不同重质渣油中间相沥青的制备
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摘要
原料组成、温度和炭化时间对中间相形成的影响截然不同而又直接相关,为调制出优质的中间相沥青,必须在三者之间找一个平衡关联点。在本实验过程中,考虑芳烃含量、胶质及沥青质含量、炭化温度和炭化反应时间对中间相沥青制备的影响。
将轻芳烃和重芳烃分别加入反应釜,在常压下,氮气吹扫,带走反应产生的轻组分。常压下,温度设定180℃/h升温速率升温至400℃,在不断搅拌的前提下,炭化反应8h。将轻芳烃和芳烃分别加入反应釜,在常压下,氮气吹扫,带走反应产生的轻组分。常压下,温度设定180℃/h升温速率升温至400℃,在不断搅拌的前提下,炭化反应8h。轻芳烃原料,常压条件, 380℃、400℃、420℃,炭化时间8h。轻芳烃原料,常压条件, 400℃炭化反应时间4h、6h、8h、10h。上述条件下制备的中间相沥青在偏光显微镜下进行观察分析。
取出固化后的样品,首先加水用耐水粗磨纸进行粗磨,用粗磨纸将样品磨平之后,再用砂纸(金相)进行细磨,最后再用抛光机将细磨后的样品进行抛光处理直至样品光亮,这样中间相样品就处理完成,就可以在偏光显微镜之下进行观察。
轻芳烃具有芳烃含量高,饱和烃含量低,胶质沥青质含量低的特点,是制备中间相沥青的优质原料,适宜的温度400℃,适宜的炭化时间8h。
Raw material composition, temperature and carbonization time among the influence of phase formation of different and directly related to modulation of high quality, of mesophase pitch, must find a balance between the different connection spot. In this experiment process, considering aromatic content, gelatin and bituminous content, carbonization temperature and carbonization reaction time on the influence of mesophase pitch preparation.
Will light aromatics and heavy aromatics adds the reaction kettle in the atmosphere, nitrogen purging, take away the reaction that produces light component. Atmospheric pressure, temperature setting 180℃/h and 400℃temperature heating rate, stirring constantly, under the precondition of carbonization reaction. Will light aromatics and aromatic reaction kettle, respectively, to join in the atmosphere, nitrogen purging, take away the reaction that produces light component. Atmospheric pressure, temperature setting 180℃/h and 400℃temperature heating rate, stirring constantly, under the precondition of carbonization reaction Light aromatics raw materials, atmospheric conditions,380℃and 400℃, 420℃, carbonized time. Light aromatics raw materials, atmospheric conditions, 400℃carbonization reaction time 4h, 6h, 10h, The above conditions in the preparation of mesophase pitch under polarizing microscope observation analysis.
Remove after curing samples, first add water use water resistant coarse grinding the coarse grinding with paper, paper will sample the coarse grinding whet flat, then sanded (metallographic) fine grinding, final reoccupy polishing machine will fine grinding the samples after polishing among brightness, so until samples in sample is complete the processing, it can be performed under the polarizing microscope observation. Light aromatics with aromatic content saturated hydrocarbon content high, low, the colloid bituminous content low characteristic, is preparation mesophase pitch of high quality raw materials, appropriate temperature 400℃, the suitable carbonized time.
将轻芳烃和重芳烃分别加入反应釜,在常压下,氮气吹扫,带走反应产生的轻组分。常压下,温度设定180℃/h升温速率升温至400℃,在不断搅拌的前提下,炭化反应8h。将轻芳烃和芳烃分别加入反应釜,在常压下,氮气吹扫,带走反应产生的轻组分。常压下,温度设定180℃/h升温速率升温至400℃,在不断搅拌的前提下,炭化反应8h。轻芳烃原料,常压条件, 380℃、400℃、420℃,炭化时间8h。轻芳烃原料,常压条件, 400℃炭化反应时间4h、6h、8h、10h。上述条件下制备的中间相沥青在偏光显微镜下进行观察分析。
取出固化后的样品,首先加水用耐水粗磨纸进行粗磨,用粗磨纸将样品磨平之后,再用砂纸(金相)进行细磨,最后再用抛光机将细磨后的样品进行抛光处理直至样品光亮,这样中间相样品就处理完成,就可以在偏光显微镜之下进行观察。
轻芳烃具有芳烃含量高,饱和烃含量低,胶质沥青质含量低的特点,是制备中间相沥青的优质原料,适宜的温度400℃,适宜的炭化时间8h。
Raw material composition, temperature and carbonization time among the influence of phase formation of different and directly related to modulation of high quality, of mesophase pitch, must find a balance between the different connection spot. In this experiment process, considering aromatic content, gelatin and bituminous content, carbonization temperature and carbonization reaction time on the influence of mesophase pitch preparation.
Will light aromatics and heavy aromatics adds the reaction kettle in the atmosphere, nitrogen purging, take away the reaction that produces light component. Atmospheric pressure, temperature setting 180℃/h and 400℃temperature heating rate, stirring constantly, under the precondition of carbonization reaction. Will light aromatics and aromatic reaction kettle, respectively, to join in the atmosphere, nitrogen purging, take away the reaction that produces light component. Atmospheric pressure, temperature setting 180℃/h and 400℃temperature heating rate, stirring constantly, under the precondition of carbonization reaction Light aromatics raw materials, atmospheric conditions,380℃and 400℃, 420℃, carbonized time. Light aromatics raw materials, atmospheric conditions, 400℃carbonization reaction time 4h, 6h, 10h, The above conditions in the preparation of mesophase pitch under polarizing microscope observation analysis.
Remove after curing samples, first add water use water resistant coarse grinding the coarse grinding with paper, paper will sample the coarse grinding whet flat, then sanded (metallographic) fine grinding, final reoccupy polishing machine will fine grinding the samples after polishing among brightness, so until samples in sample is complete the processing, it can be performed under the polarizing microscope observation. Light aromatics with aromatic content saturated hydrocarbon content high, low, the colloid bituminous content low characteristic, is preparation mesophase pitch of high quality raw materials, appropriate temperature 400℃, the suitable carbonized time.
引文
[1]张忠清,陶宗乾.重渣油加氢过程反应特征和技术特点[J].石油学报(石油加工), 1994,(9),10,(3):1-9
[2]汪道明.多环芳烃树脂的制备性能及应用[J].石油石化,2001(3):235-235
[3]查庆芳.催化裂化油浆溶剂抽提及中间相沥青[J].碳素技术,2001(2):1-5
[4]史权.催化裂化油浆及其窄馏分芳烃组成分析[J].石油学报(石油加工)2000,16 (2):90-94
[5]张荣德,刘淑琼,范耀华.几种薄膜烘箱试验方法对沥青性质的影响.石油沥青, 1992,(2):27-29
[6]丁国靖,范耀华.石油沥青及组分吸氧性能研究.石油炼制,1991,(8):33-35
[7]水恒福,冯映桐.不同喹啉不溶物的特性及其对中间相转化过程的影响[J].燃料化学学报,1995(3),23(1):62-67
[8]李玉财,魏中振等.针状焦的工业化生产[J].市场资讯,2002,[13]
[9]薛锐生,沈曾民.中间相沥青微球的活化[J].炭素技术,2001(5):1-4
[10]宋怀河,刘朗等.合成中间相沥青[J].炭素技术,1994,6:24-29
[11]张静棣.中间相沥青制镁碳砖结合剂软化点的测定[J].梅山科技,1997,1:20-22
[12]史景力,冀勇,查庆芳.中问相沥青流变性的研究[J].炭素技术,1990,2:6-10
[13]彭颖,刘朗,沈曾民.新中间相沥青的制取和性质的研究[J].石油学报(石油加工)
[14]冯德胜,刘洪国,郝京诚.胶体化学[M].北京:化学工业出版社,2005:121-130
[15]李美荣,李新贵.中间相沥青的制备与应用[J].石油学报,1998,28 :62-66
[16]商红岩,韩哲茵,查庆芳.中间相沥青显微结构的研究[J].石油沥青,1998(6),18(2):25-29
[17]李志.煤焦油沥青的利用.六盘水师专学报(自然科学版),1996,4:63-64
[18]宋怀河,刘朗.沥青-重油共炭化机理的研究:Ⅱ共炭化反应前后结构分析共炭化结构的推断[J].燃料化学学报,1994(6),22(2):164-168.
[19]张家埭.炭材料工程基础[M].冶金工业出版社,1992.87-125
[20]赵瑶兴,宋祥玉.光谱解析与有机结构鉴定[M].天津科技出版社,1981.99-100
[21]李兆敏.非牛顿流体力学[M].东营:石油大学出版社,1998.34-41
[22]商红岩,查庆芳,钱树安,中间相沥青可溶组分的结构表征[J].新型炭材料料,1999,(6),14(2):32-38
[23]关德林译.晶体的高温塑性变形[M].大连:大连理工大学出版社,1989.2-11
[24]王长安,吴育良,许凯.影响乳化沥青稳定性的主要因素[M].新型炭料,2005,32(1):52-54
[25]卢永权,邓正华.实用红外光谱解析[M].合肥:中国科技大学出版社,1992
[26]史景利,刘朗,查庆芳.沥青流变性质的研究方法[J].炭素技术,1996,15(3):18-23
[27]刘智强,丁宗禹.高液体收率焦化技术的进展[J].炼油设计,1997,27(1):7-9
[28]高凤萍.国外针状焦的质量现状分析[J].炭素技术,2003,(1):27-31
[29]许斌.中间相沥青[J].炭素技术,2000,(6),10(2):14-24
[17] Peng Y. Schobert H H, Song et al.PriprintsSymposia (Div of Petro Chem of ACS), 1992, 37(2): 505
[31] Peter J. Pappano et al, Dependence of physical properties of isostatically molded on crystallite height. Carbon , 2004, 42 : 3003-3042
[32] Savage P E, Jacobs G E, Javanmardiam M Ind Eng Chem Res, 1989, 28(6): 645
[33] P.Glogar, et al. Factor analysis of physical properties of electrode graphite. Carbon, 1992, 30(2): 129-134
[34] F. Rodriguez-Reinoso. et al, Pyrolysis of petroleum reduesⅣ: Kinetics of pyrolysis. Carbon, 2001, 39(1): 222-234
[35] E. A. Heintz. et al, Effect of calcinations rate on petroleum coke properties. Carbon, 1995 , 33(6): 817-820
[36] F. Rodriguez-Reinoso et al, Delayed: Industrial and laboratory aspects. Carbon, 1998,36 (1): 105-116
[37] E. A. Heintz. et al, Review: The characterization of petroleum coke. Carbon, 1996, 34(6): 699-709
[38] P.glogar.et al, Factor analysis of chemcal physical propertyof eletrode graphite. Carbon[J],1992 ,30(2):129-134
[39] S. J. Park, B. J. Kim, Ammonia removal of activated carbon fibers produced by oxyfluorination, J. Colloid Interf. Sci. 291(2005): 597-599
[40] S. J. Park, S. Y. Jin. Effect of ozone treatment on ammonia removal of activated carbon, J. Colloid Interf. Sci. 286(2005): 417-419
[41] Nazem F F. Flow of molten masophase pitch[J]. Carbon, 1982, 20 (4): 345-358
[42] G. H. Tayloy, G. M. Pennock. Carbon, 1993, 31 (2): 341-354
[43] March H, Latham C S, Gray E M. Carbon, 1985, 23(5): 555
[44] Rand B. Petroleum derived carbons[C].Washington:ACS Symposium Series 303, 1986
[45] Anthony D. Cato, Dan D. Edie. F low behavior of mesophase pitch[J]. Carbon , 2003, 41: 1411–1417
[46] Fitzer E, Kompalik D, Yudate K. Rheological characterization of coal-tar Pitches [J]. Fuel, 1987, 66(11): 1505-1512
[47] L. R. Radovic, F. Rodriguez-Reinoso, in: Thrower(Ed.), Chemistry and Physics of Cabon, vol. 25, Dekker, New York, 1997, p. 243
[2]汪道明.多环芳烃树脂的制备性能及应用[J].石油石化,2001(3):235-235
[3]查庆芳.催化裂化油浆溶剂抽提及中间相沥青[J].碳素技术,2001(2):1-5
[4]史权.催化裂化油浆及其窄馏分芳烃组成分析[J].石油学报(石油加工)2000,16 (2):90-94
[5]张荣德,刘淑琼,范耀华.几种薄膜烘箱试验方法对沥青性质的影响.石油沥青, 1992,(2):27-29
[6]丁国靖,范耀华.石油沥青及组分吸氧性能研究.石油炼制,1991,(8):33-35
[7]水恒福,冯映桐.不同喹啉不溶物的特性及其对中间相转化过程的影响[J].燃料化学学报,1995(3),23(1):62-67
[8]李玉财,魏中振等.针状焦的工业化生产[J].市场资讯,2002,[13]
[9]薛锐生,沈曾民.中间相沥青微球的活化[J].炭素技术,2001(5):1-4
[10]宋怀河,刘朗等.合成中间相沥青[J].炭素技术,1994,6:24-29
[11]张静棣.中间相沥青制镁碳砖结合剂软化点的测定[J].梅山科技,1997,1:20-22
[12]史景力,冀勇,查庆芳.中问相沥青流变性的研究[J].炭素技术,1990,2:6-10
[13]彭颖,刘朗,沈曾民.新中间相沥青的制取和性质的研究[J].石油学报(石油加工)
[14]冯德胜,刘洪国,郝京诚.胶体化学[M].北京:化学工业出版社,2005:121-130
[15]李美荣,李新贵.中间相沥青的制备与应用[J].石油学报,1998,28 :62-66
[16]商红岩,韩哲茵,查庆芳.中间相沥青显微结构的研究[J].石油沥青,1998(6),18(2):25-29
[17]李志.煤焦油沥青的利用.六盘水师专学报(自然科学版),1996,4:63-64
[18]宋怀河,刘朗.沥青-重油共炭化机理的研究:Ⅱ共炭化反应前后结构分析共炭化结构的推断[J].燃料化学学报,1994(6),22(2):164-168.
[19]张家埭.炭材料工程基础[M].冶金工业出版社,1992.87-125
[20]赵瑶兴,宋祥玉.光谱解析与有机结构鉴定[M].天津科技出版社,1981.99-100
[21]李兆敏.非牛顿流体力学[M].东营:石油大学出版社,1998.34-41
[22]商红岩,查庆芳,钱树安,中间相沥青可溶组分的结构表征[J].新型炭材料料,1999,(6),14(2):32-38
[23]关德林译.晶体的高温塑性变形[M].大连:大连理工大学出版社,1989.2-11
[24]王长安,吴育良,许凯.影响乳化沥青稳定性的主要因素[M].新型炭料,2005,32(1):52-54
[25]卢永权,邓正华.实用红外光谱解析[M].合肥:中国科技大学出版社,1992
[26]史景利,刘朗,查庆芳.沥青流变性质的研究方法[J].炭素技术,1996,15(3):18-23
[27]刘智强,丁宗禹.高液体收率焦化技术的进展[J].炼油设计,1997,27(1):7-9
[28]高凤萍.国外针状焦的质量现状分析[J].炭素技术,2003,(1):27-31
[29]许斌.中间相沥青[J].炭素技术,2000,(6),10(2):14-24
[17] Peng Y. Schobert H H, Song et al.PriprintsSymposia (Div of Petro Chem of ACS), 1992, 37(2): 505
[31] Peter J. Pappano et al, Dependence of physical properties of isostatically molded on crystallite height. Carbon , 2004, 42 : 3003-3042
[32] Savage P E, Jacobs G E, Javanmardiam M Ind Eng Chem Res, 1989, 28(6): 645
[33] P.Glogar, et al. Factor analysis of physical properties of electrode graphite. Carbon, 1992, 30(2): 129-134
[34] F. Rodriguez-Reinoso. et al, Pyrolysis of petroleum reduesⅣ: Kinetics of pyrolysis. Carbon, 2001, 39(1): 222-234
[35] E. A. Heintz. et al, Effect of calcinations rate on petroleum coke properties. Carbon, 1995 , 33(6): 817-820
[36] F. Rodriguez-Reinoso et al, Delayed: Industrial and laboratory aspects. Carbon, 1998,36 (1): 105-116
[37] E. A. Heintz. et al, Review: The characterization of petroleum coke. Carbon, 1996, 34(6): 699-709
[38] P.glogar.et al, Factor analysis of chemcal physical propertyof eletrode graphite. Carbon[J],1992 ,30(2):129-134
[39] S. J. Park, B. J. Kim, Ammonia removal of activated carbon fibers produced by oxyfluorination, J. Colloid Interf. Sci. 291(2005): 597-599
[40] S. J. Park, S. Y. Jin. Effect of ozone treatment on ammonia removal of activated carbon, J. Colloid Interf. Sci. 286(2005): 417-419
[41] Nazem F F. Flow of molten masophase pitch[J]. Carbon, 1982, 20 (4): 345-358
[42] G. H. Tayloy, G. M. Pennock. Carbon, 1993, 31 (2): 341-354
[43] March H, Latham C S, Gray E M. Carbon, 1985, 23(5): 555
[44] Rand B. Petroleum derived carbons[C].Washington:ACS Symposium Series 303, 1986
[45] Anthony D. Cato, Dan D. Edie. F low behavior of mesophase pitch[J]. Carbon , 2003, 41: 1411–1417
[46] Fitzer E, Kompalik D, Yudate K. Rheological characterization of coal-tar Pitches [J]. Fuel, 1987, 66(11): 1505-1512
[47] L. R. Radovic, F. Rodriguez-Reinoso, in: Thrower(Ed.), Chemistry and Physics of Cabon, vol. 25, Dekker, New York, 1997, p. 243