CN1832900A - 制备合成气的方法 - Google Patents

制备合成气的方法 Download PDF

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CN1832900A
CN1832900A CNA2004800100790A CN200480010079A CN1832900A CN 1832900 A CN1832900 A CN 1832900A CN A2004800100790 A CNA2004800100790 A CN A2004800100790A CN 200480010079 A CN200480010079 A CN 200480010079A CN 1832900 A CN1832900 A CN 1832900A
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steam
product
steam reformer
reactor
temperature
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W·D·比尔根
F·J·A·马腾斯
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Shell Internationale Research Maatschappij BV
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Abstract

一种由碳质原料制备含氢气与一氧化碳的气体的方法，该方法进行下述步骤：(a)在上端包括燃烧器(52)的垂直取向管式部分氧化反应器(51)中部分氧化碳质原料，从而得到氢气和一氧化碳的第一气态产品，(b)在对流蒸汽重整区(44)中在蒸汽存在下催化蒸汽重整碳质原料，从而得到蒸汽重整产品，(c)将步骤(a)的第一气态产品与步骤(b)的蒸汽重整产品(57)混合，以此降低步骤(a)的第一气态产品的温度，(d)将步骤(c)中得到的混合物与后重整催化剂(53)接触，和(e)通过在步骤(d)中得到的混合物与蒸汽重整反应区之间对流换热为步骤(b)中的对流蒸汽重整反应区提供所需的热量，从而得到温度下降的含氢气和一氧化碳的气体。

Description

制备合成气的方法
技术领域
本发明涉及通过进行部分氧化反应和吸热蒸汽重整反应由碳质原料制备包括一氧化碳和氢气的混合物的方法。
背景技术
EP-A-168892描述了一种吸热蒸汽重整反应，该反应在位于至少一个管内的固定床中进行，通过使部分氧化反应的至少部分热产品气沿管运行而使管内温度保持为800-950℃。根据该公开的专利文献，部分氧化反应(POX)和吸热生产合成气的组合可以提高合成气的产率，提高H2/CO的比，降低每得到一立方米合成气产品使用的氧气量，降低用于生产含CO和H2的气体混合物的设备的投资费用(与部分氧化相比)。
DE-A-3345088描述了进行蒸汽重整反应的反应器和方法。该公开专利文献描述了由天然气原料开始进行蒸汽重整反应的反应器。该反应器由管板组成，多个充填有合适催化剂的管从管板伸入反应器。通过使天然气部分氧化反应的热流出物从反应器管外部通入反应器，以此提供反应需要的热。这种蒸汽重整反应器也称为所谓的对流蒸汽重整反应器(CSR)。
适宜地，需要操作对流蒸汽重整装置和利用部分氧化的热气体。将这些工艺组合在一起时的问题是部分氧化反应得到的气体温度很高，例如是1100-1500℃。如果用这些气体在对流蒸汽重整装置中供热，则必须解决一些实际问题，例如，必须避免CSR反应器中使用的材料因机械疲劳而断裂。因此，目前需要得到一种克服这些实际问题的组合POX和CSR工艺。
发明内容
下述方法可以实现本发明的目的。
一种由碳质原料制备含氢气与一氧化碳的气体的方法，该方法进行下述步骤：
(a)在上端包括燃烧器的垂直取向管式部分氧化反应器中部分氧化碳质原料，从而得到氢气和一氧化碳的第一气态产品，
(b)在对流蒸汽重整区中催化蒸汽重整碳质原料，从而得到蒸汽重整产品，
(c)将步骤(a)的第一气态产品与步骤(b)的蒸汽重整产品混合，以此降低步骤(a)的第一气态产品的温度，
(d)将步骤(c)中得到的混合物与后重整催化剂接触，和
(e)通过在步骤(d)中得到的混合物与蒸汽重整反应区之间对流换热为步骤(b)中的对流蒸汽重整反应区提供所需的热量，从而得到温度下降的含氢气和一氧化碳的气体。
申请人发现：将部分氧化流出物与蒸汽重整装置流出物混合，然后进行后重整步骤，这样可以降低部分氧化流出物的温度，可以在较低温度下运行CSR。由于在较低温度下操作CSR，所以蒸汽重整装置产品中的甲烷含量较高，这可以通过催化后重整步骤进行平衡，在催化后重整步骤中，部分甲烷转化为合成气。
附图说明
图1示出在本发明的装置中的POX和CSR反应器。
具体实施方式
步骤(a)中的碳质原料优选是气态烃，合适的是甲烷、天然气、伴生气或C1-4烃的混合物。气态烃的例子是天然气、炼油气、伴生气或(煤层)甲烷等。合适的气态烃主要包括，即大于90v/v％、特别是大于94v/v％的C1-4烃，特别是包括至少60v/v％的甲烷，优选至少75％，更优选90％的甲烷。优选使用天然气或伴生气。优选脱除原料中所有的硫。
步骤(a)和步骤(b)中的碳质原料优选是上述气态原料。在这种优选实施方案中，步骤(a)和(b)的全部气态原料的10-90wt％、更优选20-50wt％供给步骤(b)。
在步骤(a)中，可以根据公知的原理如Oil and Gas Journal，1971年9月6日，第85-90页中所述Shell Gasification Process进行部分氧化。描述部分氧化工艺例子的公开文献有EP-A-291111、WO-A-9722547、WO-A-9639354和WO-A-9603345。在这些工艺中，优选在没有催化剂的情况下使原料与含氧气体在部分氧化条件下接触。
含氧气体可以是空气(含有约21％的氧气)，优选富氧空气，合适的是最高含有100％氧气的空气，优选含有至少60vol％的氧气，更优选含有至少80vol％的氧气，更优选含有至少98vol％的氧气。可以用深冷技术生产富氧空气，但是优选用膜基法生产，例如WO93/06041中描述的方法。
在步骤(a)中，原料与含氧气体的接触优选在置于反应器内的燃烧器中进行。为了调节步骤(a)中部分氧化反应得到的气态产品中的H2/CO比，可以在原料中加入二氧化碳和/或蒸汽。以气态产品的量计，至多15vol％，优选至多8vol％，更优选至多4vol％的二氧化碳或蒸汽加入原料。作为合适的蒸汽源，可以使用任选的下游烃合成如费-托合成中生产的水。
步骤(a)中部分氧化反应的气态产品的温度通常是1100-1500℃，H2/CO摩尔比是1.5-2.6，优选1.6-2.2。
可以用公知的蒸汽重整工艺实施步骤(b)，其中蒸汽和气态烃原料在CSR反应器中与合适的重整催化剂接触。CSR反应区优选存在于位于POX反应器之后的一个独立反应器中。对流蒸汽反应区优选包括配有一个或多个装有重整催化剂的管的管式反应器。这种反应器的各种设计都是已知的，都适用于本发明。设计应当使用于供热的蒸汽重整产品和合成气在该反应器中作为单独的物流得到。这种反应器概念的例子描述在US-A-6224789中。相对于步骤(b)的原料中以烃存在的碳，蒸汽重整产品中的甲烷含量可以是1-30mol％碳。在优选的实施方案中，相对于步骤(b)的原料中以烃存在的碳，甲烷含量是1-10mol％碳，优选2-5mol％碳。
应用于蒸汽重整反应器管的催化剂和工艺条件可以是蒸汽重整领域的普通技术人员熟知的那些催化剂和工艺条件。合适的催化剂包括任选负载在载体如氧化铝上的镍。气态原料的空速优选是700-1000L(S.T.P.)/L催化剂/hr，其中S.T.P.表示15℃的标准温度和1bar(绝对)的标准压力。蒸汽与碳(烃和CO)的摩尔比优选低于1，更优选0.5-0.9。如果在步骤(b)中使用这种低的蒸汽与碳的比，则催化剂优选包括VIII族金属。催化剂更优选包括(a)氧化物载体材料和(b)包括约0.1wt％至约7.0wt％的至少一种选自Pt、Ni、Pd和Co的金属的涂层，金属优选是铂；所述载体材料包括：(i)至少80wt％的在涂布所述涂层前已经在最高约670℃的温度下煅烧的ZrO2；(ii)0.5-10mol％的至少一种选自Y、La、Al、Ca、Ce和Si的氧化物，优选La2O3。这种催化剂的例子例如在EP-A-695279中描述的催化剂。原料优选还包括一定量的CO2，其中CO2与碳(烃和CO)的摩尔比优选是0.5-2。步骤(b)的产品气的温度优选是600-1000℃，H2/CO摩尔比是0.5-2.5。
在步骤(c)中，将步骤(a)的第一气态产品与步骤(b)的蒸汽重整产品混合，以此降低步骤(a)的第一气态产品的温度。这种混合可以在部分氧化反应器、单独的混合容器或单独的CSR反应器中进行。如果在POX反应器中混合，则优选通过将蒸汽重整产品供给POX反应器的下端，优选远离燃烧器的下半部分进行。使用这种方式时，在混合过程中不会有大量甲烷转化，而温度会下降。因为温度为1100-1500℃的部分氧化反应产品和温度低得多的蒸汽重整产品是在远离燃烧器的位置处混合，所以其温度比部分氧化反应产品的温度下降250-500℃。
在步骤(d)中，步骤(c)中得到的混合物与后重整催化剂接触。这适于通过使气态混合物流经合适的重整催化剂床来实现。这种催化剂床可以位于POX反应器、单独容器或CSR反应器中，这也取决于进行步骤(c)的位置。当在POX反应器中进行步骤(c)时，优选在位于所述容器中的蒸汽重整产品入口的正下方的催化剂床中进行步骤(d)。
甲烷优选在步骤(d)中转化，其中温度下降值适宜为20-70℃，优选40-60℃。步骤(d)中得到的甲烷含量下降的混合物温度优选是950-1100℃，更优选980-1050℃。步骤(d)中的甲烷转化率适宜为10-50wt％。
催化剂床可以是任何公知的重整催化剂，如含镍催化剂或步骤(b)中所述催化剂。
步骤(d)的流出物随后供给CSR反应区，其中气体为所述区供热，得到冷却的最终合成气产品。在步骤(e)中，在CSR反应器中，内构件材料的金属壁表面温度优选保持低于1100℃。
上述方法可以在图1所示的工艺装置中进行。图1示出CSR反应器(44)和POX反应器(51)。CSR反应器(44)上配有充填有蒸汽重整催化剂床(22)的一个或多个平行放置的反应器管(21)，包括用于热气体即步骤(d)的流出物的通道(23)。一个反应器管(21)适合装备1-10个通道(23)。第三个管板(32)在反应器(44)的下端，定义出空间(33)，空间(33)使用于步骤(d)得到的混合物的反应器入口(38)与通道(23)的入口流体连接，通道(23)通过开孔(34)穿过管板(32)，开孔(34)优选比通道(23)本身大。通道不固定在管板(32)上的这一事实是有利的，因为它能使组合的反应器管(21)和通道(23)在启动和冷却条件下在反应器(44)中自由热膨胀。伸入下部空间(33)的通道下端优选用耐热材料如陶瓷制成，因为在所述空间中由于步骤(d)得到的混合物通过反应器入口(38)进入CSR反应器而具有很高的温度。
包括催化剂床(22)的反应器管(21)的出口开孔(35)正好位于所述管板(32)的正上方。所述开孔(35)排出的蒸汽重整产品进入空间(36)，空间(36)定义为管板(40)和(32)之间的空间。这个空间(36)使用于蒸汽重整产品的反应器出口(39)与开孔(35)流体连接。空间(36)中可以适当设置导流片，引导蒸汽重整产品流以之字形流经所述空间，从而优化热蒸汽重整产品气与所述空间中存在的反应器管(21)外表面的接触。在使用时，开孔(35)排出的部分蒸汽重整产品通过出口(39)离开反应器，通过操作反应器，使空间(36)中的压力高于空间(33)中的压力，使另一部分通过开孔(34)离开空间(36)进入空间(33)。在使用时，开孔(35)排出的蒸汽重整产品的优选0-60wt％、更优选0-40wt％进入空间(33)，与步骤(d)的流出物混合。
图1还示出用于天然气和蒸汽的反应器入口(43)、用于热气态介质的反应器入口(38)、用于蒸汽重整产品的反应器出口(39)和用于由通道(23)排出的气体的反应器出口(42)。存在的管板(40)和(41)是为了固定反应器管(21)，定义通道(23)排出气体的收集空间(45)和入口空间(46)，入口空间(46)使用于天然气和蒸汽的反应器入口(43)和包括催化剂床(22)的反应器管(21)流体连接。
图1还示出配有燃烧器(52)的POX反应器(51)，也向燃烧器(52)中供给天然气和氧气(50)。(39)处排放的蒸汽重整产品通过管道(55)和开孔(57)供给POX反应器(51)，以基本在燃烧器(52)周围的循环流外侧的燃烧器(52)下方一定距离处进行混合步骤(c)，循环流存在于反应器上部区域中。这样不会导致存在于蒸汽重整产品中的甲烷大量转化。图1还示出后重整催化剂床(53)和连接管道(56)，将步骤(d)中得到的混合物供给步骤(e)。在步骤(e)中，该混合物供给通道(23)，为蒸汽重整催化剂床(22)供热。
上述工序得到的合成气可有利地用作费-托合成工艺、甲醇合成工艺、二甲醚合成工艺、醋酸合成工艺、氨合成工艺的原料，或者供给使用合成气混合物作为原料的其他工序如涉及羰基化和加氢甲酰化反应的工序。优选向步骤(a)和(b)中供应再循环气。这些再循环气例如在前面例举的使用本发明方法制备的合成气的工艺得到的。这些再循环气可以包括C1-5烃，优选C1-4烃，更优选C1-3烃。这些烃或其混合物在5-30℃(1bar)、特别是20℃(1bar)下是气态。还可以存在氧化化合物如甲醇、二甲醚、醋酸。
本发明特别涉及制备含氢气和一氧化碳的气体(合成气)的方法，其中还可以实施附加步骤(f)和(g)。在步骤(f)中，用费-托催化剂将合成气催化转化为包括烃的物流。在步骤(g)中，步骤(f)的包括烃的物流分离成烃产品和气态再循环物流。适宜的烃产品是具有5个或更多个碳原子、优选4个或更多个碳原子、更优选3个或更多个碳原子的那些产品。气态再循环物流可以包括合成工艺中生产的普通气态烃、氮气、未转化的甲烷和其他原料烃、未转化的一氧化碳、二氧化碳、氢气和水。
在步骤(g)中，再循环物流供给步骤(a)和/或(b)。再循环物流优选供给步骤(a)的燃烧器，或者直接供给部分氧化反应器的上部区域。
任选地，再循环物流供给步骤(a)之前，将再循环物流中存在的部分或全部二氧化碳从再循环物流中分离。部分二氧化碳适于供给步骤(a)。
步骤(f)和(g)可以用公知的费-托工艺如Sasol工艺和ShellMiddle Distillate工艺实施。合适的催化剂的例子基于铁和钴。一般的反应器结构包括浆液反应器和管式反应器。这些工艺和其他工艺例如详细描述在EP-A-776959、EP-A-668342、US-A-4943672、US-A-5059299、WO-A-9934917和WO-A-9920720中。

Claims (8)

1、一种由碳质原料制备含氢气与一氧化碳的气体的方法，该方法进行下述步骤：
(a)在上端包括燃烧器的垂直取向管式部分氧化反应器中部分氧化碳质原料，从而得到氢气和一氧化碳的第一气态产品，
(b)在对流蒸汽重整区中在蒸汽存在下催化蒸汽重整碳质原料，从而得到蒸汽重整产品，
(c)将步骤(a)的第一气态产品与步骤(b)的蒸汽重整产品混合，以此降低步骤(a)的第一气态产品的温度，
(d)将步骤(c)中得到的混合物与后重整催化剂接触，和
(e)通过在步骤(d)中得到的混合物与蒸汽重整反应区之间对流换热为步骤(b)中的对流蒸汽重整反应区提供所需的热量，从而得到温度下降的含氢气和一氧化碳的气体。
2、权利要求1的方法，其中步骤(b)原料中的蒸汽与碳的摩尔比是0.5-0.9。
3、权利要求1-2任一项的方法，其中步骤(a)中得到的氢气和一氧化碳的第一气态产品的温度是1100-1500℃，该温度在步骤(c)中下降300-750℃。
4、权利要求1-3任一项的方法，其中步骤(c)通过将蒸汽重整产品供给部分氧化反应器的下端进行。
5、权利要求4的方法，其中在位于蒸汽重整产品供给所述反应器的位置正下方的部分氧化反应器的下端的催化剂床中进行步骤(d)。
6、权利要求1-5任一项的方法，其中蒸汽重整产品中的甲烷含量相对于步骤(b)的碳质原料中作为烃存在的碳是1-10mol％。
7、权利要求1-6任一项的方法，其中步骤(d)中的甲烷转化率是10-50wt％。
8、权利要求1-7任一项的方法，其中步骤(d)中得到的混合物温度是950-1100℃，优选980-1050℃。
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