature, the light molecular or pyrolysis gas released from the mesophase pitch were formed a core around the QI component, and then aggregated, grow up and finally became stable pores. During the further heating process, the interior pressure of pitch was higher than the exterior one, resulting in that some volatile materials would be driven and escape from the inner of molten pitch under the pressure difference. As a consequence, some closing pores would turn into opening pores. It was worthy to note that the pressure difference was determined by the amount and the generating rate of the light component.
2) A series of carbon foams with pore size of20-200μm were prepared through supercritical toluene technique. Toluene and mesophase would firstly form a homogeneous phase at the supercritical toluene condition. When the pressure was relieved quickly, toluene should separated from the mixture phase owing to the supersaturate status. Besides the Gibbs freedom energy of interface between QI and light components was lower than that of pitch matrix, the toluene would prefer to form the core at the interface, then diffusion, coalescence, growing up and finally turned into pores.
3) During the graphitization process, the thermal stress and its gradient distribution along the pore wall and ligament would lead to the occurrence of micro-cracks. The texture and shape of the micro-cracks was greatly detemined by the thermal stress, the release rate and the properties of the precursor carbons. The micro-cracks could be controlled to some content by adusting the composition of the precursor mesophase pitch.
4) The homogenous dispersion of CNTs in the mesophase pitch was realized through the ultrasonic wave combined with magnetic stirring method. When the mass concentration of CNTs was3.5%, the as-prepared carbon foams owned uniform pore distribution, and the strength of pore wall was greatly enhanced and the amount of micro-cracks was greatly reduced. The compression strength was as high as4.7MPa.
5) A certain amount of mesopore and macropore was created when the carbon foams were subjected to HNO3oxidaiton treatment. The oxidation could improve the hydrophilic properties, which was beneficial for the dispersion of metal catalysis. After impregnated with metal nanoparticles, carbon nanofiber could be grown on the surface of carbon foams through CVD technique, which could effectively increase the external surface area without the loss of the pore structure. MnOx-CeO2hybird oxides could be homogeneously supported on the CNFs/carbon foams composites for NO removal. When the temperature was in the range of180-220℃, the removal efficiency of NO was as high as90%.
6) The hydrophilic surface of carbon foams would be obtained by mild HNO3oxidaiton. The active bacteria could be immobilized on the surface of oxidized carbon foams after the bacterination and domestication. Due to the large total bacterial count and high acitive, the immobilized microorganism exhibited high degradation efficiency for the COD, BOD and NH3-N, which was81%,81%and75%, respectively. The performance of carbon foams-based biofilm was superior to those of bioceramic particles significantly, revealing the good biocompatibility of carbon foams.
本论文针对泡沫炭的孔结构控制和自发泡、超临界发泡机理以及石墨化泡沫炭微裂纹的产生机制,形成了较具特色的研究,并得出如下主要结论：
1)以中间相沥青为原料,采用自发泡技术,制得结构可控的中大孔泡沫炭,系统考察了中间相沥青的性质、自发泡条件、炭化、石墨化工艺对泡沫炭孔结构的影响。通过对中间相沥青进行预氧化,结合沥青的簇组成及其粘-温特性,推断自发泡机理如下：在发泡温度下,中间相沥青中的轻组分或裂解气将优先在喹啉不溶物(QI组分)处成核、聚集和膨胀,然后形成泡孔；在升温至发泡温度的过程中,当沥青内部由裂解产生气体的压力高于外界压力时,部分气体在内外压差的作用下从沥青内部逸出,导致泡沫炭的开孔率较高。
2)以甲苯为发泡剂,采用超临界发泡制得孔径为100-200μm的泡沫炭,并结合不同工艺条件对泡沫炭的结构进行了有效调控,推断发泡机理如下：在超临界条件下,当甲苯和中间相沥青形成均相体系后,在快速卸压过程中,溶解在中间相沥青中的甲苯处于过饱和状态,进而与熔融沥青分相：由于轻组分/QI界面处的Gibbs自由能比沥青主体相要低,于是甲苯则优先在轻组分/QI界面处成核,并逐渐扩散、聚集和膨胀,最终形成泡孔。
3)通过调控不同程度萃取的中间相沥青的簇组成,考察不同石墨化泡沫炭微裂纹结构,推断其产生机制如下：泡沫炭在石墨化过程中,由于孔壁及韧带处存在热应力梯度分布,导致热应力的释放速度不同,进而产生微裂纹。其中,微裂纹的产生及其形状与石墨化过程中产生的热应力、热应力的释放速度和碳基体的物理性质有关。通过调节中间相沥青的族组成可以有效控制石墨化泡沫炭微裂纹的产生。
4)协同超声和磁力搅拌分散功效,实现了CNTs在中间相沥青中的均匀分散,并成功自发泡制备出CNT增强的泡沫炭。当CNTs分散量为3.5wt.%时,所制泡沫炭孔结构的均一性最好,压缩强度达4.7MPa。
5)泡沫炭经HNO3适当氧化后,孔壁表面形成新的中孔、大孔,并有效的改进了其界面的亲水性,从而有利于金属催化剂的均匀分散；通过化学气相沉积法,可以在改性泡沫炭表面均匀生长一层致密的纳米碳纤维,在不影响泡沫炭的孔结构和强度的同时,大大增强了材料的有效界面,从而有利于MnOx-CeO2纳米催化剂在泡沫炭界面的高度分散。MnOx-CeO2/CNFs-泡沫炭催化剂具有极高的NO的催化脱除能力,在180-220℃范围内,对NO的脱硝效率可以达到90%以上。
6)泡沫炭经过HNO3氧化、水洗、生物接种、生物驯化之后,成功的在其表面生长出致密的高活性生物膜。生物菌种类和数量较多,对多种污水成分具有一定的普适性降解效果。其中,生物泡沫炭对COD、BOD和NH3-N等典型污染物降解率分别高达81%、81%和75%,明显优越于生物陶瓷颗粒,揭示了泡沫炭良好的生物相容性和作为微生物固定化载体的应用前景。
Carbon foams, which exhibit an interconnected structure and a large porosity made up of macrospores, are important in many areas of modern science and technology, including aerospace, heat exchanger, catalyst support and electrode material due to their remarkable properties, such as low density, high open-cell ratio, low coefficient of thermal expansion, resistance to corrosion, easy machining and other superior performances. However, the tailor of pore architecture and enforcement of mechanical performance of carbon foams for some special application were still a challenging task. This therefore, calls for research into more economic and effecitive ways to prepare high qulitiy carbon foams with controlled structure and porperties. In this thesis, we focused on these issues and developed two methods (self-foaming and supercritical foaming) to foam mesophase pitch. The pore texture (pore shape, pore size, ligament structure, and opening/closing pore) and mechanical properties have been systematically investigated by adjusting the physical chemistry parameters of mesophase pitch, self-foaming and supercritical foaming conditions. The mechanisms of self-foaming and supercritical foaming were clarified and the occurrence of micro-cracks in graphitized carbon foams was explained. Meanwhile, the applications of carbon foams in gas-solid catalysis and the water treatment were also preliminarily studied.
The major innovations of the thesis were from three aspects:tailoring of pore structure (especially pore range from10to200μm), the mechanism of self-foaming and supercritical foaming and the foming mechanism for the micro-crack in the matrix. The main research contents are summaried as follows.
1) Carbon foams with pore size of100to600μm were prepred by self-foaming approach, using mesophase pitches as precusors. The pore control has been systematically studied. The mechanisms of self-foaming have been revealed. Under the foaming temperature, the light molecular or pyrolysis gas released from the mesophase pitch were formed a core around the QI component, and then aggregated, grow up and finally became stable pores. During the further heating process, the interior pressure of pitch was higher than the exterior one, resulting in that some volatile materials would be driven and escape from the inner of molten pitch under the pressure difference. As a consequence, some closing pores would turn into opening pores. It was worthy to note that the pressure difference was determined by the amount and the generating rate of the light component.
2) A series of carbon foams with pore size of20-200μm were prepared through supercritical toluene technique. Toluene and mesophase would firstly form a homogeneous phase at the supercritical toluene condition. When the pressure was relieved quickly, toluene should separated from the mixture phase owing to the supersaturate status. Besides the Gibbs freedom energy of interface between QI and light components was lower than that of pitch matrix, the toluene would prefer to form the core at the interface, then diffusion, coalescence, growing up and finally turned into pores.
3) During the graphitization process, the thermal stress and its gradient distribution along the pore wall and ligament would lead to the occurrence of micro-cracks. The texture and shape of the micro-cracks was greatly detemined by the thermal stress, the release rate and the properties of the precursor carbons. The micro-cracks could be controlled to some content by adusting the composition of the precursor mesophase pitch.
4) The homogenous dispersion of CNTs in the mesophase pitch was realized through the ultrasonic wave combined with magnetic stirring method. When the mass concentration of CNTs was3.5%, the as-prepared carbon foams owned uniform pore distribution, and the strength of pore wall was greatly enhanced and the amount of micro-cracks was greatly reduced. The compression strength was as high as4.7MPa.
5) A certain amount of mesopore and macropore was created when the carbon foams were subjected to HNO3oxidaiton treatment. The oxidation could improve the hydrophilic properties, which was beneficial for the dispersion of metal catalysis. After impregnated with metal nanoparticles, carbon nanofiber could be grown on the surface of carbon foams through CVD technique, which could effectively increase the external surface area without the loss of the pore structure. MnOx-CeO2hybird oxides could be homogeneously supported on the CNFs/carbon foams composites for NO removal. When the temperature was in the range of180-220℃, the removal efficiency of NO was as high as90%.
6) The hydrophilic surface of carbon foams would be obtained by mild HNO3oxidaiton. The active bacteria could be immobilized on the surface of oxidized carbon foams after the bacterination and domestication. Due to the large total bacterial count and high acitive, the immobilized microorganism exhibited high degradation efficiency for the COD, BOD and NH3-N, which was81%,81%and75%, respectively. The performance of carbon foams-based biofilm was superior to those of bioceramic particles significantly, revealing the good biocompatibility of carbon foams.
引文
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