CN101151094A - 催化反应器 - Google Patents
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Abstract
用于费-托合成的紧凑型催化反应器,在反应器内限定交替排列的多重第一流动通道和第二流动通道,分别用于携载进行费-托合成的气体混合物,和冷却液。各第一流动通道包括结合金属基体的可移动透气性催化剂结构。通过该催化剂结构限定多重流动通路,和空隙率,即由所述多重流动通路构成的第一流动通道横断面积的比率在25%至75%之间。这提供生产力和选择性之间的最佳平衡,因此反应器的操作是经济的和可控的。
Description
本发明涉及催化反应器,该反应器适用于将天然气转化成长链烃,尤其是进行费-托(Fischer-Tropsch)合成的化学方法,和涉及包括该催化反应器进行处理的设备。
在WO 01/51194和WO 03/048034(Accentus plc)中描述了一种方法:其中在第一催化反应器中甲烷和蒸气反应,产生一氧化碳和氢气;所产生的气体混合物然后用于在第二催化反应器中进行费-托合成。总的结果是将甲烷转化成较高分子量的烃,该烃在环境条件下通常是液体或蜡状物。该方法的两个步骤,即蒸气/甲烷重整和费-托合成,需要不同的催化剂,和分别将热量转移到反应气体或从反应气体转移热量,因为反应分别是吸热和放热的。用于这些反应的反应器可成型为层式板,在板之间限定流动通道,用于不同流体的流动通道在堆叠层中交替。在那些需要催化剂的通道中,这优选为在陶瓷涂层中携带催化剂的金属基体形式,当催化剂用尽时可从通道中除去这样的结构。该催化剂结构提供大表面面积,用于在反应气体和催化材料之间接触,但同时它抑制反应气体穿过通道的流动。
依照本发明,提供用于费-托合成的紧凑型催化反应器,在反应器内限定交替排列的多重第一流动通道和第二流动通道,分别用于携载进行费-托合成的气体混合物,和冷却液;
其中各第一流动通道包含可移动的透气性催化剂结构,该催化剂结构包括无孔金属基体,在该基体的至少一个表面上具有不大于200μm的基本上均匀厚度的连续陶瓷涂层,该陶瓷涂层掺入催化材料,该催化剂结构限定提供在80-120m2/g范围的孔表面面积的中孔和大孔,和将催化剂结构成型以便限定在其中通过的多重总体流动通路,其中空隙率,即由所述多重总体流动通路构成的第一流动通道横断面积的比率在25%至77%之间。
优选空隙率在约35%至75%之间,更优选在60%至72%之间。
应理解,费-托反应是比较慢的反应。费-托合成的目的是产生其中碳链比甲烷的长的烃,并的确优选至少C5,所以一般是液体和/或蜡状物。因此,实用的反应器必须每单位时间产生大量这样的长链烃,和应该选择性形成这样的长链烃而非甲烷。已经发现假如空隙率小于约25%,那么产率太低而不经济,而假如空隙率超过约77%,产率可能高,但甲烷的产量将变得过多。
费-托反应典型地在约200℃进行,这样可在宽范围内选择反应器的材料。例如反应器可由铝合金、不锈钢、高镍合金或其它钢合金制备。
优选催化剂结构的金属基体是当加热后形成氧化铝附着表面涂层的钢合金,例如含铝的铁素体钢,例如含15%铬、4%铝和0.3%钇的铁(例如Fecralloy(TM))。当这种金属在空气中加热时,它形成附着的氧化铝氧化物涂层,防止合金被进一步氧化和腐蚀。当陶瓷涂层为氧化铝时,这显然结合到在表面上的氧化物涂层。基体优选为薄的金属箔,例如厚度小于100μm,和基体可以是波面的、褶状的或其它形状的,以便限定多重流动通路。
催化剂结构优选包含厚度在40μm-200μm之间的陶瓷涂层,更优选厚度在60μm-100μm之间。该涂层限定孔,并掺入催化金属颗粒。
可将这样的掺入催化材料的催化剂结构插入反应器的流动通道中,其中用于费-托反应的流动通道与除去热量的流动通道交替。在流动通道内催化剂结构的金属基体增强热传递和增加催化剂表面积。在组件中催化剂结构可从通道除去,因而假如催化剂用尽时它们可被替换。由催化剂结构限定的流动通路可具有任何合适的截面形状。至少一些流动通路可沿着它们的长度互相连通,或者所有流动通路可被催化剂结构互相分开。优选所有形成表面的催化剂结构掺入催化材料。
如果通道深度不超过约3mm,则催化剂结构可例如为单一的成型箔。或者,特别在通道深度大于约2mm时,优选的催化剂结构包含许多由基本上平的箔分开的这样的成型箔;成型箔和平的箔可互相结合,或者可作为独立的物品插入。为了保证必需的良好热接触,用于费-托反应的通道优选小于20mm深度,更优选小于10mm深度。期望在通道宽度内,使通道内的温度均匀保持在约2-4℃内,通道越大,这实现起来就越困难。
反应器组件可包含堆叠的板。例如,可由各板中的槽限定第一和第二流动通道,将板堆叠,然后结合在一起。或者可由堞形的和与平片交替堆叠的薄金属片限定流动通道;可由密封带限定流动通道的边缘。例如,通过扩散粘结、铜焊接或热等静压将形成反应器组件的堆叠板结合在一起。
因此,加工天然气以获得长链烃的设备可加入使甲烷和蒸气反应形成合成气体的蒸气/甲烷重整反应器,和产生长链烃的本发明费-托反应器。
现在,本发明仅通过实施例,并结合附图进一步和更具体地描述,其中:
图1显示适用于费-托合成的反应器的部分剖视图;
图2显示用于图1中反应器的催化剂载体。
本发明是关于将天然气(主要是甲烷)转化成长链烃的化学方法。该方法的第一步涉及蒸气重整,即以下类型的反应:
H2O+CH4→CO+3H2
该反应是吸热的,可由流动通道中的铑或铂/铑催化剂催化。通过易燃气体例如甲烷或氢气的燃烧,可提供引起该反应所需的热量,该燃烧是放热的,可由临近第二气体流动通道中的铂/钯催化剂催化。
通过蒸气/甲烷重整所产生的气体混合物然后用于进行费-托合成,以产生长链烃,即:
nCO+2nH2→(CH2)n+nH2O
该反应是放热反应,在催化剂例如铁、钴或熔融磁铁矿存在下,在通常190℃-280℃之间的高温,和通常1.5MPa-2.5MPa(绝对值)之间的高压下发生。费-托合成的优选催化剂包含比表面积140-230m2/g的γ-氧化铝涂层,具有约10-40%钴(与氧化铝相比的重量比),和具有小于10%重量钴的助催化剂例如钌、铂或钆,和碱性助催化剂例如氧化镧。在陶瓷的沉积和浸渍,然后还原提供催化剂颗粒之后,比表面积优选为约80-110m2/g(通过BET气体吸附技术测量),例如90m2/g。通过压汞法测量,提供(as-supplied)的氧化铝的比孔体积优选为0.37-0.47cm3/g,而含催化剂的陶瓷的比孔体积为0.20-0.26cm3/g(通过BET技术测量),例如0.24cm3/g。
将蒸气甲烷重整所产生的高压一氧化碳和氢气流冷却和压缩至高压,即2.0MPa,然后加到催化费-托反应器中,该反应器是由上述板堆叠形成的紧凑型催化反应器;反应物混合物流动穿过一组通道,同时冷冻剂流动穿过另一组通道。
通过穿过热交换器和旋风分离器,然后是分离室的通路,将费-托合成的反应产物(主要是水和烃例如石蜡)冷却以使液体凝结,其中三相水、烃和尾气分离,在大气压下烃产物是稳定的。收集和分离保留在气相和过量氢气(费-托尾气)中的烃。一部分可通过减压阀,在重整器(如上述)中提供催化燃烧处理的燃料。剩下的尾气可加入准备发电的燃气轮机中。所必需的主要电力设备是压缩机,该压缩机用于将压力提高到费-托反应所必需的压力;也可用电运转真空蒸馏单元,为蒸气的产生提供方法用水。
现在参考图1,该图显示了适合用作费-托反应器的反应器10的一部分,为了清晰,反应器10以截面显示并具有分开的组件。反应器10由厚度1mm的平板12堆叠组成,平板12被间隔开以便限定用于冷却液的通道以及与之交替的费-托合成的通道。由厚度0.75mm的堞形板14限定冷却液通道。在该实施例中堞形物的高度(通常在1至4mm范围内)为2mm,沿侧面提供2mm厚的固体边缘带16,连续的连接带间隔6mm。用于费-托合成的通道为5mm高,由条18限定,条18为正方形横截面,5mm高,间隔350mm并因此限定直通的通道。(或者,可由堞形板代替限定用于费-托合成的通道,所以个别通道可为例如5mm高和10mm宽,或例如3mm高和20mm宽。)平板12、条18和其它构造组件可以是铝合金,例如3003级(含约1.2%锰和0.1%铜的铝)。
按上述装配堆叠件,然后例如通过铜焊接结合在一起,形成反应器10。如图2所示,现在结合图来看,掺入适当催化剂的催化剂载体22然后插入用于费-托合成的通道,催化剂载体22具有和相应通道一样的宽度和高度。在这种情况下,在用于费-托合成的各通道中,载体22由3个波面箔23制成,其中波面1.3mm高,被名义上的平箔24分开,所有这些箔厚度为50μm。名义上的平箔24优选以非常小的幅度成波状,例如给出约0.1mm的总高度,因为这使它们稍微少的弯曲,所以易于操作和插入。在各箔的每个表面涂覆厚度约80μm的催化剂层25,优选氧化铝陶瓷。陶瓷具有中孔,该中孔的特征尺寸在2nm至20nm的范围内,为分散的催化剂金属提供大多数位置。优选这些中孔的尺寸在10-16nm之间,更优选在12-14nm之间。对于该费-托合成,也必需有更大的中孔和大孔,即孔的尺寸为至少50nm及以上。例如,可通过喷涂含比较大的氧化铝颗粒,例如在5-40μm范围内的不可分散的γ氧化铝颗粒,以及用作支持剂和粘合剂的一些氧化铝溶胶的液滴,获得这样的大孔含量。氧化铝颗粒之间所得间隙提供需要的大孔。陶瓷层也必须掺入合适的催化剂,例如贵金属促进的钴;可将催化金属以硝酸盐的形式沉积至陶瓷层中,然后加热和还原成金属。
可认识到箔的横断面积由总箔厚度、波面高度和由波面波长决定。在该实施例中,每个箔的总厚度(包括陶瓷涂层)为约210μm,和波面总高度为1.5mm;波面波长为约2.5mm。空隙率,即由流动通路确定的横断面积的比率因此为约71%。可认识到空隙率仅考虑总体气体流动通路;陶瓷的孔隙率对流动通路无贡献(因为孔隙率太低和因为孔太小)。在使用期间,主要由液烃占据陶瓷内的孔,所以不提供气流通路。可认识到所有流动通路在至少一些它们的表面上具有催化剂;在箔之间通过的所有流动通路在它们的所有表面上均有催化剂。
在该实施例中,通过喷涂方法,波面箔23和平箔24分别涂覆催化剂,互相之间不固定;仅将它们插入流动通道。或者至少一些箔表面可能相反不提供催化剂涂层25,例如名义上平箔24可能根本不涂覆,或可能仅涂覆一个侧面。作为另一个替代,在插入流动通道之前箔可互相固定。也可认识到,波面可有不同的显示形状,例如它们可以是由平部分分开的Z字形波面或尖峰。关于幅度和关于波长,它们可以有不同的尺寸。也应该认识到:通道的尺寸可以和上述的不同。然而,流动通道优选深度为至少1mm,优选深度为至少2mm,以为催化剂提供足够的空间;和优选深度不大于20mm,更优选深度不大于10mm,因为难于保证基本上均匀的温度遍及这样深的通道。
C5+烃的产率取决于:通过反应器的一氧化碳质量流;转化率(经历反应的一氧化碳比率);和选择性(为C5+的烃产物比例)。对于特定的催化剂类型和催化剂厚度,和对于反应器内的固定压力和温度,转化率和选择性主要由空间速度(定义为在STP下供给气体的体积流速除以可用于流体流动的反应器通道体积)决定。因此可选择空间速度,以提供最佳的转化率和选择性。
假如空隙率小于约25%,产率变得不经济。这是因为假如空间速度保持不变(对于最佳转化率和选择性),空隙率的减小对应于一氧化碳通过反应器的流速下降,因而产率降低。假如流速不与空隙率减小成比例下降,那么空间速度增加,从而降低二氧化碳的转化率。总C5+产率减少。
在另一方面,假如空隙率太大,如在77%以上,那么暗示在通道体积内有比较低的催化剂负荷,和因此有太少的可用于烃分子产生的催化剂位点。即使空间速度具有最佳值,转化率和选择性均将下降。空隙率增加所导致的气流增加不足以补偿这些下降,因此C5+产率又下降。
因而,最佳催化剂结构将例如提供在约25%-77%之间,更优选在约35%-75%之间例如约71%的空隙率。催化剂应该例如提供每小时每克催化剂至少0.5g C5+的产率。具有该空隙率,催化剂不会被过量的气体清除,流速提供选择性和产率的最佳平衡。此外,气流足够大以保证良好的温度控制,因此一氧化碳的转化率保持在所期望的限度内。
可认识到通过改变波面高度和波长或波面形状,可改变空隙率,因为这些改变了提供波面箔所必需的初始-平箔的宽度,该波面箔的宽度等于流动通道的宽度。通过改变箔的厚度,和通过改变陶瓷涂层的厚度,也可改变空隙率。
Claims (6)
1.一种用于费-托合成的紧凑型催化反应器,在所述反应器内限定交替排列的多重第一流动通道和第二流动通道,该第一流动通道和第二流动通道分别携载进行费-托合成的气体混合物,和冷却液;其中各第一流动通道含有可移动的透气性催化剂结构,该催化剂结构包括无孔金属基体,并且在该基体的至少一个表面上具有不大于200μm的基本上均匀厚度的连续陶瓷涂层,该陶瓷涂层掺入催化材料,所述催化剂结构限定提供在80-120m2/g范围内孔表面面积的中孔和大孔,和将所述催化剂结构成型,以便限定从其中穿过的多重总体流动通路,其中空隙率,即由所述多重总体流动通路构成的第一流动通道的横断面积的比率在25%-77%之间。
2.权利要求1的反应器,其中所述空隙率在约35%-75%之间。
3.权利要求1或2的反应器,其中所述催化剂结构的金属基体包含含铝的铁素体钢。
4.前述权利要求中任一项的反应器,其中所述催化剂结构的金属基体包含厚度小于100μm的金属箔。
5.前述权利要求中任一项的反应器,其中所述催化剂结构包含厚度在60-100μm之间的陶瓷涂层。
6.一种将天然气转化成长链烃的设备,其中将天然气加入蒸气重整反应器,产生合成气体,并加入前述权利要求中任一项的费-托反应器,产生长链烃。
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