原位晶化材料合成及加氢裂化催化应用研究
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摘要
原位晶化催化材料合成制备的核心就是将分子筛合成与原位生长概念相结合,将一种最重要的石油裂解分子筛Y沸石晶粒直接生长在基质上而得到的催化材料。本文从传统原位FCC催化剂制备特点出发,针对现有原位晶化工艺的不足,进一步依据加氢裂化催化剂的应用要求,分别提出了各种改进性和独创性的原位催化材料合成概念和技术方案。首先,不仅实现了廉价煤系高岭土原位合成的工业化可行路线,而且通过合成条件和参数优化实现了快速原位合成,将现有长达近30h的晶化时间能缩短到12h甚至6h;其次,将一系列分子筛合成与创新的广义原位生长概念相结合,通过扩大基质选择范围提出金属原位复合方法并制备了一系列多元改性载体或原位分子筛材料,包括涉及多孔无定形材料的固相原位合成方式,也包括将稀土、钛、锌、锆等结构性或电子性助剂原位引入形成多元原位复合材料的方法,如一种锌改性原位催化材料,原位负载量高达3.5%时结晶度高仍可达56%;同时应用原位自转晶方式通过异种分子筛转化得到了具有独特形貌、孔结构及催化特质的新材料,方法涉及无外加硅源或外加固相硅源的高岭土原位合成以及独特的介孔材料自转晶原位合成,特别地,后者是在不同方法制备的螺旋和纳米粒状形貌介孔分子筛基础上,利用介孔材料自转晶得到了接近纳米大小品粒和孔容比传统法高出60%的新型高硅B分子筛。
通过本文新型原位合成法,制备了在形态和性能上都有别于传统分子筛的原位晶化材料,同时各种表征手段和分析也显示了其晶粒变小、孔径增大的趋势,且形态和酸度特征上也表现了与传统分子筛的差异化,而这些特征经过论证都更有利于应用在处理重要质大分子原料的加氢裂化催化剂上,例如100～200hm的小晶粒、40%甚至60%以上的集中的4～20nm中孔分布、更高的B/L酸比例等。在这些新型原位晶化催化材料的基础上,也基于拓展原位催化概念应用范围的需要,本文强化了新型原位催化材料在工业催化应用特性的研究,尤其是跳出原位晶化FCC催化剂范畴,转向代表清洁化生产的加氢裂化催化剂领域,进一步研究完善加氢裂化催化剂设计内涵并实践了新型原位概念的加氢裂化催化剂开发。实验结果表明,原位分子筛材料不仅表现了具有更高本征催化效率的特点,而且突出表现了优异的开环裂解性能,所涉及的所谓原位型加氢裂化催化剂能获得比常规催化剂低2～3个单位的低BMCI值尾油。低尾油BMCI值尾油是需求量很大的优质制乙烯原料,而炼厂加工重质高芳烃劣质原料比例的增加也越来越需要开环性能更优异的分子筛材料,因此原位型催化材料的研究不仅为未来加氢裂化催化剂应用发展提供了一个全新的材料平台,也为加氢裂化催化剂的发展进步拓展了一个新的空间。
This dissertation focus on the research and development of an in-situ synthesis catalytic material which is important in the field of petroleum cracking. Such special material is featured for which a famous FAU zeolite, Y type zeolite, crystallized in hydrothermal condition and directly grows on the surface of a kind of matrix. Referring to characteristic of traditional in-situ synthesis FCC catalyst and concerning about the shortcomings of present in-situ synthesis technology while basing on the requirements of hydrocracking catalyst, this research presents a series of modified schemes or novel methods according innovative in-situ synthesis concept. Firstly, while a low-cost industrial in-situ Y zeolite can be produced by the use of various cheap coal series kaolin matrix, a fast in-situ synthesis technology by optimizing preparation condition or parameters can be realized with crystallization time declining from present about 30h to less 12h or even more 6h. Secondly, by combining zeolite synthesis with expanding in-situ concept, a series of new multi-component zeolites can be prepared by in-situ compounding referring to not only solid synthesis process using porous amorphous material as feed but also in-situ recombination of electrical or structure auxiliaries such as titanium, zinc and rare earth, etc., which, for example, a zinc-incorporate in-situ Y zeolite has crystallinity 56% with as high as 3.5m% zinc content. Moreover, by the new concept of in-situ crystal self-transformation, different modified in-situ synthesis methods are developed related to free-of silica source or solid silica present and kinds of zeolie are attained with different appearance or granular-size, which, for example, a micro screw-form or nanometer sphere-form mesoporous zeolite was assembleded and then a new crystal self-transformation (3 zeolite with 60% more pore volume than traditionalβ zeolite was also synthesized by the use of these mesoporous materials.
Depending on the new in-situ synthesis given by our research, a series of novel in-situ synthesis catalytic materials are prepared, whose characteristics differ from traditional material as they show super-micro crystal granular with 100-200 nm size, high B/L acidity ratio and concentrated mesoporous pore distribution in the range of 4-20nm with 40% or more than 60% ration. Furthermore, this dissertation and related research does much more effort on catalytic application of new in-situ synthesis. Getting rid of limitation of in-situ concept in the scope of FCC catalyst, much more works have been done on dual-function catalyst design, recipe optimization, hydrocracking process evaluation, hydrocracing operating way and product-cut scheme in order to coordinate properties of new in-situ material with requirement of hydrocracking process and its catalyst. It is demonstrated that, in one aspect, in-situ zeolite has more effective catalytic capability based on unit active site, in another aspect, it has excellent ring-open activity as so called in-situ type hydrocracking catalyst can produce tail oil with generally 2-3 unit lower than traditional hydrocracking catalyst on BMCI index. While low BMCI index tail oil is high quality ethylene feed, refineries have to treat more and more inferior feeds with high aromatic content. Thus, in-situ catalytic material or zeolite will provide a new material application reservoir and give hydrocracking catalyst R&D more space on selection and change. Also, a new opportunity for advancement for hydrocracking technology is presented.
通过本文新型原位合成法,制备了在形态和性能上都有别于传统分子筛的原位晶化材料,同时各种表征手段和分析也显示了其晶粒变小、孔径增大的趋势,且形态和酸度特征上也表现了与传统分子筛的差异化,而这些特征经过论证都更有利于应用在处理重要质大分子原料的加氢裂化催化剂上,例如100～200hm的小晶粒、40%甚至60%以上的集中的4～20nm中孔分布、更高的B/L酸比例等。在这些新型原位晶化催化材料的基础上,也基于拓展原位催化概念应用范围的需要,本文强化了新型原位催化材料在工业催化应用特性的研究,尤其是跳出原位晶化FCC催化剂范畴,转向代表清洁化生产的加氢裂化催化剂领域,进一步研究完善加氢裂化催化剂设计内涵并实践了新型原位概念的加氢裂化催化剂开发。实验结果表明,原位分子筛材料不仅表现了具有更高本征催化效率的特点,而且突出表现了优异的开环裂解性能,所涉及的所谓原位型加氢裂化催化剂能获得比常规催化剂低2～3个单位的低BMCI值尾油。低尾油BMCI值尾油是需求量很大的优质制乙烯原料,而炼厂加工重质高芳烃劣质原料比例的增加也越来越需要开环性能更优异的分子筛材料,因此原位型催化材料的研究不仅为未来加氢裂化催化剂应用发展提供了一个全新的材料平台,也为加氢裂化催化剂的发展进步拓展了一个新的空间。
This dissertation focus on the research and development of an in-situ synthesis catalytic material which is important in the field of petroleum cracking. Such special material is featured for which a famous FAU zeolite, Y type zeolite, crystallized in hydrothermal condition and directly grows on the surface of a kind of matrix. Referring to characteristic of traditional in-situ synthesis FCC catalyst and concerning about the shortcomings of present in-situ synthesis technology while basing on the requirements of hydrocracking catalyst, this research presents a series of modified schemes or novel methods according innovative in-situ synthesis concept. Firstly, while a low-cost industrial in-situ Y zeolite can be produced by the use of various cheap coal series kaolin matrix, a fast in-situ synthesis technology by optimizing preparation condition or parameters can be realized with crystallization time declining from present about 30h to less 12h or even more 6h. Secondly, by combining zeolite synthesis with expanding in-situ concept, a series of new multi-component zeolites can be prepared by in-situ compounding referring to not only solid synthesis process using porous amorphous material as feed but also in-situ recombination of electrical or structure auxiliaries such as titanium, zinc and rare earth, etc., which, for example, a zinc-incorporate in-situ Y zeolite has crystallinity 56% with as high as 3.5m% zinc content. Moreover, by the new concept of in-situ crystal self-transformation, different modified in-situ synthesis methods are developed related to free-of silica source or solid silica present and kinds of zeolie are attained with different appearance or granular-size, which, for example, a micro screw-form or nanometer sphere-form mesoporous zeolite was assembleded and then a new crystal self-transformation (3 zeolite with 60% more pore volume than traditionalβ zeolite was also synthesized by the use of these mesoporous materials.
Depending on the new in-situ synthesis given by our research, a series of novel in-situ synthesis catalytic materials are prepared, whose characteristics differ from traditional material as they show super-micro crystal granular with 100-200 nm size, high B/L acidity ratio and concentrated mesoporous pore distribution in the range of 4-20nm with 40% or more than 60% ration. Furthermore, this dissertation and related research does much more effort on catalytic application of new in-situ synthesis. Getting rid of limitation of in-situ concept in the scope of FCC catalyst, much more works have been done on dual-function catalyst design, recipe optimization, hydrocracking process evaluation, hydrocracing operating way and product-cut scheme in order to coordinate properties of new in-situ material with requirement of hydrocracking process and its catalyst. It is demonstrated that, in one aspect, in-situ zeolite has more effective catalytic capability based on unit active site, in another aspect, it has excellent ring-open activity as so called in-situ type hydrocracking catalyst can produce tail oil with generally 2-3 unit lower than traditional hydrocracking catalyst on BMCI index. While low BMCI index tail oil is high quality ethylene feed, refineries have to treat more and more inferior feeds with high aromatic content. Thus, in-situ catalytic material or zeolite will provide a new material application reservoir and give hydrocracking catalyst R&D more space on selection and change. Also, a new opportunity for advancement for hydrocracking technology is presented.
引文
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