CN1844067A - 在炔烃和二烯的选择性氢化反应中操作下流式沸点反应器的方法 - Google Patents
在炔烃和二烯的选择性氢化反应中操作下流式沸点反应器的方法 Download PDFInfo
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Abstract
本发明公开了使下述流中的炔烃和二烯在下流式沸点反应器中被氢化的方法，所述流包含：氢、甲烷、C2－C6烯烃和烷烃、C2－C6炔烃和二烯、苯、甲苯、二甲苯和其它C6+组分，其中反应热被反应器中的液体吸收，这产生了蒸汽。除了到反应器的进料外，还提供了循环流，其流量足以保证反应器中催化剂粒子被润湿。由第二下游液/汽分离器提供的第三股流被供给到反应器，该第三股流的来源是：对应于反应器中蒸发物料的、来自第一下游液/汽分离器的部分冷凝蒸汽。第三股流的组成控制了流经反应器的液体的稳态组成。
Description
发明领域
本发明涉及一种改进方法，用于在下流式沸点反应器中选择性地氢化烃流中的炔烃和二烯。
背景技术
来自烃蒸汽裂化器骤冷系统的蒸汽产物流典型地主要由氢、甲烷、C2-C6烯烃和烷烃、C2-C6炔烃和二烯、苯、甲苯、二甲苯和其它C6+组分组成。在高压低温箱系统中，首先将氢与甲烷分离之后，通常在后续的蒸馏系统中完成碳数产物的分离和回收。由于相同碳数的烯烃、炔烃和二烯的相对挥发性差异很小，难以生成纯的烯烃产物，这使得蒸馏系统的设计复杂化。解决此问题的一种方法是首先分离碳数馏分，然后选择性地氢化处理每种馏分，以将炔烃和/或二烯转化成相应的烯烃或烷烃。这种所谓的“后段”方法要求针对每种碳数馏分的分离氢化处理系统，而且要将必需量的氢添加到每个系统中。另一种方法是在分离前，使用所含的氢作为转化用的氢源，对进料流进行氢化处理。这种所谓的“前段”方法的优点在于：除去了从进料流到低温箱的大部分氢，从而降低了对低温箱尺寸和冷却的要求。
美国专利出版物2003-0233017-A1(12/18/2003)公开了一种通过如下方式维持经过下流式沸点反应器的混合相流动和温度控制的方法，该方式为：从C5/C6分流器中除去较大量的富含C6+组分的液体流，将该液体流与净蒸汽进料和反应器液体循环流一起供给到反应器，由此将蒸汽馏分中的C6+组分从反应器汽/液分离罐返回到分流器。
本发明的优点是取消了C6+组分从C5/C6分流器的提取和返回。另一个优点是需要较小的C5/C6分流器、和相关的再沸器与冷凝器。
发明概述
本发明提供了一种改进的“前段”氢化处理系统，其允许有效地控制催化剂床内的温度，该催化剂选择性地氢化下述流中的炔烃和二烯，所述流包含氢、甲烷、C2-C6烯烃和烷烃、C2-C6炔烃和二烯、苯、甲苯、二甲苯和其它C6+组分。本发明利用下流式沸点反应器，其中反应热被反应器中的液体吸收，从而产生蒸汽。除了到反应器的进料外，还有来自第一下游液/汽分离器的循环流，其进料速率要足以保证反应器中的催化剂粒子被润湿。
循环到反应器的第三股液体流通过部分冷凝来自第一下游液/汽分离器的一定量蒸汽而被提供，该蒸汽对应于反应器中蒸发的质量，所述蒸汽量通常优选为来自第一下游液/汽分离器的蒸汽流的约30％至50％这一范围，将部分冷凝流输送到第二下游液/汽分离器。第三股流的组成控制了流经反应器的液体的稳态组成。流经反应器的物料的稳态组成与压力一起确定了反应器的温度曲线。
在“沸点反应器”中要一直维持液相，即使反应组分由于反应放热被汽化也是如此。在反应流易于汽化的任何反应中，可以添加惰性的较高沸点的组分来维持液相。
附图简述
该图是本发明一个实施方案的示意性流程图。
优选实施方案详述
有用的催化剂包括VIII族金属。催化剂可以以单独的VIII族金属组分形式使用，或者以彼此掺合或与本领域已知的改性剂(尤其是VIB族和IB族元素)掺合的形式使用。可用于炔烃和二烯的选择性氢化的催化剂包括：负载于氧化铝上的氧化钯。镍催化剂也能催化1，2-丁二烯和炔烃的选择性氢化。然而，对于这些反应，优选钯催化剂。一种此类催化剂包含负载于1/8英寸球上的0.34wt.％钯，商品名为G68C，由Süd-Chemie(以前的United Catalyst Inc.)提供。另一种催化剂包括负载于8-12筛目球上的0.5wt.％钯，商品名为E144SDU，由Calcicat，Catalyst and Performance Chemicals Division，Mallinckrodt，Inc.提供。为了得到最佳结果，将催化剂负载于整装填料中，其公开于共同拥有的美国专利5,730,843中。然而，催化剂可以简单地放置于反应器中。
现在参照附图，烃流中炔烃和二烯的选择性氢化反应在下流式沸点反应器中进行，所述烃流包含比炔烃和二烯的量(按摩尔计)显著多的氢和烯烃。下流式沸点反应器被表示为塔10，其为垂直放置的反应器，包含负载于整装填料12中的颗粒催化剂。气相进料流通过流送管101供给到塔10的顶部。源于分离器20的流送管102和源于液/汽分离器30的流送管104中的液体也供给到流送管101中，这在下面有更加具体的描述。气体和液体流同时向下流经塔，流动方式是气相连续的。气体和液体的并流消除了失控(runaway)反应的可能性。补偿(trim)加热器(未示出)可以安装在流送管101内，以确保反应器的入口进料温度足以引发选择性氢化反应。
反应器10进行绝热操作，以使反应热优选通过蒸发轻质液相组分而被吸收。流送管105中来自反应器的流出物被供给到汽/液分离器20，在那里蒸汽与液体分离。流送管106中的蒸汽被输送到冷凝器70，运行该冷凝器70以冷凝足够的蒸汽，用于补充反应器10中蒸发的物料、和来自分离器30的流送管104中回收的液体。流送管102中的液体被供给回到反应器10。流送管102中流的流速是可变的，并且被维持为至少足以确保反应器10中所有位置的催化剂粒子都被充分润湿。流送管104中的流提供了补偿物料，其对应于反应器中蒸发的物料，该蒸发物料作为流送管103中流的一部分离开反应器系统。流送管104中流的组成控制了流经反应器10的液体的稳态组成。这是重要的控制参数，它与反应器压力一起确定了反应器温度曲线。滑流被流送管107导出，以控制汽/液分离容器20中的液体存量。
塔40是C5/C6分流器。该塔的进料是来自分离器30的流送管103中的蒸汽。塔40被设计为通过流送管108来回收蒸汽馏分，其基本不含C6+组分；并通过流送管109回收底部液体产物，其基本不含C5以及更轻的组分。塔顶馏出物通过流送管130导出，经过分凝器50，在那里重组分被冷凝。塔顶馏出物在接受分离器60中被收集，在那里液烃通过流送管120被提取，并作为回流返回到塔40中。水通过流送管110被导出。注意，蒸馏产物通过流送管108被移去。
实施例
如图所示，系统进料是来自产生烯烃的蒸汽裂化器的骤冷塔并经过压缩和酸性气体(CO2和H2S)脱除后生成的蒸汽产物。反应器装有约14,000ft3整装填料，该填料中装有氢化催化剂。床尺寸为：直径约15ft，长70ft。反应器的操作条件为：反应器的顶部/底部压力为250/240psia；液体循环速率(流送管102中的流)为4,792,100lbs./hr；流送管107中的滑流流量为2854lbs./hr。蒸馏塔40被构造为：20级(理论)顶部段的直径为16.4ft，20级(理论)底部段的直径为10.5ft。蒸馏塔40的设计条件是：回流比0.18；回流温度136；冷凝器压力为238psia；塔的压降为2psi。热量和物料的衡算结果如下表所示。
表
热量和物料的衡算
| 101 | 102 | 103 | 104 | 105 | 106 | 107 | 108 | 109 | 110 | |
| 温度压力psi蒸汽馏分摩尔流量lb/mol/hr质量流量lb/hr体积流量cuft/hr焓MMBtu/hr质量流量lb/hrH2COCO2H2S甲烷乙炔乙烯 | 205.32500102,5096,113,9701,030,270-468.6959,4091,6170.00.0130,9404,589314,462 | 223.5240064,3064,792,100115,181-354.083130650.00.010,34025857,820 | 122.8240128,127786,912670,898-123.2496,1231,5410.00.0118,388846243,092 | 23.424008,4156527,10512,946-131.63119120.00.02,1957214,926 | 223.42400100,8956,108,3901,133,170-470.6116,2711,6170.00.0130,9241,178315,852 | 223.5240136,5881,316,2901,019,730-116.5246,1411,5520.00.0120,584919258,032 | 224.724001047,854189-0.532000.00.017094 | 80.62381027,527748,504604,109-121.2856,1231,5410.00.0118,405847243,187 | 397.9240052343,0001,210-2.5730.00.00.00.00.00.00.0 | 80.6238571,02617-6.9910.00.00.00.00.00.00.0 |
表(续)
| 乙烷 | 74,413 | 17,235 | 54,817 | 4,696 | 76,755 | 59,520 | 28 | 54,845 | 0.0 | 0.0 |
| 丙酮丙二烯丙烯丙烷丁二烯叔丁烯1-丁烯顺-2-丁烯异丁烯异丁烷丁烷1-戊烯己烷辛烷苯甲苯间二甲苯邻二甲苯 | 5,9909,659288,27410,52743,69269,576176,07974,82360,11422,35129,539456,502419,239330,9711,910,1701,293,4707,2235,416 | 7033,512114,1965,0483,34742,798125,47447,38434,81112,30618,297346,437363,810318,5001,728,9401,235,3407,0525,302 | 5263,022144,9196,1571,33415,00554,13314,82415,4226,4646,86841,3648,94440621,5012,57432 | 2121,01033,8661,51392611,70135,15912,5369,8243,5614,96973,61145,91511,478158,90653,510153102 | 1,4467,560293,18612,7275,60369,273214,56674,47460,02422,36030,040462,722418,925330,3391,907,7201,291,3807,2075,406 | 7434,047178,9907,6792,25626,47489,09227,09025,21310,05411,744116,28555,11511,839178,77356,040155104 | 161868671206795720305515845942,7762,0561410 | 5273,028145,1046,1651,34015,07654,33814,90315,4796,4846,89841,7473390.033600.00.0 | 0.00.00.00.00.00.00.00.00.00.00.01689,1891,00023,9414,6301812 | 0.00.00.00.00.00.00.00.00.00.00.00.00.00.00.00.00.00.0 |
表(续)
| 对二甲苯 | 7,937 | 7,745 | 4 | 171 | 7,920 | 175 | 16 | 0.0 | 20 | 0.0 |
| 乙苯苯乙烯壬烷癸烷十一烷十二烷十三烷十四烷十五烷水丙二烯异戊二烯己二烯己烯戊烷 | 10,4384,429331000053,9587,9648,0853,897149,072119,144 | 10,1704,338331000039,749365223131,69298,612 | 6200000004,45506313,76910,340 | 2408200000009,7031123317,38020,532 | 10,4164,421331000054,278483826152,927130,003 | 24583000000014,5291186321,23531,391 | 208000000050010.0212154 | 0.00.000000001,2420560.030310,193 | 261000000000.00.0813,678301 | 0.00.000000001,0260.00.00.00.00.0 |
Claims (4)
1.一种用于氢化下述流中的炔烃和二烯的方法，所述流包含：氢、甲烷、C2-C6烯烃和烷烃、C2-C6炔烃、二烯、苯、甲苯、二甲苯和其它C6+组分，该方法包括以下步骤：
(a)使所述流通过下流式沸点反应器中所含的氢化催化剂，该下流式沸点反应器在反应器中混合物的沸点温度下操作，反应热被沸腾液体吸收以产生第一液/汽流出物，一部分炔烃和二烯被转化为相应的相同碳数的烯烃和烷烃；
(b)将第一液/汽流出物分离为第一液体和第一蒸汽；
(c)将一定量的一部分第一液体返回到所述下流式沸点反应器中，该量确保在所述下流式沸点反应器中所有位置的催化剂都被充分润湿；
(d)冷凝对应于反应器中蒸发物料的一部分第一蒸汽，以产生第二液/汽流出物；
(e)将第二液/汽流出物分离为第二液体和第二蒸汽；和
(f)使所述第二液体返回到所述下流式沸点反应器，从而控制流经反应器的物料的稳态组成。
2.如权利要求1所述的方法，其中所述第二蒸汽被供给到C5/C6分流器，其中C5和较轻的物料作为顶部馏出物被导出，C6和较重的物料作为底部馏出物被导出。
3.如权利要求1所述的方法，其中第一液体和所述第二液体被循环回到所述下流式沸点反应器的顶部。
4.如权利要求1所述的方法，其中被冷凝的部分第一蒸汽占蒸汽总量的约30％至50％。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11/101,098 | 2005-04-07 | ||
| US11/101,098 US7408090B2 (en) | 2005-04-07 | 2005-04-07 | Method of operating downflow boiling point reactors in the selective hydrogenation of acetylenes and dienes |
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| CN (1) | CN1844067A (zh) |
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| WO (1) | WO2006110201A2 (zh) |
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| US8471082B2 (en) * | 2008-03-14 | 2013-06-25 | Catalytic Distillation Technologies | Process for converting methane to ethylene |
| US8324442B2 (en) * | 2009-03-03 | 2012-12-04 | Amyris, Inc. | Microbial derived isoprene and methods for making the same |
| EP2976367B1 (de) | 2013-03-20 | 2021-04-28 | BYK-Chemie GmbH | Verfahren zur herstellung funktionalisierter thermoplastischer elastomere |
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| US4316997A (en) | 1976-02-23 | 1982-02-23 | Varen Technology | Alkylation process and apparatus useful therein |
| US4317949A (en) | 1976-02-23 | 1982-03-02 | Varen Technology | Alkylation process and apparatus useful therein |
| US4419328A (en) | 1981-07-30 | 1983-12-06 | Mobil Oil Corporation | Controlled fluidized bed reactor for testing catalysts |
| US4529573A (en) | 1982-06-17 | 1985-07-16 | Uop Inc. | Gas injection control |
| US5177289A (en) | 1982-11-17 | 1993-01-05 | Chemical Research & Licensing Company | Method for conducting exothermic reactions |
| US5003124A (en) | 1982-11-17 | 1991-03-26 | Chemical Research & Licensing Company | Oligomerization process |
| US5190730A (en) | 1982-11-17 | 1993-03-02 | Chemical Research & Licensing Company | Reactor for exothermic reactions |
| US4950803A (en) | 1982-11-17 | 1990-08-21 | Chemical Research & Licensing Company | Etherification process |
| US4621062A (en) | 1984-04-27 | 1986-11-04 | Phillips Petroleum Company | Control of an isomerization process |
| US5840259A (en) | 1993-04-05 | 1998-11-24 | Catalytic Distillation Technologies | Boiling point reactor with heat removal |
| US5792428A (en) | 1994-07-18 | 1998-08-11 | Chemical Research & Licensing Company | Apparatus for conducting exothermic reactions |
| US6413413B1 (en) | 1998-12-31 | 2002-07-02 | Catalytic Distillation Technologies | Hydrogenation process |
| US7273957B2 (en) | 1999-05-04 | 2007-09-25 | Catalytic Distillation Technologies | Process for the production of gasoline stocks |
| FR2810991B1 (fr) * | 2000-06-28 | 2004-07-09 | Inst Francais Du Petrole | Procede pour l'hydrogenation de coupes contenant des hydrocarbures et notamment des molecules insaturees contenant au moins deux doubles liaisons ou au moins une triple liaison |
| US6596913B1 (en) | 2001-02-23 | 2003-07-22 | Catalytic Distillation Technologies | Recovery of tertiary butyl alcohol |
| US6858770B2 (en) | 2001-08-21 | 2005-02-22 | Catalytic Distillation Technologies | Paraffin alkylation |
| US6620965B1 (en) | 2002-03-08 | 2003-09-16 | Catalytic Distillation Technologies | Process for vinyl acetate |
| US6824676B1 (en) | 2002-03-08 | 2004-11-30 | Catalytic Distillation Technologies | Process for the selective desulfurization of a mid range gasoline cut |
| US6867338B2 (en) | 2002-03-15 | 2005-03-15 | Catalytic Distillation Technologies | Selective hydrogenation of acetylenes and dienes in a hydrocarbon stream |
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| US20060229477A1 (en) | 2006-10-12 |
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| WO2006110201A2 (en) | 2006-10-19 |
| WO2006110201A3 (en) | 2007-11-01 |
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