CN102177326B - 控制燃烧产物的方法与装置 - Google Patents
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- Y02E20/34—Indirect CO2mitigation, i.e. by acting on non CO2directly related matters of the process, e.g. pre-heating or heat recovery
Abstract
本发明涉及控制燃烧反应及其产物的方法和系统。一种实施方式包括燃烧控制系统,该系统具有氧化流,所述氧化流主要包括氧和CO2并具有一定的氧与CO2的比例,然后将所述氧化流与燃料流混合并在燃烧室内燃烧,产生具有一定温度和组成的燃烧产物流,所述温度和组成分别由温度传感器和氧分析仪检测,所得数据被用于控制所述氧化流和所述燃料流的流量和组成。系统还可包含具有膨胀器的燃气轮机,所述膨胀器具有一定的负载和反馈布置的负载控制器。
Description
相关申请的交叉参考
本申请要求在2008年10月14日提交的美国临时申请号61/105,331的权益。
发明领域
本发明的实施方式涉及控制燃烧产物的方法与装置。更具体地,提供了用于在氧-燃料型燃烧反应中获得基本化学计量燃烧的方法与装置。
发明背景
本部分旨在介绍与本公开内容的示例性实施方式相关的本领域的多个方面。可以相信此讨论有助于提供一个框架,帮助读者更好地理解本发明的特定方面。因此,应当理解该部分应当从这个角度去阅读,并非一定作为对现有技术的承认。
一些降低CO2排放的方法包括燃料脱碳或燃烧后捕获。然而,这两种解决方案成本高,并且降低了发电效率,导致发电量降低,燃料需求增长,电价上涨以满足国民电力需求。另一种方法是联合循环式氧-燃料燃气轮机(an oxy-fuel gas turbine in a combined cycle)。然而,市场上还没有能以这种循环工作的燃气轮机。
最初的氧-燃料理论基于烃与纯氧的燃烧,这导致极高的温度。这样的高温导致燃烧室寿命的问题,还有多环芳烃(PAH)的形成,这些多环芳烃导致产生油烟。已经尝试了多种解决这些问题的方法并获得不同水平的成功,包括用二氧化碳代替空气作为燃气轮机的质流气体。然而,这种方法和其他方法需要专门的涡轮设备,该设备尚不能在市场上买到。
美国专利号5,724,805公开了一个使用燃气轮机的发电厂,该燃气轮机用烃和氧/二氧化碳混合物相混合后作为燃料。然而,该公开内容陈述到O2/CO2混合物具有比空气更多的O2,因此在非常高的温度下燃烧,这需要巨大的燃烧室以允许燃烧气体有时间逐渐冷却,从而产生更少的一氧化碳(CO)。因此,对于要实施的‘805参考文献中的技术来说,必须使用一种专门的非标准燃烧室。
因此,对有效控制燃烧产物流的温度和组成的方法和系统依然有实际的需求。
发明概述
本发明的一种实施方式公开了一种燃烧控制系统。此燃烧控制系统包括:燃烧室(combustor),该燃烧室至少由初级燃烧区和燃尽区组成;高浓度二氧化碳(CO2)供给(稀释剂供给);氧供给流,该流被配置以至少与高浓度CO2流的第一部分(即初级稀释剂流)组合形成氧化流,该氧化流主要由氧和CO2组成,并具有一定的氧与CO2比例;以及具有一定流量和组成的燃料流。此系统进一步包括:燃烧室,该燃烧室被配置以能在初级燃烧区和燃尽区混合并燃烧氧化流和燃料流,其中加入稀释剂供给的第二部分(即次级稀释剂流)以形成具有一定温度和组成的燃烧产物流;至少一个温度传感器,该传感器被配置以测量燃烧产物流离开燃烧室后的温度,其中此燃烧产物流的温度被用于调节次级稀释剂流的流速,以在燃烧室出口获得所需的温度;以及至少一个氧分析仪,该分析仪被配置以测量燃烧产物流组成中的氧含量,其中燃烧产物中的氧含量被用于调节氧供给流的流速,以实现基本化学计量燃烧。
在一些实施方式中,燃料流可至少由以下成分组成:高质量燃料流,低热值燃料流,以及任选地,高浓度CO2补充流。单独流可以通过各个流的流量控制器与总控制器有效连接,从而控制燃料流的流量和组成以调节燃烧温度,避免熄火。在一些实施方式中,各个流可以被连接到由中央控制系统控制的流量控制器。
在另外的实施方式中,燃烧室可以包括:第一混合区,用以混合高浓度CO2流的第一部分与氧供给流,以形成氧化流;初级燃烧区,该燃烧区被配置以进行燃烧反应,该燃烧反应产生燃烧产物流;以及燃尽区,该燃尽区被配置以将高浓度CO2流的第二部分输送到燃烧室,以调节燃烧室和燃烧产物流的温度。在一个示例性实施方式中,向初始高温燃烧区中添加催化剂以催化燃烧反应。在另一可选实施方式中,第二混合区可被配制以预混合氧化流和燃料流,或者在燃烧反应进行的同时混合所述流。
本发明的另一种实施方式公开了燃烧控制方法。此方法包括:提供高浓度的CO2流,氧供给流,以及燃料流,其中各种流都具有一定的流速和组成;组合至少第一部分高浓度CO2流和氧供给流,形成氧化流;在燃烧室中燃烧氧化流和燃料流,以形成具有一定温度和组成的燃烧产物流;检测燃烧产物流的氧含量;以及调整氧供给流的流速直到燃烧产物流是基本化学计量的。
在本发明的第三种实施方式中,提供了燃烧系统。此燃烧系统包括:燃料流,其主要包括烃和二氧化碳(CO2)并具有初始的燃料和CO2比例;氧化流,其主要包括氧和二氧化碳(CO2),其中燃料流和氧化流被组合以形成燃烧反应物流,该燃烧反应物流中燃料与氧的组合比例被调节以满足所需的平衡比例(其被定义为燃料-氧化剂的实际比例与燃料-氧化剂的化学计量比例的比值),同时该燃烧反应物流中初始CO2与燃料的组合比例被调节以提供初级燃烧区所需的燃烧温度;次级稀释剂流,其主要包括二氧化碳(CO2);和燃烧室,该燃烧室被配置以燃烧该燃烧室入口流以产生主要包括水和二氧化碳的初级燃烧产物,其中初级燃烧产物与次级稀释剂流混合形成燃烧产物流,其具有一定的温度和一定的CO2和燃料终比例。
附图简述
本发明的前述和其它优势可以通过阅读以下对非限制性实施实例的详细说明和附图而变得明显,其中:
图1A-1E说明了四种可选的依照本发明某些方面的示例性控制示意图;
图2图解了一个示例性燃烧室的示意图,此燃烧室可被配置以用于图1A-1E的可选的示例性系统。
图3是一个操作图1A-1E的系统的方法的示例性流程图;
发明详述
在下面的详细说明部分中,本发明的具体实施例将会结合优选实施例进行描述。但是,就下面的说明具体到本发明的特定实施方式或特定应用来说,这仅是为了示例性的目的且仅提供对示例性实施例的说明。因此,本发明并不局限于下面描述的具体实施方式,相反,本发明包括涵盖于附属权利要求的真正精髓和范围内的所有可选方式、修改和等同物。
如本文所用,术语“化学计量燃烧(stoichiometric combustion)”是指燃烧反应具有一定体积的烃(比如燃料)和一定体积的氧,其中所述体积的氧恰好能使所述体积的烃完全或几乎完全燃烧,以产生一定体积的几乎没有氧残余且几乎没有烃残余的燃烧产物。
如本文所用,术语“初级停留时间(primary residence time)”是指在压力和温度的局部条件下,燃烧室产生近似平衡状态的燃烧产物所需的时间。
本公开内容的实施方式提供了设计用于燃气轮机中氧-燃料燃烧的燃烧方法和系统。本发明的优选实施方式解决了与高温氧-燃料燃烧相关的问题,例如能导致油烟的多环芳烃(PAH)的形成,以及有问题的燃烧产物如氧和一氧化碳(或类似的不完全燃烧产物)的产生。燃烧系统设计的一个示例性实施方式包括高浓度二氧化碳(CO2)流,此流被分成至少初级稀释剂流和次级稀释剂流,以及氧供给流,此供给流被配置以与初级稀释剂流组合形成主要包括氧(O2)和二氧化碳(CO2)的氧化流(例如“合成空气”)。此系统还包含燃料流和燃烧室,其中此燃烧室至少由初级燃烧区和燃尽区组成,该燃烧室被配置以混合燃料流和氧化流,并在基本上化学计量燃烧的反应中使其燃烧,形成主要包括水(蒸气)和二氧化碳的初级燃烧产物流。此初级燃烧产物流可经次级稀释剂流稀释形成次级燃烧产物流。
注意,在一些实施方式中,可以采用高压燃烧(例如高于约10个大气压)方法。初级燃烧区的绝热火焰温度可通过改变形成氧化流时CO2与氧的混合比例来控制。燃烧产物流的温度可以独立控制,以在燃烧室出口处获得燃烧产物所需的温度或其他性质。因此,在一些实施方式中,系统将包括用于测量燃烧产物流的温度传感器,并且可以增加燃烧产物流中CO2百分含量以降低燃烧产物流的温度,或者减少CO2百分含量以提高燃烧产物流的温度。
在本发明的一些实施方式中,将CO2和氧混合以制备“合成空气”(例如氧化流)。与氧混合的CO2的量提供了一种控制初级燃烧产物流温度的方法,同时也为辅助控制燃烧产物的组成提供了另一个变量。燃烧室设计可以包括骤冷(熄灭,quench)孔,为燃尽区提供额外的CO2,以防止燃烧产生的高温对燃烧室壳体的冲击。该系统的另外实施方式包括控制系统,此控制系统测量进入燃烧室的烃的量,计算并控制燃烧所需的氧的正确量。该控制系统还利用测量燃烧产物的设备反馈的信息来更新氧供给流流量控制器以确保实现所需的燃烧,从而向氧化流提供正确量的氧。还任选地提供了催化后燃烧步骤,根据燃烧室所用的烃混合物可能需要此步骤。该催化步骤能将初级燃烧产物流中氧降至所需的低水平,以避免提高采收率法采油(EOR)设备中严重的腐蚀问题。
本发明的一些实施方式包括操作氧-燃料燃烧系统的方法,以提供所公开的系统的益处和优势。例如,一种实施方式包括将燃料流与氧化流组合,并将其在燃烧室里燃烧以形成燃烧产物流。燃料流和氧化流可以预先混合或者同时混合和燃烧,并且在一些实施方式中还包括催化剂,这取决于不同流的组成和流速。此方法还包括探测或检测燃烧产物流的温度和/或组成,并调整燃料流和氧化流中至少一种的流速,直至燃烧处于基本化学计量的条件。
本公开内容的方法和装置可用于多种应用,包括燃气轮机燃烧器系统。此燃气轮机燃烧器系统可以是单轴运行的集成气轮机、多轴系统或者具有外置燃烧器的非集成系统,并且根据特定系统的温度、体积和其他变量,甚至可以与独立的压缩机和热气膨胀器一起使用。这些方法和系统可被用来有利地提高燃烧效率(例如,减少未燃烧或部分燃烧燃料和/或氧的量),并且提供在一定负载条件范围内对气轮机入口温度的更好控制。
本专利公开的系统和方法的至少一个优点包括使用商用燃气轮机燃烧罐型系统(combustion can type system)与氧-燃料/联产型系统(oxy-fuel/co-generation type of system)的灵活性,诸如美国专利申请号61/072,292中公开的超低排放发电系统和方法。通过控制与氧混合形成氧化流的CO2的量,也可以控制初级燃烧产物流的温度和组成。所公开的系统和方法的应用可以避免开发展新的燃气轮机燃烧罐的需要,使得“现成(off-the-shelf)”的燃气轮机燃烧室技术应用于这类系统中。
采用的燃烧室可以类似于气化方法中所用的那些,在气化方法中,氧和烃在低于大气压的环境中反应,温度用水蒸气调节。本发明中将用CO2取代水蒸气调节温度。使用水蒸气成本昂贵并也将导致燃烧产物中生成额外的氢气,氢气在本循环中是不需要的。通过混合CO2和氧,还可以使用更传统的扩散型燃烧室,这种燃烧室与现有的燃气轮机使用的那些类似,其中将用CO2取代空气以冷却燃烧衬管(liner)。优选在近似化学计量的条件下燃烧以消除过量氧去除的开支。
本发明的实施方式提供另外的益处。本系统和方法允许操作员或自动化系统分别控制初级燃烧区的温度和燃烧产物流的温度,以及控制燃烧产物,例如限制燃烧产物中腐蚀性一氧化碳和氧的量,因此使燃烧产物能用于提高采收率法采油操作,该操作要求去除这类腐蚀性成分。此外,所公开的系统和方法可以适应可用燃气质量的变化。例如,如果提供的是低热值燃料(例如低于40%的甲烷),例如来自低质量气体储存器或CO2突破后的储存器(a reservoir after CO2breakthrough),则所述系统和方法可以调节氧化流中氧的比例,和/或向燃烧步骤添加高质量燃料或强化燃料(例如氢气)或增加其量,从而维持燃烧产物流适当的温度和组成。
现在来看附图,图1A-1D说明了四种可选的依照本发明某些方面的示例性控制示意图。具体地,图1A是一个基本的示例性系统。系统100包含:高浓度二氧化碳(CO2)流102,该流至少可被分成初级稀释剂流102a和次级稀释剂流102b;和氧供给流104,该流可与初级稀释剂流102a混合形成具有一定氧和CO2比例的氧化流106。还提供了燃料流108,取决于来源,此流可主要由甲烷(CH4)组成,或可包括轻烃、重烃、氢气(H2)和惰性气体例如二氧化碳的混合物。还提供了燃烧室(例如燃烧罐)110,该燃烧室在优选实施方式中被分为两部分,初级燃烧区110a和燃尽区110b,并且该燃烧室被配置以至少接收氧化流106和燃料流108,在初级燃烧区110a混合氧化流106和燃料流108并使之在所需的火焰温度和在燃烧室内足以产生近似平衡状态的热产物流(未显示)的初级停留时间下燃烧,然后在燃尽区110b用次级稀释剂流稀释热产物流,形成燃烧产物流112a,燃烧产物流112a被注入膨胀装置111(例如燃气轮机或者热气膨胀器),该膨胀装置与负载控制器111’有效连接,形成膨胀后产物流112b。该膨胀后产物流112b可被分开形成流113和次级流128,流113可形成高浓度CO2流102的至少一部分,而次级流128可被用于提高采收率法采油(EOR),捕获或另外的用途。系统100还包括温度传感器114和氧分析仪126中至少一个,温度传感器114和氧分析仪126分别被配置以测量燃烧产物流112a或膨胀后产物流112b的温度和氧含量。来自温度传感器114的温度数据被用以控制次级稀释剂流102b的流速以及调整燃烧产物流112a的温度。氧供给104的流速被调整为与燃料供给108的流速成正比。来自氧分析仪126的氧数据被用于调整氧供给流104与燃料供给108的流速的比例系数,直至达到基本化学计量燃烧。
继续参考图1,系统100还包括中央控制器115,该中央控制器115被有效连接到第一流速控制器116a,用于控制初级稀释剂流102a;第二流速控制器118,用于控制氧供给流104;第三流速控制器120,用于控制燃料流108;和第四流速控制器116b,用于控制次级稀释流102b。中央控制器115还可连接到温度传感器114和氧分析仪126,以确定燃烧产物流112a或膨胀后产物流112b中未燃烧氧的量,并用这些测量结果控制氧供给流104的流量。中央控制器115还可以随着负载条件改变,控制燃料流108和氧供给流104的流速以维持所需的化学计量。
高浓度二氧化碳(CO2)流(即“稀释剂供给流”)102可来自任何方便的来源。例如,至少一部分稀释剂供给流102可通过循环流113转用或分离至少一部分膨胀后产物流112b而获得。然而,此系统100可置于另一高浓度CO2来源附近,例如外部管网,高浓度CO2气井,气体处理厂或其他来源。此外,循环流113可包括一些处理,例如过滤系统像膜、分子筛、吸收剂、吸附剂,或其他系统,以除去具有潜在危险性或不需要的成分,例如未反应的氧或烃。特别是,如果氧分析仪检测到膨胀后产物流112b具有高水平的氧,则膨胀后产物流112b不应当用作稀释剂,例如次级稀释剂流102b。类似地,高水平的未反应烃,根据燃烧室110可能也是不可接受的,并且在用作次级稀释剂流102b之前可能需要除去或分离。然而,优选并预期燃烧产物流112a已经经历基本化学计量的燃烧,所以它应具有低于约3.0体积百分数(vol%)的氧,或低于约1.0vol%的氧,或低于约0.1vol%的氧,或甚至低于约0.001vol%的氧,以及低于约3.0体积百分数(vol%)的烃,或低于约1.0vol%的烃,或低于约0.1vol%的烃,或甚至低于约0.001vol%的烃。
次级流(即“残余流”)128可用于出售,用于其它需要高浓度二氧化碳的过程,或被压缩并注入陆地储存器(terrestrial reservoir),用于提高采收率法采油(EOR),捕获(sequestration)或其它用途。与循环流113类似,流128使用前可能需要经过一些处理以除去潜在污染物或反应物,如氮氧化合物(NOx)或氧。同样,优选并预期流104基本不含氮,而流112a已经经历基本化学计量的燃烧,所以它应具有低于约3.0体积百分数(vol%)的氧,或低于约1.0vol%的氧,或低于约0.1vol%的氧,或甚至低于约0.001vol%的氧,以及低于约3.0体积百分数(vol%)的NOx,或低于约1.0vol%的NOx,或低于约0.1vol%的NOx,或甚至低于约0.001vol%的NOx。
氧供给流104可由空气分离单元(air separation unit)或其它提供高纯度氧的过程或系统提供。分离出的氮可用于其它相关过程,例如美国专利申请号61/072,292所公开的氮注入井。在一个示例性实施方式中,氧供给流104可含有约90vol%至约99.9vol%的氧及残余的氩,并且可含有痕量的氮和二氧化碳。在另一示例性实施方式中,氧供给流可含有约95vol%至约96vol%的氧与约4vol%至约5vol%的氩以及少于约0.2vol%的二氧化碳。
中央控制器115可以是任何类型的控制系统,该系统被配置以接受数据输入,例如流速和组成,并发出信号以通过例如阀门、泵、压缩机以及任意其它可用于调整流速的设备控制流速。在一个示例性实施方式中,中央控制器115可包括一台可编程的计算机,该计算机有用户输入设备如键盘和鼠标,用户输出设备如显示器和喇叭,并且能使用有源存储器(RAM)工作,并通过LAN、WAN、Wi-Fi或无线网或其它外部网络与硬盘驱动器、光盘驱动器、网络驱动器和数据库可操作地连接。
流速控制器116a,116b,118和120可包括用于接收和处理来自中央控制器115的信号的可编程自动化控制器,并可与流速阀或叶片、通风孔或其它能增加或减少主要为气态的流的流量的设备可操作地连接。此外,在一个示例性实施方式中,流速控制器116a,116b,118和120可与流量和/或组成传感器可操作地连接,这些传感器能提供额外的数据输入,例如以确认流量控制器所控制的各流流速的变化。为维持火焰稳定和有效控制,任何或所有控制器116a,116b,118和120都使用高速控制器可能是有利的。
尽管流速控制器116b可以是如上所述的有源传感器(activesensor),但是次级稀释剂流102b的流速在一示例性实施方式中可能是不受控制的。例如,燃烧室110可包括衬管,该衬管具有一个或多个骤冷孔(例如稀释孔),这些冷却孔具有特定的样式和容纳大小,被设计以在燃烧室中提供稀释和控制温度。因此,次级稀释剂流102b的流速可主要取决于燃烧室110中骤冷孔的硬件设计,以及稀释剂供给流102的压力、温度和组成。此外,流速控制器116b仍可用于在关机、次级稀释剂102b污染或一些其它原因下切断次级稀释剂102b的流动。在一些实施方式中,中央控制器115还可包括某些传感器的2/3表决系统,例如温度传感器114和氧分析仪126。包括中央控制器115在内的控制系统还可被设置有至少一种安全互锁和/或关机逻辑,以及报警器,用以在系统100失去控制时保护下游设备。
温度传感器114可以是单个传感器,或者可以额外包括备用传感器作为备份,或者一系列分布于燃烧产物流112a或膨胀后产物流112b内部及周围的传感器,以确保精确的温度读取。可以使用任何类型的适用的温度传感器,但所选的传感器应有高耐热性,能在约华氏2,000度(℉)或以上或者甚至约2,200℉以上的温度下有效工作。在所述发明系统100的一些示例性实施方式中,温度传感器114可直接向CO2流量控制器116b发送数据,或者可向中央控制器115发送数据,而中央控制器115控制流量控制器120的响应。可选地,温度传感器114也可直接向燃料流流量控制器120发送数据。此外,可选地,温度传感器114可以从燃烧室110内部排出口附近或者排出后在燃尽区110b下游采集数据,在沿着燃烧产物流112a和膨胀后产物流112b的多个位点采集数据,或者上述采集方法的组合。流112a和112b的温度应该被限制在一定的操作参数内,此参数很大程度上取决于所用的设备,可利用的燃料流和其他输入流的种类,残余流128的潜在用途以及其他因素。
总体而言,初级燃烧区110a的温度应低于约3,500℉以避免NOx产生,同时也因为大部分商用燃烧室110不能在此温度以上工作,但如果燃烧室110的材料可以在更高的温度下工作且系统100中也没有氮,则此限制可设定得更高。膨胀器111入口处的温度优选地低于约2,500℉。如此的高温也有助于生成不需要的多环芳烃(PAH’s),而多环芳烃会导致油烟产生。然而,初级燃烧区110a的温度必须足够高以避免熄火,所述避免熄火是根据进入初级燃烧区的反应物的温度和从特定燃料108可得到的释放热,通过调节氧与CO2比例而实现的;并且足够高以有效地燃烧掉几乎全部的氧(O2)和烃(例如化学计量的燃烧温度),以使形成的膨胀后产物流112b只需要有限的处理就可以用于提高采收率法采油(EOR)或用作系统100的稀释剂。对于许多情况,燃烧产物流112a的优选温度将在至少约1,500℉至最大约2,500℉或者至少约1,600℉至最大约1,900℉。对于许多情况,初级燃烧区的优选绝热火焰温度将在至少约2,450℉至最大约3,500℉,除非在采用了改进的结构材料并且燃烧反应物中没有氮的情况下所述上限可以提高。
氧分析仪126可以是单个传感器,也可以包括额外的传感器作为备用,或者是一系列位于多个位置的传感器以确保精确测量。例如,可以使用多个lambda或宽带氧化锆O2传感器为中央控制器115和/或氧供给流流量控制器118二者之一提供反馈。如果使用lambda传感器,由于燃烧产物流112a中氧含量在化学计量系数1.0上下变化,可设置中央控制器115,使燃料流108中的燃料与氧供给流104中的氧的比值高频振动。该高频振动过程与汽车工业中内燃机中所使用的类似。在任何情况下,燃烧产物流中的氧含量优选地低,其从低于约3.0体积百分数(vol%),至低于约1.0vol%,至低于约0.1vol%,至低于约0.001vol%。如果氧含量过高,则氧供给流104的流速会被降低。反过来,如前文所述,这可降低火焰温度,需要调整燃料流108的流速。
图1B图解了图1A中所示的的基本示例性系统,但具有另外的任选特征,这些特征被配置以进一步处理或调节产物流112a和112b。因此,参照图1A能最好地理解图1B。系统140包括所公开的与图1A相关的所有特征,但它另外包含以下装置:燃烧后催化装置146,此装置被配置以减少产物流112a和112b以及燃料旁路流142中的氧和一氧化碳含量,燃料旁路流142具有一定的流速和组成并具有用于控制燃料旁路流142流速的流量控制器144。氧分析仪126可直接或通过中央控制器115间接地与流量控制器144有效连接。在某些特定的实施方式中,燃料旁路流142具有分支,或者流128有回路,可能需要额外的流量控制器和氧分析仪(未显示),参见下文进一步的讨论。
催化装置146可以是单个设备,或者多个串联或并联的设备,但优选工作能耗小的小型设备。特别地,催化装置146可以是一氧化碳还原催化器和/或氧还原催化器,这些催化器通常用于余热回收蒸汽发生器(HRSG’s)以满足排放要求。此类系统通常不是设计用于除去大量的氧,但如果膨胀后产物流112b中有大量的氧,膨胀后产物流112b在被压缩并注入用于提高采收率法采油(EOR)之前,可能需要多次循环通过催化装置146。因此,在一些实施方式中,催化装置146后端需要另一个氧分析仪(未显示)以确保注入流128含有足够低量的氧(例如低于约0.5体积分数(vol%)的氧或低于约0.1vol%),以避免压缩和注入设备被腐蚀,并避免通过注入可与储存器中残留的烃反应的氧而使储存器酸化。
燃料旁路流(例如燃料流的第二部分)142被配置以与膨胀后产物流112b在循环流113从膨胀后产物流112b分离的下游混合,并优选地在催化装置146的上游引入以便可在催化装置146中使用额外的烃以提高氧的去除效率。然而,在一些可选的实施方式中,旁路流142可在催化装置146的前后被分流并引入。在EOR流128环流回催化装置146的实施方式中,在EOR流128环流回催化装置146之前向EOR流128中引入一部分旁路流142可能是有益的。有益处地,旁路流142被配置以在EOR流128被压缩并注入储存器前降低其中氧的体积分数,以基本避免压缩和注入设备的腐蚀和注入储存器中残留的烃的酸化。
图1C是图1A所述系统的第三种示例性实施方式的图示,此实施方式可包括或者可不包括图1B实施方式的图示中所公开的特征。因此,参照图1A和图1B能最好地理解图1C。系统150包含:烃分析仪152,其被配置以测量产物流112a和/或112b组成中烃的含量;高质量燃气供给108a,由流量控制器154控制;以及低热值燃气供给108b,由流量控制器156控制。流量控制器156可以直接连接至烃传感器152和/或可以通过中央控制器115连接。流量控制器154、156以及任选地120可有效连接至总控制器(summation controller)158,其可直接或通过氧供给控制器118与中央控制器115连接。
高质量燃料气流108a可由基本纯的甲烷(例如,约99vol%)组成,并可选地可以含有“强化(spiking)”燃气例如氢气,较重的烃(C3+)或其任意组合。高质量燃料气流108a的组成主要依据系统150的需要和不同燃料种类的可利用性变化,但优选地将不包括大量惰性气体(例如氮气,二氧化碳等)或酸性气体(例如二氧化硫,硫化氢等)。高质量燃料气流108a可来自任意合理的气源,但优选地来自附近的产气田而不是从显著的远处引入。特别地,如果流108a是氢,则其可从自附近的产气田(未显示)所产气流的自热重整(ATR)过程中提供。
低热值燃气气流108b可由低于约80vol%的甲烷,低于约60vol%的甲烷,低于约40vol%的甲烷,或者甚至低于约20vol%的甲烷组成。低热值流108b也可含有少量的重烃例如乙烷和丙烷。在多数情况下,流108b剩余部分主要是惰性气体如二氧化碳,但在某些情况下,将会有少量的氮气、硫化氢、氦气和其他气体。优选地,除了二氧化碳外的所有非烃和所有惰性气体都要在混合和燃烧之前从流108b中分离。
在一个示例性实施方式中,两个含烃流108a和108b的流量和组成被用于计算燃烧室110运转所需的氧量,并将该设定值提供给氧供给流量控制器118。该计算可提供燃烧室110中进行化学计量燃烧所需的氧量。系统150寿命期间,各种流的流量和组成可根据流108a和108b的来源变化。例如,低热值燃气108b可能来自EOR井,该井在早期生产中具有高的甲烷含量(例如约80vol%以上)。在这样的情况下,高质量燃气流108a的流量可以很低甚至没有。然而,当发生突破时,来自低热值燃气流108b的流量可能含非常低的甲烷含量(例如低于约20vol%)。在那种情况下,高质量燃气流108a的流量需要增加以向燃料流108中加入烃。
图1D是图1A系统的第四种示例性实施方式的图示,该实施方式可包括或者可不包括图1B和图1C实施方式图示中所公开的特征。因此,参考图1A-1C能最好地理解图1D。系统160还包含高浓度CO2补给流108c,该流具有一定的流量和组成,以及与其有效连接的流量控制器162。CO2补给流108c可与流108a和108b组合形成燃料气流108,所述燃料流108在系统160寿命期间具有基本恒定的组成。此方法与系统150类似,但燃烧室的物理特征可根据108的组成特别设计,并且仍可燃烧具有不同组成的燃料108b。CO2流108c可以由膨胀后产物流112b分流或来自另外的来源。
图1E是图1A至1D系统的第四种示例性实施方式的图示。因此,参考图1A-1D能最好地理解图1E。系统170包括:燃料流108,其主要包括烃和二氧化碳(CO2)并且具有一个燃料与CO2的初始比例;氧化流106,其主要包括氧和二氧化碳(CO2),其中燃料流108和氧化流106组合形成燃烧室入口流172,其具有被配置以满足最优平衡比例的燃料与氧的组合比例以及被配置以提供最优燃烧温度的二氧化碳与燃料的组合初始比例;次级稀释剂流102b;和燃烧室110,其被配置以燃烧燃烧室入口流172,产生主要包括水和二氧化碳的热产物流174,其中该热产物流174与次级稀释剂流102b混合形成燃烧产物流112a,该燃烧产物流112a具有一定的温度和CO2与燃料的终比例。
在一些示例性实施方式中,燃料流108中的烃主要由甲烷组成,燃料与氧的摩尔比为从约1.9∶1的mol燃料/mol氧至约2.1∶1的mol燃料/mol氧,或从约1.95∶1的mol燃料/mol氧至约2.05∶1的mol燃料/mol氧。这些摩尔比几乎等同于化学计量比例,即0.9∶1至约1.1∶1。在另一些的示例性实施方式,燃料流108中的烃主要由甲烷组成,并且CO2与燃料的终比例为从约10∶1的mol CO2/mol燃料至约30∶1的molCO2/mol燃料,或从约15∶1的mol CO2/mol燃料至约25∶1的molCO2/mol燃料,或从约20∶1mol CO2/mol燃料至23∶1的mol CO2/mol燃料。
在至少一种示例性实施方式中,系统170还包括:高质量燃气流108a,其具有一定的流量和组成;低热值燃料流108b,其具有一定的流量和组成;高浓度CO2补给流108c,其被配置以与高质量燃气流108a和低热值燃料流108b组合形成燃料流108,并维持该燃料流108中恒定的燃料与CO2的初始比例。额外的实施方式还包括:氧供给流104,其具有一定的流量和组成;高浓度CO2混合流102a,其具有一定的流量和组成,被配置以与氧供给流104组合形成氧化流106。
在又一示例性实施方式中,系统170还额外包括:至少一个温度传感器114,其被配置以测量燃烧产物流112a和/或膨胀后产物流112b(以及任选地,热产物流174)的温度,其中流112a或112b的温度被用于计算高浓度CO2混合流102a、高浓度CO2补给流108c和次级稀释剂流102b中至少一个的流速,以调节燃烧温度;至少一个氧分析仪126,其被配置以测量产物流112a和/或112b组成中的氧含量,其中产物流112a-112b中氧含量被用于优化氧供给流104的流速,以达到基本化学计量燃烧;和至少一个烃分析仪152,其被配置以测量产物流112a-112b组成中的烃含量,其中产物流112a-112b组成中的烃含量被用于优化氧供给流104的流速以达到基本化学计量燃烧。系统170还可包括具有一定负载的燃气轮机111和被配置以测量该负载的负载控制器111’,其中负载测量结果被用于根据负载变化维持燃料与氧的组合比例。
图2图解了一个示例性燃烧室的示意图,此燃烧室可被配制用于图1A-1D的可选示例性系统。因此,参考图1A-1D能最好地理解图2。燃烧室系统200包括:第一混合区202,第二混合区204,初始高温初级燃烧区205,燃尽区206,以及任选的燃料喷嘴208a和208b。热产物流(或“初级燃烧产物流”)212产自初级燃烧区205。注意,在一些示例性实施方式中,可采用高压燃烧过程(例如高于约10个大气压)。
第一混合区202被配置以混合初级稀释剂流102a和氧供给流104,以形成氧化流106。第二混合区204被配置以混合氧化流106和燃料流108。在一种实施方式中,流106和108可以在第二混合区204预先混合,然后直接流入初级燃烧区205。在另一种实施方式中,即非预混方式中,第二混合区204与初级燃烧区205重合并同时出现,类似于扩散燃烧器型布置。初级燃烧区205包括燃烧器,火焰和燃烧反应本身,燃烧反应产生热产物流212。燃尽区206将次级稀释剂流102b输送到燃烧室110,以调节燃烧室110和燃烧产物流112a的温度。
在燃烧室110的一些示例性实施方式中,燃尽区206包含下列之一:被动稀释区,其具有一系列用于冷却和骤冷燃烧室110的衬管的孔;主动稀释区,其具有至少一个骤冷孔,该骤冷孔被配置以主动将至少一部分次级稀释剂流102b输送入燃烧室110并与初级燃烧产物流212混合;一系列分级骤冷孔,以主动控制燃尽区206内的温度模式;以及其任意组合。此外,燃尽区206可包括压力传导器或其他传感器210,以监测和测量燃烧室110内的压力振荡,这种压力振荡是火焰熄灭的迹象。燃烧室110还可包含氧分析仪(未显示),为氧反馈回路提供另一个输入信号。
在非预混布置的一种示例性实施方式中,燃料流108a和108b可在单独的喷嘴208a和208b引入,这些喷嘴基于各自流的体积流量进行配置,或者混合并作为燃料流108混合组合物由一个喷嘴注入。
氧化流106和燃料流108在燃烧室110内的组合被配置以维持最低的绝热火焰温度和火焰稳定性,以燃烧掉氧化流106中的全部或几乎全部氧(例如,化学计量反应是优选的)。就热值而言,氧化流106没有热值,高质量燃气流108a可具有相对高的热值(例如,从至少500英热单位/标准立方英尺(BTU/scf)至约950BTU/scf),而低热值燃气流108b具有相对低的热值(例如从约150BTU/scf至约450BTU/scf)。
燃烧室110可以是标准外部燃烧室,或者可以是定制或改良的燃烧室。可采用的燃烧室种类的实例包括:富氧克劳斯(oxyClaus)燃烧室、部分氧化(POX)燃烧室、自热重整(ATR)燃烧室和燃气轮机扩散燃烧室。注意每种类型的燃烧室可能需要一些改良才能使用基本上CO2流工作。
在一种示例性实施方式中,第二混合区204和喷嘴208a和208b被配置以高度湍流的方式混合燃料流108和氧化流106以确保得到均匀的混合物。在运行期间,初级燃烧区205产生高达约2,200℃的温度。加入骤冷气流102b后,燃烧产物流112a进入燃尽区206时的温度有望达到约1,400℃。通过燃尽区206的外壁可引入额外的骤冷气流102b,生产一种“气膜(gas envelope)”,以保证燃烧室110的室壁比火焰205显著冷。在一种示例性实施方式中,如有必要,冷却流102b可以去除烃,以使油烟形成最少。在另一种示例性实施方式中,燃烧在高于大气压力的环境中进行,例如约10个大气压以上。反应生成水(蒸汽)和二氧化碳,如以下的方程式所示(进入该室的二氧化碳基本未参与反应):
CH4+2O2=2H2O+CO2
图3是操作图1A-1D系统的方法的示例性流程图。因此,参考图1A-1D能最好地理解图3。方法300从步骤(框,block)302开始,包括以下步骤:供给304高浓度CO2流102、氧供给流104和燃料流108,其中每个流都有一定的流速和组成;分流306高浓度CO2流102为初级稀释剂流102a和次级稀释剂流102b,每个流都有一定的流速;调整308初级稀释剂流的流速,这独立于高浓度CO2流的总流速;组合310初级稀释剂流102a和氧供给流104形成氧化流(例如“合成空气”)106;在燃烧室110的初级燃烧区110a燃烧312氧化流106和燃料流108,形成具有一定温度和组成的燃烧产物流112a;检测314燃烧产物流112a中的氧含量;以及利用了检测到的氧含量调整316氧供给流104的流速,直到燃烧产物流112a是基本化学计量的。在一种实施方式中,方法300包括:检测314燃烧产物流112a的温度;以及利用检测到的温度调整316初级稀释剂流102a的流速以调节燃烧温度。在一种实施方式中,此方法包括:将318燃烧产物流112a的一部分引导至提高采收率法采油(EOR)过程。
实施例
作为单一产气田或不同产气田中不同生产阶段气流的实例,下表提供了一些示例性气流组成。表1提供了生产开始时或附近生产井的具体流组成和流速。
表1:初始
表2提供了CO2突破后生产井中具体的流组成和流速。
表2:突破后
尽管本发明可以容许各种修改和可选形式,仅以示例的方式展示了上面所讨论的示例性实施方式。然而,同样应该理解的是并不希望本发明被局限于这里所公开的具体实施方式。实际上,本发明包括落在附属权利要求的真正精髓和范围之内的所有可选形式、修改和等同形式。
Claims (38)
1.一种燃烧系统,其包括:
高浓度二氧化碳(CO2)流;
至少一个CO2流量调节装置,其被配置以调整所述高浓度CO2流的总流速,并将所述高浓度CO2流分成具有一定流速的初级稀释剂流和具有一定流速的次级稀释剂流,其中所述至少一个流量调节装置进一步被配置以调整初级稀释剂流的流速,这独立于所述高浓度CO2流的总流速;
具有一定流速的氧供给流;
至少一个氧流量调节装置,其被配置以调整氧供给流的流速;
混合装置,其被配置以组合初级稀释剂流和氧供给流,以形成氧化流,所述氧化流具有一定的流速和一定的氧与CO2的比例;
燃料流,其具有一定的流速和组成;以及
燃烧室,其至少由初级燃烧区和燃尽区组成,其中所述燃烧室被配置以在所述初级燃烧区内混合所述氧化流和所述燃料流并使之在一定的火焰温度和足以产生近似平衡状态的热产物流的初级停留时间下燃烧,
其中所述燃烧室被配置以在所述燃尽区内用所述次级稀释剂稀释所述热产物流以形成具有低于3.0vol%的氧的燃烧产物流。
2.权利要求1所述的系统,其中所述燃烧产物流具有低于所述热产物流的温度。
3.权利要求2所述的系统,还包括:
控制系统,其包括:
第一控制器,其被配置以调节所述氧供给流的流速与所述燃料流的流速成比例,以便在所述初级燃烧区内产生近似化学计量的燃烧;
第二控制器,其被配置以通过控制所述初级稀释剂流的流速调节所述氧化流中氧与CO2的比例,以产生一定的初级燃烧区火焰温度,所述火焰温度被配置以在燃烧室平均速度、所述燃烧室的排气极限、和在所述燃烧室内足以产生近似平衡状态下燃烧产物流的所述初级停留时间之间提供足够的余量。
4.权利要求3所述的系统,还包括膨胀装置,所述膨胀装置被配置以使燃烧产物流膨胀,形成温度低于所述燃烧产物流的膨胀后产物流。
5.权利要求4所述的系统,所述控制系统还包括至少一个温度传感器,其与所述控制系统和所述CO2流量调节装置有效连接并且被配置以测量所述燃烧产物流的温度并向所述控制系统发送信号,所述控制系统被配置以根据所述燃烧产物流的温度调整所述次级稀释剂的流速,以在所述燃烧系统出口后方一定位置形成具有所需温度的次级燃烧产物流。
6.权利要求5所述的系统,还包括至少一个氧传感器,所述至少一个氧传感器位于所述膨胀后产物流中,离所述膨胀装置出口有一定距离,所述至少一个氧传感器被配置以测量所述膨胀后产物流中氧含量并向所述控制系统发送信号,其中所述控制系统被配置以调整所述氧化流中氧与所述燃料流中燃料的氧与燃料的比例,以达到基本化学计量燃烧,所述基本化学计量燃烧的标志为所述膨胀后产物流中氧含量接近0,以及当少量增加氧比例时,所述膨胀后产物流中氧含量是可检测的。
7.权利要求6所述的系统,还包括:
至少一个负载控制器,其被配置以控制所述燃料流的流速,以维持所述膨胀装置中所需的负载条件。
8.权利要求1所述的系统,其中,根据所述高浓度CO2流和所述次级稀释剂流流径中至少一个节流器的压降,被动地控制所述次级稀释剂流的流速。
9.权利要求6所述的系统,还包括中央控制器,所述中央控制器被有效连接至:
所述至少一个温度传感器和至少一个氧分析仪;
控制所述初级稀释剂流的第一流速控制器;
控制所述氧供给流流速的第二流速控制器;
控制所述燃料流流速的第三流速控制器;和
控制所述次级稀释剂流的第四流速控制器。
10.权利要求4所述的系统,其中所述燃烧产物流主要由水和二氧化碳(CO2)组成,并且所述高浓度CO2流至少部分地由所述膨胀后产物流的CO2部分组成。
11.权利要求10所述的系统,其中所述膨胀后产物流的CO2部分的至少一部分被用于提高采收率法采油(EOR)。
12.权利要求11所述的系统,还包括燃烧后催化装置,其被配置以在用于提高采收率法采油(EOR)之前,减少所述燃烧产物流中的氧含量。
13.权利要求12所述的系统,还包括位于所述燃料流上的分流器,其被配置以将所述燃料流分成第一部分和第二部分,所述第一部分被配置以进入所述燃烧室,所述第二部分被配置以绕过所述燃烧室,并且在燃烧后催化装置上游,与所述膨胀后产物流混合,以形成提高采收率法采油的注入流。
14.权利要求1所述的系统,所述燃烧系统还包括第一混合区,所述第一混合区位于所述燃烧室上游并且被配置以混合所述初级稀释剂流和所述氧供给流,形成所述氧化流。
15.权利要求1所述的系统,还包括催化剂,其中所述催化剂被加入所述初级燃烧区,催化所述燃烧反应。
16.权利要求14所述的系统,还包括第二混合区,所述第二混合区被配置以在一位置预混所述氧化流和所述燃料流,所述位置选自:所述初级燃烧区上游和所述初级燃烧区内,从而所述氧化流和所述燃料流的混合与燃烧几乎同时进行。
17.权利要求12所述的系统,其中所述燃尽区包含选自下列的特征:具有一系列用于使燃烧室衬管冷却和骤冷的孔的被动稀释区;具有至少一个骤冷孔的主动稀释区,该骤冷孔被配置以将所述次级稀释剂主动输送到所述燃烧室以与所述燃烧产物流混合;一系列分级骤冷孔,用于主动控制所述燃尽区的温度模式;及其任意组合。
18.权利要求9所述的系统,其中所述氧化流包含至少5体积百分数的氧到至少40体积百分数的氧,并且所述氧化流的其余部分包含至少95体积百分数的CO2到99.9体积百分数的CO2。
19.权利要求9所述的系统,还包括:
具有一定流量和组成的高质量燃气流;
具有一定流量和组成的低热值燃气流,其被配置以与所述燃气流组合形成所述燃料流。
20.权利要求19所述的系统,还包括:
用于控制所述高质量燃气流的第五流量控制器;
用于控制所述低热值燃气流的第六流量控制器;和
与所述第五和第六流量控制器有效连接的总控制器,其被配置以控制所述燃料流的流量和组成,以调节燃烧温度,避免熄火。
21.权利要求20所述的系统,还包括至少一个烃分析仪,其被配置以测量所述燃烧产物流组成中烃的量,并至少与所述第六流量控制器有效连接,以控制低热值燃气的量,以避免所述燃烧室中熄火。
22.权利要求19所述的系统,还包括具有一定的流量和组成的高浓度CO2补充流,其被配置以与所述低热值燃气流和所述高质量燃气流组合形成所述燃料流,其中所述高浓度CO2补充流与第七流量控制器有效连接,所述第七流量控制器与所述总控制器有效连接,所述总控制器被配置以调整每种流的流量,以在所述燃料流中产生基本恒定的流量和组成。
23.燃烧控制方法,包括:
提供高浓度CO2流、氧供给流和燃料流,其中每种流具有一定的流速和组成;
将所述高浓度CO2流分流为均具有一定流速的初级稀释剂流和次级稀释剂流;
调整所述初级稀释剂流的流速,这独立于高浓度CO2流的总流速;
组合所述初级稀释剂流和所述氧供给流,形成氧化流;
在燃烧室的初级燃烧区燃烧所述氧化流和所述燃料流以形成热产物流;和
在所述燃烧室的燃尽区内用所述次级稀释剂稀释所述热产物流以形成具有一定温度和组成的燃烧产物流,
其中所述燃烧产物流具有低于3.0vol%的氧。
24.权利要求23所述的方法,还包括:
检测所述燃烧产物流中的氧含量;和
利用所述检测到的氧含量,调整所述氧供给流的流速,直到所述燃烧产物流是基本化学计量的。
25.权利要求24所述的方法,还包括:
检测所述燃烧产物流的温度;和
利用所述检测到的温度,调整进入所述燃烧室燃尽区的所述次级稀释剂流的流速,以调节燃烧温度。
26.权利要求25所述的方法,还包括提供高质量燃气流、低热值燃气流和所述初级稀释剂流;并将所述高质量燃气流与所述低热值燃气流和所述初级稀释剂流组合以形成所述燃料流。
27.权利要求26所述的方法,还包括使用流量控制器控制所述高浓度二氧化碳流、所述氧供给流、所述高质量燃气流、所述低热值燃气流和所述初级稀释剂流的流量,其中所述流量控制器与中央控制器有效连接。
28.权利要求23所述的方法,还包括在所述燃烧室的所述初级燃烧区预混所述氧化流和所述燃料流。
29.权利要求23所述的方法,还包括通过向所述初级燃烧区加入催化剂,催化所述燃烧。
30.权利要求26所述的方法,还包括:
检测所述燃烧产物流中未反应烃的量;和
根据所述燃烧产物流中未反应烃的量,控制所述低热值燃气流的流量。
31.权利要求26所述的方法,还包括通过控制所述高质量燃气流、所述低热值燃气流和所述初级稀释剂流每一个的流量,维持所述燃料流基本恒定的流量和组成。
32.燃烧室系统,包括:
燃料流,其主要包括烃和二氧化碳(CO2)并具有一定的烃与CO2的初始比例;
氧化流,其主要包括氧和二氧化碳(CO2),其中所述燃料流和所述氧化流被组合以形成燃烧室入口流,所述燃烧室入口流具有满足最优平衡比例的燃料与氧的组合比例,以及提供最优燃烧温度的CO2与燃料的组合初始比例;
稀释剂流,其主要包括二氧化碳(CO2);和
燃烧室,其被配置以燃烧燃烧室入口流,产生主要包括水和二氧化碳的热产物流,其中所述热产物流与所述稀释剂流混合,形成具有一定温度和CO2与燃料的终比例的燃烧产物流,
其中所述燃烧产物流具有低于3.0vol%的氧。
33.权利要求32所述的系统,其中所述烃主要由甲烷组成,并且燃料与氧的比例为0.9∶1的mol燃料/mol氧至1.1∶1的mol燃料/mol氧。
34.权利要求32所述的系统,其中所述烃主要由甲烷组成,并且所述CO2与燃料的终比例为20∶1的mol CO2/mol燃料至25∶1的molCO2/mol燃料。
35.权利要求32所述的系统,还包括:
具有一定流量和组成的高质量燃气流;
具有一定流量和组成的低热值燃气流;和
高浓度CO2补充流,其被配置以与所述高质量燃气流和所述低热值燃气流组合形成所述燃料流,并维持所述燃料流中恒定的燃料与CO2的初始比例。
36.权利要求35所述的系统,还包括:
具有一定流量和组成的氧供给流;和
具有一定流量和组成的高浓度CO2混合流,其被配置以与所述氧供给流组合形成所述氧化流。
37.权利要求36所述的系统,还包括:
至少一个温度传感器,其被配置以测量所述燃烧产物流的温度,其中所述燃烧产物流的温度被用于计算选自以下的流的流速:所述高浓度CO2混合流,所述高浓度CO2补充流,所述稀释剂流及其任意组合,以调节燃烧温度;
至少一个氧分析仪,其被配置以测量所述燃烧产物流组成中的氧含量,其中所述燃烧产物流中的氧含量被用于优化所述氧供给流的流速,以达到基本化学计量的燃烧;和
至少一个烃分析仪,其被配置测量所述燃烧产物流组成中的烃含量,其中所述燃烧产物流组成中的烃含量被用于优化所述氧供给流的流速,以达到基本化学计量的燃烧。
38.权利要求37所述的系统,还包括流量控制器,其与所述稀释剂流有效连接并被配置以主动控制所述稀释剂流的流速,以优化所述燃烧产物流的温度。
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- 2009-08-31 WO PCT/US2009/055544 patent/WO2010044958A1/en active Application Filing
- 2009-08-31 PL PL09820963T patent/PL2344738T3/pl unknown
- 2009-08-31 US US13/062,442 patent/US9222671B2/en active Active
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EP2344738A4 (en) | 2017-11-29 |
US20110300493A1 (en) | 2011-12-08 |
US9222671B2 (en) | 2015-12-29 |
CA2737133A1 (en) | 2010-04-22 |
EP3489491B1 (en) | 2020-09-23 |
EP2344738A1 (en) | 2011-07-20 |
AU2009303735B2 (en) | 2014-06-26 |
MX2011002770A (es) | 2011-04-26 |
SG195533A1 (en) | 2013-12-30 |
US20170241638A1 (en) | 2017-08-24 |
AU2009303735A1 (en) | 2010-04-22 |
JP5580320B2 (ja) | 2014-08-27 |
US10495306B2 (en) | 2019-12-03 |
US9719682B2 (en) | 2017-08-01 |
WO2010044958A1 (en) | 2010-04-22 |
BRPI0920139A2 (pt) | 2015-12-22 |
PL2344738T3 (pl) | 2019-09-30 |
EP3489491A1 (en) | 2019-05-29 |
EP2344738B1 (en) | 2019-04-03 |
JP2012505987A (ja) | 2012-03-08 |
US20140318427A1 (en) | 2014-10-30 |
CA2737133C (en) | 2017-01-31 |
CN102177326A (zh) | 2011-09-07 |
EA026915B1 (ru) | 2017-05-31 |
EA201170573A1 (ru) | 2011-10-31 |
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