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Structural characterization of semicokes produced from the pyrolysis of petroleum pitches

机译:石油沥青热解产生的半焦的结构表征

摘要

Semicokes obtained from the pyrolysis of petroleum pitches are important materials that are used in the manufacture of many carbonaceous products. Therefore, new structural information of the semi-cokes will extend their utilization. The structural analysis of anisotropic semicokes of the pyrolysis of petroleum pitches obtained under various experimental conditions of temperature and time was investigated. The overall objective is to provide further detailed information of factors which influence formation of anisotropy or turbostratic structures in resultant semicokes. Experiments were carried out under an argon atmosphere at the temperature range of 500-1000 degrees C for 30, 60 and 120 min in a tube furnace. FTIR, H-1-NMR, and C-13 NMR results showed that the aromatic structure of the semicokes was increasing with respect to increasing temperature as well as increasing time. Aromaticity of the semicokes was calculated as 0.54 and 0.64, for Pitch A at 500 degrees C after 120 min, and Pitch B at 600 degrees C after 120 min, respectively. The intensity ratio between Raman "D" and "G" peaks, I-D/I-G (commonly used to characterize disorder in graphene structures) was observed to increase approximately linearly from 0.65 to 0.92 when the pyrolysis temperature of Pitch A was increased from 500 degrees C to 900 degrees C. XRD patterns of the semicokes showed the formation of some crystalline material with time and temperature. The average number of layers, calculated by the Debye-Scherer technique using the XRD patterns of the semicokes, was between 5 and 10. SEM images of the semicokes indicated the presence of turbostratic structures. All the results of characterizations were consistent and indicated the formation of highly amorphous hydrocarbon materials that contain turbostratic structures. Treatments at higher temperatures increased formations of aromatic structure with increased crystallinity. Temperature seemed to be the dominating parameter of the pyrolysis reactions. As the pyrolysis temperature was increased, aromatic structure formation was favored with increased crystallinity in the semicokes. We expect that findings of the present work will open new uses for the anisotropic semicokes obtained from petroleum pitches. The pitches can be widely applied to the templating synthesis of carbon nanostructures and other carbon nanomaterials.
机译:从石油沥青的热解中获得的半焦是用于制造许多含碳产品的重要材料。因此,新的半焦结构信息将扩展其利用。研究了在温度和时间的各种实验条件下获得的石油沥青热解各向异性半焦的结构分析。总体目的是提供影响最终焦炭中各向异性或涡轮层状结构形成的因素的进一步详细信息。在管式炉中在氩气气氛中在500-1000摄氏度的温度范围内进行了30、60和120分钟的实验。 FTIR,H-1-NMR和C-13 NMR结果表明,半焦的芳族结构随温度的升高和时间的增加而增加。对于120分钟后500摄氏度的沥青A和120分钟后600摄氏度的沥青B,半焦的芳香度分别计算为0.54和0.64。当沥青A的热解温度从500摄氏度提高时,观察到拉曼“ D”峰与“ G”峰之间的强度比ID / IG(通常用于表征石墨烯结构的无序)从0.65线性升高至0.92。到900℃。半焦的XRD图表明随着时间和温度的形成一些结晶物质。通过Debye-Scherer技术使用半焦炭的XRD图计算出的平均层数在5到10之间。半焦炭的SEM图像表明存在涡轮层状结构。所有表征结果都是一致的,并表明含有涡轮层状结构的高度无定形烃材料的形成。在较高温度下的处理增加了具有增加的结晶度的芳族结构的形成。温度似乎是热解反应的主要参数。随着热解温度的升高,半焦中的芳族结构形成与结晶度的增加是有利的。我们希望当前工作的发现将为从石油沥青中获得的各向异性半焦开辟新的用途。该沥青可广泛应用于碳纳米结构和其他碳纳米材料的模板合成。

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