催化裂化催化剂新材料的合成、表征及其裂化反应性能的研究
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摘要
本论文的主要内容是合成了流化催化裂化(FCC)催化剂新材料,并通过深入表征催化裂化催化剂新材料的孔结构参数,开展了催化裂化催化剂新材料的分析及其孔结构与反应性能的关联研究;建立X射线荧光光谱法测定催化裂化催化剂新材料磷、铁、镧和稀土元素的分析方法,获得了满意的结果。本论文的工作目的在于从分析理论水平上对催化剂的形态、孔径和结构的影响进行研究,从而指导催化反应工艺的设计以及新型催化裂化催化剂材料的研究。
论文包括三个部分。
第一部分催化裂化催化剂新材料的合成、表征及其裂化反应性能的研究进展
第一章催化裂化催化剂新材料的研究进展
介绍了流化催化裂化(FCC)反应及其催化裂化催化剂技术进展,对FCC催化剂新材料及其工艺进行了归纳和总结,展望了设计开发具有高裂化活性和低结焦性能的催化裂化催化剂新材料的发展趋势和应用前景。
第二章催化裂化催化剂的孔结构与反应性能关系的研究进展
催化裂化催化剂在制备过程中,存在着孔隙结构与表面积的变化,孔隙结构变化特征的准确分析是高效研发FCC催化剂的基础。本章从FCC催化剂的孔隙结构的表征分析、反应过程中孔隙结构变化以及孔隙结构模型三方面总结了FCC催化剂孔结构分析方法的研究现状,并且对各种方法的特点进行了评述;同时对FCC催化剂分析方法的研究重点催化剂制备过程中孔隙结构的变化影响,孔隙结构与反应性能的关系等几个方面进行了展望,。
第三章X射线荧光光谱分析的研究应用进展
介绍了X射线荧光光谱分析的基本原理和仪器装置,对X射线荧光光谱法分析在催化剂分析领域的应用研究进行了归纳和总结,展望了X射线荧光光谱法在催化裂化催化剂新材料领域分析研究的发展趋势和应用前景。
第四章论文选题意义及主要研究内容
介绍了本论文的研究目的意义、研究内容和实验中的表征手段。
第二部分催化裂化催化剂新材料及其孔结构与反应性能的研究
在实验室进行了山西金洋土的性质及其原位晶化工艺所制催化剂的研究。结果表明,山西金洋土的基本性质符合全白土型原位晶化催化剂的要求,该高岭土在原位晶化体系中具有适度活性硅和较快活性铝的碱溶速度,以及良好的晶化性能和裂化性能。与现用的苏州高岭土采用相同工艺制备的对比剂相比,山西金洋土的比表面积和孔体积更大。以新疆减压宽馏分和减压渣油的混合油为原料,进行了裂化性能的考察。结果表明,高岭土经过热和化学改性,形成了一定活性的中孔结构,所设计的新型重油催化剂具有较好的重质油转化能力和良好的裂化产物选择性。
第三部分X射线荧光光谱法测定催化剂新材料的分析应用
第一章X射线荧光光谱法测定助催化剂中磷和铁的研究
使用X射线荧光光谱仪,采用人工合成标样,设计合成了一套磷和铁总含量分别为0.15%-2.30%、0.20%-2.40%的标准样品;采用数学校正法中的经验系数法校正元素间的互相干扰,样品不经任何处理,粉末直接压片,经验系数法校正基体效应,建立了分析测定助催化剂中磷和铁含量的方法。讨论了样品制作方法,合适的测量条件,探讨了试样中元素间的相互影响。实验结果表明,该方法重现性好,准确度和精密度较高,测定磷和铁的相对标准偏差分别为:0.34%和0.59 %;测定范围磷为0.01-2.50%,铁为0.01-2.50%。分析结果与化学法、等离子发射光谱法测定结果吻合。本方法操作简便、样品处理简单,不用分解试样,结果准确,分析速度远快于其它分析方法,单次测量一个样品只需要5分钟,适用范围广,满足了科研和工业生产的需要。
第二章X射线荧光光谱法测定分子筛中镧含量的研究
根据准确快速测定分子筛中改性元素镧含量的需求,本论文采用粉末样品压片制样,用X射线荧光光谱仪对分子筛中稀土元素镧进行测定。以离子交换法制备标准样品,通过充分地研磨,来克服粒度效应和矿物效应。论文主要讨论了吸收-增强效应对镧元素分析的影响;使用经验系数法校正基体效应,本方法得到的分析结果与化学方法一致;同时该方法测定范围宽,满足了科研和工业生产的需求。
The main contents of this paper describe how to synthesize the new materials of the fluid catalytic cracking (FCC) catalysts.By analyzing the pore structure parameters of the new materials FCC catalyst, the associated study on analysis of the new catalytic cracking catalyst and their pore structure and reaction properties are carried out. As a result, the satisfactory analytical methods of phosphorus, iron, lanthanum and rare earth elements contained in the new materials FCC catalyst were determined by using X-ray fluorescence spectrometry. The objective of this paper is to guide the design of catalytic reaction process and enhance the further research of the new FCC catalyst materials through studying the catalyst shape, size and structure in the view of analytical theories.
This paper consists of the following three parts:
Part One A review on study progress of new fluid catalytic cracking catalyst in synthesis, analysis, characterization and reaction properties
Chapter One A review on study progress of the new material of fluid catalytic cracking catalyst
The fluid catalytic cracking (FCC) reaction and its catalytic cracking catalysts are introduced when the new materials for FCC catalyst and its process are summarized and categorized. Then, the potential development and application prospects of FCC catalysts and new materials with the high cracking activity and low coking properties are predicted.
Chapter Two Study progress of the fluid catalytic cracking catalyst in relation between reaction capability and pore structure
In the preparation process of FCC catalyst, there is the existence of pore structure and surface area changes. Therefore, the accurate analysis of high-performance research on changes of pore structure characteristics will become the basis of FCC catalyst synthesis. In this paper, the characterization of pore structure analysis, reaction course of changes in pore structure and pore structure model are summarized on the three aspects of FCC catalyst pore structure analysis method, and the characteristics of various methods are compared too. In meantime, the FCC catalyst analysis methods focusing on the prosperous development are discussed. A particular study on the relations between the change of pore structure and reaction properties in the catalyst preparation process is introduced referring to literatures.
Chapter Three A review on the X-ray Fluorescence Spectrometry analysis
This chapter introduces the basic principles and the instrumentation of the X-ray fluorescence spectrometry analysis. It mainly summarizes and categorizes the applications of X-ray Fluorescence Spectrometry, and vistas the newly developing techniques and further trends of the X-ray Fluorescence Spectrometry method to analyze the elements used in the new material catalyst based on the published references.
Chapter Four Significance and the main research contents of the thesis
Significance and objectives of this research, main contents, innovative points, experiments and the characterization approaches in this thesis are introduced.
Part Two Study on the reaction capability and the pore structure of new material with FCC catalyst
The properties of Jinyang soil taken from Shanxi Province and the catalyst from its in-situ crystallization were studied in the laboratory. The result showed that the essential properties of Jinyang soil met with the requirement for making catalyst by in-situ crystallization, which possessed the stronger and appropriate alkaline dissolvable rates for active alumina and active silica respectively, as well as good performance of crystallization and cracking. After the thermal treatment and chemical modification of kaolin, the certain reactive mesoporous structure was formed in CLS material, and the novel FCC catalyst containing CLS exhibited the excellent heavy oil cracking capability and superior selectivity to desired products.
Part Three Determination of the new material catalyst by X-ray Fluorescence Spectrometry
Chapter One Determination of Phosphorus and Iron in Co-catalyst by X-ray Fluorescence Spectrometry
The aim of this work was to develop a new technique for quantitative analysis of phosphorus and iron contents in co-catalyst by X-ray fluorescence spectrometry (XRFS). A set of synthesized standard samples were prepared for the experiments with this purpose when the interferences of inter-elements were corrected by the Empirical Coefficient Method. The standard samples were manually synthesized, and the powder pellets were used for sample preparation while and the matrix effects were corrected by the experience coefficients. The characteristic X-rays of phosphorus and iron elements could selectively be determined with the enhanced accuracy and reduced time consumption within a range without signal interference from main-component elements. Manufacturing sample and measurement conditions of the new method were brought up; The matrix effects of Co-catalyst samples were verified by Empirical Coefficient Method. The results of experiment showed that the accuracy and precision of this method satisfactorily had the high repeatability. The measuring ranges of elements were w 0.01-2.50% for phosphorus and w 0.01-2.50% for Iron with the relative deviations of 0.34% for Phosphorus and 0.59% for Iron, respectively. This method showed the satisfactory accordant results in comparison with the chemical method and inductively coupled plasma (ICP). It also has provided the analytical values for phosphorus and iron in co-catalyst. This new method has the advantages of satisfactory accuracy, high precision, less interference, easy sample handling and high efficiency. In addition, the samples are not decomposed during the analysis process when each sample only requires 5 minutes to be taken for measurement. This new method will be able to meet the growing demands of quantitative analysis of phosphorus and iron content in co-catalysts. This method had the satisfactory accuracy and precision, so the analytical range was large, and had been successfully applied to the determine phosphorus and iron in co-catalyst.
Chapter Two Determining the content of La on modified zeolite by X-ray Fluorescence Spectrometry
After eliminating particle size effects and mineral effects by sufficiently grinding and using proper preparation methods of standards, absorption-enhancement effects of the XRFS to determine the content of La2O3 on modified zeolite were mainly discussed in this paper. If the absorption-enhancement effects were corrected by the experience coefficients, the results appeared to be in good agreement with the classical chemical method, and can meet the requirements of scientific research analysis and industrial analysis.
论文包括三个部分。
第一部分催化裂化催化剂新材料的合成、表征及其裂化反应性能的研究进展
第一章催化裂化催化剂新材料的研究进展
介绍了流化催化裂化(FCC)反应及其催化裂化催化剂技术进展,对FCC催化剂新材料及其工艺进行了归纳和总结,展望了设计开发具有高裂化活性和低结焦性能的催化裂化催化剂新材料的发展趋势和应用前景。
第二章催化裂化催化剂的孔结构与反应性能关系的研究进展
催化裂化催化剂在制备过程中,存在着孔隙结构与表面积的变化,孔隙结构变化特征的准确分析是高效研发FCC催化剂的基础。本章从FCC催化剂的孔隙结构的表征分析、反应过程中孔隙结构变化以及孔隙结构模型三方面总结了FCC催化剂孔结构分析方法的研究现状,并且对各种方法的特点进行了评述;同时对FCC催化剂分析方法的研究重点催化剂制备过程中孔隙结构的变化影响,孔隙结构与反应性能的关系等几个方面进行了展望,。
第三章X射线荧光光谱分析的研究应用进展
介绍了X射线荧光光谱分析的基本原理和仪器装置,对X射线荧光光谱法分析在催化剂分析领域的应用研究进行了归纳和总结,展望了X射线荧光光谱法在催化裂化催化剂新材料领域分析研究的发展趋势和应用前景。
第四章论文选题意义及主要研究内容
介绍了本论文的研究目的意义、研究内容和实验中的表征手段。
第二部分催化裂化催化剂新材料及其孔结构与反应性能的研究
在实验室进行了山西金洋土的性质及其原位晶化工艺所制催化剂的研究。结果表明,山西金洋土的基本性质符合全白土型原位晶化催化剂的要求,该高岭土在原位晶化体系中具有适度活性硅和较快活性铝的碱溶速度,以及良好的晶化性能和裂化性能。与现用的苏州高岭土采用相同工艺制备的对比剂相比,山西金洋土的比表面积和孔体积更大。以新疆减压宽馏分和减压渣油的混合油为原料,进行了裂化性能的考察。结果表明,高岭土经过热和化学改性,形成了一定活性的中孔结构,所设计的新型重油催化剂具有较好的重质油转化能力和良好的裂化产物选择性。
第三部分X射线荧光光谱法测定催化剂新材料的分析应用
第一章X射线荧光光谱法测定助催化剂中磷和铁的研究
使用X射线荧光光谱仪,采用人工合成标样,设计合成了一套磷和铁总含量分别为0.15%-2.30%、0.20%-2.40%的标准样品;采用数学校正法中的经验系数法校正元素间的互相干扰,样品不经任何处理,粉末直接压片,经验系数法校正基体效应,建立了分析测定助催化剂中磷和铁含量的方法。讨论了样品制作方法,合适的测量条件,探讨了试样中元素间的相互影响。实验结果表明,该方法重现性好,准确度和精密度较高,测定磷和铁的相对标准偏差分别为:0.34%和0.59 %;测定范围磷为0.01-2.50%,铁为0.01-2.50%。分析结果与化学法、等离子发射光谱法测定结果吻合。本方法操作简便、样品处理简单,不用分解试样,结果准确,分析速度远快于其它分析方法,单次测量一个样品只需要5分钟,适用范围广,满足了科研和工业生产的需要。
第二章X射线荧光光谱法测定分子筛中镧含量的研究
根据准确快速测定分子筛中改性元素镧含量的需求,本论文采用粉末样品压片制样,用X射线荧光光谱仪对分子筛中稀土元素镧进行测定。以离子交换法制备标准样品,通过充分地研磨,来克服粒度效应和矿物效应。论文主要讨论了吸收-增强效应对镧元素分析的影响;使用经验系数法校正基体效应,本方法得到的分析结果与化学方法一致;同时该方法测定范围宽,满足了科研和工业生产的需求。
The main contents of this paper describe how to synthesize the new materials of the fluid catalytic cracking (FCC) catalysts.By analyzing the pore structure parameters of the new materials FCC catalyst, the associated study on analysis of the new catalytic cracking catalyst and their pore structure and reaction properties are carried out. As a result, the satisfactory analytical methods of phosphorus, iron, lanthanum and rare earth elements contained in the new materials FCC catalyst were determined by using X-ray fluorescence spectrometry. The objective of this paper is to guide the design of catalytic reaction process and enhance the further research of the new FCC catalyst materials through studying the catalyst shape, size and structure in the view of analytical theories.
This paper consists of the following three parts:
Part One A review on study progress of new fluid catalytic cracking catalyst in synthesis, analysis, characterization and reaction properties
Chapter One A review on study progress of the new material of fluid catalytic cracking catalyst
The fluid catalytic cracking (FCC) reaction and its catalytic cracking catalysts are introduced when the new materials for FCC catalyst and its process are summarized and categorized. Then, the potential development and application prospects of FCC catalysts and new materials with the high cracking activity and low coking properties are predicted.
Chapter Two Study progress of the fluid catalytic cracking catalyst in relation between reaction capability and pore structure
In the preparation process of FCC catalyst, there is the existence of pore structure and surface area changes. Therefore, the accurate analysis of high-performance research on changes of pore structure characteristics will become the basis of FCC catalyst synthesis. In this paper, the characterization of pore structure analysis, reaction course of changes in pore structure and pore structure model are summarized on the three aspects of FCC catalyst pore structure analysis method, and the characteristics of various methods are compared too. In meantime, the FCC catalyst analysis methods focusing on the prosperous development are discussed. A particular study on the relations between the change of pore structure and reaction properties in the catalyst preparation process is introduced referring to literatures.
Chapter Three A review on the X-ray Fluorescence Spectrometry analysis
This chapter introduces the basic principles and the instrumentation of the X-ray fluorescence spectrometry analysis. It mainly summarizes and categorizes the applications of X-ray Fluorescence Spectrometry, and vistas the newly developing techniques and further trends of the X-ray Fluorescence Spectrometry method to analyze the elements used in the new material catalyst based on the published references.
Chapter Four Significance and the main research contents of the thesis
Significance and objectives of this research, main contents, innovative points, experiments and the characterization approaches in this thesis are introduced.
Part Two Study on the reaction capability and the pore structure of new material with FCC catalyst
The properties of Jinyang soil taken from Shanxi Province and the catalyst from its in-situ crystallization were studied in the laboratory. The result showed that the essential properties of Jinyang soil met with the requirement for making catalyst by in-situ crystallization, which possessed the stronger and appropriate alkaline dissolvable rates for active alumina and active silica respectively, as well as good performance of crystallization and cracking. After the thermal treatment and chemical modification of kaolin, the certain reactive mesoporous structure was formed in CLS material, and the novel FCC catalyst containing CLS exhibited the excellent heavy oil cracking capability and superior selectivity to desired products.
Part Three Determination of the new material catalyst by X-ray Fluorescence Spectrometry
Chapter One Determination of Phosphorus and Iron in Co-catalyst by X-ray Fluorescence Spectrometry
The aim of this work was to develop a new technique for quantitative analysis of phosphorus and iron contents in co-catalyst by X-ray fluorescence spectrometry (XRFS). A set of synthesized standard samples were prepared for the experiments with this purpose when the interferences of inter-elements were corrected by the Empirical Coefficient Method. The standard samples were manually synthesized, and the powder pellets were used for sample preparation while and the matrix effects were corrected by the experience coefficients. The characteristic X-rays of phosphorus and iron elements could selectively be determined with the enhanced accuracy and reduced time consumption within a range without signal interference from main-component elements. Manufacturing sample and measurement conditions of the new method were brought up; The matrix effects of Co-catalyst samples were verified by Empirical Coefficient Method. The results of experiment showed that the accuracy and precision of this method satisfactorily had the high repeatability. The measuring ranges of elements were w 0.01-2.50% for phosphorus and w 0.01-2.50% for Iron with the relative deviations of 0.34% for Phosphorus and 0.59% for Iron, respectively. This method showed the satisfactory accordant results in comparison with the chemical method and inductively coupled plasma (ICP). It also has provided the analytical values for phosphorus and iron in co-catalyst. This new method has the advantages of satisfactory accuracy, high precision, less interference, easy sample handling and high efficiency. In addition, the samples are not decomposed during the analysis process when each sample only requires 5 minutes to be taken for measurement. This new method will be able to meet the growing demands of quantitative analysis of phosphorus and iron content in co-catalysts. This method had the satisfactory accuracy and precision, so the analytical range was large, and had been successfully applied to the determine phosphorus and iron in co-catalyst.
Chapter Two Determining the content of La on modified zeolite by X-ray Fluorescence Spectrometry
After eliminating particle size effects and mineral effects by sufficiently grinding and using proper preparation methods of standards, absorption-enhancement effects of the XRFS to determine the content of La2O3 on modified zeolite were mainly discussed in this paper. If the absorption-enhancement effects were corrected by the experience coefficients, the results appeared to be in good agreement with the classical chemical method, and can meet the requirements of scientific research analysis and industrial analysis.
引文
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