CN109863229A - 半渗透膜在裂化盘管中的用途 - Google Patents
半渗透膜在裂化盘管中的用途 Download PDFInfo
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- CN109863229A CN109863229A CN201780065968.4A CN201780065968A CN109863229A CN 109863229 A CN109863229 A CN 109863229A CN 201780065968 A CN201780065968 A CN 201780065968A CN 109863229 A CN109863229 A CN 109863229A
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- Prior art keywords
- coil pipe
- smelting furnace
- gas
- furnace coil
- metal
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Classifications
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Abstract
在链烷烃裂化器的盘管中的通路或管或其一段或“U”形管,其具有在金属基材中孔径为约0.001‑0.5微米的外涂有致密的金属膜的段,允许来自裂化气的H2、CH4、CO和CO2中的一种或多种的渗透,将反应平衡移动至生产乙烯,并降低在蒸汽裂化器的下游分离系列上的载荷。
Description
技术领域
本发明涉及热裂化链烷烃的领域。更具体地,本发明涉及在盘管通路或其部分或“U”形管的一种或多种中结合至少对于氢的可渗透膜,以从输送管线上游的裂化气中至少除去氢,以降低在分离系列上的载荷。
背景技术
在乙烯蒸汽裂化器的后端,使用巨大量的资金设备和能量来从甲烷和其他组分(包括H2、CO和CO2)分离裂化气的组分,以得到相对纯的乙烯。如果H2、CH4、CO和CO2中的一些或全部可在裂化器中从裂化气分离,则将驱动化学平衡朝向形成乙烯。此外,这样的分离将降低在分离系列上的载荷。
来自转让给Worcester Polytechnic Institute,Worcester Mass的最早提交日期为1997年12月15日的申请、于2000年11月28日授权给Ma等人的美国专利6,152,987教导了具有氢可渗透性膜的表面涂层的微多孔不锈钢管道。所得到的管或管道可用于从气体混合物分离氢。该参考文献未提议在用于热裂化链烷烃至烯烃的熔炉的通路中结合这样的管道结构。
转让给Worcester Polytechnic Institute的Ma等人名下的系列专利也通过2010年6月1日授权的美国专利7,727,596说明,其教导在高达约500℃的温度下从气态混合物分离氢。这低于裂化链烷烃的典型的温度。气体混合物看起来主要是H2和氦,而不是裂化气流。未讨论从烯烃(乙烯)分离氢、CH4、CO、CO2中的一种或多种。有趣的是,该专利公开了孔径为0.1微米至15微米(在一些情况下,0.1-0.5微米)的高温合金,其可用作用于分离膜的基材(第7栏,第16-60行)。
转让给Bettergy的Tang等人名下的2015年2月12日公布的美国专利申请20150044130教导了用钯掺杂沸石来制备可在高达约450℃的温度下使用的半渗透膜,该温度同样低于链烷烃的裂化温度(参见实施例中的表格)。实施例中的表格显示,在高达约450℃的温度下,比起分子诸如CO2和CH4,对氢的选择性高。该说明书未教导或提议膜可在超过450℃的温度下使用。
转让给美国能源部的2014年7月29日授权给Berchtold等人的美国专利8,791,037公开了在高达约1000℃的温度下稳定的来自聚合物前体的非氧化物(Si/C/N)陶瓷膜。说明书教导了孔径可通过单体组成、共聚单体官能度、光聚合条件和热解条件来控制(第6栏,第40-50行)。然而,该专利中未公开条件的细节。
本发明试图提供了一种在熔炉盘管中从裂化气的流分离H2、CH4、CO和CO2中的一种或多种的方法。
发明内容
在一种实施方案中,本发明提供了一种用于[蒸汽]裂化器的熔炉盘管,其包含一个或多个由以下组成的段:
i) 熔化温度大于1000℃的连续金属通道,其允许裂化气在其中流过,适合与盘管中的通路共同操作;
所述金属具有一个或多个包含以下的区域:
a) 孔隙率,其使得5-75%、优选10-50%的孔具有0.001-0.5微米的尺寸;或
b) 在所述金属内的陶瓷衬套或在所述金属上的外涂层,所述陶瓷衬套或外涂层具有大于900℃的熔点和使得5-75%、优选10-50%的孔具有0.001微米至0.5微米的尺寸的孔隙率;
所述区域外涂有厚度为0.1-10微米的致密的气体-选择性膜,允许H2、CH4、CO和CO2中的至少一种在500℃至900℃的温度下扩散离开所述通道。
在其他实施方案中,陶瓷由选自以下的氧化物、二氧化物、氮化物、碳化物和磷酸盐形成:多孔二氧化硅、熔融二氧化硅、多孔氧化铝、二氧化钛、二氧化锆、二氧化钍、氧化镧、氧化镁、氧化钙、氧化钡、氧化锡、二氧化铈、氧化锌、氧化硼、氮化硼、碳化硼、磷酸硼、磷酸锆、氧化钇、硅酸铝、氮化硅、碳化硅和其混合物。
在其他实施方案中,致密的气体-选择性膜包含铁、镍、钛、铬、铝和钼中的一种或多种。
在其他实施方案中,致密的气体-选择性膜进一步包含一种或多种选自Pd、Ta、V、Pt、Nb和Zr的金属。
在其他实施方案中,致密的气体-选择性膜进一步包含一种或多种选自Al2O3、BaTiO3、SrTiO3和ZrO2的金属氧化物陶瓷。
在其他实施方案中,致密的气体-选择性膜为致密的金属氧化物膜。
在其他实施方案中,致密的气体-选择性膜包含Pd。
在其他实施方案中,致密的气体-选择性膜包含氧化钇稳定的ZrO2。
在其他实施方案中,致密的气体-选择性膜包含氧化钙稳定的ZrO2。
在其他实施方案中,致密的气体-选择性膜不少于理论密度的约95%。
在其他实施方案中,陶瓷为通过以下形成的Si/C/N陶瓷:
使单体和/或低聚硅氮烷陶瓷前体与包含烯(乙烯基)官能化、低聚、无机或有机硅氮烷、二官能硫醇和四官能硫醇的一种或多种的共聚单体组合;
使所述组合作为基材上的薄膜成形;
使所述薄膜光聚合;和
使所述经光聚合的薄膜热解,以产生基本上不含氧化物的陶瓷膜。
在其他实施方案中,所述单体和/或低聚硅氮烷含有选自硼、钛、铝、磷和其组合的杂原子。
在其他实施方案中,连续金属通道为形成盘管的一部分的管状通道。
在其他实施方案中,连续金属通道为形成盘管的一部分的90°弯管(肘管)或180°弯管(U形管)。
其他实施方案提供了一种在熔炉盘管中从裂化气除去H2、CH4、CO和CO2中的一种或多种的方法,所述方法通过结合一个或多个上述段进行。
其他实施方案提供了一种裂化熔炉,其包含一种或多种上述盘管。
其他实施方案提供了一种裂化链烷烃的方法,所述方法通过在850℃至950℃的温度下使链烷烃通过权利要求1的熔炉盘管进行。
其他实施方案提供了上述方法,其中所述链烷烃为C2-4链烷烃。
其他实施方案提供了上述方法,其中所述链烷烃为乙烷。
实施方案的描述
数字范围
除了在操作实施例中或另外指示,在说明书和权利要求书中使用的涉及成分的量、反应条件等的所有数字或表述应被理解为在所有情况下被术语“约”修饰。因此,除非指示为相反的情况,否则在以下说明书和所附权利要求书中描述的数字参数为近似值,其可根据本发明期望得到的性质而变。至少,并且不试图将等价物原则的适用限制于权利要求的范围,每一个数字参数应至少根据报道的有效数字的数量并且通过应用通常的四舍五入技术来解释。
虽然描述本发明宽泛范围的数字范围和参数为近似值,但是在具体实施例中描述的数值尽可能精确地报道。然而,任何数值固有地含有由其相应的测试测量中存在的标准偏差必然得到的某些误差。
另外,应理解的是,本文引用的任何数值范围旨在包括其中包括的所有子范围。例如,“1-10”的范围旨在包括列举的最小值1和列举的最大值10之间的所有子范围,并且包括1和10;也就是,具有等于或大于1的最小值以及等于或小于10的最大值。由于所公开的数值范围为连续的,它们包括最小值和最大值之间的每一个值。除非明显另外指示,否则在本申请中指定的各种数值范围为近似值。
在实践中,本文表述的所有组成范围总数限于100% (体积百分数或重量百分数)并且不超过100%。当在组合物中可能存在多个组分时,每一个组分的最大量的总和可超过100%,应理解,并且如本领域技术人员容易理解的,实际使用的组分的量将符合100%的最大值。
在链烷烃(诸如石脑油和低级烷烃诸如C2-4链烷烃)的蒸汽裂化中,将物料与蒸汽一起进料至管或盘管,通过裂化器的对流段,其中将物料加热至接近裂化温度(约750℃)。物料随后在熔炉的辐射段中在约0.001-2.0秒(在一些实施方案中,0.001-1秒)的时间内通过盘管。在熔炉的辐射段中,盘管包含多个通过肘管(90°)或“U”形管(180°)连接的直段或通路,以提供蛇形构造。在熔炉的辐射段中,壁安装的燃烧器和/或底板安装的燃烧器将壁加热至它们辐射热量到盘管表面上的温度。盘管的温度在约800℃至约975℃的范围内。在这些温度下,分子被裂化,例如乙烷分解成其原子组分并重排,以形成多个产物,包括乙烯、H2、CH4、CO和CO2。该重排为化学反应,并且在盘管中从气体流除去H2、CH4、CO和CO2副产物的一种或多种将移动转化至期望的产物乙烯。
离开熔炉的气体的组合物含有许多物类,包括自由基,并且需要快速淬灭,以防止流中的分子进一步重排。裂化气流通过输送管线通向热交换器,在这里将气体快速淬灭至某一温度,以防止气体中分子的任何显著重排。淬灭的气体随后进入分离系列。在分离系列中,将气体序贯冷却至低温,以冷凝甲烷、乙烷和丙烷,以及提余液和其他副产物。副产物可包括乙炔和其他重质产物,诸如苯、甲苯和二甲苯(BTX)。来自裂化器的产物流还含有氢、甲烷、一氧化碳和二氧化碳。这些组分也被冷却,并且通过分离系列的各部分。这样对分离系列产生了额外的载荷。期望在进入分离系列之前,优选在进入输送管线之前,降低裂化气中的H2、CH4、CO和CO2的量。
根据本发明,提供了一种用于蒸汽裂化器的熔炉盘管,其包括一个或多个包含通道的段,即金属的通路、肘管或“U”形管的任何段。
通道(例如,通路、管道、肘管或“U”形管)管线通常由熔点大于1000℃、理想地大于1100℃的金属铸成。通路、肘管或“U”形管可由任何高温钢制成。在一些实施方案中,通路或“U”形管为不锈钢,其可选自锻造不锈钢、奥氏体不锈钢和HP、HT、HU、HW和HX不锈钢、耐热钢以及基于镍的合金。通路、肘管或“U”形管可为高强度低合金钢(HSLA);高强度结构钢或超高强度钢。这样的钢的分类和组成为本领域技术人员已知的。
合适的金属组分的其他实例包括,但不限于,铁、镍、钛、铬、铝及其合金,例如,钢、不锈钢、HASTELLOY®合金(例如,HASTELLOY C-22) (Haynes International,Inc.,Kokomo,Ind.的商标)和INCONEL®合金(例如,INCONEL合金625) (INCONEL为Huntington AlloysCorp.,Huntington W. Va.的商标)。在一种实施方案中,输送管线包括含有铬和镍的合金(例如,INCONEL合金625)。在另外的实施方案中,合金含有铬、镍和钼,例如,HASTELLOY C-22或INCONEL合金625。
在一种实施方案中,不锈钢(优选耐热不锈钢)通常包含13-50,优选20-50,最优选20-38重量%的铬。不锈钢可进一步包含20-50,优选25-50,最优选25-48,理想地约30-45重量%的Ni。不锈钢的余量可基本上为铁。
在本发明的一些实施方案中,钢可进一步包含多种微量元素,包括至少0.2重量%,至多3重量%,通常1.0重量%,至多2.5重量%,优选不多于2重量%的锰;0.3-2,优选0.8-1.6,通常小于1.9重量%的Si;小于3,通常小于2重量%的钛、铌(通常小于2.0,优选小于1.5重量%的铌)和所有其他微量金属;和其量小于2.0重量%的碳。存在微量元素,其量使得钢的组成共计100重量%。
在一种实施方案中,不锈钢(优选耐热不锈钢)通常包含13-50,优选20-50,最优选20-38重量%的铬。不锈钢可进一步包含20-50,优选25-50,最优选25-48,理想地约30-45重量%的Ni。不锈钢的余量可基本上为铁。
本发明还可与基于镍和/或钴的极端奥氏体高温合金(HTA)一起使用。通常合金包含主要量的镍或钴。通常基于镍的高温合金包含约50-70,优选约55-65重量%的Ni;约20-10重量%的Cr;约20-10重量%的Co;和约5-9重量%的Fe和余量的以下描述的一种或多种微量元素,使得组成达到100重量%。通常,基于钴的高温合金包含40-65重量%的Co;15-20重量%的Cr;20-13重量%的Ni;小于4重量%的Fe和余量的以下描述的一种或多种微量元素,以及至多20重量%的W。组分的总和加起来达到100重量%。
在本发明的一些实施方案中,钢可进一步包含多种微量元素,包括至少0.2重量%,至多3重量%,通常1.0重量%,至多2.5重量%,优选不多于2重量%的锰;0.3-2,优选0.8-1.6,通常小于1.9重量%的Si;小于3,通常小于2重量%的钛、铌(通常小于2.0,优选小于1.5重量%的铌)和所有其他微量金属;和其量小于2.0重量%的碳。存在微量元素,其量使得钢的组成共计100重量%。
用于通路或通路的一部分、肘管或“U”形管的基材金属可为多孔的。例如,适合用作基材的多孔不锈钢可得自Mott Metallurgical Corporation (Farmington,Conn.)和得自Pall Corporation (East Hills,N.Y.)。
本领域的普通技术人员可使用本领域已知的技术来选择基材厚度、孔隙率和孔径分布。可基于最终复合气体分离模块的操作条件(诸如操作压力)以及其它因素来选择期望的基材厚度、孔隙率和孔径分布。具有通常较高孔隙率和通常较小孔径的基材特别适用于生产复合气体分离模块。在一些实施方案中,基材的孔隙率可在约5-约75%或约10-约50%的范围内。虽然基材的孔径分布可变化,但是基材的孔直径范围可为约0.001微米或更少至约0.1微米或更多,通常0.001-0.05微米,任选0.001-0.01微米。
通常,优选较小孔径。然而,在一些实施方案中,使用具有较大孔的基材,并且在多孔基材上形成具有通常较小孔径的中间层,通常如以下公开的陶瓷(例如,形成梯度支撑)。
在一些实施方案中,基材的平均或中值孔径可在约0.001-约0.05微米,例如,约0.001微米至约0.03或0.05微米的范围。在一些情况下,基材中的孔可为约0.01微米至约0.05微米,例如,可存在0.01微米、0.02微米和0.05微米尺寸的孔。
在一些情况下,多孔金属基材中的孔径可足够大,以允许并非期望的那些的分子(例如,H2、CO、CO2和CH4)通过金属。多孔金属基材需要涂布有致密的气体-选择性膜,如以下描述的。在其他实施方案中,多孔金属基材可首先涂布有陶瓷,随后涂布有致密的气体-选择性膜。
在本发明的一些实施方案中,金属基材可涂布有陶瓷或具有陶瓷衬套(例如,通过金属的通路填充有陶瓷)。陶瓷需要在不小于450℃,优选不小于500℃,在一些实施方案中,不小于550℃,通常850℃至900℃,理想地高达1000℃的温度下稳定。
陶瓷应为由选自以下的氧化物、二氧化物、氮化物、碳化物和磷酸盐形成的多孔陶瓷:多孔二氧化硅、熔融二氧化硅、多孔氧化铝、二氧化钛、二氧化锆、二氧化钍、氧化镧、氧化镁、氧化钙、氧化钡、氧化锡、二氧化铈、氧化锌、氧化硼、氮化硼、碳化硼、磷酸硼、磷酸锆、氧化钇、硅酸铝、氮化硅、碳化硅和其混合物。在一些实施方案中,陶瓷膜可为致密的气体-选择性膜,如以下描述的。
用于形成陶瓷膜的优选的组分包括钛、锆、铝(例如,α氧化铝和γ氧化铝)、镁、硅的氧化物和其混合物。混合氧化铝和氧化硅的陶瓷为沸石,钛等价物为ETS型陶瓷。在陶瓷材料结构中的孔径可为0.0003-1.0微米,在一些实施方案中,0.001-1微米或更大,在一些实施方案中,0.01-0.05微米。该孔径足以允许H2、CH4、CO和CO2中的一种或多种扩散或渗透通过陶瓷。
在本发明的一些实施方案中,陶瓷可掺杂有或含有帮助氢、甲烷、一氧化碳和二氧化碳中的一种或多种运输的金属的颗粒、纤维或晶须。钯、铌、钽、锆、钒及其合金可用于氢的传送。
陶瓷可以干或湿的形式施用。如果以湿的形式(溶液或悬浮液),通常通过热处理除去溶剂/稀释剂,以得到干涂层。该步骤可在达到约400℃的温度下发生。干涂层随后在达到约1500℃的温度下,在惰性气氛(通常为氮气)下烧结约2-48小时的时间段。干燥和烧结过程为本领域技术人员公知的。
在本发明的其他实施方案中,气体选择性(陶瓷)膜由无机聚合物前体形成,所述无机聚合物前体通过光引发交联,随后热解。
进一步有用地用于本发明的聚合物陶瓷方面的材料分为两类:单体或低聚陶瓷前体和多官能硫醇单体。主要感兴趣的陶瓷前体为乙烯基官能化、无机-有机硅氮烷。硫醇化的共聚单体的组成和官能度为另一种变量,其可用于控制交联的聚合物产物性质。四硫醇和具有不同链长的不含氧烷烃二硫醇(独立和串联二者)是优选的。
共聚单体浓度(硅氮烷/硫醇)、共聚单体官能度(例如,二硫醇相对四硫醇,以及当串联使用时二者的比率)以及二硫醇链长为系统变量,其允许受控操纵聚合动力学、网络形成特性,以及相应地,聚合物产物的最终性质。
聚合物膜应利用本发明的光诱导的自由基阶梯式生长硫醇-烯聚合来形成,其中“烯”官能度经由硅氮烷陶瓷前体掺入。聚合将优选在本体材料上进行,即,不需要溶剂。通常的UV光引发剂2,2-二甲氧基-2-苯基苯乙酮将优选用于调节引发动力学。这些硫醇-烯反应的独特的特性是它们能够自引发;因此,使用单独的光引发剂是任选的,对聚合物产物的分子组成和同质性提供另外的控制水平。
聚合物材料性质与单体/低聚反应物的性质、利用的聚合机理、反应条件(温度、气氛、引发速率(照射强度、引发剂浓度和自引发单体浓度以及引发波长))以及反应性官能团的转化程度密切关联。所有这些因素累积规定聚合动力学,以及相应地,聚合物产物的材料和化学性质,和因此其分离特性。
无定形陶瓷膜的形成优选通过加热和热解经由前面描述的阶梯式生长光聚合制造的聚合物陶瓷前体来完成。正像聚合物制造条件和动力学在性质确定中起到重要的作用,热解条件和动力学也一样。因此,聚合物/陶瓷结构/性质对材料的热经历的依赖性的理解是必要的。
交联的聚合物陶瓷前体的热解应优选在若干不同的气氛下,即,在空气、真空、氮、氩和氨下进行,其中气氛规定热解化学,和因此具有从纯SiC到纯Si3N4范围的可达到组成的最终产物的相对Si-C-N组成。加热速率、最终的温度、在某温度下的浸泡时间和冷却速率也优选用于控制聚合物到无定形陶瓷转换,和因此产物的性质。
本发明的聚合反应可在各种条件下实施。例如,反应步骤任选包括以下的一个或多个:例如,照射包含所述单体的组合物,加热包含所述单体的组合物,向包含所述单体的组合物加入至少一种催化剂,和/或等等。所用的辐射可为例如电磁辐射、电子轰击或原子核辐射。在某些实施方案中,例如,将涂布有本文描述的可聚合的组合物的制品或其他基材暴露于辐射源(例如,UV或电子束辐射源)达所选的时间段。为了进一步说明,任选利用一个光子和/或两个光子聚合。关于单一和多个光子聚合的另外的细节在以下中提供:例如,Macak等人(2000) “Electronic and vibronic contributions to two-photonabsorption of molecules with multi-branched structures(对具有多分枝结构的分子的双光子吸收的电子和电子振动贡献)”,J. Chem. Phys. 113(17):7062;Luo等人(2000)“Solvent induced two-photon absorption of push-pull molecules(推-拉分子的溶剂诱导的双光子吸收)”,J. Phys. Chem. 104:4718;和Luo等人(1994) “One- and two-photon absorption spectra of short conjugated polyenes (短共轭多烯的单光子和双光子吸收光谱)”,J. Phys. Chem. 98:7782,各自通过引用结合到本文。用于聚合本发明的单体的光的强度通常为约1-约1000 mW/cm2,更通常约20-约800 mW/cm2,再更通常约50-约500 mW/cm2,例如,在约315-365 nm波长下。此外,辐射暴露时间也变化,例如,根据所用的具体单体、期望的双键转化程度等。为了说明,通常将本文描述的可聚合的组合物暴露于具体的辐射源达几毫秒到几分钟或更久。在一些实施方案中,在5 mW/cm下,本发明的单体在小于60秒(例如,约20秒或更少)内实现基本上完全或定量的双键转化,即,在通常小于0.1 J/cm2的剂量下,实现基本上定量的双键转化。此外,聚合温度通常为0℃-100℃。在优选的实施方案中,聚合在室温(例如,20-25℃)或接近室温下实施。
在聚合反应之后,通常将所得到的聚合物材料热解,以形成陶瓷材料。例如,取决于用于热处理的条件,可得到无定形或结晶结构。当热解在约700-1200℃,优选900-1200℃的温度范围下进行时,通常特别得到无定形结构。当热处理在较高温度下进行时,例如1200-2000℃,优选1500-2000℃,通常得到至少部分结晶结构。热解通常在保护性气体覆盖或反应气体覆盖(例如,氦、氩、氮、氨等)下或在真空中进行。此外,热解通常实施约0.5-2小时,以将聚合物材料转化为陶瓷材料。任选,在热解之后,陶瓷材料经历另外的加工。例如,在至多2000℃,优选1600-2000℃的温度下0.5-2小时的烧结程序之后,通常得到稳定的主体。
最终的陶瓷涂层或衬套的孔隙率应使得5-75%,优选10-50%的孔具有0.001微米至0.05微米的尺寸。
陶瓷或金属基材随后外涂有致密的气体选择性膜。
在一种实施方案中,气体选择性膜为对氢选择性可渗透的致密的气体-选择性膜,并且可包括一种或多种氢-选择性金属或其合金。氢-选择性金属包括,但不限于,铌(Nb)、钽(Ta)、钒(V)、钯(Pd)、铂(Pt)、锆(Zr)及其氢-选择性合金。优选钯和钯的合金。例如,钯可与至少一种选自金、铂、钌、铑、钇、铈和铟的金属成合金。在选择用于合金的组分时需要一些考虑。已提议铜和银作为合金组分。然而,由于裂化气可能含有乙炔和蒸汽,人们将避免银和铜作为合金组分,因为可存在形成乙炔化银或乙炔化铜的倾向,它们呈现爆炸性危险。金属组分可具有约0.3-约3微米的粒径。
致密的气体-分离膜可包括一种或多种不是气体-选择性材料的组分,例如,不是氢-选择性材料的组分,诸如金属氧化物陶瓷,其优选选自氧化铝(Al2O3)、钛酸钡(BaTiO3)、钛酸锶(StTiO3)、被氧化钇或氧化钙稳定或部分稳定的氧化锆(ZrO2)和其各种组合。当使用时,金属氧化物陶瓷可以金属和金属氧化物陶瓷的共混物的10-90 wt.%,优选30-70 wt.%,理想地40 wt.%-60 wt.%的量存在。
致密的气体-选择性膜可具有约0.1-10微米的厚度。例如,在一种实施方案中,致密的气体-选择性膜的厚度为小于约10微米、诸如约3-8微米的基本均匀厚度。
致密的气体-选择性膜的金属组分通常通过以下而活化:使其与SnCl2的溶液(例如,1 g/l,pH约2)接触,随后在接触之后不久从溶液过滤粉末,洗涤,并任选干燥,以得到活化的金属(PdCl2)。活化的金属与金属氧化物陶瓷(如果存在)一起可作为粉末使用,或分散(浆料)或再溶解于合适的溶剂或稀释剂(例如,水)中。
通过用于将微粒材料(例如,粉末)施用于多孔表面的本领域技术人员已知的任何合适的方法,使形成致密的气相选择性膜的微粒材料的层与多孔陶瓷或金属衬套的上表面或外表面(相对于裂化气的流动路径)接触。例如,通过用气体输送,或通过施用微粒材料的糊膏、浆料或悬浮液,或通过在多孔衬套的表面上挤压或摩擦微粒材料的粉末,可将微粒材料施用于多孔金属基材或陶瓷的表面。
在一种实施方案中,进行至少一个接触步骤,同时横过基材(例如,任选涂布有陶瓷的多孔金属基材)施用较高压力和较低压力的压差,其中较高的压力施用于基材的上表面或外表面的一侧。通过使用负压(即,施用于基材的另一个表面(例如,下表面或内表面)的真空),或正压(即,施用于基材的外表面的压力),或二者的组合,可完成施用压差。在优选的实施方案中,在向多孔基材的第二表面(即,内表面)施用真空下,微粒材料作为浆料沉积。
施用于多孔衬套的上表面或外表面(相对于裂化气的流动路径)的微粒材料的量和尺寸可稍有变化,取决于用于沉积微粒材料的方法。在施用微粒材料时,主要目标是完全覆盖多孔基材的表面,其将最终支撑致密的气体选择性(分离)膜。
在微粒材料与多孔基材的上表面或外表面接触以形成第一涂布的表面之后,除去在衬套上存在的任何过量的第一微粒材料。除去方法可变化,取决于施用方法,但是在大多数情况下,可通过摩擦(例如,机械或手动摩擦)而除去。优选,当将真空施用于基材的下表面或内表面(与施用的微粒材料相对的表面)时,进行除去过量的微粒材料的步骤。如果使用湿法(例如,浆料或悬浮液)沉积微粒材料,则应在除去过量的微粒材料之前干燥已涂布的基材,以避免除去湿微粒饼的厚片,这可从多孔基材的孔牵引微粒材料。
在一些实施方案中,施用平均颗粒直径范围为例如约0.001-约0.05微米的较小粒径的微粒材料(金属)组分可用于降低所得到的涂布的多孔基材(支撑)的平均孔径和降低多孔基材的表面粗糙度。实现这些目标涉及解决在微粒材料的选择(例如,微粒材料、施用方法、粒径等的选择)中的若干变量。
致密的气相-选择性膜的沉积可在一个步骤或在多个步骤中进行,优选在每一个步骤之后退火。
用于退火的一种可用的方法涉及在较低温度下在惰性气氛中并随后在氢存在下热处理经涂布的多孔基材。更具体地,在不存在氢下发生退火,直至退火温度为至少250℃,优选至少300℃,更优选至少350℃。一旦退火温度达到250℃,优选300℃,更优选350℃,在退火步骤中可存在氢和氧。换句话说,在优选的实施方案中,在含氢气氛中进行退火步骤,但是仅在温度已达到最低300℃,优选至少350℃,更优选至少400℃之后。虽然退火步骤可采用非常高的温度(例如,600℃或更大),但是在大多数情况下,退火步骤在350℃-550℃,最优选400℃-500℃的温度下发生。在通过连续涂层建立膜的实施方案中,在沉积步骤之间当膜冷却时,从系统吹扫氢。通常,当膜开始冷却时,通过使系统充满惰性气体来吹扫氢,使得当膜达到300℃,优选400℃时,不存在氢。
可用于该热处理步骤的惰性气体包括氮、氦、氩、氖和二氧化碳。用于退火步骤的优选的惰性气体为选自氮、氩、氖和二氧化碳的气体,用于热处理的最优选的惰性气体为氮。
一旦退火温度达到至少300℃(优选更高),进行退火步骤的气态气氛在其中应具有一些氢。在电镀多孔基材的退火步骤过程中使用的气态气氛应包含3-100%的氢和97-0%的惰性气体的混合物。
退火在足以处理覆盖多孔基材(金属或涂布有陶瓷的金属)的外表面的气体-选择性材料(金属)的薄层的温度下进行。虽然所需的退火温度多少取决于在多孔基材上电镀的具体金属或金属合金和其层的厚度,通常,热处理温度应在至少300℃至800℃的范围内。优选的热处理温度在325℃至700℃的范围内,最优选的热处理温度在350℃至550℃的范围内。
进行退火步骤达足以提供气体-选择性材料的层的必要处理的时间段,并且如果需要,将其制备用于接下来的一系列电镀、抛光和退火。因此,退火时间段可在向上高达48或更多小时的范围,但是典型的退火时间段在0.1小时-12小时的范围。然而,优选退火时间最少至仅这样的时间,即,提供实现本发明的益处所需的气体-选择性金属的层的处理所需的时间。预期这样的时间段在0.2-10小时的范围内,或甚至在0.3小时至4小时的范围内。
进行退火的压力可在0.5个大气压(绝对压力)至20个大气压的范围内。更通常,热处理压力在0.8 atm-10 atm的范围内。
认为沉积的金属的晶粒生长参数提高膜稳定性,并且帮助其在升高的温度下耐变化。通过提高退火温度来促进晶粒生长看起来具有有益效果,特别是当在沉积步骤之间将气体选择性材料的层抛光时。抛光步骤在以下更详细地讨论。认为在抛光晶粒中存在一些积极效果,以将它们有效涂抹在敞开的孔中并形成均匀的金属层。已观察到采用这样的方式形成的气体分离系统在高操作温度下耐裂化。
退火后,将具有其退火的支撑的膜层的多孔基材抛光/研磨。通过使表面畸形和缺损最小化和通过填充开口诸如裂缝、针孔和在薄膜层中可能存在的其他缺陷,抛光改进沉积的层的表面,用于进一步沉积。示例性的研磨和抛光方法公开于转让给Shell OilCompany的在Del Paggio等人名下的于2012年5月1日授权的美国专利8,167,976。
在制备本发明的通路、肘管或“U”形管中,人们需要试图尽可能匹配各种组分的热膨胀系数,以使得在部分的不同层之间的内应力最小化和使涂层内的内应力最小化。
根据本发明的管或“U”形管可具有光滑的内部或可具有旋脊内部,以促进湍流。这样的内部旋脊在转让给Kubota Corporation的1999年9月14日授权给Sugitani等人的美国专利5,959,718中公开。不束缚于理论,认为在通道的内表面处湍流将促进裂化气混合物中的较轻气体的扩散。当气体经历离心力而围绕“U”形管穿行时,在“U”形管中分离可更有效(每单位长度)。
“U”形管的壁厚度可能不均匀,以解释内壁的腐蚀。
本发明的通路可任选具有围绕它们的金属护套。护套应由熔化温度不小于约1000℃,理想地大于1100℃的金属制成,如上文关于可制成管或“U”形管的金属所述的。
通路或管道应为相对短的段,长度不大于约4米。如果通路段具有护套,它们的布置应使得它们在其中通路暴露于相对较低量的辐射能量的熔炉的区域中。这使得在整个通路(管和“U”形管)中表面能量的损失最小化。从裂化通路分离的气体将累积至护套和管道或“U”管的外表面之间。护套可具有开口,以允许气体离开进入熔炉,在那里其将被燃烧。在一些实施方案中,设计护套中的开口,使得经过开口的燃烧气体的通路吸引在护套和通路或“U”形管之间的气体至熔炉中(例如,文丘里型管)。在熔炉的辐射段中的温度足够高,使得来自盘管的气体将被燃烧。
对由在盘管表面处燃烧氢引起的盘管温度的提高,需要给予一些考虑。这可提高盘管内的温度,其可能导致在盘管内部的碳沉积。这样的沉积可堵塞孔。对所得到的水对熔炉(特别是通路或管)的辐射段的影响,也需要给予一些考虑。燃烧产物应为水蒸气,但是其可能对引导至盘管的辐射能量具有不利的影响。
在一些实施方案中,护套可将氢引导至熔炉外部的收集工具。
在一些实施方案中,可将基材金属机械加工,以产生敞开的段,其覆盖有或具有包含本发明的陶瓷或致密的气体-选择性膜中的一种或多种的衬套。
护套用作另外的安全性目的,因为如果通道的基材金属故障,则护套将为通路提供一些残余的结构完整性,允许设备处理这种情况。
工业适用性
在熔炉盘管中产生区域,其具有a) 使得5-75%、优选10-50%的孔具有0.001-0.5微米的尺寸的孔隙率;或b) 在所述金属内的陶瓷衬套或在所述金属上的外涂层,所述陶瓷衬套或外涂层具有大于900℃的熔点和使得5-75%、优选10-50%的孔具有0.001微米至0.5微米的尺寸的孔隙率;外涂有厚度为0.1-10微米的致密的气体-选择性膜,允许H2、CH4、CO和CO2中的至少一种在500℃至900℃的温度下扩散离开所述熔炉盘管,移动盘管中的化学平衡,以提高乙烯的产量。
Claims (20)
1.用于蒸汽裂化器的熔炉盘管,其包含一个或多个由以下组成的段:
i) 熔化温度大于1000的连续金属通道,其允许裂化气在其中流过,适合与盘管中的通路共同操作;
所述金属具有一个或多个包含以下的区域:
a) 孔隙率,使得5-75%的孔具有0.001-0.05微米的尺寸;或
b) 在所述金属内的陶瓷衬套或在所述金属上的外涂层,所述陶瓷衬套或外涂层具有大于900℃的熔点和使得5-75%的孔具有0.001微米至0.5微米的尺寸的孔隙率;
所述区域外涂有厚度为0.1-10微米的致密的气体-选择性膜,允许H2、CH4、CO和CO2中的至少一种在500℃至900℃的温度下扩散离开所述通道。
2.权利要求1的熔炉盘管,其中所述金属或陶瓷衬套或外涂层的孔隙率使得10-50%的孔具有0.001-0.05微米的尺寸。
3.权利要求2的熔炉盘管,其中所述陶瓷由选自以下的氧化物、二氧化物、氮化物、碳化物和磷酸盐形成:多孔二氧化硅、熔融二氧化硅、多孔氧化铝、二氧化钛、二氧化锆、二氧化钍、氧化镧、氧化镁、氧化钙、氧化钡、氧化锡、二氧化铈、氧化锌、氧化硼、氮化硼、碳化硼、磷酸硼、磷酸锆、氧化钇、硅酸铝、氮化硅、碳化硅和其混合物。
4.权利要求3的熔炉盘管,其中所述段中致密的气体-选择性膜包含铁、镍、钛、铬、铝和钼中的一种或多种。
5.权利要求4的熔炉盘管,其中所述致密的气体-选择性膜进一步包含一种或多种选自Pd、Ta、V、Pt、Nb和Zr的金属。
6.权利要求5的熔炉盘管,其中所述致密的气体-选择性膜进一步包含一种或多种选自Al2O3、BaTiO3、SrTiO3和ZrO2的金属氧化物陶瓷。
7.权利要求6的熔炉盘管,其中所述致密的气体-选择性膜为致密的金属氧化物膜。
8.权利要求7的熔炉盘管,其中所述致密的气体-选择性膜包含Pd。
9.权利要求7的熔炉盘管,其中所述致密的气体-选择性膜包含氧化钇稳定的ZrO2。
10.权利要求7的熔炉盘管,其中所述致密的气体-选择性膜包含氧化钙稳定的ZrO2。
11.权利要求7的熔炉盘管,其中所述致密的气体-选择性膜不少于理论密度的约95%。
12.权利要求2的熔炉盘管,其中所述陶瓷为通过以下形成的Si/C/N陶瓷:
使单体和/或低聚硅氮烷陶瓷前体与包含烯(乙烯基)官能化、低聚、无机或有机硅氮烷、二官能硫醇和四官能硫醇的一种或多种的共聚单体组合;
使所述组合作为基材上的薄膜成形;
使所述薄膜光聚合;和
使所述经光聚合的薄膜热解,以产生基本上不含氧化物的陶瓷膜。
13.权利要求12的熔炉盘管,其中所述单体和/或低聚硅氮烷含有选自硼、钛、铝、磷和其组合的杂原子。
14.权利要求1的熔炉盘管,其中所述连续金属通道为形成盘管的一部分的管状通道。
15.权利要求1的熔炉盘管,其中所述连续金属通道为形成盘管的一部分的90°弯管或180°弯管。
16.从熔炉盘管中的裂化气除去H2、CH4、CO和CO2的一种或多种的方法,所述方法通过结合一个或多个权利要求1的段进行。
17.一种裂化熔炉,其包含一种或多种权利要求1的盘管。
18.一种用于裂化链烷烃的方法,所述方法通过在850℃至950℃的温度下使链烷烃通过权利要求1的熔炉盘管进行。
19.权利要求18的方法,其中所述链烷烃为C2-4链烷烃。
20.权利要求19的方法,其中所述链烷烃为乙烷。
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