CN102791373A - 烯烃裂化催化剂和制造方法 - Google Patents

烯烃裂化催化剂和制造方法 Download PDF

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CN102791373A
CN102791373A CN2011800128813A CN201180012881A CN102791373A CN 102791373 A CN102791373 A CN 102791373A CN 2011800128813 A CN2011800128813 A CN 2011800128813A CN 201180012881 A CN201180012881 A CN 201180012881A CN 102791373 A CN102791373 A CN 102791373A
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zeolite
silica
steam
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T·V·沃斯科博伊尼科夫
M·H·奎克
J·J·塞内塔
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Honeywell UOP LLC
Universal Oil Products Co
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Abstract

本发明提供了新型催化剂和制备该催化剂的方法。该催化剂是用于裂化烯烃的分子筛，并具有改进的选择性，以提高丙烯收率和降低生成的芳烃和甲烷的量。该催化剂已被离子交换以减少该催化剂中的碱成分。

Description

烯烃裂化催化剂和制造方法
优先权声明
本申请要求2010年3月16日提交的美国申请No.12/724,446的优先权。
技术领域
本发明涉及用于烯烃裂化的催化剂和制造烯烃裂化催化剂的方法。
背景技术
乙烯和丙烯分别是每分子具有两个或三个原子的轻烯烃，是用于制造其它有用材料（例如聚乙烯和聚丙烯）的重要化学品。聚乙烯和聚丙烯是如今使用的两种最常见塑料，并具有用于材料制造和用作包装材料的多种用途。乙烯和丙烯的其它用途包括氯乙烯、环氧乙烷、乙基苯和醇的生产。轻烯烃的生产主要通过较大的烃的蒸汽裂化或热解进行。用作轻烯烃生产的原料的烃包括天然气、石油液体和碳质材料，包括煤、再生塑料或任何有机材料。
提高由沸石裂化法制造乙烯时产物部分的转化率的已知方法是通过烯烃的歧化或复分解产生更多乙烯和丙烯。在US 5,026,935和US 5,026,936中公开了这类方法，其中结合使用复分解反应步骤与催化裂化步骤，以通过C4和更重分子的复分解产生更多乙烯和丙烯。催化裂化步骤使用沸石催化剂转化每分子具有4个或更多碳原子的烃流，以制造每分子具有较少碳原子的烯烃。送往沸石催化剂的烃进料流通常含有40至95重量％的每分子具有4个或更多碳原子的链烷烃和5至60重量％的每分子具有4个或更多碳原子的烯烃的混合物。US 5,043,522中公开了用于此类沸石裂化法的优选催化剂是酸沸石，实例包括ZSM-型沸石或硼硅酸盐中的数种。在ZSM-型沸石中，ZSM-5是优选的。据公开，可用于制造乙烯和丙烯的裂化法的其它含沸石的材料包括沸石A、沸石X、沸石Y、沸石ZK-5、沸石ZK-4、合成丝光沸石、脱铝丝光沸石、以及天然生成的沸石，包括菱沸石、八面沸石、丝光沸石等。经过离子交换以替换沸石中存在的碱金属的沸石是优选的。优选的阳离子交换阳离子是氢、铵、稀土金属及其混合物。
欧洲专利No.109,059B1公开了一种方法，其中通过使进料流与具有小于或等于300的硅铝原子比的ZSM-5或ZSM-11沸石在400至600℃的温度下接触而将含有每分子具有4至12个碳原子的烯烃的进料流转化成丙烯。ZSM-5和ZSM-11沸石与氢或铵阳离子交换。该参考文献还公开了，尽管每分子少于4个碳原子的任何烯烃的再循环提高了转化成丙烯的转化率，但没有反应的链烷烃往往积聚在再循环流中。该参考文献提供了附加的低聚步骤，其中使具有4个碳原子的烯烃低聚以促进难以通过常规分馏法与C4烯烃分离的链烷烃（例如丁烷，特别是异丁烷）的脱除。在相关欧洲专利109060B1中，公开了将丁烯转化成丙烯的方法。该方法包括使丁烯与选自硅沸石、boralites、铬硅酸盐和硅铝摩尔比大于或等于350的那些沸石ZSM-5和ZSM-11的沸石化合物接触。该转化在500至600℃的温度和每千克纯沸石化合物5至200千克/小时丁烯的空速下进行。欧洲专利109060B1公开了与选自铬、镁、钙、锶和钡的改性元素一起使用离子交换的、浸渍的或共沉淀形式的硅沸石-1。
催化剂是烃加工中最资本密集的支出之一。催化剂中的改进可改进该催化剂的寿命周期，以使该催化剂可以在裂化和再生之间的周期中更长时间地发挥其裂化功能，由此改进催化剂中的投资收益率。
发明概述
本发明提供了用于烯烃裂化的新型催化剂。该催化剂包含已被蒸汽处理以将碱金属含量降至低于100重量ppm、然后酸洗的分子筛。在一个实施方案中，该催化剂是沸石。优选用于裂化烯烃的沸石是硅沸石（silicalite）沸石。
在另一实施方案中，该催化剂包括粘合剂，例如无机氧化物、二氧化硅、氧化铝、二氧化硅-氧化铝、磷酸铝、二氧化钛、氧化锆和富含二氧化硅的粘土，例如高岭土。
从下列发明详述中可以获得本发明的其它目的、实施方案和细节。
发明详述
轻烯烃生产是一种重要工艺，且轻烯烃的量和质量可以通过较大烯烃的选择性裂化提高。用于生产轻烯烃的正常商业方法是烃原料（例如石脑油）的例如蒸汽裂化和催化裂化。这些裂化法通常产生价值低于乙烯或丙烯的较大烯烃。生成烯烃原料的典型工艺装置包括蒸汽裂化器、精炼厂FCC装置、MTO装置和炼焦器装置。该方法是烯烃裂化法并集成到生成烯烃流的精炼厂系统中，以将较大烯烃转化成轻烯烃。典型进料流包含链烷烃和具有C4至C8烃的烯烃组合物。
该方法使用固定床反应器，其中该方法包括多个反应床，且该方法在不同的反应床之间切换。然后在联机反应床工作过程中将脱机反应床再生。使反应器保持联机对烯烃生产而言是重要的，具有较长循环时间的催化剂能使反应器较长时间保持联机。
烯烃裂化法的运行条件包括500℃至600℃的温度和200至600kPa的运行压力。该方法使用沸石催化剂并提供高丙烯收率。该方法以高空速运行，以在不使用惰性稀释剂流的情况下实现高转化率和高选择性，并使反应器尺寸和运行成本最小化。
本发明是具有较长循环时间的用于裂化烯烃的催化剂。该催化剂是分子筛，该分子筛已经与硝酸铵溶液进行离子交换以将碱金属含量降至低于总分子筛重量的100ppmw。该催化剂然后被蒸汽处理和酸洗。用于烯烃裂化的优选催化剂是沸石，优选的沸石是硅沸石（silicalite）。硅沸石具有高的二氧化硅与氧化铝的比率，该比率优选大于400。
对该催化剂进行离子交换以除去碱金属和碱土金属离子。用铵化合物进行离子交换，其中所述铵化合物可包含硝酸铵、硫酸铵、磷酸铵或氯化铵。优选的铵化合物是硝酸铵。
使该催化剂与硝酸铵溶液进行离子交换以除去碱离子，特别是钠离子Na+。蒸汽处理包括在蒸汽和惰性气氛下在大于500℃的温度下对该催化剂进行蒸汽加工。优选地，蒸汽加工温度为700℃至800℃，更优选的蒸汽加工温度为720℃至740℃。可以用100％蒸汽对所述催化剂进行蒸汽处理，或蒸汽处理步骤可包括蒸汽和惰性气体的组合。惰性气体包括不与催化剂反应的任何惰性气体，包括氮气和氩气，或惰性气体的混合物。
然后用无机酸将该催化剂酸洗。优选的无机酸是硝酸。催化剂的酸洗可除去非骨架氧化铝，以产生更稳定的催化剂。
该催化剂可进一步包括粘合剂。粘合剂为该催化剂提供硬度和耐磨性。粘合剂可占催化剂总重量的10％至90％。粘合剂有助于形成晶粒或使晶粒团聚。
在形成催化剂产品时，催化剂具有干燥催化剂产品的15重量％至50重量％的组成。催化剂产品中的粘合剂构成干燥催化剂产品的10重量％至90重量％。粘合剂优选为该催化剂的10至80重量％，更优选20至70重量％。
可用的粘合剂包括无机氧化物、二氧化硅、氧化铝、二氧化硅-氧化铝、磷酸铝、二氧化钛、氧化锆和富含二氧化硅的粘土，例如高岭土。优选地，粘合剂包含二氧化硅。术语二氧化硅-氧化铝不仅是二氧化硅和氧化铝的物理混合物，还指已共胶凝或共沉淀的酸性和非晶材料。在这方面，可以形成也有效充当吸附剂的其它共胶凝或共沉淀的非晶材料。这些包括二氧化硅-氧化镁、二氧化硅-氧化锆、二氧化硅-氧化钍、二氧化硅-氧化铍、二氧化硅-二氧化钛、二氧化硅-氧化铝-氧化钍、二氧化硅-氧化铝-氧化锆、铝磷酸盐、这些的混合物，等等。然后将该催化剂在至少600℃的温度煅烧。
任选地，可以将粘土添加到该催化剂中。在将催化剂与粘合剂混合之前将粘土添加到催化剂浆料中，并将所得浆料混合和喷雾干燥。在添加粘土时，粘土构成干燥催化剂产品的40重量％至80重量％。
用于制造催化剂的标准程序是首先制备煅烧的沸石。然后用粘合剂（例如二氧化硅）粘合和挤出沸石。然后将挤出的催化剂煅烧，离子交换，蒸汽加工，然后酸洗，再次煅烧。
在一个实施方案中，制成的催化剂是包含硅沸石的沸石，该硅沸石具有大于400的二氧化硅与氧化铝的比率。使该催化剂与硝酸铵进行离子交换以将碱金属和碱土金属离子含量降至低于100ppmw。然后将该催化剂在高于400℃、优选高于500℃的温度下蒸汽处理。该蒸汽处理是蒸汽和惰性气体气氛，其中惰性气体是氮。然后用硝酸将该催化剂酸洗。在最优选的实施方案中，该催化剂包含60重量％至90重量％的沸石和10重量％至30重量％的含二氧化硅化合物的粘合剂。
进行的实验表明，钠离子（Na+）的存在对于最终催化剂（即已经被蒸汽加工和洗涤的催化剂）的选择性是有害的。所用催化剂是硅沸石沸石，形成的催化剂包含70重量％沸石和30重量％非晶二氧化硅。在将催化剂上的钠离子浓度降至低于该催化剂的100重量ppm（通过对形成的催化剂进行ICP（电感耦合等离子体）分析测得）时，选择性显著提高。该催化剂是在实验室中使用商业设备制备的。在催化剂具有降低的钠离子浓度时，选择性提高且并不合意的产物减少。结果显示在下表中。
表：丙烯的收率
Figure BDA00002111528500051
结果是以标准方式制成的催化剂A和C（其中钠浓度大于100ppmw）与催化剂B和D（其中钠浓度已降至小于100ppmw）的比较。催化剂A和B是在实验室中制备的，催化剂C和D是商业制备的催化剂。对于每对样品（A和B，C和D）的蒸汽加工条件是相同的。然后在试验反应器中使用所述催化剂。使40％异丁烯和60％异丁烷的混合物在催化剂上在反应条件下反应。反应条件包括580℃的进料入口温度和13.5hr-1的WHSV。来自反应器的出口压力为150kPa（7psig）。
数据表明，对高-Na催化剂而言，蒸汽处理剧烈性需要高于低-Na材料。如果蒸汽处理剧烈性相同，则催化剂选择性低。
尽管已经用目前被视为优选实施方案的内容描述本发明，但要理解的是，本发明不限于所公开的实施方案，而是意在涵盖所附权利要求的范围内包含的各种修改和等效布置。

Claims (10)

1.用于裂化烯烃的具有较长循环时间的催化剂，其包含：
分子筛，该分子筛：
被离子交换以将碱金属含量降至低于100ppmw；并被蒸汽处理和酸洗。
2.权利要求1的催化剂，其中所述分子筛是沸石。
3.权利要求2的催化剂，其中所述沸石是硅沸石。
4.权利要求3的催化剂，其中所述沸石具有等于或大于400的二氧化硅与氧化铝的比率。
5.权利要求1的催化剂，其中所述沸石被离子交换以除去碱金属和碱土金属离子。
6.权利要求5的催化剂，其中将所述沸石与选自由硝酸铵、硫酸铵、磷酸铵、氯化铵及其混合物组成的组的铵化合物离子交换。
7.权利要求1的催化剂，进一步以催化剂总重量的10重量％至90重量％的量包含粘合剂，其中所述粘合剂选自由无机氧化物、二氧化硅、氧化铝、二氧化硅-氧化铝、磷酸铝、二氧化钛、氧化锆、富含二氧化硅的粘土及它们的混合物组成的组。
8.权利要求7的催化剂，其中所述粘合剂包含二氧化硅。
9.权利要求1的催化剂，其中所述蒸汽处理包括在蒸汽和惰性气氛下在大于500℃的温度下对所述催化剂进行蒸汽加工。
10.权利要求9的催化剂，其中所述蒸汽处理包括蒸汽气氛，或包含蒸汽和惰性气体的气氛。
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