石油焦的理化性质及其催化气化反应特性研究
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摘要
石油焦是渣油延迟焦化的副产物,而高温气化则是实现其高效、清洁利用的有效方法。然而,石油焦的气化活性很低,这制约了石油焦用做大规模高效气化原料的可行性。因此,研究石油焦的理化性质及其气化反应特性以寻找制约其气化活性的关键因素显的尤为重要。催化气化技术可有效改善石油焦的气化反应活性以实现其高效利用,而建立一个准确、普适性的催化气化反应动力学模型对于解决石油焦催化气化的现实性问题,如气化炉的设计和优化,具有极其重要的意义。本文的主要研究内容和结果如下：
在热解温度为350-500℃范围内,以减压渣油、煤沥青和生物质沥青为原料分别制备了三类液相炭化焦,并对三类液相炭化焦的理化性质和气化反应特性进行了研究,在此基础上进一步考察了三类液相炭化焦在高温煅烧过程中理化性质和气化反应特性的演变规律。结果表明：①液相炭化焦中可溶有机质的含量高达14.12～66.69%,经CS2处理后,液相炭化焦碳微晶结构的变化很小,而BET比表面积和孔体积均大幅增加,从而导致其气化反应活性的大幅提高；②液相炭化焦中存在的大量小分子有机物质是制约其气化反应活性的一个重要因素；③三种液相炭化焦经高温煅烧后的碳微晶结构的有序化程度存在如下关系,即煤沥青焦>石油焦>生物质沥青焦,而三者的气化反应活性则完全相反。
以五种煤气化灰渣为研究对象,对其物相组成、表面形态和粒度分布等理化性质进行了分析表征,并考察了不同煤气化灰渣对石油焦/CO2和石油焦/水蒸气气化反应特性的影响。结果表明：①煤气化灰渣的组成极不均匀,不同粒度气化灰渣的化学组成有很大的差异,可通过简单的筛分过程初步实现气化灰渣的分级利用；②气化灰渣残炭及其原煤的快速热解焦的碳结构有序化程度存在如下关系,即DSHHZ>DSHFH>SF-RP1400,而气化灰渣残炭的气化反应活性则要优于其原煤的快速热解焦；③不同气化灰渣对石油焦/CO2气化反应促进作用的大小顺序为：SHFH≈SHHZ>GTHZB≈GTHZA>LNHZ,气化灰渣对气化反应促进作用的大小与气化灰渣中Fe2O3+CaO和Fe2O3+CaO+Na2O+K2O含量近似成线性关系。
在气化温度为800～1000℃范围内,分别考察了气化温度、原煤掺入量以及煤种对不同煤阶原煤与石油焦共气化反应特性的影响。结果表明：①随着神府煤掺入量的增加,神府煤/石油焦共气化的气体产物中H2产率以及气体产物的总产率均逐渐增加,气体产物中H2的含量逐渐从石油焦单独气化时的51.88%增加至共气化时的62.05%；②不同煤阶原煤与石油焦的共其气化反应速率存在如下关系：即XLT>SF>GP;三种原煤/石油焦共气化过程中水煤气变换反应均未达到平衡状态,但水煤气变换反应的发生程度存在如下关系：即XLT>SF>GP;③原煤/石油焦共气化,尤其是褐煤/石油焦共气化技术,可实现石油焦和褐煤资源的高效、清洁利用,是一条可行、具有推广前景的技术。
对石油焦在水蒸气/CO2混合气氛下的非催化和催化气化反应特性进行了研究,主要考察了气化剂组成、气化温度等参数对石油焦在水蒸气/CO2混合气氛下的气化反应活性、气体产物中H2+CO的总产率以及H2/CO比值的影响。结果表明：①催化气化条件下单位质量的碳完全气化所产生的气体产物中H2+CO总产率以及H2/CO比值均大非催化气化；②石油焦在水蒸气/CO2混合气氛下催化气化一步法定向调控气体产物中H2/CO比值以生产费托合成反应的原料气经初步试验表明是可行的。
考察了单种金属盐、复合金属盐以及可弃催化剂作用下石油焦/CO2的气化反应特性,并提出了一个普适性的催化气化反应动力学模型。结果表明：①本文所提出的修正随机孔模型不仅能很好地解释单种金属盐的催化气化行为,而且能很好地解释复合金属盐、甚至可弃催化剂的催化气化反应行为,是一个普适性的催化气化反应动力学模型；②所提出的催化气化反应动力学模型中的模型参数α和β值的大小可在一定烈度上表征催化剂的催化能力,具有一定的物理意义。
Petroleum coke is the by-product of crude oil delayed coking unit, and gasification technology can realize its efficient and clean use. However, the gasification activity of petroleum coke is extremely low, which greatly restricts the applicability of petroleum coke as the feedstock of gasifiers. Therefore, it is very important to investigate the physico-chemical properties and gasification characteristics of petroleum coke and to find out main reasons leading to the low gasification activity of petroleum coke. Catalytic gasification technology can effectively improve the gasification activity of petroleum coke, and establish a accurate and universal catalytic gasification kinetic model for solving the reality problems of catalytic gasification of petroleum coke, such as the design and optimization of the gasifiers, is of great significance. The main contents and results of this study were summarized as follows.
Three kinds of Liquid-Phase Carbonization Cokes (LPCCs) were separately prepared from vacuum residue, coal tar pitch and biomass tar pitch at the pyrolysis temperatures of350～500℃, and the physico-chemical properties and gasification characteristics of LPCCs were investigated. Furthermore, the effects of high temperature calcination on the physico-chemical properties and gasification characteristics of LPCCs were also investigated. The following results were obtained.①A large number of CS2-soluble fraction existed in LPCCs (as high as14.12～66.69%), although the carbon crystalline structures of LPCCs after extraction were almost unchanged, the BET surface areas and total pore volumes of extracted LPCCs increased significantly, which resulted in a greatly increasing gasification activity of LPCCs;②The soluble fractions contained in LPCCs were the most important factor of affecting on the gasification activity of LPCCs;③The ordering of carbon microcrystalline structures of the high temperature calcined cokes from three LPCCs was as follows:coal pitch coke>petroleum coke>biomass pitch coke, while the ordering of gasification activities of the three high temperature calcined cokes was completely opposite.
The physico-chemical properties of five coal gasification slag, such as chemical composition, surface morphologies, particle size distribution,and so on,were investigated, and the effects of coal gasification slag on the CO2and steam gasification of petroleum coke were studied. The following results were obtained.①The composition of coal gasification slag is very uneven, the chemical composition of coal gasification slag of different particle sizes are very different, that means the classification and utilization of coal gasification slag can realized through screening process;②The ordering of carbon microcrystalline structures among the different types of residual carbon from coal gasification slag and their rapid pyrolysis char was as follows:DSHHZ>DSHFH>SF-RP1400, while the gasification activities of residual carbon are superior to the rapid pyrolysis char;③The ordering of the catalytic action of different coal gasification slag on the CO2gasification reaction was:SHFH≈SHHZ>GTHZB≈GTHZA>LNHZ, and the catalytic action of coal gasification slag is approximately linear with the Fe2O3+CaO and Fe2O3+CaO+Na2O+K2O contents.
The effects of gasification temperatures and loading contents of coal on the gasification activity, gas yields and H2production characteristics of petroleum coke and coal co-gasification processes were investigated. The following results were obtained.￤ith the increasing loading contents of Shenfu coal, the H2yields and total yields of gaseous products from co-gasification increased, and the H2contents increased from51.88%to62.05%;②The ordering of co-gasification reactivity of petroleum coke with coals of different ranks was as follows:XLT>SF>GP; The water-gas shift reactions did not reach equilibrium during the co-gasification of petroleum coke with coals of different ranks, and the extent of the water-gas shift reaction was:XLT>SF>GP;③Coal and petroleum coke co-gasification, especially lignite and petroleum coke co-gasification technology can realize the efficient and clean use of petroleum coke.
The effects of composition of gasifying agent and gasification temperature on the non-catalytic and catalytic gasification characteristics of petroleum coke gasified in steam and CO2mixed atmosphere were investigated.①The H2+CO yields and H2/CO ratio in gaseous products from the catalytic gasification are larger than those of non-catalytic gasification;②A single-step to control the composition of synthesis gas with desirable H2/CO ratio to produce the feed gas of FT synthesis reaction from catalytic gasification of petroleum coke in steam and CO2mixed environment is feasible.
The CO2catalytic gasification characteristics of petroleum coke catalyzed by different catalysts at the gasification temperature of900℃were investigated,and a universal catalytic gasification kinetic model were established.①The extended random pore model (ERPM) proposed in this paper can not only explain the catalytic gasification characteristics of various metal salts, but also can explain the catalytic gasification characteristics of composite metal salts, even disposable catalysts;②The value of parameters α and β in proposed ERPM can characterization the catalytic ability of catalysts to a certain extent.
在热解温度为350-500℃范围内,以减压渣油、煤沥青和生物质沥青为原料分别制备了三类液相炭化焦,并对三类液相炭化焦的理化性质和气化反应特性进行了研究,在此基础上进一步考察了三类液相炭化焦在高温煅烧过程中理化性质和气化反应特性的演变规律。结果表明：①液相炭化焦中可溶有机质的含量高达14.12～66.69%,经CS2处理后,液相炭化焦碳微晶结构的变化很小,而BET比表面积和孔体积均大幅增加,从而导致其气化反应活性的大幅提高；②液相炭化焦中存在的大量小分子有机物质是制约其气化反应活性的一个重要因素；③三种液相炭化焦经高温煅烧后的碳微晶结构的有序化程度存在如下关系,即煤沥青焦>石油焦>生物质沥青焦,而三者的气化反应活性则完全相反。
以五种煤气化灰渣为研究对象,对其物相组成、表面形态和粒度分布等理化性质进行了分析表征,并考察了不同煤气化灰渣对石油焦/CO2和石油焦/水蒸气气化反应特性的影响。结果表明：①煤气化灰渣的组成极不均匀,不同粒度气化灰渣的化学组成有很大的差异,可通过简单的筛分过程初步实现气化灰渣的分级利用；②气化灰渣残炭及其原煤的快速热解焦的碳结构有序化程度存在如下关系,即DSHHZ>DSHFH>SF-RP1400,而气化灰渣残炭的气化反应活性则要优于其原煤的快速热解焦；③不同气化灰渣对石油焦/CO2气化反应促进作用的大小顺序为：SHFH≈SHHZ>GTHZB≈GTHZA>LNHZ,气化灰渣对气化反应促进作用的大小与气化灰渣中Fe2O3+CaO和Fe2O3+CaO+Na2O+K2O含量近似成线性关系。
在气化温度为800～1000℃范围内,分别考察了气化温度、原煤掺入量以及煤种对不同煤阶原煤与石油焦共气化反应特性的影响。结果表明：①随着神府煤掺入量的增加,神府煤/石油焦共气化的气体产物中H2产率以及气体产物的总产率均逐渐增加,气体产物中H2的含量逐渐从石油焦单独气化时的51.88%增加至共气化时的62.05%；②不同煤阶原煤与石油焦的共其气化反应速率存在如下关系：即XLT>SF>GP;三种原煤/石油焦共气化过程中水煤气变换反应均未达到平衡状态,但水煤气变换反应的发生程度存在如下关系：即XLT>SF>GP;③原煤/石油焦共气化,尤其是褐煤/石油焦共气化技术,可实现石油焦和褐煤资源的高效、清洁利用,是一条可行、具有推广前景的技术。
对石油焦在水蒸气/CO2混合气氛下的非催化和催化气化反应特性进行了研究,主要考察了气化剂组成、气化温度等参数对石油焦在水蒸气/CO2混合气氛下的气化反应活性、气体产物中H2+CO的总产率以及H2/CO比值的影响。结果表明：①催化气化条件下单位质量的碳完全气化所产生的气体产物中H2+CO总产率以及H2/CO比值均大非催化气化；②石油焦在水蒸气/CO2混合气氛下催化气化一步法定向调控气体产物中H2/CO比值以生产费托合成反应的原料气经初步试验表明是可行的。
考察了单种金属盐、复合金属盐以及可弃催化剂作用下石油焦/CO2的气化反应特性,并提出了一个普适性的催化气化反应动力学模型。结果表明：①本文所提出的修正随机孔模型不仅能很好地解释单种金属盐的催化气化行为,而且能很好地解释复合金属盐、甚至可弃催化剂的催化气化反应行为,是一个普适性的催化气化反应动力学模型；②所提出的催化气化反应动力学模型中的模型参数α和β值的大小可在一定烈度上表征催化剂的催化能力,具有一定的物理意义。
Petroleum coke is the by-product of crude oil delayed coking unit, and gasification technology can realize its efficient and clean use. However, the gasification activity of petroleum coke is extremely low, which greatly restricts the applicability of petroleum coke as the feedstock of gasifiers. Therefore, it is very important to investigate the physico-chemical properties and gasification characteristics of petroleum coke and to find out main reasons leading to the low gasification activity of petroleum coke. Catalytic gasification technology can effectively improve the gasification activity of petroleum coke, and establish a accurate and universal catalytic gasification kinetic model for solving the reality problems of catalytic gasification of petroleum coke, such as the design and optimization of the gasifiers, is of great significance. The main contents and results of this study were summarized as follows.
Three kinds of Liquid-Phase Carbonization Cokes (LPCCs) were separately prepared from vacuum residue, coal tar pitch and biomass tar pitch at the pyrolysis temperatures of350～500℃, and the physico-chemical properties and gasification characteristics of LPCCs were investigated. Furthermore, the effects of high temperature calcination on the physico-chemical properties and gasification characteristics of LPCCs were also investigated. The following results were obtained.①A large number of CS2-soluble fraction existed in LPCCs (as high as14.12～66.69%), although the carbon crystalline structures of LPCCs after extraction were almost unchanged, the BET surface areas and total pore volumes of extracted LPCCs increased significantly, which resulted in a greatly increasing gasification activity of LPCCs;②The soluble fractions contained in LPCCs were the most important factor of affecting on the gasification activity of LPCCs;③The ordering of carbon microcrystalline structures of the high temperature calcined cokes from three LPCCs was as follows:coal pitch coke>petroleum coke>biomass pitch coke, while the ordering of gasification activities of the three high temperature calcined cokes was completely opposite.
The physico-chemical properties of five coal gasification slag, such as chemical composition, surface morphologies, particle size distribution,and so on,were investigated, and the effects of coal gasification slag on the CO2and steam gasification of petroleum coke were studied. The following results were obtained.①The composition of coal gasification slag is very uneven, the chemical composition of coal gasification slag of different particle sizes are very different, that means the classification and utilization of coal gasification slag can realized through screening process;②The ordering of carbon microcrystalline structures among the different types of residual carbon from coal gasification slag and their rapid pyrolysis char was as follows:DSHHZ>DSHFH>SF-RP1400, while the gasification activities of residual carbon are superior to the rapid pyrolysis char;③The ordering of the catalytic action of different coal gasification slag on the CO2gasification reaction was:SHFH≈SHHZ>GTHZB≈GTHZA>LNHZ, and the catalytic action of coal gasification slag is approximately linear with the Fe2O3+CaO and Fe2O3+CaO+Na2O+K2O contents.
The effects of gasification temperatures and loading contents of coal on the gasification activity, gas yields and H2production characteristics of petroleum coke and coal co-gasification processes were investigated. The following results were obtained.￤ith the increasing loading contents of Shenfu coal, the H2yields and total yields of gaseous products from co-gasification increased, and the H2contents increased from51.88%to62.05%;②The ordering of co-gasification reactivity of petroleum coke with coals of different ranks was as follows:XLT>SF>GP; The water-gas shift reactions did not reach equilibrium during the co-gasification of petroleum coke with coals of different ranks, and the extent of the water-gas shift reaction was:XLT>SF>GP;③Coal and petroleum coke co-gasification, especially lignite and petroleum coke co-gasification technology can realize the efficient and clean use of petroleum coke.
The effects of composition of gasifying agent and gasification temperature on the non-catalytic and catalytic gasification characteristics of petroleum coke gasified in steam and CO2mixed atmosphere were investigated.①The H2+CO yields and H2/CO ratio in gaseous products from the catalytic gasification are larger than those of non-catalytic gasification;②A single-step to control the composition of synthesis gas with desirable H2/CO ratio to produce the feed gas of FT synthesis reaction from catalytic gasification of petroleum coke in steam and CO2mixed environment is feasible.
The CO2catalytic gasification characteristics of petroleum coke catalyzed by different catalysts at the gasification temperature of900℃were investigated,and a universal catalytic gasification kinetic model were established.①The extended random pore model (ERPM) proposed in this paper can not only explain the catalytic gasification characteristics of various metal salts, but also can explain the catalytic gasification characteristics of composite metal salts, even disposable catalysts;②The value of parameters α and β in proposed ERPM can characterization the catalytic ability of catalysts to a certain extent.
引文
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