纳米氧化锌对中间相炭微球粒径的影响
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摘要
以精制煤沥青为原料,在反应温度、压力和时间一定的条件下研究了添加纳米氧化锌对热缩聚反应得到的中间相炭微球(MCMB)粒径的影响。MCMB的形貌用偏光显微镜和扫描电镜(SEM)进行观察;其晶体结构用X射线衍射仪(XRD)进行表征;比表面积的变化采用电化学工作站分析。结果表明,在反应温度为410℃、时间为4 h和压力为0.5 MPa的条件下,纳米氧化锌的加入可使MCMB粒径变小、粒径分布范围变窄以及产率提高,但石墨化度降低;而且,纳米氧化锌的添加比例对MCMB粒径的影响程度不同,随着氧化锌添加比例的增大,MCMB粒径减小的程度变得越来越小,分布范围更窄。此外,对形成MCMB的机理及出现的实验现象进行了分析和讨论。该研究为制备粒径分布范围窄、粒径小且产率高的MCMB提供了一条新途径。
Mesocarbon microbeads(MCMB) with a narrow size distribution were prepared by means of polymerization at certain reaction temperature, time and pressure. The effect of adding nano-zinc oxide to refined coal tar pitch on the particle size of MCMB was investigated. The morphology of MCMB was observed by polarized optical microscope and SEM. The crystal structure of MCMB was characterized by XRD. The change of specific surface area of MCMB was analyzed by electrochemical workstation. The results reveal that the addition of nano-zinc oxide reduces the particle size of MCMB, narrows the size distribution and increases the yield of MCMB at the reaction temperature of 410 ℃ for 4 h under the pressure of 0.5 MPa.. But the addition of nano-zinc oxide reduces graphitization degree of MCMB. And the proportion of nano-zinc oxide has different impacts on particle size of MCMB. With the increase of nano-zinc oxide, the particle size of MCMB becomes small increasingly slowly, but the distribution range of particle size gets narrower. In addition, the possible formation mechanism and experimental phenomena were analyzed and discussed. The research provides a new channel for getting MCMB with small particle size and high yield.
Mesocarbon microbeads(MCMB) with a narrow size distribution were prepared by means of polymerization at certain reaction temperature, time and pressure. The effect of adding nano-zinc oxide to refined coal tar pitch on the particle size of MCMB was investigated. The morphology of MCMB was observed by polarized optical microscope and SEM. The crystal structure of MCMB was characterized by XRD. The change of specific surface area of MCMB was analyzed by electrochemical workstation. The results reveal that the addition of nano-zinc oxide reduces the particle size of MCMB, narrows the size distribution and increases the yield of MCMB at the reaction temperature of 410 ℃ for 4 h under the pressure of 0.5 MPa.. But the addition of nano-zinc oxide reduces graphitization degree of MCMB. And the proportion of nano-zinc oxide has different impacts on particle size of MCMB. With the increase of nano-zinc oxide, the particle size of MCMB becomes small increasingly slowly, but the distribution range of particle size gets narrower. In addition, the possible formation mechanism and experimental phenomena were analyzed and discussed. The research provides a new channel for getting MCMB with small particle size and high yield.
引文
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[16]Hu X B,Cheng G,Zhao B Y,et al.Catalytic effect of dopants on microstructure and performance of MCMB-derived carbon laminations[J].Carbon,2004,42(2):381-386.
[17]Yu G H,Xie X,Pan L J,et al.Hybrid nanostructured materials for high-performance electrochemical capacitors[J].Nano Energy,2013,2(2):213-234.
[18]Zhang X H,Meng X Y,Gong S L,et al.Synthesis and characterization of 3D MnO2/carbon microtube bundle for supercapacitor electrodes[J].Materials Letters,2016,179:73-77.
[2]张永刚,王成扬,闫裴.低温CoCl2催化热处理中间相炭微球用作锂离子电池负极材料[J].新型炭材料,2007,22(1):35-39.
[3]Tokumitsu K,Fujimoto H,Mabuchi A,et al.High capacity carbon anode for Li-ion battery:A theoretical explanation[J].Carbon,1999,37(10):1599-1605.
[4]Zhou C,Mcginn P J.The effect of oxygen on the processing of mesocarbon microbeads to high-density carbon[J].Carbon,2006,44(9):1673-1681.
[5]Norfolk C,Mukasyan A,Hayes D,et al.Processing of mesocarbon microbeads to high-performance materials:Part I.Studies towards the sintering mechanism[J].Carbon,2004,42(1):11-19.
[6]Yokono T,Nakahara M,Makino K,et al.Application of carbon microbeads for column packing for high-performance liquid chromatography[J].Journal of Materials Science Letters,1988,7(8):864-866.
[7]李铁虎,常天杰,冀勇斌,等.活性中间相炭微球的制备及机理研究[J].新型炭材料,2008,23(4):374-377.
[8]Huang C C,Chen Y Z.Electrochemical performance of supercapacitors with KOH activated mesophase carbon microbead electrodes[J].Journal of the Taiwan Institute of Chemical Engineers,2013,44(4):611-616.
[9]Ridham D,Saroj K,Rajeev K,et al.Mesocarbon microsphere composites with Fe3O4nanoparticles for outstanding electromagnetic interference shielding effectiveness[J].RSC Advances,2015,5(54):43279-43289.
[10]朱秋荣,侯文生,史晟,等.碳微球的研究进展[J].化工进展,2014,33(7):1780-1785.
[11]王红强,李新海,郭华军,等.中间相炭微球的结构对其电化学性能的影响[J].中南大学学报(自然科学版),2003,34(2):140-143.
[12]Yang Y J,Lin Q L,Huang Y Q,et al.Efficient preparation of mesocarbon microbeads by pyrolysis of coal-tar pitch in the presence of rosin[J].Journal of Analytical&Applied Pyrolysis,2011,91(2):310-315.
[13]Yang Y S,Wang C Y,Chen M M.Preparation and structure analysis of nano-iron/mesocarbon microbead composites made from a coal tar pitch with addition of fer-rocene[J].Journal of Physics&Chemistry of Solids,2009,70(10):1344-1347.
[14]Li T Q,Wang C Y,Liu X J,et al.Characteristics of mesocarbon microbeads generated from a coal tar pitch with addition of micro-alumina powder[J].Fuel Processing Technology,2005,87(1):77-83.
[15]Cao Q,Xie X L,Li J P,et al.A novel method for removing quinoline insolubles and ash in coal tar pitch using electrostatic fields[J].Fuel,2012,96(7):314-318.
[16]Hu X B,Cheng G,Zhao B Y,et al.Catalytic effect of dopants on microstructure and performance of MCMB-derived carbon laminations[J].Carbon,2004,42(2):381-386.
[17]Yu G H,Xie X,Pan L J,et al.Hybrid nanostructured materials for high-performance electrochemical capacitors[J].Nano Energy,2013,2(2):213-234.
[18]Zhang X H,Meng X Y,Gong S L,et al.Synthesis and characterization of 3D MnO2/carbon microtube bundle for supercapacitor electrodes[J].Materials Letters,2016,179:73-77.