CN1171835C - 流化床催化裂化过程中选择性生产轻质烯烃的方法 - Google Patents

流化床催化裂化过程中选择性生产轻质烯烃的方法 Download PDF

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CN1171835C
CN1171835C CNB998058149A CN99805814A CN1171835C CN 1171835 C CN1171835 C CN 1171835C CN B998058149 A CNB998058149 A CN B998058149A CN 99805814 A CN99805814 A CN 99805814A CN 1171835 C CN1171835 C CN 1171835C
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P・K・雷德威格
P·K·雷德威格
艾斯皮林
J·E·艾斯皮林
斯图恩兹
G·F·斯图恩兹
沃啻特尔
W·A·沃啻特尔
亨瑞
B·E·亨瑞
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ExxonMobil Technology and Engineering Co
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    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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Abstract

本发明涉及一种将来源于催化裂化或热裂化的石脑油料流选择性生产C2-C4烯烃的方法。石脑油料流与含约从10到50%(重)平均孔径低于约0.7nm结晶沸石的催化剂进行接触，反应条件包括温度从约500到650℃且烃分压从10到40psia。

Description

流化床催化裂化过程中选择性生产轻质烯烃的方法
发明领域
本发明涉及一种将来源于催化裂化或热裂化的石脑油料流选择性生产C2-C4烯烃的方法。石脑油料流与含约从10到50％(重)平均孔径低于约0.7nm结晶沸石的催化剂进行接触，反应条件包括温度从约500到650℃，烃分压从10到40psia。
发明背景
对低排放燃料的需要导致对用于烷基化、低聚、MTBE和ETBE合成过程的轻质烯烃的需求增加。另外，对用作聚烯烃特别是聚丙烯生产原料的低成本轻质烯烃特别是丙烯的需求也不断扩大。
可用来提高烯烃产量的轻质链烷烃固定床脱氢工艺方法近来重新受到注意。但此类方法所需的投资成本及操作费用较高，因而，最好使用投资成本较低的工艺方法来提高烯烃产率。在催化裂化过程中提高烯烃产率的方法会特别有利。
美国专利4,830,728披露了一种能按烯烃产量最大化操作的流化床催化裂化(FCC)装置。FCC装置有两个分别引入不同料流的分开的立管。立管操作设计成其中一个立管中一种适宜的催化剂用来转化重质瓦斯油，而另一个立管中一种适宜的催化剂用来裂解轻质烯烃/链烷烃进料。重质瓦斯油立管内的反应条件可改进成使汽油或烯烃产量最大化。使所期望产物最大化的主要手段是使用了一种特殊催化剂。
另外授权Arco的美国专利5,026,936提出一种通过裂化和复分解反应组合从C4或更高碳进料生产丙烯的工艺方法，其中高碳烃裂化成乙烯和丙烯，且至少一部分乙烯复分解成丙烯。另外参见美国专利5,026,935、5,171,921和5,043,522。
美国专利5,069,776提出通过将进料与包括孔径0.3到0.7nm沸石的移动床沸石催化剂在高于约500℃温度和少于约10秒的停留时间条件下进行接触而将烃进料转化的方法。生产烯烃的同时形成少量饱和气态烃。另外，授权Mobil的美国专利3,928,172提出一种将烃进料转化的方法，是通过烃进料在ZSM-5催化剂存在下进行反应来生产烯烃。
采用FCC装置生产烯烃产品的方法本身所固有的问题是生产过程依赖于特殊催化剂对最大化生产轻质烯烃同时也达到343℃的最高转化率加上进料组成的平衡。此外，即使特殊催化剂平衡可维持总烯烃产量的最大化，由于不期望的副反应，如彻底裂解、异构化、芳化和氢转移反应，使烯烃的选择性一般很低。由不期望的副反应产生的轻质饱和气体导致要增加回收所期望烯烃的费用。因此，希望在能够对C2-C4烯烃选择性高度控制的生产过程中使烯烃产量最大化。
发明概述
按照本发明，提供一种选择性生产C2-C4烯烃的方法，包括将含链烷烃和烯烃的催化裂化或热裂化石脑油料流与含约从10到50％(重)平均孔径低于约0.7nm结晶沸石的催化剂进行接触，反应条件包括温度从约500到650℃，烃分压从10到40psia，烃停留时间为1到10秒，且催化剂与进料的重量比约为2-10，其中约不大于20％(重)链烷烃转化为烯烃。
在优选的具体方案中，提供一种在包括反应区、汽提区和催化剂再生区的生产装置中选择性生产C2-C4烯烃的方法。石脑油料流与反应区所包含的催化剂床，优选为流化态催化剂床接触。催化剂由平均孔径低于约0.7nm的沸石构成，且反应区的操作条件为温度从约500到650℃，烃分压从约10到40psia，烃停留时间为1到10秒，且催化剂与进料的重量比约为2-10，其中约不大于20％(重)链烷烃转化为烯烃。
在本发明另一具体方案中，催化剂为ZSM-5型催化剂。
在本发明另一优选具体方案中，原料含约10到30％(重)链烷烃和从约20到70％(重)烯烃。
在本发明另一具体方案中，反应区的操作温度从约525到600℃。
发明详细说明
能用来生成较高产率C2、C3和C4烯烃的适宜原料是在石脑油沸程范围内且含从约5到35％(重)，优选从约10到30％(重)，且更优选从约10到25％(重)链烷烃和从约15％(重)，优选从约20％(重)到70％(重)烯烃的料流。进料中也可包含环烷烃和芳烃。石脑油沸程料流一般是指沸程从约18℃到约221℃，优选从约18℃到约149℃的料流。石脑油可以是热裂化或催化裂化石脑油。这类料流可从任何适当来源得到，例如可以从瓦斯油或渣油的流化床催化裂化(FCC)得到，或从渣油的延迟焦化或流化焦化得到。本发明实际使用的石脑油料流优选从瓦斯油或渣油的流化床催化裂化得到。这类石脑油富含烯烃和/或二烯烃且链烷烃量相对贫乏。
本发明方法在包括反应区、汽提区、催化剂再生区和分馏区的生产装置中实施。将石脑油料流送入反应区，与热的再生催化剂源接触。在从约500到650℃，优选从约500到600℃的温度下，热催化剂将进料汽化并裂化。裂化反应会在催化剂上沉积含碳烃或焦碳，从而使催化剂失活。裂化产物与结焦催化剂分离并被送入分馏塔。结焦催化剂通过汽提区，用蒸汽从催化剂颗粒中汽提出挥发物。为保留吸附烃用于热平衡，汽提操作可在低深度条件下进行。然后将汽提后的催化剂通过再生区，在含氧气体，优选空气存在下烧去催化剂上的焦碳，将催化剂再生。除焦步骤恢复了催化剂活性，同时将催化剂加热到例如650℃到750℃。然后将热催化剂再循环回反应区与新鲜石脑油料流反应。可将再生器内烧焦形成的烟道气进行处理，除去颗粒物和转化一氧化碳，然后通常将烟道气排放到大气中。从反应区出来的裂化产物被送至分馏区，回收不同产品，尤其是C3馏分和C4馏分。
尽管已设法使FCC生产装置本身增加轻质烯烃的产率，但本发明的实际操作中使用自己一套如上所述的独特生产装置接收来自炼油厂任何适当来源的石脑油。反应区在能使C2到C4烯烃，尤其是丙烯选择性最大化的同时C5+烯烃转化率较高的工艺条件下操作。适用于本发明实际操作的催化剂是由平均孔径低于约0.7纳米(nm)的结晶沸石构成，所述结晶沸石占总流化催化剂的10％到50％(重)。优选结晶沸石选自中孔径(＜0.7nm)结晶硅铝酸盐或称沸石系列。其中特别令人感兴趣的是氧化硅与氧化铝摩尔比小于75∶1，优选小于50∶1且更优选小于40∶1的中孔沸石。孔径有时也称作有效孔径是通过用标准吸附技术和已知最小动力学直径的烃化合物测定的。参见Breck.的《沸石分子筛》和Anderson等人在J.Catalysis 58，114(1979)发表的论文，引入此两篇文献作为参考。
可用于实施本发明的中孔径沸石在W.H.Meier和D.H.Olson编辑的《沸石结构类型图册》(Butterworth-Heineman，第三版，1992)中述及，引入此文献作为参考。中孔径沸石的孔径一般从约0.5nm到约0.7nm，例如包括MFI、MFS、MEL、MTW、EUO、MTT、HEU、FER和TON结构类型的沸石(IUPAC委员会制定的沸石命名法)。这类中孔径沸石的非限定性实例包括ZSM-5、ZSM-12、ZSM-22、ZSM-23、ZSM-34、ZSM-35、ZSM-38、ZSM-48、ZSM-50、Silicalite和Silicalite 2。最优选是在美国专利3,702,886和3,770,614中述及的ZSM-5，在美国专利3,709,979中述及的ZSM-11，在美国专利3,832,449中述及的ZSM-12，在美国专利3,948,758中述及的ZSM-21和ZSM-38，在美国专利4,076,842中述及的ZSM-23，和美国专利4,016,245中述及的ZSM-35。引入所有上述专利作为参考。其它适用的中孔径沸石包括硅铝磷酸盐类(SAPO)，如在美国专利4,440,871中述及的SAPO-4和SAPO-11；铬硅酸盐类；硅酸镓类；硅酸铁类；磷酸铝类(ALPO)，如在美国专利4,310,440中述及的ALPO-11；铝硅酸钛类(TASO)，如EP-A229,295中述及的TASO-45；在美国专利4,254,297中述及的硅酸硼类；铝磷酸钛类(TAPO)，如在美国专利4,500,651中述及的TAPO-11；和铝硅酸铁类。在本发明的一个具体实施方案中，所述沸石的Si/Al比约大于40。
中孔径沸石可包括被认为是由于沸石合成过程中晶体内或晶体表面发生错位造成的“结晶混合物”。引为参考的美国专利4,229,424中披露了ZSM-5和ZSM-11结晶混合物的实例。结晶混合物本身为中孔径沸石，且与沸石物理混合物有所区别，在同样的催化剂复合物或水热反应混合物中，后者中明显有不同沸石结晶或晶粒存在。
本发明催化剂与无机氧化物基体组分结合在一起。无机氧化物基体组分将催化剂组分粘结起来，使催化剂成品的硬度能经受粒子间和反应器壁的撞击。无机氧化物基体可由无机氧化物溶胶或凝胶制成，经干燥后将催化剂组分“粘结”起来。无机氧化物基体优选无催化活性，且由硅和铝氧化物构成。还优选在无机氧化物基体中引入另外的氧化铝相。可采用氢氧化铝-g-氧化铝类，勃姆石，水铝石和过渡氧化铝类如a-氧化铝、b-氧化铝、g-氧化铝、d-氧化铝、e-氧化铝、k-氧化铝和r-氧化铝。优选的氧化铝种类是三氢氧化铝如三水铝石、三羟铝石、新三水氧化铝或doyelite。基体材料可含磷或磷酸铝。
优选的工艺条件包括温度从约500到650℃，优选从约525到600℃；烃分压从约10到40psia，优选从约20到35psia；且催化剂与石脑油之比(重量/重量)从约3到12，优选从约4到10，其中催化剂重量为催化剂复合物总重量。还优选将蒸汽与石脑油料流一起引入反应区，蒸汽包括约50％(重)以内的烃进料。另外，优选石脑油在反应区的停留时间少于10秒，例如从约1到10秒。上述条件应使石脑油料流中的C5+烯烃至少约60％(重)转化为C4-产物，和少于约25％(重)，优选少于约20％(重)的链烷烃转化为C4-产物，且应使丙烯约占总C3反应产物的至少90％(摩尔)，优选大于约95％(摩尔)，同时丙烯/总C2-产物之重量比大于约3.5，优选大于约4.0。还优选乙烯约占总C2产物的至少90％(摩尔)，同时丙烯∶乙烯之重量比大于约4，且“全馏程”C5+石脑油产品的马达法辛烷值和研究法辛烷值都较石脑油进料有所提高。为进一步改善对丙烯的选择性，在供料之前先将催化剂预焦化的步骤属于本发明范围。将有效量的单环芳烃送入反应区来改善丙烯对乙烯的选择性也属于本发明范围。芳烃可以由外部来源供应如来自重整生产装置，或是由来自本过程的重质石脑油循环产物组成。
下面所提出的实施例仅仅是用来例示说明本发明，并不以任何方式限定本发明。
实施例1-12
下面的实施例例示说明能维持化学纯丙烯所采用的临界工艺操作条件，所用样品为经已在815.5℃下蒸热16小时来模拟工业平衡的ZCAT-40(一种含ZSM-5的催化剂)催化裂化的石脑油。比较实施例1和2可以看出提高催化剂/油比能改善丙烯收率，但会牺牲丙烯纯度。比较实施例3和4及5和6可以看出降低油的分压能大大改善丙烯纯度，同时不会损害丙烯收率。比较实施例7和8及9和10可以看出提高温度能使丙烯收率和纯度都得到改善。比较实施例11和12可以看出减少催化剂停留时间能改善丙烯收率和纯度。实施例13示出在采用传统FCC反应器/再生器设计的二段所能达到的反应器温度和催化剂/油比条件下获得高丙烯收率和纯度的实例。
                                                   表1
实施 例 进料烯烃重％ 温度℃ 催化 剂/油  油 psia 油停留时间秒 催化剂停留时间秒 重％C 3 ＝ 重％C 3 - 丙烯纯度％
  1   38.6   566     4.2   36     0.5   4.3   11.4   0.5   95.8
  2   38.6   569     8.4   32     0.6   4.7   12.8   0.8   94.1
  3   22.2   510     8.8   18     1.2   8.6   8.2   1.1   88.2
  4   22.2   511     9.3   38     1.2   5.6   6.3   1.9   76.8
  5   38.6   632     16.6   20     1.7   9.8   16.7   1.0   94.4
  6   38.6   630     16.6   13     1.3   7.5   16.8   0.6   96.6
  7   22.2   571     5.3   27     0.4   0.3   6.0   0.2   96.8
  8   22.2   586     5.1   27     0.3   0.3   7.3   0.2   97.3
  9   22.2   511     9.3   38     1.2   5.6   6.3   1.9   76.8
  10   22.2   607     9.2   37     1.2   6.0   10.4   2.2   82.5
  11   22.2   576     18.0   32     1.0   9.0   9.6   4.0   70.6
  12   22.2   574     18.3   32     1.0   2.4   10.1   1.9   84.2
  13   38.6   606     8.5   32     1.0   7.4   15.0   0.7   95.5
                               续表1
实施例 重％C 2 ＝ 重％C 2 - C 3 ＝/C 2 ＝ C 3 ＝/C 2 - 重％C 3 ＝
    1     2.35     2.73  4.9   4.2     11.4
    2     3.02     3.58  4.2   3.6     12.8
    3     2.32     2.53  3.5   3.2     8.2
    4     2.16     2.46  2.9   2.6     6.3
    5     6.97     9.95  2.4   1.7     16.7
    6     6.21     8.71  2.7   1.9     16.8
    7     1.03     1.64  5.8   3.7     6.0
    8     1.48     2.02  4.9   3.6     7.3
    9     2.16     2.46  2.9   2.6     6.3
    10     5.21     6.74  2.0   1.5     10.4
    11     4.99     6.67  1.9   1.4     9.6
    12     4.43     6.27  2.3   1.6     10.1
    13     4.45     5.76  3.3   2.6     15.0
                 
上面的实施例(1、2、7和8)表明通过选择适当的反应器条件可以达到C3＝/C2＝＞4和C3＝/C2-＞3.5。
实施例14-17
石脑油料流(例如FCC石脑油、焦化石脑油)中所含烯烃和链烷烃经小或中孔径沸石如ZSM-5裂化可生产较大量乙烯和丙烯。对乙烯或丙烯的选择性或对丙烯/丙烷的选择性随催化剂和工艺操作条件而变动。已发现通过将蒸汽与催化石脑油馏分一起同时送入反应器的方法能够提高丙烯收率。催化剂可以是ZSM-5或其它小或中孔径沸石。下表2例示说明将5％(重)蒸汽与含38.8％(重)烯烃的FCC石脑油同时送入时丙烯收率得到的提高情况。尽管丙烯收率提高，但丙烯纯度有所降低。因此，需要调整其它操作条件来维持目标丙烯的选择性。
                                                 表2
实施例 蒸汽同时进料 温度℃ 催化 剂/油 油 psia 油停留时间，秒 催化剂停留时间，秒 重％丙烯 重％丙烷 丙烯纯度％
  14   非   630     8.7     18   0.8   8.0   11.7   0.3   97.5
  15   是   631     8.8     22   1.2   6.0   13.9   0.6   95.9
  16   非   631     8.7     18   0.8   7.8   13.6   0.4   97.1
  17   是   632     8.4     22   1.1   6.1   14.6   0.8   94.8

Claims (7)

1.一种选择性生产C2-C4烯烃的方法，包括将含从10到30重量％链烷烃和15到70重量％烯烃的催化裂化或热裂化石脑油原料与含10到50重量％平均孔径低于0.7nm结晶沸石的催化剂进行接触，反应条件包括温度从500到650℃，烃分压从10到40psia，烃停留时间为1到10秒，且催化剂与进料的重量比为2-10，其中不大于20重量％链烷烃转化为烯烃，丙烯占总C3反应产物的至少90％(摩尔)。
2.按权利要求1的方法，其中催化剂为ZSM-5。
3.按权利要求2的方法，其中反应温度从500到600℃。
4.按权利要求3的方法，其中进料流中的C5+烯烃至少60重量％转化为C4-产物，和少于25重量％的链烷烃转化为C4-产物。
5.按权利要求4的方法，其中丙烯占总C3反应产物的至少95％(摩尔)。
6.按权利要求5的方法，其中丙烯与总C2-产物之重量比大于3.5。
7.按权利要求6的方法，其中丙烯与总C2-产物之重量比大于4.0。
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