在超临界二氧化碳体系中处理废弃塑料制备碳材料的研究
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摘要
废弃塑料产生的“白色污染”对生态环境和人类的生存带来污染和多种潜在危害。对废弃塑料进行回收再利用,将会大大节约能源和原材料,缓解社会的生态压力,实现可持续发展。由于塑料种类混杂,而目前的塑料分类技术效率太低,导致难以实现经济可行的回收。因此,需要开发一种广谱有效的工艺可以兼顾各种不同塑料的处理,并能生产出高附加值的碳材料,进而可最大限度地利用废弃塑料。在本论文中,笔者将超临界二氧化碳(scCO2)体系用于废弃塑料(主要是PET、PP、PE)和废弃油脂(地沟油)的回收处理以制备碳材料,并探讨其作为锂离子电池电极材料应用的可行性。
开发了一种在超临界C02体系中处理废弃PET制备碳微球的工艺。碳微球产物的石墨化程度、分散性和产率与反应温度及时间成正相关。最佳反应条件是650℃反应3h,碳微球产率可达28.0%。超临界C02体系中PET前驱物分解为联苯、甲苯等小分子芳香烃,并进一步脱氢碳化聚合生成碳微球结构。制备的碳微球在电流100mA/g的条件下,首次放电容量达504.9mAh/g,充电容量为258.5mAh/g,二十次循环后仍然可达初次放电的40%。通过混酸超声湿氧化处理,可以使碳微球做成的电极20次循环后容量提高21.9%,预计高温石墨化处理可使其储锂性能变得更好,有可能应用于锂离子电池电极。添加催化剂可改变产物的形貌。碳微球经1500℃退火氧化处理后出现两种形貌,层状碳微球和各向同性的多孔结构,反映了碳产物内部结构的差别。
将废弃聚烯烃PP或PE在scCO2体系中650℃反应3h均获得分散均匀的碳微球产物,产率分别可达42.0%和43.5%。1500℃退火氧化处理可使碳微球变为层状结构,这种碳微球只有这一种结构。用Hummers方法进一步氧化和退火后的碳微球产物变成椭球型层状结构,理论上分析了形成机制。
开发了一种在scCO2体系下直接裂解废弃食用油(地沟油)获得碳微球的工艺技术,可以用于废弃油类,地沟油等处理。碳微球产物呈球形、纺锤形或者卵形。600℃时,碳微球产率最高可达42.2wt%,这时二氧化碳使用量为14g。在1300-1500℃下进一步真空退火后发现,碳微球内部其实是由石墨碳层沿轴线层层堆叠而成。获得这种层状碳微球的最佳条件是在600℃下反应6h,然后再将碳微球置于1500℃真空退火1-2h。这种碳微球和层状多孔碳微球在电极,化学储能,色谱分离技术和润滑等领域有应用潜力。
分别用金属钠、钾和锂在480-500℃还原scCO2,制备了多孔碳材料,比表面积为110.9-571.6m2g-1,孔径3.88-3.94nm。笔者提出了碱金属纳米液滴以自身为还原剂和模板形成多孔结构的机制。利用铜带融化实验检测釜中实际的反应温度,发现实际反应温度远高于设定温度,这个发现有助于对碱金属-scCO2体系反应机理的了解。经测量,这种多孔碳材料由于比表面积大,首次电化学储锂放电容量巨大,最高为1704mAh/g,20循环后,放电容量为200mAh/g,但不可逆容量过多。不过有望通过提高石墨化程度或复合过渡金属氧化物提高储锂性能。
The "white pollution" caused by waste plastic brings heavy pollution and a variety of potential hazards on the ecological environment and human survival. Recycling of waste plastic will be, significant in savings energy and materials, helpful to reduce the ecological pressure and achieve sustainable development. As the complexity of the plastic mixtures, current sorting techniques are inefficient for economically feasible recycling. Therefore, a general approach which is compatible with different kinds of plastics to generate value-added products is important. Here in this dissertation, supercritical carbon dioxide (SC-CO2) was used in processing waste plastics (mainly including PET, PP and PE), as well as discarded oil (cooking oil) to produce novel carbon materials.
A simple chemical route to prepare carbon microspheres by pyrolyzing PET waste in a SC-CO2system has been illustrated. The graphitization of carbon products is mainly determined by the reaction time and temperature. A higher temperature tends to generate a higher yield of solid carbon product. The spherical particles were obtained with a carbon yield as high as28%at650℃for3h. It is found that the SC-CO2system favors the dissociation of the PET precusor to aromatic hydrocarbons, which further decompose to yield carbon spheres. The material exhibits a first discharge capacity of504.9(mA h)/g at a constant current density of100mA/g and maintains a capacity retention of40%after the20th cycle. The acid-mixture-sonicate process could improve22%higher of the capacity. An annealing-oxidation at1500℃leads to the microspheres from PET converting into two distinctive structures, layer-by-layer stacking and porous golf ball structure.
Carbon microspheres were also synthesized by pyrolyzing PP or PE wastes in a SC-CO2system. The yield of Carbon microspheres was42.0%and43.5%, respectively. An annealing-oxidation treatment at1500℃results in carbon microspheres from PP or PE converting into layer-by-layer stacking structure. The layer-by-layer stacking carbon microspheres were further changed into layer-by-layer stacking carbon microellipses by treatment via a Hummers-Method.
A simple route for efficient production of carbon microspheres by direct pyrolysis of discarded oil in a scCO2system was demonstrated. The solid carbon product was obtained in spherical, filament-or egg-like morphologies. The yield of solid carbon reached42.2wt%when the treatment was conducted at600℃using14g dry ice. Moreover, microspheres formed by layer-by-layer stacking were obtained after further vacuum annealing at1300-1500℃. The optimal conditions for producing high-yield layer-structured carbon spheres were600℃for6h, followed by annealing at1500℃for1-2h. Also, microporous carbon spheres have potential for use in electrodes, chemical energy storage, separation technologies, and lubricants.
It was found that the carbon materials formed by reduction of scCO2with alkali metals (Na, K, and Li) demonstrate porous structure with an average pore size of3.88-3.94nm and surface area of110.9-571.6m2g-1. A formation mechanism was proposed that nanodroplets of alkali metals take the roles both as reductants for CO2reduction to carbon and as templates for the production of porous carbon. It was found the actual reaction temperature was much higher than the oven temperature, it helps to get deeper understanding of the reaction of alkali metals-scCO2system. Porous carbon as anode material of lithium ion batteries was tested. The first discharge capacity for the porous carbon reaches1704mAh/g, which is ascribed to its large pore volume providing abundant space to catch Li ions. After20discharge-charge cycles, the discharge capacity stabilizes at200mAh/g, the large irreversible capacity is mainly due to the formation of SEI film on the surface of the electrode material during the first charge-discharge process. It is suggested that further graphitization of the porous carbon materials could lead to better electrochemical performance.
开发了一种在超临界C02体系中处理废弃PET制备碳微球的工艺。碳微球产物的石墨化程度、分散性和产率与反应温度及时间成正相关。最佳反应条件是650℃反应3h,碳微球产率可达28.0%。超临界C02体系中PET前驱物分解为联苯、甲苯等小分子芳香烃,并进一步脱氢碳化聚合生成碳微球结构。制备的碳微球在电流100mA/g的条件下,首次放电容量达504.9mAh/g,充电容量为258.5mAh/g,二十次循环后仍然可达初次放电的40%。通过混酸超声湿氧化处理,可以使碳微球做成的电极20次循环后容量提高21.9%,预计高温石墨化处理可使其储锂性能变得更好,有可能应用于锂离子电池电极。添加催化剂可改变产物的形貌。碳微球经1500℃退火氧化处理后出现两种形貌,层状碳微球和各向同性的多孔结构,反映了碳产物内部结构的差别。
将废弃聚烯烃PP或PE在scCO2体系中650℃反应3h均获得分散均匀的碳微球产物,产率分别可达42.0%和43.5%。1500℃退火氧化处理可使碳微球变为层状结构,这种碳微球只有这一种结构。用Hummers方法进一步氧化和退火后的碳微球产物变成椭球型层状结构,理论上分析了形成机制。
开发了一种在scCO2体系下直接裂解废弃食用油(地沟油)获得碳微球的工艺技术,可以用于废弃油类,地沟油等处理。碳微球产物呈球形、纺锤形或者卵形。600℃时,碳微球产率最高可达42.2wt%,这时二氧化碳使用量为14g。在1300-1500℃下进一步真空退火后发现,碳微球内部其实是由石墨碳层沿轴线层层堆叠而成。获得这种层状碳微球的最佳条件是在600℃下反应6h,然后再将碳微球置于1500℃真空退火1-2h。这种碳微球和层状多孔碳微球在电极,化学储能,色谱分离技术和润滑等领域有应用潜力。
分别用金属钠、钾和锂在480-500℃还原scCO2,制备了多孔碳材料,比表面积为110.9-571.6m2g-1,孔径3.88-3.94nm。笔者提出了碱金属纳米液滴以自身为还原剂和模板形成多孔结构的机制。利用铜带融化实验检测釜中实际的反应温度,发现实际反应温度远高于设定温度,这个发现有助于对碱金属-scCO2体系反应机理的了解。经测量,这种多孔碳材料由于比表面积大,首次电化学储锂放电容量巨大,最高为1704mAh/g,20循环后,放电容量为200mAh/g,但不可逆容量过多。不过有望通过提高石墨化程度或复合过渡金属氧化物提高储锂性能。
The "white pollution" caused by waste plastic brings heavy pollution and a variety of potential hazards on the ecological environment and human survival. Recycling of waste plastic will be, significant in savings energy and materials, helpful to reduce the ecological pressure and achieve sustainable development. As the complexity of the plastic mixtures, current sorting techniques are inefficient for economically feasible recycling. Therefore, a general approach which is compatible with different kinds of plastics to generate value-added products is important. Here in this dissertation, supercritical carbon dioxide (SC-CO2) was used in processing waste plastics (mainly including PET, PP and PE), as well as discarded oil (cooking oil) to produce novel carbon materials.
A simple chemical route to prepare carbon microspheres by pyrolyzing PET waste in a SC-CO2system has been illustrated. The graphitization of carbon products is mainly determined by the reaction time and temperature. A higher temperature tends to generate a higher yield of solid carbon product. The spherical particles were obtained with a carbon yield as high as28%at650℃for3h. It is found that the SC-CO2system favors the dissociation of the PET precusor to aromatic hydrocarbons, which further decompose to yield carbon spheres. The material exhibits a first discharge capacity of504.9(mA h)/g at a constant current density of100mA/g and maintains a capacity retention of40%after the20th cycle. The acid-mixture-sonicate process could improve22%higher of the capacity. An annealing-oxidation at1500℃leads to the microspheres from PET converting into two distinctive structures, layer-by-layer stacking and porous golf ball structure.
Carbon microspheres were also synthesized by pyrolyzing PP or PE wastes in a SC-CO2system. The yield of Carbon microspheres was42.0%and43.5%, respectively. An annealing-oxidation treatment at1500℃results in carbon microspheres from PP or PE converting into layer-by-layer stacking structure. The layer-by-layer stacking carbon microspheres were further changed into layer-by-layer stacking carbon microellipses by treatment via a Hummers-Method.
A simple route for efficient production of carbon microspheres by direct pyrolysis of discarded oil in a scCO2system was demonstrated. The solid carbon product was obtained in spherical, filament-or egg-like morphologies. The yield of solid carbon reached42.2wt%when the treatment was conducted at600℃using14g dry ice. Moreover, microspheres formed by layer-by-layer stacking were obtained after further vacuum annealing at1300-1500℃. The optimal conditions for producing high-yield layer-structured carbon spheres were600℃for6h, followed by annealing at1500℃for1-2h. Also, microporous carbon spheres have potential for use in electrodes, chemical energy storage, separation technologies, and lubricants.
It was found that the carbon materials formed by reduction of scCO2with alkali metals (Na, K, and Li) demonstrate porous structure with an average pore size of3.88-3.94nm and surface area of110.9-571.6m2g-1. A formation mechanism was proposed that nanodroplets of alkali metals take the roles both as reductants for CO2reduction to carbon and as templates for the production of porous carbon. It was found the actual reaction temperature was much higher than the oven temperature, it helps to get deeper understanding of the reaction of alkali metals-scCO2system. Porous carbon as anode material of lithium ion batteries was tested. The first discharge capacity for the porous carbon reaches1704mAh/g, which is ascribed to its large pore volume providing abundant space to catch Li ions. After20discharge-charge cycles, the discharge capacity stabilizes at200mAh/g, the large irreversible capacity is mainly due to the formation of SEI film on the surface of the electrode material during the first charge-discharge process. It is suggested that further graphitization of the porous carbon materials could lead to better electrochemical performance.
引文
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