渣油加氢体系胶体性质的研究
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摘要
渣油热反应过程中,体系胶体稳定性下降会导致沥青质聚沉,进而生焦。渣油加氢反应过程中伴随着热反应的发生,沥青质在催化剂上聚沉、结焦会造成催化剂迅速失活,影响装置的长周期运转。因此,本文比较系统地研究了不同渣油在不同反应条件下的加氢转化和胶体稳定性。
采用质量分数电导率法考察了分别搀兑催化裂化油浆和减四线抽出油对渣油体系胶体稳定性的影响,发现搀兑催化裂化油浆或减四线抽出油均使渣油体系的稳定性下降。研究表明,馏分油组分与渣油组分极性的差距决定了体系胶体稳定性的变化。
不同渣油加氢转化性能的研究表明,渣油的加氢转化性能与沥青质的性质和反应条件密切相关,其中沥青质的分子单元结构大小和硫含量对渣油加氢转化性能具有重要影响。分子尺寸小、硫含量高的沥青质易于转化,相应的渣油转化率较高;反应条件影响渣油的转化和液相产物的胶体稳定性。在加氢过程中,伴随着热反应的发生,液相产物胶体稳定性下降,使沥青质易于析出、生焦。在氢初压为8MPa,剂油比1:10,反应时间为2h的条件下,反应温度升高,渣油转化率增大,液相产物胶体稳定性下降,焦炭产率明显增加;反应温度为420℃时,液相产物的胶体稳定性被完全破坏,沥青质分相析出,生焦量显著增加。提高反应氢初压,一定程度上抑制了渣油转化,但液相产物的胶体稳定性有所改善,生焦率降低。延长反应时间,渣油转化率提高,但液相产物的胶体稳定性变差,生焦量增加。对不同渣油加氢反应的液相产物胶体稳定性的研究表明,组分组成、组分性质和平均结构均影响液相产物的胶体稳定性;饱和分与沥青质含量增加,芳香分与胶质含量减少,液相产物的胶体稳定性变差;胶质与沥青质的极性差距加大,不利于液相产物的稳定;沥青质与胶质的芳香结构差距加大,液相产物的胶体稳定性变差。
沥青质中的杂原子含量及类型严重影响催化剂失活和沥青质的反应性能,对沥青质加氢反应前后杂原子含量及类型进行了研究。加氢过程中,C-S键能小于C-C键能,因此沥青质中的硫S易于脱除,随着反应的进行沥青质中硫含量减少。氮主要位于芳香环内,难于脱除,随反应的进行沥青质中氮含量增加。采用X射线光电子能谱(XPS)和X射线吸收近边谱(XANES)对沥青质中杂原子类型进行分析,发现渣油沥青质中的氮主要以吡咯类氮形式存在,含少量吡啶类氮;氧主要以C-O单键形式存在;硫主要以噻吩硫形式存在,含有少量亚砜。硫、氮官能团的特点决定了其脱除的难易程度。加氢反应后沥青质中吡啶类氮(碱性氮)相对含量增多,羧基氧相对数量显著增加,噻吩硫、亚砜相对数量减少。加氢后沥青质中亚砜含量的减少与沥青质极性变小相一致。
渣油中沥青质的胶粒形态影响其流变性质和扩散传质效率,尤其是沥青质的加氢反应行为。利用小角X射线散射技术(SAXS)对渣油及其加氢反应样品中沥青质的胶粒尺寸进行了测定。研究发现,渣油中沥青质的胶粒尺寸在6-9nm,沥青质的胶粒尺寸与其含量无关;渣油搀兑馏分油及热反应生焦诱导期内样品的研究表明,组分性质的不配伍性以及可溶质溶剂化作用的减弱使沥青质发生絮凝,胶粒尺寸变大;加氢过程中,沥青质分子发生加氢裂化和缩合生焦反应,沥青质的胶粒尺寸变小。
采用安东帕Physical MCR101型流变仪研究渣油的流变性。在压力为6MPa、温度160℃-280℃的实验条件下发现,渣油属于牛顿型流体;粘度与温度呈指数关系,升高温度,不同渣油间粘度差距减小;压力对粘度的影响较小。
The decline in the colloidal stability of residue would cause asphaltene to aggregate and ultimately transform into coke during thermal reaction. Asphaltene deposited on the catalyst and transformed int coke, making catalyst deactived rapidly, during hydroprocessing of heavy oils. So asphaltenes would limit the efficiency of conversion and run time of unit greatly. Therefore, the hydroprocessing performance of residue and the relationship between the colloidal stability variation and coking characteristics were investigated in this thesis.
Effect of FCC slurry oil and HVGO on the colloidal stability of residue was studied by mass fraction conductivity method. It was shown that the addition of two fractions exhibited negative effect on the colloidal stability of residue. The disparity in polarity between heavy fraction and residue was the main reason for altering the colloidal stability of residue.
Through the investigation on the hydroprocessing performance of different residue, it could be seen that asphaltenes with small size and high sulfur content were easy to convert, and the conversion of corresponding residue was high. The product distribution and colloidal stability were invarious with reaction condition. As the reaction temperature increased, the conversion of residue increased or the colloidal stability of system decreased, and the coke yield increased. At reaction temperature of 420℃, the colloidal stability of residue system was destroyed totally, the sludge formation was found and the coke yield increased remarkablely. As the initial hydrogen pressure increased, the conversion of residue reduced and the colloidal stabililty increased, and the coke yield decreased. As reaction time increase, the conversion of residue increased and the colloidal stability decreased, and the coke yield increased. The change of the colloidal stability was deterimined by the company action of SARA composition and the properties of them.
The reaction performance of asphaltenes was influenced by heteroatom content and types of them. The sulfur-carbon bond was weaker than the carbon-carbon bond, so the sulfur-carbon bond was easy to rupture, and the sulfur content in asphaltene decreased as hydroprocessing processed. Nitrogen was mainly present in the aromatic rings located inside the asphaltene molecule, and was difficult to remove. So the nitrogen in asphaltene increased. X-ray photoelectron spectroscopy(XPS) and X-ray absorption near-edge structure spectrum(XANES) were carried out to investigate the type of heteroatom in asphaltene. After hydroprocessing, basic nitrogen relative content increased, carbonoxylate oxygen relative content increased, and thiophene sulfur and sulfoxide relative content decreased. The decreased contene of sulfoxide was consistent with the downtrend of polarity of asphaltene.
The rheology and diffused efficiency of residue were influenced by morphology of colloidal particle of asphaltene. The colloidal particle size of asphaltene was characterized by small angle X-ray scattering technology(SAXS). The size of colloidal particle in residue was between 6-9nm. When the SARA compostion was uncomfatible and the solvated power of maltene decreased, asphalene aggregated together and the size increased. After hydroprocessing, the size of asphaltenes particles decreased.
At high temperature and pressure, the residue, mixed system and the liquid product after hydroprocessing were shown to be Newton rheology. The viscosity and temperature character fitted to exponential law. Pressure had little impact on the viscosity.
采用质量分数电导率法考察了分别搀兑催化裂化油浆和减四线抽出油对渣油体系胶体稳定性的影响,发现搀兑催化裂化油浆或减四线抽出油均使渣油体系的稳定性下降。研究表明,馏分油组分与渣油组分极性的差距决定了体系胶体稳定性的变化。
不同渣油加氢转化性能的研究表明,渣油的加氢转化性能与沥青质的性质和反应条件密切相关,其中沥青质的分子单元结构大小和硫含量对渣油加氢转化性能具有重要影响。分子尺寸小、硫含量高的沥青质易于转化,相应的渣油转化率较高;反应条件影响渣油的转化和液相产物的胶体稳定性。在加氢过程中,伴随着热反应的发生,液相产物胶体稳定性下降,使沥青质易于析出、生焦。在氢初压为8MPa,剂油比1:10,反应时间为2h的条件下,反应温度升高,渣油转化率增大,液相产物胶体稳定性下降,焦炭产率明显增加;反应温度为420℃时,液相产物的胶体稳定性被完全破坏,沥青质分相析出,生焦量显著增加。提高反应氢初压,一定程度上抑制了渣油转化,但液相产物的胶体稳定性有所改善,生焦率降低。延长反应时间,渣油转化率提高,但液相产物的胶体稳定性变差,生焦量增加。对不同渣油加氢反应的液相产物胶体稳定性的研究表明,组分组成、组分性质和平均结构均影响液相产物的胶体稳定性;饱和分与沥青质含量增加,芳香分与胶质含量减少,液相产物的胶体稳定性变差;胶质与沥青质的极性差距加大,不利于液相产物的稳定;沥青质与胶质的芳香结构差距加大,液相产物的胶体稳定性变差。
沥青质中的杂原子含量及类型严重影响催化剂失活和沥青质的反应性能,对沥青质加氢反应前后杂原子含量及类型进行了研究。加氢过程中,C-S键能小于C-C键能,因此沥青质中的硫S易于脱除,随着反应的进行沥青质中硫含量减少。氮主要位于芳香环内,难于脱除,随反应的进行沥青质中氮含量增加。采用X射线光电子能谱(XPS)和X射线吸收近边谱(XANES)对沥青质中杂原子类型进行分析,发现渣油沥青质中的氮主要以吡咯类氮形式存在,含少量吡啶类氮;氧主要以C-O单键形式存在;硫主要以噻吩硫形式存在,含有少量亚砜。硫、氮官能团的特点决定了其脱除的难易程度。加氢反应后沥青质中吡啶类氮(碱性氮)相对含量增多,羧基氧相对数量显著增加,噻吩硫、亚砜相对数量减少。加氢后沥青质中亚砜含量的减少与沥青质极性变小相一致。
渣油中沥青质的胶粒形态影响其流变性质和扩散传质效率,尤其是沥青质的加氢反应行为。利用小角X射线散射技术(SAXS)对渣油及其加氢反应样品中沥青质的胶粒尺寸进行了测定。研究发现,渣油中沥青质的胶粒尺寸在6-9nm,沥青质的胶粒尺寸与其含量无关;渣油搀兑馏分油及热反应生焦诱导期内样品的研究表明,组分性质的不配伍性以及可溶质溶剂化作用的减弱使沥青质发生絮凝,胶粒尺寸变大;加氢过程中,沥青质分子发生加氢裂化和缩合生焦反应,沥青质的胶粒尺寸变小。
采用安东帕Physical MCR101型流变仪研究渣油的流变性。在压力为6MPa、温度160℃-280℃的实验条件下发现,渣油属于牛顿型流体;粘度与温度呈指数关系,升高温度,不同渣油间粘度差距减小;压力对粘度的影响较小。
The decline in the colloidal stability of residue would cause asphaltene to aggregate and ultimately transform into coke during thermal reaction. Asphaltene deposited on the catalyst and transformed int coke, making catalyst deactived rapidly, during hydroprocessing of heavy oils. So asphaltenes would limit the efficiency of conversion and run time of unit greatly. Therefore, the hydroprocessing performance of residue and the relationship between the colloidal stability variation and coking characteristics were investigated in this thesis.
Effect of FCC slurry oil and HVGO on the colloidal stability of residue was studied by mass fraction conductivity method. It was shown that the addition of two fractions exhibited negative effect on the colloidal stability of residue. The disparity in polarity between heavy fraction and residue was the main reason for altering the colloidal stability of residue.
Through the investigation on the hydroprocessing performance of different residue, it could be seen that asphaltenes with small size and high sulfur content were easy to convert, and the conversion of corresponding residue was high. The product distribution and colloidal stability were invarious with reaction condition. As the reaction temperature increased, the conversion of residue increased or the colloidal stability of system decreased, and the coke yield increased. At reaction temperature of 420℃, the colloidal stability of residue system was destroyed totally, the sludge formation was found and the coke yield increased remarkablely. As the initial hydrogen pressure increased, the conversion of residue reduced and the colloidal stabililty increased, and the coke yield decreased. As reaction time increase, the conversion of residue increased and the colloidal stability decreased, and the coke yield increased. The change of the colloidal stability was deterimined by the company action of SARA composition and the properties of them.
The reaction performance of asphaltenes was influenced by heteroatom content and types of them. The sulfur-carbon bond was weaker than the carbon-carbon bond, so the sulfur-carbon bond was easy to rupture, and the sulfur content in asphaltene decreased as hydroprocessing processed. Nitrogen was mainly present in the aromatic rings located inside the asphaltene molecule, and was difficult to remove. So the nitrogen in asphaltene increased. X-ray photoelectron spectroscopy(XPS) and X-ray absorption near-edge structure spectrum(XANES) were carried out to investigate the type of heteroatom in asphaltene. After hydroprocessing, basic nitrogen relative content increased, carbonoxylate oxygen relative content increased, and thiophene sulfur and sulfoxide relative content decreased. The decreased contene of sulfoxide was consistent with the downtrend of polarity of asphaltene.
The rheology and diffused efficiency of residue were influenced by morphology of colloidal particle of asphaltene. The colloidal particle size of asphaltene was characterized by small angle X-ray scattering technology(SAXS). The size of colloidal particle in residue was between 6-9nm. When the SARA compostion was uncomfatible and the solvated power of maltene decreased, asphalene aggregated together and the size increased. After hydroprocessing, the size of asphaltenes particles decreased.
At high temperature and pressure, the residue, mixed system and the liquid product after hydroprocessing were shown to be Newton rheology. The viscosity and temperature character fitted to exponential law. Pressure had little impact on the viscosity.
引文
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