CN1031981A - 合成氨用气体的生产方法 - Google Patents

合成氨用气体的生产方法 Download PDF

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CN1031981A
CN1031981A CN88101475A CN88101475A CN1031981A CN 1031981 A CN1031981 A CN 1031981A CN 88101475 A CN88101475 A CN 88101475A CN 88101475 A CN88101475 A CN 88101475A CN 1031981 A CN1031981 A CN 1031981A
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methane
temperature
heat exchanger
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克里斯托弗
格哈德·格鲁夫利德
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Metal Co ltd
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Abstract

从富含H2和CO，且含杂质甲烷的混合物生产 合成氨用H2和N2。先将混合物催化转化成含CO 量为2～8％的混合物，再将其预冷到-50℃以下，经 换热区再冷却到-160℃以下。且在换热区将高H气 体混合物冷致甲烷露点以下，除去高甲烷冷凝物。然 后，用液氮涤气以除去CO。在换热区至少蒸发部分 高CO冷凝物，再送到转化器。H2和N2气态混合 物从液氮涤气器得到且也通过换热区。

Description

这项发明涉及一种供合成氨使用的由氢和氮气组成的混合气体的生产工艺流程。在该流程中一种主要由氢和一氧化碳组成且含有杂质甲烷在内的混合气体在10到60bar左右的压力，大约在350℃到550℃的温度下，经过催化转化反应生成一种变化反应过的含有CO2和占体积2%到8%之间的CO的混合气体。在从这种所谓转化反应过的混合气体中除去CO2后，预冷到温度不超过-50℃，这种预冷过的高H2混合气体在热交换器中进一步冷却到温度不超过-160℃。
德国专利2007441披露了一种供氨合成使用的气体是如何生产出来的，烃类物质气化后生成一种原料气体，这种原料气体经脱硫、转化反应和清除CO后用液氮洗涤气体以除去残留杂质同时一氧化碳也被除去并掺夹在杂质混合物中。
本发明的目的是尽量减少一氧化碳中的甲烷含量，用液氮涤气方法把它从氢气中分离以便使全部或大部分一氧化碳能够重新循环回转化器中。在转化反应中，CO用来产生氢气以增加H2的产率，从而增加合成气体的生产速度。
在上面描述的工艺过程中，我们的目标之所以能够达到是由于采取了下列步骤：高H2混合气体的温度在热交换器中降低到甲烷露点温度以下，高甲烷冷凝液从混合气体中清除;用液氮洗涤混合气体以除去一氧化碳冷凝液;至少部分高CO冷凝液在热交换器中蒸发并被送入转化器;以及含H2和N2的混合气体从涤气器中提取出来再通过热交换区。
如果高H2混合气体除含有甲烷外还含有氩气，则混合气体的温度在热交换器中降至氩气的露点温度以下以使含有氩气的高甲烷冷凝液能够被分离出来。
根据本项发明，在这个流程中包含在混合气体中的大部分甲烷和所有氩气在用液氮洗涤这种混合气体之前，已从高H2混合气体中分离出来，接着又从本工艺流程中除去。仍然包含在高H混合气体中的一氧化碳用液氮涤气的方法除去后，又可以重新循环回转化器。由于这个原因，转化器可以工作在相当高的温度下和使用相当不敏感的催化剂，例如一种含铁催化剂。这种催化剂不会使转化反应CO+H2O＝H2+CO2进行到一氧化碳完全反应为止。
在以前所了解的工艺流程中，部分没有转化的一氧化碳将随着用液氮涤气的办法排除出来的杂质一起被排除并随着所谓的杂质一起被遗弃。在按照本项发明所采用的流程中，甲烷和氩气是大量存在的杂质、它们得以清除是由于高氢混合气体在热交换器中被冷却，而这是由液氮涤气后的产物提供的致冷作用。
预冷过的高H2混合气体在20到60巴的压力下，被适当地送入热交换器使得高甲烷冷凝液在相当高的压强下也变成可以利用的东西了。如果这种冷凝液随着它部分地被释放而降压，则它的温度进一步降低，因此当这种冷凝液流过热交换器时它能够起附加冷凝剂的作用。
该工艺流程的可能实施方法将根据附图加以说明。
管线1用来供给原料气体。这种气体已经脱硫并主要由氢和一氧化碳组成，此外还包含甲烷，一氧化碳，以及在大多数情况下还有氩。这种原料气体通常是由气化烃类物质或煤得到。这种由气化产生的气体用通常熟知的方法脱硫。管线1中的这种混合气体用来转化为用于合成氨所需气体的有用物质是氢和CO。在包括级间冷却器3在内的二级转化器2a，2b中，CO至少实际上被用来同水蒸汽催化转化成H2和CO2。转化器的第一级2a工作温度，大约在450℃和550℃之间。转化器第二级2b工作温度在350℃和430℃之间。一种众所周知的相当不灵敏转化反应催化剂，如含铁催化剂，可以用在这二级转化器中。同样鉴于转化器工作在10到大约60巴范围的高压下，刚才所说的催化剂比低温催化剂更合乎要求。
来自第二级转化器2b并含有占体积大约2%到8%CO的混合气体经管线4导出。在涤气器5中用已知的办法尽可能完全除去CO2。例如在大约-70℃到-20℃的范围内用甲醇涤气就有效。在涤气器5中进行有效地冷却对进一步处理混合气体也是所希望的。
完全除去了CO2的高H2混合气体经管线6从涤气器5中导出。如果需要的话，可以让这种混合气体通过更冷的冷却器7。
建议使用一种分子筛8来清除混合气体中残留的CO2和涤气液。在温度不超过-50℃时高H2气体经管经10送入热交换器11。在这个热交换器中通过同冷流体间换热而把气体进一步冷却到甲烷的露点温度以下。如果混合气体中还含有干扰量的氩气，则气体温度在热交换器11中要降到这种隋性气体露点温度以下。混合气体的各种成分有下列压力-温度关系：
1bar    10bars
H2-253 -242
N2-196 -169
CO    -191    -161
Ar    -186    -157
CH4-162 -125
一种主要由液化了的甲烷，也可能含有氩的冷凝液在高H2气体中形成。这种冷凝液经分离器13分离后通过管线14导向减压阀15。在这个减压阀中甲烷温度随着它的压强降低而进一步降低，就这样甲烷被分离出来了。此时甲烷作为一种冷却剂通过热交换器11，然后甲烷或氢-甲烷混合物经管线16被提取出来。热交换器11可以由板式换热器构成。
清除了冷凝了的甲烷和氩后的高H2气体经管线18送入液氮涤气器20。如果需要的话，在管线18处可装入一个冷却器（图中未画出）。在热交换器11中冷却到某种程度以后液化了的氮从管线21并经管线22在大致为-180℃到-200℃的温度范围内送入涤气器20。一种H2，N2混合气体在涤气器20的顶端经管线24脱离涤气器20。该气体经热交换器11稍微加热后经管线25以供使用。该气体中氢气同氮气的摩尔数比3∶1是通过本来已知的方法调节。例如掺入来自管线21或22的氮。
在液氮涤气器20中形成的并把杂质也聚集在内的冷凝液主要包含CO和N2，可能还有少量的CH4和Ar。这种冷凝液起初通过减压阀26，经管线27流向热交换器11。在热交换器11中它也起冷却剂的作用。然后经管线28到压缩机29，再经管线30回到转化器2a。即使在涤气器20中形成的全部冷凝液这样循环回到转化器2a也不需担心会提高流经管线25的混合气体中杂质含量，因为分离器13特别把甲烷分离出来并经管线16从工艺流程中清除出去。
在一个改进的方法中从涤气器20来的冷凝液只稍微在减压阀26中减压，而部分气流通过减压阀32减压后掺入高甲烷冷凝液。这样将使CO有一定损失但却给热交换器11提供了一个额外的制冷作用和使管线27和28处于较高压强下，因而减少了压缩机29的能量消耗。在另一项改进方法中用一个泵代替压缩机装入管线27中。
实例
例一是根据本项发明如附图所示那样配置，但缺少减压阀32和冷却器7。作为比较例二缺少分离器13，管线14和16以及阀15。涤气器20的槽底生成物也直接经管线28遗弃。在这二个例子中，这种供合成氨用的气体在每天生产1000吨氨的工厂中生产。
在二例中原料由气化重油并经脱硫的原料气体组成。这种气体含有下列成分：
CO24.4 摩尔百分数
CO    48.7    摩尔百分数
H246.2 摩尔百分数
CH40.5 摩尔百分数
N20.1 摩尔百分数
Ar    0.1    摩尔百分数
在例一中原料气体的进气速率是88，460sm3/n，例二中进气速率是93，465sm3/h。在二个例子中都用含铁催化剂供转化反应使用。在第一级转化器2a的输入端压强大约是52巴，输出端温度是498℃。第二级转化器输出端温度是385℃。大约在-62℃时用甲醇在涤气器5中清除CO2。
下列气体成分（用摩尔百分数表示）和进气速率（单位是sm3/h）是从用下列参考数字标明的工厂设备中得到的。在实例一中获得的数据标在前面。
参考号    4    4    6    6    28    28
CO233.3 33.6 - - - -
CO    3.2    3.2    4.8    4.8    45.3    43.6
H260.6 62.6 90.7 94.4 12.5 12.9
CH40.5 0.4 0.7 0.5 2.4 4.7
N22.0 0.1 3.2 0.1 34.9 27.5
Ar    0.4    0.1    0.6    0.2    4.9    1.3
速率    138872    134635    92495    89143    8133    9866
在二个例子中，合成气体以110，492sm3/h速率经管线25获得。这种气体由摩尔比为3∶1的氢和氮组成。在例一中氮以2，857sm3/h的速率送入涤气器20，而在例二中以31，235sm3/h的速率送入。涤气器20工作在45巴的压强下，它的顶端和槽底之间的温度为-192℃到-186℃。
在这二个例子中几处管线的压强和温度值如下：
管线    6    10    16    18    21    25    28
压强（bars）    48    47    1.5    46    49    44    1.5
温度（℃）    -62    -62    25    -185    35    25    25
例一的方法是根据本项发明实施的。同例二比较，它的优点特别表现在只需以较低的速率输送原料且将较少的氮送入管线21。由于这个原因，尽管需要较多资金，本项发明中提供的方法还是较经济的。

Claims (4)

1、一种由氢和氮组成的用于合成氨的混合气体的生产方法，这种方法包括：一种主要含有大量氢和一氧化碳，以及甲烷作为杂质也包含在内的混合气体在10到大约60巴(bars)之间的压强下和在大约350℃到550℃之间的温度下经过催化转化反应产生一种转化反应过的含有CO2和含量占体积大约2%到8%之间的CO的混合气体；从这种所谓的转化反应过的混合气体中清除CO2后再把这种气体预冷到温度不超过-50℃；再将这种预冷过的高H混合气体在热交换器中进一步冷却到温度不超过-160℃；其特点在于，高H混合气体的温度在热交换器中降至甲烷的露点温度以下，高甲烷冷凝液从这种混合气体中排除出去，用液氮洗涤该种气体以除去一氧化碳冷凝液；至少部分高CO冷凝液在热交换区中蒸发并被送入转化器；以及含H2和N2的混合气体从涤气器提取出来并通过热交换器。
2、按权利要求1的方法，其特点是混合气体中除甲烷外还包含杂质氩气以及高H2混合气体的温度在热交换区中降至氩气的露点温以下并把含氩气的高甲烷冷凝液分离出来。
3、按权利要求1或2的方法，其特点是预冷过的高H2混合气体在20到60bar之间的压力下送入热交换器;至少有部分分离出来了的高甲烷冷凝液减压后通过热交换器。
4、按上述任何一项权利要求的方法，其特点是部分CO冷凝液流减压掺入高甲烷冷凝液中以便混合冷凝液通过热交换器后从工艺流程中排除出去。
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CN102353233A (zh) * 2011-08-03 2012-02-15 成都蜀远煤基能源科技有限公司 煤制气甲烷化后气体深冷分离液化的工艺方法和装置
CN102435045A (zh) * 2011-12-14 2012-05-02 杭州中泰深冷技术股份有限公司 液氮洗涤净化合成气及其深冷分离回收lng装置
CN102533365A (zh) * 2011-12-12 2012-07-04 航天长征化学工程股份有限公司 一种液化天然气及合成氨联产工艺
CN103121662A (zh) * 2012-07-13 2013-05-29 上海国际化建工程咨询公司 液氮洗净化制氨合成新鲜气并联产sng或／和lng的方法及装置

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DE10055818A1 (de) * 2000-11-10 2002-05-23 Ammonia Casale Sa Verfahren zum Herstellen von Ammoniak aus einem Stickstoff-Wasserstoff-Gemisch aus Erdgas
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IN160585B (zh) * 1983-02-14 1987-07-18 Exxon Research Engineering Co
GB2192703B (en) * 1986-07-17 1989-12-13 Boc Group Plc Gas treatment method and apparatus

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CN1498190B (zh) * 2001-03-31 2011-10-05 金属技术股份有限公司 从甲醇生产氨的方法
CN102353233A (zh) * 2011-08-03 2012-02-15 成都蜀远煤基能源科技有限公司 煤制气甲烷化后气体深冷分离液化的工艺方法和装置
CN102353233B (zh) * 2011-08-03 2014-05-07 成都蜀远煤基能源科技有限公司 煤制气甲烷化后气体深冷分离液化的工艺方法和装置
CN102533365A (zh) * 2011-12-12 2012-07-04 航天长征化学工程股份有限公司 一种液化天然气及合成氨联产工艺
CN102533365B (zh) * 2011-12-12 2014-07-30 航天长征化学工程股份有限公司 一种液化天然气及合成氨联产工艺
CN102435045A (zh) * 2011-12-14 2012-05-02 杭州中泰深冷技术股份有限公司 液氮洗涤净化合成气及其深冷分离回收lng装置
CN103121662A (zh) * 2012-07-13 2013-05-29 上海国际化建工程咨询公司 液氮洗净化制氨合成新鲜气并联产sng或／和lng的方法及装置
CN103121662B (zh) * 2012-07-13 2016-03-02 上海国际化建工程咨询公司 液氮洗净化制氨合成新鲜气并联产sng或/和lng的方法及装置

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DE3731055A1 (de) 1989-04-06
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PT88512B (pt) 1993-03-31
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BR8802526A (pt) 1989-03-21

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