CN1037760C - 碳氢化合物的蒸汽重整方法 - Google Patents

碳氢化合物的蒸汽重整方法 Download PDF

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CN1037760C
CN1037760C CN94105617A CN94105617A CN1037760C CN 1037760 C CN1037760 C CN 1037760C CN 94105617 A CN94105617 A CN 94105617A CN 94105617 A CN94105617 A CN 94105617A CN 1037760 C CN1037760 C CN 1037760C
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I·I·普林达尔
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Abstract

碳氢化合物在蒸汽重整催化剂存在下进行高温蒸汽重整的方法，其中催化剂放置在至少包括上下两层的固定床中，其特征在于催化剂床上层厚度为0.30-0.60米并且上层催化剂颗粒的活性是下层催化剂颗粒的活性的1-50%。所述的催化剂床下层还可分成许多亚层，而相对上层催化剂而言，各亚层催化剂的蒸汽重整活性不断提高。

Description

碳氢化合物的蒸汽重整方法
本发明的目的是制备富含氢气和一氧化碳的气体。具体地说，本发明涉及通过碳氢化合物原料的高温催化蒸汽重整来制备这种气体的方法和反应器。
富含有氢气和一氧化碳的气体主要用作生产氨和甲醇的合成气体原料，还有用于炼钢以及作为燃料或家用煤气。
目前工业制备方法包括高温蒸汽重整方法如碳氢化合物的自热催化重整或初次和二次蒸汽重整。
高温蒸汽重整方法中碳氢化合物原料和空气、氧气、或富氧空气在安装在反应器顶部的燃烧炉中一起燃烧。氧气的供应量应低于完全燃烧所需的量，流出气体中的氢气和一氧化碳主要通过燃烧反应而成：
       (1)
       (2)无论何种碳氢化合物原料，这种反应都是强放热反应。这种方法最常用于较轻质原料的重整，其中原料范围可从天然气到沸点最高达200℃的粗汽油馏分。
在该过程中，只有部分碳氢化合物原料在上述燃烧反应(1，2)中被含氧气氛氧化。燃烧后气流中残留的碳氢化合物通过吸热反应进行催化蒸汽重整：
催化蒸汽重整过程在约900-1400℃下完成。在进料中加入蒸汽是为了调节火焰温度和提高炉流出气体中的碳氢化合物转化率。
在反应器的上部，与蒸汽混合的碳氢化合物进料与含氧气氛一起燃烧。燃烧后气体中残存的碳氢化合物在反应器下部以固定床形式放置的催化剂存在下进行蒸汽重整。吸热的蒸汽重整反应所需的热能通过反应器上部催化床上方的燃烧段流出的热气供给。随着燃烧气体和催化剂接触，催化剂床中的蒸汽重整反应使气体温度降至900-1100℃。
为了能够承受放热燃烧反应(1，2)产生的高温，反应器壳体内壁通过耐火绝热材料衬里而得到保护。
目前，上述类型的常用工业反应器的衬里材料含有90％以上的氧化铝。尽管这些材料是具有良好耐热和耐磨性的高强度铸件或砖，但通过与含有碳氧化物，蒸汽和氢气的热燃烧气体接触而使反应器上部燃烧区周围常发生严重损坏。气体的还原性使耐火材料中的氧化铝还原成低级铝氧化物，这种低级铝氧化物在反应器上部的高温环境中易挥发。
反应器衬里的挥发性降解产物与原料气中所含高温下易挥发的杂质一起在温度低于降解产物和杂质的气化温度的反应器区域和下游的反应设备中沉淀下来。
包含高活性蒸汽重整催化剂床的反应器中，床上部催化剂表面温度比燃烧气体温度低很多，因此固体主要沉积在催化剂床的最上层。
因此，固体基本上是在催化剂床最上部沉积成薄层并使该层中气体传送受到限制，从而使床的次层中气流分布不均匀，最终在催化剂床上形成不利的通道。
现已发现在碳氢化合物的高温催化蒸汽重整方法中，在催化剂床的最上层采用对碳氢化合物的蒸汽重整过程具有低活性的催化剂颗粒，而在后续层中逐渐提高催化剂颗粒的活性，即可避免出现上述问题。催化剂床中进行的吸热蒸汽重整反应时大面积的催化剂表面上的温度降低程度得以减缓，从而使床最上部分只有少量固体沉积。这样可在催化剂床中的大面积上进行固体沉积并且使催化剂床中的气体传送得以大幅度改善。
按照这一发现，本发明提出在重整反应器中以固定床形式放置的蒸汽重整催化剂存在下进行碳氢化合物高温蒸汽重整的改进方法，其中催化剂床至少包括上下两层，其中上层的催化剂颗粒对碳氢化合物蒸汽重整过程的活性低。
按照本发明，在催化剂床上层使温度下降程度足够降低，其中将上层催化剂颗粒的活性降低，从而使其活性达到下层催化剂颗粒的活性的1-50％。
在本发明方法和反应器的操作过程中，将预热至约400-700℃的碳氢化合物原料引入具有耐火衬里的反应器上部燃烧炉中。在该燃烧炉中，原料与氧气和含氧气氛混合。氧气用量使氧/碳摩尔比优选达到0.5-0.7，蒸汽/碳摩尔比优选达到0.5-2.0。本发明方法在自热催化重整条件下进行操作时，适用于本发明方法的碳氢化合物原料范围可从甲烷到沸点最高达200℃的粗汽油馏分，其中包括天然气，液化石油气和一次重整气体。
燃烧炉流出的气体含有未转化的碳氢化合物，然后让其通过重整反应器中燃烧炉燃烧段下面以固定床形式放置的蒸汽重整催化剂。
在燃烧段常用的1000-1500℃下，反应器衬里的分解产物，燃烧炉或工艺原料气体中的外来组分可挥发并随流出气体进入催化剂床。
由于流出气体中的残留碳氢化合物在催化剂上进行吸热蒸汽重整，所以催化剂床上层的催化剂表面温度要比采用具有常规蒸汽重整活性的催化剂如含镍和/或钼的已知催化剂时的周围气体温度低约100-150℃。当常规蒸汽重整催化剂的活性降低到5％时，上层催化剂的温度降低程度降低到约25℃。结果是随着催化剂床上层的催化剂表面温度变化减缓，使得固体化合物在催化剂表面的沉积过程分散在床中的大面积上进行。
从下表2可明显看出，在给定气体组成(表1)情况下，催化剂床的表面温度可在比较大的温度范围内受到控制。所要求的催化剂表面温度将取决于流出气体中固体的挥发性。
                        表1
 气体组成(按干燥状态计)   催化剂床进口   催化剂床出口
     H2      mol％       56.7       62.4
     N2      mol％        7.0        6.1
     CO       mol％       21.4       21.5
     CO2     mol％        8.3        8.3
     CH4    .mol％        5.7       0.94
     Ar      .mol％       0.91       0.79
     H2O     mol％       33.9       28.2
                            表2
自热重整
温度分布-催化剂床：
由丹麦Haldor Tops_e A/S提供的镍重整催化剂RKS-2
  相对活性        100％        30％        10％
  轴距(m)        温度气体     催化剂        温度气体      催化剂        温度气体       催化剂
    0.00   1150    1089  1150       1109 1150        1127
    0.02   1106    1062  1119       1086 1132        1112
    0.10   1020    1008  1045       1031 1078        1067
    0.20    992     989  1007       1002 1040        1034
    0.30    985     985   993        991 1018        1014
    0.40    984     983   987        986 1005        1003
    0.60    983     983   984        984  992         991
在工业用高温重整反应器中，将30至60厘米的催化剂床上层的常规重整催化剂的活性降低90％通常就足够使催化剂床上部的固体量降低到不会不利地限制气体传送过程的程度。
将催化剂层分成许多亚层并且使在反应气体的流动方向上不断提高催化剂的活性就可固体的沉积过程分散在催化剂床的后续各层进行。
用少量活性材料浸渍合适的载体或从浸渍的催化剂颗粒中浸滤出一部分活性材料即可制成低重整活性的催化剂。
另一方面，增大催化剂床上层催化剂颗粒的粒径也可降低催化活性。

Claims (2)

1.碳氢化合物在蒸汽重整催化剂存在下进行高温蒸汽重整的方法，其中催化剂放置在包括上下两层的固定床中，其特征在于催化剂床上层厚度为0.30-0.60米并且上层催化剂颗粒的活性是下层催化剂颗粒的活性的1-50％。
2.权利要求1的方法，其中催化剂床下层分成许多亚层，而相对上层催化剂而言，各亚层催化剂的蒸汽重整活性不断提高。
CN94105617A 1993-05-17 1994-05-17 碳氢化合物的蒸汽重整方法 Expired - Lifetime CN1037760C (zh)

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US5554351A (en) 1996-09-10
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CN1098700A (zh) 1995-02-15
ES2120538T3 (es) 1998-11-01
DE69412536T2 (de) 1998-12-24
ZA943380B (en) 1995-04-04
EP0625481B1 (en) 1998-08-19
EP0625481A1 (en) 1994-11-23
DE69412536D1 (de) 1998-09-24

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