CN111542492A - 生产含氢气体的设备和方法 - Google Patents
生产含氢气体的设备和方法 Download PDFInfo
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- CN111542492A CN111542492A CN201880070615.8A CN201880070615A CN111542492A CN 111542492 A CN111542492 A CN 111542492A CN 201880070615 A CN201880070615 A CN 201880070615A CN 111542492 A CN111542492 A CN 111542492A
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- 239000001257 hydrogen Substances 0.000 title claims abstract description 23
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- 238000004519 manufacturing process Methods 0.000 title abstract description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 125
- 239000003054 catalyst Substances 0.000 claims abstract description 48
- 239000000203 mixture Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 26
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- JSKIRARMQDRGJZ-UHFFFAOYSA-N dimagnesium dioxido-bis[(1-oxido-3-oxo-2,4,6,8,9-pentaoxa-1,3-disila-5,7-dialuminabicyclo[3.3.1]nonan-7-yl)oxy]silane Chemical compound [Mg++].[Mg++].[O-][Si]([O-])(O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2)O[Al]1O[Al]2O[Si](=O)O[Si]([O-])(O1)O2 JSKIRARMQDRGJZ-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
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- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
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- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
本发明涉及用于生产氢气、氢气‑甲烷混合物或含H2的反应气体,用于生产氢气、醇、氨、二甲醚和乙烯以及用于费‑托法的设备和方法,并且可以用于处理烃类气体的气体或气体化学工业以及使用氢气‑甲烷混合物的技术。根据本发明,在用于生产含氢气体的设备中,所述设备包括在压力下运行的反应器容器,并且设有用于输送蒸汽‑甲烷混合物和蒸汽‑空气混合物的装置,生产气体出口,设置在容器的内壁上的耐火衬里,以及设置在容器内部并由上子层和下子层组成的甲烷转化催化剂层,甲烷进料安装在催化剂子层之间。反应器容器由不同直径的零件制成,使得催化剂的上子层设置在容器的直径较大的零件中,并且催化剂的下子层设置在直径较小的下部零件中。
Description
技术领域
本发明涉及用于获得含氢气体,氢气、氢气-甲烷混合物、基本上含H2和CO的合成气,用于生产氢气、醇、氨、二甲醚、乙烯,以及用于费-托法的设备和方法,并且可以用于处理烃类气体的化学工业中,并还用于涉及氢气-甲烷混合物的应用的技术中。
背景技术
现有技术描述了用于获得基本含H2和CO的合成气,用于生产醇、氨、二甲醚、乙烯,以及用于生产费-托法的甲烷转化反应器,如2004年5月20日公布的RF专利2228901号,IPCC01B3/38中所述。用于获得预设的H2/CO比在1.0至2.0范围内的合成气的现有技术反应器包括两个阶段:部分氧化步骤A)和在催化剂上用步骤A)产物转化残留甲烷的步骤B)。部分氧化步骤A)分两个阶段进行:a)以大约等于0.76-0.84的氧气与甲烷的摩尔比用氧气对天然气进行非催化部分氧化,以得到H2O和CH4的非平衡含量的产物;b)用与CO2与H2O或H20和CH4的矫正添加剂转化阶段a)反应产物,以通过在催化剂上将用水蒸气转化残留甲烷而获得气体混合物。甲烷转化反应器允许产生具有预设的CO/H2比的合成气,该合成气可用于获得氢气以及原料,所述原料用于醇、二甲醚、氨或其他碱性化学物质的进一步合成工艺。
然而,所描述的甲烷转化反应器具有若干缺点,其中,受到与高氧气消耗(超过转化天然气的重量消耗)相关的设备应用的功能限制和经济限制,其生产要求高功耗(高达1000kWh/t)和资本成本(高达1500USD/kgh-1)。烟灰(sooting)也是一个严重的问题,因为它会大大降低催化剂活性。
该设备的缺点还在于由于空气压缩的支出、中间阶段的存在和副反应而造成的低热力学效率,这显著降低了产物气体中目标组分的含量。
现有技术描述了一种用于获得氢气-甲烷混合物的反应器,其被描述在于2014年6月27日公布的RU发明专利第2520482号。它是使用至少两个包含低级石蜡烃作为原料源的并流的等效设备。那时,一个流被送入用于用含氧气体进行的部分氧化,而另一流与水蒸气混合并且经过数个后续阶段。每个阶段包括由于由第一流的部分氧化而产生的热传递而在加热热交换器中进行加热。之后,该流流过充满催化剂头的绝热转化反应器。该方案的缺点是高投资成本、高金属消耗和低的原料利用效率。
现有技术根据USSR专利第1831468号,IPC 5C01 3/38描述了“从烃进料中获得合成气的方法”。它是包括将烃类进料与氧化剂(氧气或含氧气体或蒸汽混合)并且在整装催化剂的存在下转化混合物的等效方法。此时,反应区的温度不低于混合物自燃点的93℃,并且反应区的混合物注入速度超过了回火工艺的速度。现有技术方法需要使用高选择性催化剂。USSR专利第1831468号中描述的发明的主要缺点是催化剂成本高,由于局部过热而可能造成催化剂损坏以及可能的烟灰。
目前,用于部分甲烷氧化的反应器是已知的。它包括:
·第一室,用于形成第一反应物气体的通道;
·第二室,用于形成第二反应物气体的通道;
·分隔第一室与第二室的多孔催化膜。该膜可以允许第二反应物气体(例如氧气)从第二室进入第一室。由于天然气或煤床甲烷或沼气的转化,该反应器用于获得H2/CO比为约1.8:1至约6:1的合成气。该反应器具有厚度约为25-200mm的耐火衬里,其可以承受高达约1000℃的温度(美国专利申请第20130032762号,公布于2013年6月2日)等。该发明专利申请的缺点是必须使用膜,该膜降低了反应器的可靠性和产量,并且难以调节H2/CO比率。
甲烷转化的有希望的方向是“CH4的深度氧化+非催化二氧化碳转化”的两个阶段工艺。当甲烷的完全氧化的放热阶段与二氧化碳转化的吸热阶段结合在一起时,它允许通过组合方法而实施自热工艺。这种方法是在用H2/CO进行甲烷转化的反应器中进行的,其包括:燃烧室,用于甲烷或天然气与空气氧;搅拌器;冷却系统,用于氧化产物和合成气;预热系统,用于甲烷和空气。此时,燃烧室包含点火设备并且被制成流动室的形式。带有防突破网格的搅拌器被连接到反应室入口,并且甲烷和空气输送管被连接到搅拌器。用于冷却氧化产物并加热输送至燃烧室的空气的热交换器被连接到室出口。此时,热交换器具有将氧化产物从其腔中排出的奶嘴(nipple)。该设备还具有:二氧化碳提取系统;搅拌器,用于二氧化碳和甲烷;以及安装在燃烧室中用于二氧化碳转化的室(俄罗斯联邦专利第2361809号,公布于2009年7月20日,公告号20等)。该解决方案的缺点是设备复杂、热力学损失高和金属消耗高。
目前,用于获得富含氢气和碳氧化物的气体的甲烷转化反应器是已知的。它包括:夹套,其在压力下工作并具有输送含热气体流的水蒸气和产物输出的装置;夹套的内壁上的耐火衬里和位于其内的重整催化剂层;以及射流喷嘴,用于产生含有热气体流的水蒸气。射流喷嘴与壳体的上部连接,其在压力下操作。根据该发明的反应器的显著特征是催化剂层由上子层和下子层组成。此时,催化剂的上子层的催化活性低于下子层的催化活性(专利第2119382号,公布于1998年9月27日)等。该技术方案的缺点是低级石蜡烃转化的效率低,该方法的热力学效率低,投资成本和金属消耗高,以及产物气体中杂质气体(氮气、氩气)的含量高。
目前,用于获得富含氢气和碳氧化物的气体的甲烷转化反应器是已知的(专利第2571149号,公布于2015年12月20日)。它是一个原型,包括:壳体,其在压力下操作,并且具有用于输送水蒸气、甲烷和含氧气体以及用于产物输出的装置;壳体的内壁上的耐火衬里和位于其内的甲烷转化催化剂层。它由上子层和下子层组成。在催化剂子层之间存在输送活性气体的设备,该活性气体为二氧化碳。
该设备允许增加用于合成工艺的碳氧化物含量。然而,该设备不允许增加氢气含量。
发明内容
所要求保护的发明的技术效果是提高了低级石蜡烃转化效率和甲烷转化反应器的热力学效率,并且还提高了产物气体中的H2/CO比。
关于该设备的技术效果是通过使用一种用于获得含氢气体的设备来实现的,该设备包括:具有氧化室的反应器的上壳体和具有混合室的反应器的下壳体,上壳体与下壳体通过覆盖有内壁上的衬里的连通室连通;同轴搅拌器和形成所述同轴搅拌器的管状环带的中心管;用于输送蒸汽-甲烷混合物的管道,所述蒸汽-甲烷混合物被输送到同轴搅拌器的管状环带;用于输送蒸汽-空气混合物的管道,所述蒸汽-空气混合物被输送到中心管;位于中心管的下边缘的点火器的点火源,所述中心管进入上壳体的内部空间;下壳体中的用于输送甲烷的管道;下壳体的下部中的与产物气体出口相连的出口管。每个反应器的上、下壳体依次包括:保护球;催化剂子层;火砖拱门,其通过支撑球搁置在支撑网格上。此时,催化剂搁置在具有气体端口的火砖拱门上,所述气体端口被刚玉球覆盖,以防止催化剂溢出并降低气体通过拱门的阻力。
关于方法的技术结果是由于获得含氢气体的方法来实现的,该方法包括:向安装在反应器的上壳体上的同轴搅拌器的管状环带输送蒸汽-甲烷混合物,向中心管输送蒸汽-空气混合物,以及向反应器的上壳体中的甲烷氧化室输送点火,甲烷氧化室中,甲烷燃烧反应在催化剂的上子层上发生。那时,由此输送由该反应产生的化学物质流以与额外值的甲烷混合。混合在所述反应器的上壳体与下壳体之间的自由空间中进行。在此,只要在催化剂的下子层上游的甲烷含量在水蒸气的体积含量的0.1至0.25的范围内,就输送甲烷。化学物质和甲烷的混合流被输送到催化剂的下子层,以在反应器的下壳体中进行甲烷转化,其中,由于化学物质流中气体混合物的显热而发生额外的甲烷转化反应。产生的气体通过出口管排出。
附图说明
该附图示出了设备的结构图,其中:1–用于输送蒸汽-甲烷混合物的管道;2-反应器的上壳体;3-衬里;4-搅拌器壳体;5-同轴搅拌器的管状环带;6-用于输送蒸汽-空气混合物的管道;7-中心管;8-点火源;9-甲烷氧化室;10、20-保护球;11、21-催化剂子层;12、22-火砖拱门;13、23-支撑球;14、24-支撑网格;15-化学物质流;16-连通室;17-甲烷输送管道;18-反应器的下壳体;19-混合室;25-出口管;26-产物气体出口。
具体实施方式
本发明的实施方式的实例是下述用于获得含氢气体的设备。在本发明的实施方式的所描述的实例中,空气被用作含氧气体。这允许表征本发明实施方式与处理天然气及伴生气体并且获得具有所需组成的产物气体的系统有关的特征。
用于获得含氢气体的设备包括:反应器的上壳体2;反应器的上壳体2的内壁上的衬里3;带搅拌器壳体的同轴搅拌器4;用于输送蒸汽-甲烷混合物的管道1,蒸汽-甲烷混合物被输送到同轴搅拌器的管状环带5;用于输送蒸汽-空气混合物的管道6,蒸汽-空气混合物被输送到中心管7;位于中心管7的下边缘的点火器(图中未显示)的点火源8。中心管进入甲烷氧化室9,甲烷氧化室9的下部由保护球10形成。该球保护催化剂的上层11免于过热。催化剂火砖拱门12的上层11和支撑球13的层位于支撑网格14上。化学物质流15穿过网格到达用于输送甲烷的管道17。管道与混合室19一起位于反应器的下壳体18中,混合室19通过连通室16与反应器的上壳体连通。反应器的下壳体包括:保护球20的层;催化剂的下子层21,其下的火砖拱门22和支撑球23的层位于支撑网格24上。网格位于与产物气体的出口26相连的出口管25上方。
甲烷入口可以是多孔圆柱体的形式,其实心底部与反应器的下壳体18的外壁上的奶嘴连接。用于输送甲烷的管道17可以沿着被加热侧与热交换器(图中未示出)连接。产物气体出口26可以沿着加热侧与热交换器(图中未示出)连接。
用于甲烷转化的催化剂的上子层11以及催化剂的下子层21可以搁置在火砖拱门12、22上,并且相应地搁置在位于下部和上部支撑网格14、24上的刚玉支撑球13、23的层上。网格被安装在耐火衬里3的凸耳(图中未示出)上的反应器的上壳体2和下壳体18中。耐火衬里的材料的主要成分是氧化铝,Fe2O3的含量不超过0.2%。支撑球13、23和保护球10、20也可以由氧化铝制成。
可以以允许将催化剂的下子层21上游的甲烷含量保持在水蒸气的体积含量的0.1至0.25的范围内的方式来进行甲烷进入。
用于获得含氢气体的设备如下操作。
在本发明的实施方式的描述的实例中,天然气-甲烷被用作低级石蜡烃,这允许表征本发明的实施方式关于将天然气及伴生气加工成甲烷-氢气混合物的特征。
使压力为1.0Mpa的天然气的流经历脱硫(如果天然气中包含硫化合物作为杂质),直至以硫表示的硫的质量浓度小于0.5mg/nm3;在热交换器中加热;以及与过热水蒸气混合。然后,通过用于输送蒸汽-甲烷混合物的管道1,将流输送至搅拌器壳体被安装在反应器的上壳体2上的同轴搅拌器4,并且输送至同轴搅拌器的管状环带5。将压力为1.0MPa的压缩空气加热到400℃,与过热的水蒸气混合,然后通过用于输送蒸汽-空气混合物的管道6而输送到中心管7。在管子的下部,在催化剂的上子层11上方的自由空间中,甲烷和空气的燃烧反应在水蒸气的存在下通过点火源8点燃位于中心管7下部边缘的点火器(图中未显示)而发生。作为这个反应的结果,获得了在催化剂11上进行绝热甲烷转化反应所必需的热量。从催化剂的上子层11将化学物质流15输送到混合室19,以与额外体积的甲烷混合。混合在反应器的上壳体2和下壳体18之间的自由空间中进行。当甲烷在热交换器(图中未显示)中加热到400℃时,输送甲烷。
只要在催化剂的下子层上游的甲烷含量在水蒸气的体积含量的0.1至0.25的范围内,就输送甲烷。当蒸汽/气体比超过0.25时,工艺效率降低并且资本成本增加。这是由于在以下规定的流动加热温度下转化率低而造成的需要增加气体的再循环流量;或者由于需要将催化剂的上子层11上游的加热温度增加到1000-1200℃,这将迫使对反应器使用更昂贵的材料。甲烷/水蒸气比降低到低于0.1还将由于需要产生过量的水蒸气而导致工艺效率降低。
将化学物质与甲烷的混合流输送到装有镍催化剂的绝热反应器的甲烷转化催化剂的下子层21,并且打算由于化学物质流15的气体混合物的显热而用于甲烷转化的附加反应。产物气体出口26以如下方式沿着加热侧与热交换器(图中未示出)连接,即加热的产物气体可以由于加热甲烷和压缩气体的入口流而冷却,并且还获得过热的水蒸气。在冷却后,提供包含甲烷-氢气混合物的产物气体用作燃料或反应混合物。在向客户供应之前,可以从产物气体中除去二氧化碳。根据《巴黎协定》,二氧化碳可被用作市场产品或掩埋。在掩埋中,该技术没有温室气体排放。
以下物质可用作甲烷转化催化剂:刚玉拉希格(Raschig)圈或含镍、钌、铑、钯和铱的球的颗粒层,其施用于难熔氧化物,如堇青石、莫来石、氧化铬、钛酸铝、尖晶石、二氧化锆和氧化铝。
绝热反应器的催化剂的下子层21中的温度被保持在约500℃至700℃的范围内,以提高工艺效率。催化剂的下子层21的头部含有选自以下的金属作为活性成分:铑、镍、铂、铱、钯、铁、钴、铼、钌、铜、锌,它们的混合物或化合物。可以使用Johnson Matthey KATALCO25-4Q和KATALCO 57-4Q催化剂。催化剂NIAP-03-01也是有效的。具有可变含量的类铂和金属的催化剂组合物影响通过水蒸气对碳氧化物氧化的动力学(转变反应),从而允许控制最终产物中的氢含量。
流的压力选择范围是0.1至9.0Mpa,这允许减小装置尺寸,减少气体动力损失和压缩相关的费用。
表1示出了绝热反应器中工艺的计算。
表1在压力为1.0MPa时第一流的转化的组成和热力特性及物理特性。
混合后的蒸汽-气体混合物
蒸汽/气体=2.7500;
温度=400.0℃;
压力=10.00atmg;
V甲烷=560.00m3/h;
蒸汽-气体混合物
蒸汽/气体=0.1000;
温度=400.0℃;
压力=10.00atmg;
V干气=1200.00m3/h;
颗粒层的入口处的气体
蒸汽/气体=1.281196;
V干气=1500m3/h;
压力=10.00atmg;
温度=1068.09℃;
颗粒层的出口处的气体
蒸汽/气体=0.563734;
V干气=2560m3/h;
压力=10.00atmg;
温度=673.36℃;
因此,提出的发明是一种新的设备,其允许提高低级石蜡烃转化的效率和甲烷转化反应器的热力学效率,降低资本成本和金属消耗,降低杂质气体(氮气、氩气)的含量并提高产物气体中的H2/CO比。
产生的产物——含氢气体及其衍生物(氢气、甲烷-氢混合物)随后可用于气体和气体化学工业以及用于烃类加工的冶金业,还用于能源积累和传输系统,并且用作运输和固定式发电厂的燃料。
Claims (2)
1.一种用于获得含氢气体的设备,包括:具有氧化室的反应器的上壳体和具有混合室的反应器的下壳体,所述上壳体与所述下壳体通过覆盖有内壁上的衬里的连通室连通;同轴搅拌器和形成所述同轴搅拌器的管状环带的中心管;用于输送蒸汽-甲烷混合物的管道,所述蒸汽-甲烷混合物被输送至所述同轴搅拌器的管状环带;用于输送蒸汽-空气混合物的管道,所述蒸汽-空气混合物被输送至所述中心管;位于所述中心管的下边缘的点火器的点火源,所述中心管进入所述上壳体的内部空间;所述下壳体中的甲烷输送管道;所述下壳体的下部中的与产物气体出口相连的出口管,每个反应器的壳体依次包括:保护球;催化剂子层;火砖拱门,其通过支撑球搁置在支撑网格上;催化剂,其搁置在包含气体端口的火砖拱门上,所述气体端口被刚玉球覆盖,以防止催化剂溢出并降低气体通过拱门的阻力。
2.一种用于获得含氢气体的方法,包括:向安装在反应器的上壳体上的同轴搅拌器的管状环带输送蒸汽-甲烷混合物;向中心管输送蒸汽-空气混合物;以及向反应器的上壳体中的甲烷氧化室输送点火,在甲烷氧化室中,甲烷燃烧反应在催化剂的上子层上发生,由此进料由该反应产生的化学物质流,用于与额外量的甲烷混合,所述混合在所述反应器的上壳体与下壳体之间的自由空间中进行,甲烷以催化剂的下子层上游的甲烷含量保持在水蒸气的体积含量的0.1至0.25范围内的方式进行进料,混合的化学物质和甲烷的流被输送到催化剂的下子层,用于在反应器的下壳体中进行甲烷转化,其中,由于化学物质流中的气体混合物的显热而发生额外的甲烷转化反应,产物气体通过出口管排出。
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PCT/RU2018/000782 WO2019112480A1 (ru) | 2017-12-07 | 2018-12-04 | Аппарат и способ получения водородсодержащего газа |
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RU2740755C1 (ru) * | 2019-11-05 | 2021-01-20 | Общество с ограниченной ответственностью "Газпром трансгаз Самара" | Способ получения водородсодержащего газа из природного газа и перегретого пара и устройство для его осуществления |
RU2755267C1 (ru) * | 2020-04-28 | 2021-09-14 | Общество с ограниченной ответственностью "Газпром трансгаз Томск" (ООО "Газпром трансгаз Томск") | Устройство для получения метано-водородного топлива из углеводородного газа |
US11859147B2 (en) | 2021-11-24 | 2024-01-02 | Indian Oil Corporation Limited | Single stage process for production of hydrogen enriched gas |
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