FCC油浆溶剂萃取研制针状焦
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摘要
研制石油系针状焦是出于两个目的,一是炼油加工原料油重质化趋势明显加快,无论是对进口原油还是国内生产原油来说,重质油占到40%以上,给炼化企业带来的是结焦问题和产焦量上升,油品产率和产量都受影响,因此说原油的深加工是炼化企业必须面临的十分紧迫的课题;二是近年来我国冶金工业迅速发展,特别是为满足国家节能环保形势的需要,电炉炼钢技术大规模在我国的推广应用,使得对冶金用石墨电极需求大增,也必然带来对石墨电极原料—针状焦需求的大增。因为国内生产针状焦无论质量或数量都不能满足需要,而必须依赖进口。
用催化裂化油浆或乙烯焦油作为制备针状焦的原料,不但使原来作为燃料油的渣油发挥其潜在价值,同时也满足国内对针状焦的需要。本论文正是以糠醛为萃取溶剂,萃取FCC油浆,富集芳烃馏分,并以富芳馏分或与乙烯焦油的调和料作为焦化原料,经过炭化、焦化及煅烧从而制备出了优质针状焦,性能指标达到或超过国外同类产品的水平。本论文主要工作有以下几个方面:
①原料萃取。在连续萃取装置上,进行了不同萃取温度和剂油比萃取条件下的正交实验,结果表明,选择性随剂油比增大而提高,随温度升高而下降;同时随萃取温度升高,抽出油密度减少,相对分子量和氢碳原子比增加。原料中芳烃含量高,萃取效果好。在温度50℃、剂油比2:1情况下,萃取效率最高。通过四组分分析、红外及核磁等手段研究,萃取前后的组分发生很大变化,芳烃由原来52%提高到90%,硫含量由0.36%降低至0.20%,芳碳原子数由9.36提高到16.5,环烷碳原子由6.4提高到8.52。重金属离子含量降低,热解缩聚反应趋于温和。
②通过偏光显微镜、红外和核磁等手段,分析炭化过程中中间相沥青的组成和偏光显微结构变化,研究FCC油浆及其富芳馏分(FCCRF)的热转化行为。结果表明,FLORY公式揭示了小球成型的基本规律,其生长和球体分布变化是内在必然,喹啉不溶物、高粘及多活性中心都将阻止小球的发育。认为压力、温度及原料组成对炭化过程有决定性的影响;虽然它们作用途径不同,但有相互制约的关系。对给定的原料来说,在合适的温度条件下,适当提高压力将有利于中间相及生焦的成型;另外看到,炭化过程是热解和缩聚过程,合适的原料组成是炭素材料制备的前提条件。乙烯焦油和催化裂化富芳烃馏分混合,可以起到共炭化的协同效应。以FCC油浆富芳馏分或其与乙烯焦油混合料为炭化原料,在3.5MPa,400～430℃,6～20hr/500℃, 1.0MPa,3～4hr,惰性气体保护下炭化可以得到优质针状焦。
③借助高温流变仪、偏光显微镜和X射线衍射仪等,研究了催化裂化油浆中间相(FCC-MP)及其富芳馏分中间相(FCCRF-MP)的流变性,试图揭示中间相沥青的显微组织结构和流变性间的关系,结果表明,不但剪切应力影响中间相沥青的显微组织结构,而且,中间相的显微组织结构同样影响体系的流变性能。大融并体流线结构中间相沥青显示更强的非牛顿特征,温度敏感性也更大,表观粘度更低。FCCRF-MP的流变性优于FCC-MP。
④借助X射线衍射、差热分析及红外等手段,对石油焦煅烧前后的晶体结构特征进行了研究,结果表明,用热力学熵函数结合晶格参数分析晶体结构和晶化作用是可行的。煅烧过程既是晶体重排过程也是热解缩聚过程;在晶体重排过程中其有序性增加,表现为熵值减小,颗粒增大;其热解缩聚的结果表现为红外非活性增强。200～700℃是晶化作用的关键阶段。就微观结构来说,1400℃的煅烧温度不足以改变石墨层的堆积状态,表现为d002变化不大,P1很小。
There were two purposes to study and prepare the needle coke, one of which was that the feed crude oil to be refined became heavier. The heavy oil of the imported and domestic crude oil reached over 40%, which increased the petroleum coke yield and lowered the quality of the product. In this view, crude oil's deep processing was the urgent problem for petroleum refinery enterprise. On the other hand, the metallurgical industry has been developed quickly in recent years. The electric furnace steelmaking technique was widely used for the sake of energy saving and environmental protection, which resulted the increasing demand for the needle coke. The needle coke used for preparing ultra high power (UHP) graphite electrode was supplied mainly by importation, because the quality or quantity of domestic needle coke products could not satisfy need. When catalytic cracking slurry or ethylene tar were used as raw material for carbonization, the latent value of residue oil could be raised, and the nation demand on the needle coke could also be satisfied. In this research, FCC slurry was extracted with furfuraldehyde and the aromatic hydrocarbons of FCC were enriched and used as the raw material to produce the high-grade needle coke through carbonization, coking and calcinations processes. The characteristics of the result needle coke reached or exceeded the imported products. The main work of this thesis was shown as follows:
①Feedstock extraction.An orthogonal test for extraction temperature and solvent–oil ratio had been done with a continuous extraction device. The results showed that the selectivity was increased with the increase of solvent–oil ratio and decreased with the temperature rising. At same time, with the temperature rising, the density of the extracted oil was declined but relative molecular weight and H/C value were raised with the temperature. The extraction was efficient due to higher aromaticity of the raw material after extraction. The optimum extraction condition was at 50℃and with the solvent–oil ratio of 2:1. The compositions of feedstock before and after extraction were examined respectively by four-composition analyses, FT-IR and H-NMR analyses etc. The result showed that the aromatic hydrocarbon content and the sulfur content were raised from 52% to 90% and 0.36% to 0.20% respectively. The average number of aromatic carbon atom and naphthenic carbon atom were raised from 9.36 to 16.5 and 6.4 to 8.52 per molecular. The reactivity became mild with the decreasing concentration of heavy metals iron
②Thermal conversion behaviors of FCC slurry and enriched aromatic hydrocarbon.The texture of mesophase pitches had been investigated with polarized microscope, FT-IR and 1H-NMR. Results indicated that the modified FLORY formula revealed the law of growth of Brooks-Taylor spherules, whose development and distribution was inherent necessity, and factors such as the fractions of quinoline insolubles, high viscosity and multi reactive center would all prohibit the growth of the spherules. It was considered that the pressure, temperature as well as the component all influenced the carbonization processes. The factors above showed interacting relations although they had different functions. For given raw material at suitable temperature, the increase of pressure favored the coalescence of mesophase and formation of needle coke. It could be understood that the appropriate composition of raw materials was attained by precondition for the preparation of carbon materials Ethylene tar mixed with FCCRF gives a performance of synergetic effect during carbonization. With conditions of 3.5MPa, 400～430℃, 6～20h and 500℃, 1.0MPa, 3～4h, inert atmosphere, the needle coke could be prepared by carbonization from enriched aromatic hydrocarbon of FCC slurry or its mixture with ethylene tar.
③The rheological properties of mesophase pitches derived from FCC and FCCRF.FCC-MP and FCCRF-MP had been studied with high-temperature rheometer, X-ray diffractometer (XRD) and polarized microscope. Results indicated that the microtexture of mesophase was affected the shearing stress and it also affected the rheological behaviors at the same time. The flow domain masophase pitch showed strong non-Newton rheological properties, larger temperature sensitivities and lower apparent viscosity. FCCRF-MP showed better rheological behavior than that of FCC-MP.
④The characteristics of fresh and calcined coke.The characteristics of fresh and calcined coke had been monitored by differential thermal analysis (DTA), XRD and FT-IR methods. The results showed that combination the entropy function with lattice parameters was a rational way to investigate crystal structure and crystallization. Calcination process was a crystal rearrangement stage as well as a dehydrogenation, polymerizing, aromation process. In the stage of crystal rearrangement, the molecular assembling order degree was increased. The process was appeared the decrease of entropy and increase of the crystal cell size. The temperature band between 200～700℃was the key stage for crystallization. The temperature at 1400℃was not high enough to change the stacking state of graphite layer structure because the value of d002 didn’t change much and P1 was very small.
用催化裂化油浆或乙烯焦油作为制备针状焦的原料,不但使原来作为燃料油的渣油发挥其潜在价值,同时也满足国内对针状焦的需要。本论文正是以糠醛为萃取溶剂,萃取FCC油浆,富集芳烃馏分,并以富芳馏分或与乙烯焦油的调和料作为焦化原料,经过炭化、焦化及煅烧从而制备出了优质针状焦,性能指标达到或超过国外同类产品的水平。本论文主要工作有以下几个方面:
①原料萃取。在连续萃取装置上,进行了不同萃取温度和剂油比萃取条件下的正交实验,结果表明,选择性随剂油比增大而提高,随温度升高而下降;同时随萃取温度升高,抽出油密度减少,相对分子量和氢碳原子比增加。原料中芳烃含量高,萃取效果好。在温度50℃、剂油比2:1情况下,萃取效率最高。通过四组分分析、红外及核磁等手段研究,萃取前后的组分发生很大变化,芳烃由原来52%提高到90%,硫含量由0.36%降低至0.20%,芳碳原子数由9.36提高到16.5,环烷碳原子由6.4提高到8.52。重金属离子含量降低,热解缩聚反应趋于温和。
②通过偏光显微镜、红外和核磁等手段,分析炭化过程中中间相沥青的组成和偏光显微结构变化,研究FCC油浆及其富芳馏分(FCCRF)的热转化行为。结果表明,FLORY公式揭示了小球成型的基本规律,其生长和球体分布变化是内在必然,喹啉不溶物、高粘及多活性中心都将阻止小球的发育。认为压力、温度及原料组成对炭化过程有决定性的影响;虽然它们作用途径不同,但有相互制约的关系。对给定的原料来说,在合适的温度条件下,适当提高压力将有利于中间相及生焦的成型;另外看到,炭化过程是热解和缩聚过程,合适的原料组成是炭素材料制备的前提条件。乙烯焦油和催化裂化富芳烃馏分混合,可以起到共炭化的协同效应。以FCC油浆富芳馏分或其与乙烯焦油混合料为炭化原料,在3.5MPa,400～430℃,6～20hr/500℃, 1.0MPa,3～4hr,惰性气体保护下炭化可以得到优质针状焦。
③借助高温流变仪、偏光显微镜和X射线衍射仪等,研究了催化裂化油浆中间相(FCC-MP)及其富芳馏分中间相(FCCRF-MP)的流变性,试图揭示中间相沥青的显微组织结构和流变性间的关系,结果表明,不但剪切应力影响中间相沥青的显微组织结构,而且,中间相的显微组织结构同样影响体系的流变性能。大融并体流线结构中间相沥青显示更强的非牛顿特征,温度敏感性也更大,表观粘度更低。FCCRF-MP的流变性优于FCC-MP。
④借助X射线衍射、差热分析及红外等手段,对石油焦煅烧前后的晶体结构特征进行了研究,结果表明,用热力学熵函数结合晶格参数分析晶体结构和晶化作用是可行的。煅烧过程既是晶体重排过程也是热解缩聚过程;在晶体重排过程中其有序性增加,表现为熵值减小,颗粒增大;其热解缩聚的结果表现为红外非活性增强。200～700℃是晶化作用的关键阶段。就微观结构来说,1400℃的煅烧温度不足以改变石墨层的堆积状态,表现为d002变化不大,P1很小。
There were two purposes to study and prepare the needle coke, one of which was that the feed crude oil to be refined became heavier. The heavy oil of the imported and domestic crude oil reached over 40%, which increased the petroleum coke yield and lowered the quality of the product. In this view, crude oil's deep processing was the urgent problem for petroleum refinery enterprise. On the other hand, the metallurgical industry has been developed quickly in recent years. The electric furnace steelmaking technique was widely used for the sake of energy saving and environmental protection, which resulted the increasing demand for the needle coke. The needle coke used for preparing ultra high power (UHP) graphite electrode was supplied mainly by importation, because the quality or quantity of domestic needle coke products could not satisfy need. When catalytic cracking slurry or ethylene tar were used as raw material for carbonization, the latent value of residue oil could be raised, and the nation demand on the needle coke could also be satisfied. In this research, FCC slurry was extracted with furfuraldehyde and the aromatic hydrocarbons of FCC were enriched and used as the raw material to produce the high-grade needle coke through carbonization, coking and calcinations processes. The characteristics of the result needle coke reached or exceeded the imported products. The main work of this thesis was shown as follows:
①Feedstock extraction.An orthogonal test for extraction temperature and solvent–oil ratio had been done with a continuous extraction device. The results showed that the selectivity was increased with the increase of solvent–oil ratio and decreased with the temperature rising. At same time, with the temperature rising, the density of the extracted oil was declined but relative molecular weight and H/C value were raised with the temperature. The extraction was efficient due to higher aromaticity of the raw material after extraction. The optimum extraction condition was at 50℃and with the solvent–oil ratio of 2:1. The compositions of feedstock before and after extraction were examined respectively by four-composition analyses, FT-IR and H-NMR analyses etc. The result showed that the aromatic hydrocarbon content and the sulfur content were raised from 52% to 90% and 0.36% to 0.20% respectively. The average number of aromatic carbon atom and naphthenic carbon atom were raised from 9.36 to 16.5 and 6.4 to 8.52 per molecular. The reactivity became mild with the decreasing concentration of heavy metals iron
②Thermal conversion behaviors of FCC slurry and enriched aromatic hydrocarbon.The texture of mesophase pitches had been investigated with polarized microscope, FT-IR and 1H-NMR. Results indicated that the modified FLORY formula revealed the law of growth of Brooks-Taylor spherules, whose development and distribution was inherent necessity, and factors such as the fractions of quinoline insolubles, high viscosity and multi reactive center would all prohibit the growth of the spherules. It was considered that the pressure, temperature as well as the component all influenced the carbonization processes. The factors above showed interacting relations although they had different functions. For given raw material at suitable temperature, the increase of pressure favored the coalescence of mesophase and formation of needle coke. It could be understood that the appropriate composition of raw materials was attained by precondition for the preparation of carbon materials Ethylene tar mixed with FCCRF gives a performance of synergetic effect during carbonization. With conditions of 3.5MPa, 400～430℃, 6～20h and 500℃, 1.0MPa, 3～4h, inert atmosphere, the needle coke could be prepared by carbonization from enriched aromatic hydrocarbon of FCC slurry or its mixture with ethylene tar.
③The rheological properties of mesophase pitches derived from FCC and FCCRF.FCC-MP and FCCRF-MP had been studied with high-temperature rheometer, X-ray diffractometer (XRD) and polarized microscope. Results indicated that the microtexture of mesophase was affected the shearing stress and it also affected the rheological behaviors at the same time. The flow domain masophase pitch showed strong non-Newton rheological properties, larger temperature sensitivities and lower apparent viscosity. FCCRF-MP showed better rheological behavior than that of FCC-MP.
④The characteristics of fresh and calcined coke.The characteristics of fresh and calcined coke had been monitored by differential thermal analysis (DTA), XRD and FT-IR methods. The results showed that combination the entropy function with lattice parameters was a rational way to investigate crystal structure and crystallization. Calcination process was a crystal rearrangement stage as well as a dehydrogenation, polymerizing, aromation process. In the stage of crystal rearrangement, the molecular assembling order degree was increased. The process was appeared the decrease of entropy and increase of the crystal cell size. The temperature band between 200～700℃was the key stage for crystallization. The temperature at 1400℃was not high enough to change the stacking state of graphite layer structure because the value of d002 didn’t change much and P1 was very small.
引文
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