洁净煤技术

2019, (04) 46-51

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渣油加氢转化过程结焦物分析与表征
Analyzation and characterization of coke in petroleum residue hydro-conversion process

钟金龙;毛学锋;朱肖曼;
ZHONG Jinlong,MAO Xuefeng,ZHU Xiaoman

摘要(Abstract):

渣油加氢过程中易发生结焦现象,生成的结焦物可能会导致装置堵塞、催化剂失活、产物收率降低等。为了防止结焦现象的发生,需揭示结焦物的基本特性,以便为渣油加氢工艺设计、煤油共炼工艺设计、催化剂设计和工业生产提供参考。采用间歇式高压釜装置,模拟工业装置渣油加氢裂化条件,获取渣油加氢裂化的结焦物。采用红外光谱分析(IR)、核磁共振分析(NMR)、热重分析(TG)、X射线衍射分析(XRD)、扫描电镜-能谱仪分析(SEM-EDS)、元素分析等对渣油加氢过程中的结焦物进行分析和表征。结果表明,常压渣油在450℃加氢裂解时,出现结焦现象,氢耗率为2. 19%,气产率为8. 90%,结焦物产率达6. 95%;结焦物的H/C原子比为0. 66,结焦过程发生剧烈的脱氢反应。渣油的芳香环缩合度为0. 699 4,芳碳率为0. 395 6;结焦物的芳香环缩合度为0. 400 5,芳碳率为0. 7695。结焦物中含有大量的芳香环结构,在187℃和584℃失重最为剧烈;结焦物的主要成分是C,还含有少量O、Na、Cl、Ca、V等元素;结焦物呈球状和不规则块状,尺寸为30~50 nm,部分结焦物堆积后呈多孔状,孔径为500~1 000 nm。
Coking occurs easily in the process of residue hydrogenation.The coke might cause a series of harms such as equipment blocking,catalyst deactivation,product yield reduction and so on.To prevent coking,the basic characteristics of the coke is necessary to be revealed,which might provide reference for the design of hydrogenation process,the design of kerosene co-refining process,catalyst design and industrial production.The hydro-cracking conditions of residue in industrial units were simulated by batch-type autoclave and the coke was obtained.The coke in residue hydro-conversion process was analyzed and characterized by using infrared spectroscopy (IR),nuclear magnetic resonance (NMR),thermogravimetric analysis (TG),X-ray diffraction(XRD),scanning electron microscopy-energy dispersive spectrometry (SEM-EDS) and elemental analysis.The results show that the atmospheric residue coked during hydrocracking when the reaction temperature is 450 ℃ and the hydrogen consumption ratio is 2.19%,the gas yield is 8.90%,the coke yield reaches 6.95% and the H/C atomic ratio of the coke is 0.66.Besides,severely dehydrogenated reaction is happened during the coking process.The condensation degree of aromatic nucleus of the residue is 0.699 4 and the aramid-carbon ratio is 0.395 6,the condensation degree of aromatic nucleus of the coke is 0.400 5 and the aramid-carbon ratio is 0.769 5.The coke contains a large amount of aromatic ring structures,and the weight loss of coke is most severe at the temperature of 187 ℃ and 584 ℃.The main component of coke is C and also contains several kinds of elements such as O,Na,Cl,Ca and V.The coke is globular or irregular block in shape,and the size is 30 to 50 nm.Some of the coke accumulates and becomes porous and the size is 500 to 1 000 nm.

关键词(KeyWords): 渣油;加氢转化;结焦;脱氢反应;表征
residue;hydro-conversion;coke deposition;dehydrogenated reaction;characterization

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作者(Author): 钟金龙;毛学锋;朱肖曼;
ZHONG Jinlong,MAO Xuefeng,ZHU Xiaoman

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