CN107250324B - 将天然气直接并入烃液体燃料 - Google Patents
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Abstract
本发明提供了将气态烃并入液态烃中的方法。所述方法包括以下步骤:将气态烃暴露于非热等离子体以活化气态烃,其中所述非热等离子体是使用E/N比在约10Td至约30Td范围内的减弱的电场产生的;并使活化的气态烃与液态烃接触以将气态烃并入液态烃中。该方法具有能耗低和资本支出相对较低的优点。
Description
技术领域
本发明涉及将气态烃并入液体燃料的领域。具体地,本发明涉及使用非热等离子体活化气态烃以将其并入液态燃料的方法。
背景技术
美国页岩气的近期发展提供了充足的天然气供应。这种增加的供应导致天然气价格的急剧下降。与天然气相比,原油和其他液体燃料的销售大幅溢价,基于能量当量,原油交易价格比天然气高约70%,柴油交易价格比天然气高约80%。换句话说,用于产生与一桶原油的能量相同量的天然气的成本显著低于原油价格。
此外,在石油工业中将来自油井的天然气简单燃烧的燃烧惯例浪费了大量的天然气。世界银行估计,仅在2011年就有超过1400亿立方米的天然气被燃烧,污染了大气层,且浪费了价值约500亿美元的天然气。要求结束燃烧惯例的国际压力越来越大。石油行业使用的一个解决方案是将这些大量的天然气重新注入油井,以代替燃烧,尽管该方案导致大量额外成本却未给公司提供实质的利益。大型能源公司正在积极寻求更好的方式将来自油井的天然气转化为更稳定和更易于运输的液体燃料。
用于将天然气转化为高价值油和“直接替代(drop-in)”燃料的传统技术包括将甲烷转化为合成气,然后进行Fischer-Tropsch合成(FTS)。这项技术为高端资本密集型技术。该技术采用多级工艺以将甲烷分子分解成碳和氢,然后由碳和氢重构合成油分子,最后将合成油精制为成品“直接替代”合成燃料。该合成油完全由转化的甲烷分子制成。因为该工艺是资本密集型工艺,所以其仅在附近便宜的天然气供应充足并进行大规模生产的情况下是经济上可行的。
US 2012/0297665公开了通过将轻质气体和液体燃料结合来制造混合燃料的方法。该方法包括以下步骤:将包含一种或多种轻质气体的反应物引入反应器,在足以使第一反应物重整以产生合成气、自由基和高能电子的条件下将第一反应物暴露于非热等离子体,将液体燃料引入到反应器,使反应产物与非热等离子体紧密接触并与反应器中的液体燃料接触以产生混合燃料。轻质气体可以包括例如二氧化碳和诸如甲烷、乙烷、丙烷、乙醇和甲醇的烃类。
US 2011/0190565公开了一种将气态烃转化为液态燃料的方法,其包括:将气态烃引入具有槽和由电极环绕的放电区的反应器中,将液体吸附剂引入槽中并在放电区域中产生非热的重复脉冲式滑动电弧放电,从而产生液态烃燃料。液体吸附剂可以是汽油、柴油、煤油、液态烷烃或其组合。
US 2009/0205254公开了一种使用非热等离子体将甲烷气体转化为液体燃料的方法。该方法包括以下步骤:提供具有反应室的反应器,提供甲烷气体流和反应物气体流至反应室中,在反应室中提供催化剂,在反应室中产生非热等离子体以将甲烷气体和反应物气体转化为自由基,并将自由基引导到催化剂上以将自由基结合成液体形式的烃。反应物气体可以包括例如CO2、O2和H2O。
美国第6,896,854号专利公开了一种用于将重质烃如重质原油和诸如天然气的烃气体反应性共转化为较轻质的烃材料如合成的轻质原油的***和方法。该方法依赖于使用介电阻挡放电等离子体,这使得在单一步骤中同时向重油中加入碳和氢。该***包括具有介质阻挡放电等离子体单元的反应器,该等离子体单元具有一对电极,所述电极被两者之间的介电材料和通道隔开。在反应器中可以任选地使用填充床催化剂以提高转化效率。
这些已知的方法使用非常强的电场和高电子能量来破坏诸如甲烷的气态烃以产生诸如CH3·的反应性自由基或合成气以相互反应或与重质烃反应。结果,这些方法需要大量的能量,这些方法的能量需求使得这些方法在小规模实施时在经济上没有吸引力。对于需要较低资本支出并具有相对较低运营成本的用于将产量丰富的天然气高效转化为高价值液体燃料的可扩展方法存在明确的市场需求。
本发明使用较弱的电场来产生非热等离子体,以将诸如甲烷的气态烃活化成反应状态,而不会使气态烃分子的键断裂。活化的气态烃能够与液体燃料中较长链的烃反应,从而将天然气的组分并入液体燃料中。
发明内容
一方面,本发明提供了一种将气态烃并入液态烃中的方法,其包括以下步骤:将气态烃暴露于使用E/N比在约10Td至约30Td范围内的电场产生的非热等离子体,以提供活化的气态烃,以及使活化的气态烃与液态烃接触。
另一方面,本发明的电场通过选自滑动电弧放电、微波放电、电晕放电、大气压辉光放电和介质阻挡放电的放电来产生。
附图说明
图1描绘了本发明的一个实施方案,其采用滑动电弧放电产生非热等离子体,并且具备甲烷再循环。
图2示出了本发明的一个实施方案,其采用滑动电弧放电阵列产生非热等离子体。
图3示出了本发明的一个实施方案,其采用介质阻挡放电产生非热等离子体。
图4描绘了本发明的一个替代实施方案,其采用介质阻挡放电产生非热等离子体。
图5示出了本发明的一个实施方案,其采用电晕放电产生非热等离子体。
图6A和6B示出了实施例1中进行的使用N2+CH4混合物的滑动电弧非热等离子体处理期间甲醇组成的变化。
图7为表示本发明的一个实施方案的流程图,其用于将气态烃并入液体燃料中。
图8示出了本发明的一个实施方案,其采用大气压辉光放电使用单管式HV电极产生非热等离子体。
图9示出了本发明的一个实施方案,其采用大气压辉光放电使用多个直立方向的管式HV电极产生非热等离子体。
图10示出了本发明的一个实施方案,其采用大气压辉光放电使用多个水平方向的管状HV电极产生非热等离子体。
图11A为实施例2中使用的30%甲基萘和70%十六烷的液体混合物在DBD等离子体处理之前(底线)和之后(顶线)的化学位移在1.6-4.0ppm范围内的NMR光谱。
图11B为30%甲基萘和70%十六烷的液体混合物在经历天然气存在下的介电阻挡放电等离子体处理之前(底线)和之后(顶线)的化学位移在6.3-8.7ppm范围内的NMR光谱。
图12A为实施例2中使用的30%甲基萘和70%十六烷的液体混合物在APG等离子体处理之前(底线)和之后(顶线)的化学位移在1.6-4.0ppm范围内的NMR光谱。
图12B为30%甲基萘和70%十六烷的液体混合物在经历天然气存在下的大气压辉光放电等离子体处理之前(底线)和之后(顶线)的化学位移在6.3-8.7ppm范围内的NMR光谱。
图13A示出了在进行等离子体处理之前和进行在天然气存在下的大气压辉光放电处理之后的傅立叶变换红外光谱之间的差异,其显示由于等离子体处理,饱和度增加(以新的C-H键表示),并且甲基萘中的苯环数量减少。
图13B示出了在进行等离子体处理之前和进行天然气存在下的介电阻挡放电处理之后的傅立叶变换红外光谱之间的差异,其显示由于等离子体处理,饱和度增加(以新的C-H键表示),并且甲基萘中的苯环数量减少。
具体实施方式
为了说明的目的,通过参考各种示例性实施方案来描述本发明的原理。虽然本文具体描述了某些实施方案,但是本领域普通技术人员会容易地认识到,相同的原理同样适用于并且可以用于其他***和方法中。在详细解释本发明的公开实施方案之前,应当理解,本发明的应用不限于所示的任何特定实施方案的细节。此外,本文使用的术语是为了描述而不是限制的目的。此外,尽管参照本文中以某种顺序提出的步骤描述了某些方法,但是在许多情况下,这些步骤可以以本领域技术人员可以理解的任何顺序进行。因此,新的方法不限于本文公开的步骤的具体布置。
必须注意的是,除非上下文另有明确规定,本文和所附权利要求中所使用的单数形式“一种”、“一个”和“该”包括复数指代。此外,术语“一种”(或“一个”)、“一个或多个”和“至少一个”可以在本文中互换使用。术语“包括”、“包含”、“具有”和“由...构成”也可以互换使用。
本发明提供了将一种或多种气态烃如甲烷并入液态烃的方法,优选该液态烃为液体燃料的液态烃或用于形成液体燃料的液态烃。参考图7,该方法包括以下步骤:使用E/N比在约10Td至约30Td范围内的电场产生(10)非热等离子体,将一种或多种气态烃暴露于(20)非热等离子体以活化气态烃,并使活化的气态烃与一种或多种液态烃接触(30),以提供液体燃料。活性气态烃将与液态烃反应,从而被并入到液态烃中以形成液体燃料的一部分。E/N比是减弱的电场(reduced electric field)的量度,其中E是单位为V/cm的电场,N是中性粒子的浓度或数量密度(例如,电场中的气体颗粒密度)。E/N值与产生非热等离子体的室中的压力无关。E/N比10-30Td对应于0.2-2eV范围内的电子能量(通过光谱测量)。
本发明使用非热等离子体来活化气态烃。如本文所用,“等离子体”是指电离气体,其被提供足够的能量以使电子从原子或分子中游离出来并使得离子和电子共存。如本文所用,术语“非热等离子体”或“非平衡等离子体”或“冷等离子体”是指非处于热力学平衡状态的等离子体。虽然非热等离子体中的电子具有高电子温度,但是等离子体中其他原子和分子的温度相对较低,因此该体系不处于热力学平衡状态。
与非热等离子体相比,热等离子体是作为在气体放电中的强气体加热至数千开尔文的温度的结果产生的,因此,热等离子体中的气体分子、离子和电子的能量分布处于热力学平衡状态。粒子之间,尤其是电子和重阳离子或中性粒子之间的产生的大量碰撞导致能量的快速重新分布,从而达到热力学平衡。
参考图1,在一个实施方案中,非热等离子体可以通过E/N比在约10Td至约30Td范围内的减弱的电场来产生。以这种方式产生的非热等离子体在大气压力下产生大量的振动-平动非平衡。振动-平动非平衡的程度可以通过实验(光谱学)来测量。在一些实施方案中,减弱的电场的E/N比可以在约12Td至约28Td、或约14Td至约26Td、或约14Td至约24Td、或约16Td至约22Td、或约18Td至约20Td的范围内。本发明的减弱的电场通常产生约0.2eV至约2eV、或约0.4eV至约1.8eV、或约0.6eV至约1.6eV、或约0.6eV至约1.4eV、或约0.8eV至约1.2eV、或约0.9eV至约1.2eV、或约0.9eV至约1.1eV的范围内的电子能量。
这种非热等离子体可以通过几种不同的方式产生,至少包括高气流滑动电弧放电、微波放电、电晕放电、大气压辉光放电和介质阻挡放电。
参考图7,在暴露(20)的步骤中,气态烃暴露于非热等离子体,从而被激活成反应状态。通过本发明的减弱的电场产生的非热等离子体激活了气态烃分子,但是如同许多现有技术方法中的情况,未提供足够的能量来使气态烃分子中的化学键断裂以产生自由基或合成气。在一些实施方案中,气态烃以非常低的压力(接近真空)进入非热等离子体,在一些实施方案中,压力可高于大气压。压力范围为约0.1atm至约3atm、或约0.1atm至约3atm、或约0.1atm至约3atm、或约0.3atm至约2.7atm、或约0.5atm至约2.5atm、或从约0.7atm至约2.2atm、或约0.8atm至约2atm、或约0.8atm至约1.5atm。
不受理论的约束,认为气态烃分子在接触非热等离子体之后被振动和平动地激活。这种激发不足以破坏气态烃分子的化学键(C-C或C-H),因为这通常需要E/N比在100-200Td范围内的减弱的电场。相反,活化的气态烃分子与液态烃分子反应而没有任何键断裂,并且被并入到液态烃分子中成为所生产的液体燃料的一部分。在一些实施方案中,气态烃是甲烷。活化的甲烷的振动温度约为2000-4000K,而气体温度不高于700-1100K。
如本文所用,术语“气态烃”是指在22摄氏度和1大气压下以气态存在的轻质烃材料。轻质烃材料通常是具有1-4个碳原子的低级烃。例如,这种轻烃材料可以包括但不限于甲烷、乙烷、丙烷、正丁烷、异丁烷和叔丁烷,或任何两种或更多种这类化合物的混合物。在一些实施方案中,轻质烃可以是与从石油生产获得的天然气或气体相关的轻质烃,或者该轻质烃可以是由于填埋作业或其他天然气矿藏或天然气发电而产生。
在一些实施方案中,气态烃可以存在于还含有惰性气体如二氧化碳或氮气的组合物中。这种混合物可暴露于非热等离子体,在这种情况下,只有气态烃被活化,而惰性气体保持惰性,因此不参与形成液体燃料的化学反应。
在一个优选的实施方案中,气态烃为甲烷。甲烷可以是纯甲烷气体的形式。或者,甲烷气体可以是从“化石燃料”矿床中获得的天然气成分,其通常由约90%以上的甲烷以及少量的乙烷、丙烷和“惰性气体”如二氧化碳和氮气组成。作为另一替代方案,甲烷气体可以是衍生自有机材料(如有机废物)的生物气体的形式。在一些实施方案中,甲烷气体可以由温度范围为22-300℃且压力范围为1-3atm的罐(或管道)提供。
参考图7,在使一种或多种活化的气态烃与一种或多种液态烃接触(30)的步骤中,活化的气态烃与液态烃反应,因此并入液态烃并成为液体燃料的一部分。不受理论的约束,认为活化的气态烃分子(以甲烷为例)遵循如下所述的放热等离子体催化并入过程:
CH4*+RH→CH3R(H)H,
CH4*+ROH→RCH3+H2O,
CH4*+R1=R2H→CH3R1R2H,
CH4*+Armt→CH3RH
这里CH4*是活化的甲烷分子;RH—烃的通式;Armt—芳烃。
相对于涉及使甲烷分子中的化学键断裂的现有技术方法,这些反应以低能耗进行。R表示液态烃的任何烃基。可以在本发明中发生的另一种并入方法可以通过以下步骤进行:第一步将活化的气态甲烷分子结合以形成二聚体、三聚体或更高级聚合物(乙烷、丙烷等),然后将这些二聚体、三聚体或更高级聚合物并入液态烃。
如本文所用,术语“液态烃”包括在液体燃料中发现的多种烃,其具有C5-C28、或至多C25、或至多C20的R基团。这样的液态烃包括但不限于C5-C28烷烃、C5-C28烯烃、C5-C28炔烃、其异构形式、以及任何两种或更多种这类化合物的混合物。液态烃的混合物可以在例如原油、汽油、柴油、煤油、烃蜡和烃油中找到。
液态烃通常是液体燃料的组分。如本文所用,术语“液体燃料”是指在22℃下为液体形式的任何烃基燃料。如本文所用,术语“烃基”是指在本发明的上下文中的液体燃料具有主要的烃特征。烃基燃料包括本质上完全是烃的基团,即它们只含有碳和氢。它们还可以包括含有不改变基团主要烃特征的取代基或原子的基团。这些取代基可以包括卤代-、烷氧基-、硝基-、羟基等。这些基团也可以含有杂原子。合适的杂原子对本领域技术人员是显而易见的,包括例如硫、氮和氧。因此,在本发明的上下文中这些基团保留了主要烃特征的同时,可以含有除碳原子以外的原子,其存在于原本由碳原子构成的环中。
适用于本发明的液体燃料的实例包括有机材料和烃类材料,例如汽油、煤油、石脑油、瓦斯油(gas oils)、加热油、柴油、燃料油、残余油和其他由包括重油在内的原油通过可将石油分离成不同分子量的各种馏分的分离和/或反应过程(如蒸馏和裂化)而制得的石油产品。在一些实施方案中,液体燃料可以是低级液体燃料和由煤、页岩油、沥青砂、焦油砂等通过各种液化方法衍生的合成燃料。液体燃料也可以是液体烷烃、液体烯烃或液体炔烃。也可以使用“直接替代”燃料。
在一些实施方案中,在接触步骤(20)中,为了在气态烃和液态烃之间产生更多的接触以促进并入反应,液体燃料可以以小液滴的形式引入,或者可以被雾化至平均直径范围为约1微米至约30微米、或约3微米至约27微米、或约5微米至约25微米、或约7微米至约23微米、或从约10微米至约20微米、或约12微米至约18微米。使用小液滴的液体燃料可以确保液态烃具有非常大的接触表面,以便于将气态烃并入液态烃中。在一些实施方案中,液体燃料可以作为蒸汽引入。
在一个实施方案中,可以通过本领域技术人员已知的任何合适的装置将液体燃料喷雾为小液滴组成的雾。例如,可以使用气动喷嘴或雾化器来提供所需直径范围的液滴。因此,在该实施方案中,液体燃料可以单独地或以组合的形式包括上述任意或全部液态烃,条件是液体燃料的形式为当其与超临界流体组合时能够被喷雾并形成所需的液滴尺寸。
在一些实施方案中,在接触步骤(30)中,相对于化学计量的气态烃,使用过量的液态烃。在一个实施方案中,气态烃和液态烃之间的摩尔比在约1:20至约1:2、或约1:18至约1:4、或约1:16至约1:5、或约1:14至约1:6、或约1:12至约1:7、或约1:10至约1:8的范围内。
在一些实施方案中,可以任选地存在催化剂以催化活化的气态烃并入到液态烃中。在一个实施方案中,并入发生在可设置催化剂的反应室中。这样的催化剂可以增加并入产量并减少反应时间。示例性催化剂包括但不限于金属、纳米球、线(wires)、负载型催化剂和可溶性催化剂。如本文所用,“纳米球”或“纳米催化剂”是指其中催化剂的平均直径在1nm至1μm范围内的催化剂。在一些实施方案中,催化剂是油溶性催化剂。这种催化剂在油加工过程中分散良好,不会沉淀。在一些实施方案中,催化剂可以是双官能团催化剂,例如包含无机碱的催化剂和含有过渡金属如铁、铬、钼或钴的催化剂。
在一些实施方案中,在反应过程中催化剂以总反应物质质量的约0.03%至约15%的水平存在。在一些实施方案中,催化剂以总反应物质质量的约0.5-2.0%的水平存在。在一个非限制性的示例性实施方案中,基于总反应混合物,引入反应混合物中的催化剂的浓度为约50ppm至约100ppm。在一些实施方案中,催化剂以至少约50ppm的水平存在。在一些实施方案中,催化剂以反应混合物的约50ppm至约80ppm的水平存在。
在一些实施方案中,催化剂为有机金属化合物。示例性的有机金属化合物含有过渡金属、含过渡金属的化合物或其混合物。催化剂中的示例性过渡金属包括选自元素周期表第V、VI和VIII族的元素。在某些实施方案中,催化剂的过渡金属是钒、钼、铁、钴、镍、铝、铬、钨、锰中的一种或多种。在一些实施方案中,催化剂是金属环烷酸盐(metalnaphthanate)、硫酸乙酯或多金属阴离子的铵盐。在一个实施方案中,催化剂是有机钼络合物(例如,MOLYVAWM 855(R.T.Vanderbilt Company,Inc.of Norwalk,Conn.,CAS登记号64742-52-5)),含有约7%至约15%的钼的有机酰胺的有机钼络合物。在另一个实施方案中,催化剂是HEX-CEM(Mooney Chemicals,Inc.,克利夫兰,俄亥俄州,含有约15%的2-乙基己酸钼)或H25/L605的双金属线、切削屑或粉末催化剂(Altemp Alloys,Orange Calif.),其包括约50-51%的钴、20%的铬、约15%的钨、约10%的镍、至多约3%的铁和1.5%的锰。
在另外的实施方案中,其他合适的催化剂包括在液体燃料中高度可溶同时具有较高的钼负载量的化合物。在一些实施方案中,催化剂赋予燃料润滑性,这是超低硫柴油产品所必需的。在一些实施方案中,有机金属化合物除用作催化剂外还增加了液体燃料的润滑性,从而无需向最终混合燃料产品中添加进一步的润滑性添加剂。可用于本文公开的方法的其他有机金属化合物是在第7,790,018号和第4,248,720号美国专利中公开的那些,这两篇专利通过引用并入本文。
在一些实施方案中,催化剂可以负载在沸石上。催化剂可以是微丸、颗粒、线、网筛、多孔板、棒和/或条带的形式。在一个说明性实施方案中,催化剂混合物包括铝线、钴线(含有约50%钴、10%镍、20%铬、15%钨、1.5%锰和2.5%铁的合金)、镍丝、钨丝和铸铁颗粒。在另一个实施方案中,催化剂为金属合金线的形式。这样的金属合金线包括但不限于上述的过渡金属,包括但不限于有机钼催化剂。催化剂可以与气体和液体燃料组合地布置在固定床或流化床中。
在接触步骤(30)之后,将气态烃和液体燃料的混合物输送到可以为冷凝器的收集容器中。收集容器的顶部空间中的气相主要由未并入的气态烃组成,该气态烃可以通过泵/压缩机再循环回到暴露步骤(20)。同时,收集容器中的液相包括具有并入的气态烃的液体燃料。
液相可以从收集容器中移出,并通过分离器进一步分离成重馏分、烷烃和硫化合物。分离器可以包括用于分离液体和固体以及将不同的液体馏分彼此分离的过滤器、膜、离心机、蒸馏器(still)、塔和/或其他已知的装置。
本发明具有将气态烃并入液体燃料的高转化率(即产率)。在一些实施方案中,气态烃的转化率为约5%至约50%、或约7%至约40%、或约10%至约30%、或约15%至约25%、或约17%至约22%、或约18%至约20%。在一些实施方案中,当未反应的气态烃再循环回来以与非热等离子体接触时,气态烃的整体转化率可以大于约80%、或大于约85%、或大于约88%、或大于约90%、或大于约92%、或大于约95%、或大于约98%。在一些实施方案中,气态烃的总转化率为约80%至约99.5%、约80%至约98%、约80%至约95%、约85%至约99.5%、约85%至约98%、或约85%至约95%。在一些实施方案中,气态烃的转化率为约80%至约90%。
在一个示例性实施方案中,使用本发明通过将原油暴露于非热等离子体活化的甲烷分子来处理1,000桶重质原油。活化的甲烷与原油反应并永久地并入原油中,以约30重量%的甲烷并入水平产生约1,300桶的油。除了将油的总量从1,000桶增加到1,300桶之外,该方法还增加了油的氢含量并降低了其粘度。可以使用“直接替代”燃料来重复该示例性实施方案,以扩大体积并提高“直接替代”燃料的性能品质。
可以使用等离子体液化***(PLS)来实施本发明,该***通过高气流滑动电弧放电、微波放电、电晕放电或大气压辉光放电或介质阻挡放电产生非热等离子体。
大气压辉光放电是用于产生非热等离子体的优选方法。为了使用大气压辉光放电,将气态烃置于大气压下的电场中。大气压下的辉光放电产生非热等离子体。气态烃、非热等离子体和液态烃的组合导致气态烃并入液态烃中。在一个实施方案中,气态烃作为气泡存在于电场中的液态烃中,并且在气泡中产生等离子体以活化气态烃,从而提供活化的气态烃,如本文所述的CH4*。位于液态烃内的活化的气态烃必然与液态烃接触且并入其中。在一个实施方案中,气态烃从液体的下方或较低部位引入液体,以使气态烃上升通过液体从而增加气态烃与液态烃之间的接触时间。
在液态烃中以气泡的形式提供气态烃以进行大气压辉光放电使得气态烃被有效地并入到液态烃中。这是因为产生的等离子体在大气压下是不稳定的,因此活化的气态烃分子只存在很短的时间。这为活化的气态烃接触液态烃提供了更多的机会,从而显著提高气态烃液化效率。
通过大气压辉光放电产生的等离子体的一个潜在缺点是在大气压力(而不是真空)下气态烃中分子颗粒的密度相对较高。结果,气态烃的活化物质在与另一活化的气态烃分子碰撞之前通常具有相对较短的自由程并潜在地损失能量。因此,在一些实施方案中,引入到液态烃中的含有气态烃的气泡可以进一步包含惰性气体,例如N2。在一些实施方案中,气态烃与惰性气体之间的体积比在约1:1至约20:1、或约2:1至约15:1、或约5:1至约12:1、或约7:1至约12:1、或约9:1至约11:1的范围内。
在一些实施方案中,气态烃可以在暴露于非热等离子体之前被干燥,以防止活化的气态烃被水猝灭。可以通过使气态烃经过硅胶管、分子筛或任何其他合适的干燥装置来干燥气态烃。
为了产生大气压辉光放电,使用至少一对电极、高电压(HV)电极和接地电极来产生E/N比在约10Td至约30Td的范围内的电场。在优选的实施方案中,将气态烃引入到两个电极之间的空间中。电场在电极之间产生等离子体,并且等离子体激发气态烃以产生活化的气态烃。
用于产生大气压辉光放电的电极由可以在约1kV至约5kV、或约1.2kV至约4.5kV、或约1.5kV至约4kV、或约1.7kV至约3.5kV、或约2kV至约3kV的范围内的电压驱动。电流可以在约0.2mA至约10mA、或约0.4mA至约8mA、或约0.6mA至约6mA、或约0.8mA至约4mA、或约1.0mA至约2.0mA的范围内。
在一些实施方案中,电压可以甚至更高,例如在5kV至约50kV、或约10kV至约40kV、或约20kV至约30kV的范围内。在一些实施方案中,电压可以与用于向电极施加高电压的直流电流相关联。在一些其他实施方案中,电压可以与用于驱动电极的交流电流相关联。这样的交流电的频率可以在约1kHz至约500kHz、或约5kHz至约400kHz、或约10kHz至约300kHz、或约15kHz至约200kHz、或约20kHz至约150kHz、或约20kHz至约100kHz、或约25kHz至约75kHz的范围内。
选择施加到电极的电势的参数以防止气态烃和液态烃的解离和热解,以及仅实现甲烷分子的振动/平动激发,随后并入液体燃料中。本领域技术人员可以根据该方法中使用的具体气态烃调节电压、电流和/或频率以实现这些目标。
在一些实施方案中,将气态烃连续引入液态烃中并暴露于在电极之间产生的非热等离子体以提供连续过程。在这个过程中,如果需要,液态烃也可以连续地供给到等离子体产生区。该过程的持续时间可以由液态烃的不饱和度确定。如本领域技术人员所理解的,具有较高不饱和度的液态烃通常需要更长的处理时间以使液态烃饱和。在处理过程中可以定期测试液体燃料,以便根据液态烃的饱和度来监测反应进程。在一些实施方案中,液态烃可以在气态烃和等离子体的存在下处理长达约5分钟、或长达约10分钟、或长达约15分钟、或长达约20分钟、或长达约30分钟、或长达约45分钟、或长达约1小时、或长达约1.5小时、或长达约2小时、或长达约3小时、或长达约4小时。
不希望受理论约束,示例性气态烃(例如来自天然气的甲烷)并入液态烃(R1=R2)中涉及烃分子的饱和,如下所示:
R1=R2+CH4→HR1-R2CH3,ΔH=-0.5eV/mol
该反应是放热的,因此能量消耗不超过CH4的0.3eV/mol。另一方面,涉及液态烃的可由非热等离子体引起的其他反应(例如聚合和解离)是强吸热的,因此在直接液化过程中是不利的。
使用大气压辉光放电来产生非热等离子体具有以下几个优点:
-易于扩大至工业规模,因为多对电极可以连接到用于产生等离子体的单个电源;和
-在液态烃中产生非热等离子体,其中等离子体、气态烃和液态烃的直接相互作用确保高的并入效率。
以下描述的示例性实施方案使用甲烷作为气态烃。然而,应当理解,在这些示例性实施方案中也可以使用其他气态烃,例如乙烷和丙烷。
所有这些放电应在0.1-3atm的压力范围内操作;气温为-22℃至300℃。等离子体功率与气体流量的比值(平均焓)应不大于CH4的0.3kW-h/m3。维持这个比值可确保E/N 10-30Td。
图1中示出了本发明的一个实施方案,其中,示出了包括等离子发生器105的等离子体液化***100(PLS)。图1所示的PLS 100包括等离子体反应器103、气泵110、流动管线和冷凝器114。
等离子体反应器103适于保持液体燃料104并且还包括等离子体发生器105。等离子体发生器105使用高压(HV)电极115、接地电极116和从电源(未示出)提供的能量产生滑动电弧等离子体放电106。应当理解的是,所使用的电源可以是能够提供足够能量以产生滑动电弧等离子体放电106的任何电源。
当使用PLS 100时,通过滑动电弧等离子体放电106的天然气被激活成反应状态,并且被并入到液体燃料104中,从而增加保持在等离子体反应器103内的液体燃料104的体积。
位于反应器103内的剩余的挥发性轻质烃和液体燃料微液滴可经由排气口109从等离子体反应器103中移出。然后将挥发性轻质烃和液体燃料微液滴转移到冷凝器112中。冷凝器112可以通过空气、水或适于提供冷却的其他手段(例如制冷剂)来冷却。然后,气泵110可以将未反应的天然气通过流动管线111泵送并进入入口113。未反应的天然气可以再循环回到等离子体发生器105。
PLS 100的压力可以保持在0.1-3atm之间,可以通过可操作地连接到等离子体反应器103的压力计108来维持和监测压力。在等离子体液化过程中,PLS 100中的CH4压力下降并且将新鲜天然气连续地添加到PLS 100中。其他产生的液体燃料104周期性地从等离子体反应器103和冷凝器112中去除。
在该实施方案中,通过由滑动电弧等离子体放电106产生的非热等离子体的天然气被激活为反应状态,并且并入到液体燃料中,从而增加其体积。夹带在废气流中的未反应的天然气和液体燃料微滴在水冷式冷凝器112中凝结。气泵用于将未反应的天然气再循环回滑动电弧等离子体发生器105中。发生这种情况的温度优选为室温至约300℃。温度可以由常规的加热器维持。
图2中示出了本发明的另一个实施方案。图2中的元件与图1中具有相似的编号的元件具有相同的功能。在图2中,示出了使液体燃料204的流动流连续液化的PLS 200。
在图2所示的PLS 200中,在等离子体反应器203中使用等离子体发生器205的阵列。“阵列”是指使用多于一个的等离子体发生器205。每个等离子体发生器205包含HV电极215和接地电极216,每个电极可操作地连接到电源。HV电极215和接地电极216产生滑动电弧等离子体放电206。
液体燃料管230也是PLS 200的一部分。等离子体反应器203的等离子体发生器205的阵列流体连接到液体燃料管230。液体燃料管230的尺寸可以被设定为根据需要承载尽可能多的液体燃料204。
在PLS 200中,每个等离子体发生器205作用于天然气,同时部分液体燃料204通过液体燃料入口217被注入到等离子体反应器203中。液体燃料入口217位于HV电极215内。液体燃料204通过滑动电弧等离子体放电206。甲烷通过气体入口218也被注入到等离子体发生器205中。然后液体燃料204在滑动电弧等离子体放电206中被激活,然后甲烷与液体燃料204的微滴和蒸汽反应从而提供高效的甲烷并入。
然后将该气体/液体混合物225注入到液体燃料204的连续流动流中,液体燃料204移动经过液体燃料管230,在液体燃料管230中等离子体化学反应进行至完成。
PLS 200中使用的方法可以通过增加另外的滑动电弧等离子体发生器205来扩大到任何所需的水平。未反应的天然气可以以与上述相同的方式再循环回到等离子体发生器205中,以将该反应再循环到PLS 100。
图3示出了使用DBD放电的本发明的另一实施方案。图3的实施方案中的元件与图1和图2中具有相似的编号的元件具有相同的功能。在图3中,示出了使液体燃料204的流动流连续液化的PLS 300。
PLS 300包括等离子体反应器303,其在所示实施方案中可以是包括HV电极315和接地电极316的DBD反应器。在所示实施方案中的等离子体放电306是DBD等离子体放电,其在HV电极315和接地电极316之间产生。
PLS 300使用位于液体燃料入口317和气体入口318的气动喷嘴335。液体燃料304在气动喷嘴335中被雾化成微滴尺寸。特别地,微滴的直径的范围可以是10-30微米。微滴与甲烷混合并切向注入到等离子体反应器303中。在暴露于等离子体发生器305的等离子体放电306之后,经处理的液体燃料304的液滴收集在壁上,然后收集在等离子体反应器303的底部。未反应的气体可经由HV电极315中的通道从等离子体反应器303排出。应当理解的是,以与PLS 100中再循环未反应的甲烷或天然气的相同的方式,PLS 300中的甲烷或天然气也可以再循环回到等离子体反应器303。
图4中示出了本发明的另一个实施方案。图4的实施方案中的元件与图1-3中具有相似的编号的元件具有相同的功能。在图4中,示出了使用HV电极415和接地电极416的同轴布置的PLS 400。
在PLS 400中,在HV电极415和接地电极416的同轴结构内点燃介质阻挡放电。在PLS 400中,在等离子体放电406之后使用气动喷嘴435将液体燃料404经由液体燃料入口417注入。
气动喷嘴435雾化液体燃料404。在由短脉冲提供的强过电压和快速上升时间的情况下,可以产生低电场介电阻挡放电。具体而言,大气压下,所施加的电压脉冲优选少于约1000ns,更优选地少于约100ns,最优选地少于约10ns,上升时间少于优选100ns,更优选少于约10ns,最优选少于1ns。施加的电压脉冲越短,上升时间越快,越好。当电极之间存在1cm的间隙时,施加的电压脉冲的振幅应大于30kV,并且当电极之间存在约2-3mm的间隙时,施加电压脉冲的振幅应大于10kV。施加电压脉冲的振幅优选基于电极之间的间隙进行调整。
气体入口418位于等离子体反应器403的底部。这里,等离子体活化的甲烷在等离子体放电406之后立即与液体燃料404混合,从而使甲烷并入液体燃料404中。这使得等离子体放电406能够被稳定可控地点燃,并使甲烷有效活化。
图5中示出了本发明的另一实施方案。图5的实施方案中的元件与图1-4中具有相似的编号的元件具有相同的功能。在图5中,PLS500同样采用HV电极515和接地电极516的同轴布置。
类似于PLS 400,在PLS 500中,液体燃料504通过使用气动喷嘴535经由液体燃料入口517被注入到通过等离子体放电506进行甲烷活化的位置的下游。气动喷嘴535使液体燃料504雾化。气体入口518位于等离子体反应器503的底部。然而,在PLS 500中,电晕放电506被用于将甲烷活化和并入到液体燃料504中。在这种情况下,HV电极515由多个针状电极519组成,其有助于电晕放电506的点燃。电晕放电506可以以稳定的直流模式或脉冲模式点燃。
在一个实施方案中,如图8所示,PLS500可以使用大气压辉光放电508用于气态烃510如天然气的液化。在该实施方案中,接地电极514和HV电极525浸没在液态烃504中。大气压辉光放电508在接地电极514和HV电极525的接近接地电极514的尖端516之间产生。接地电极514可以为例如如图8所示的棒状形式,HV电极525可以为如图8所示的管状电极。管状HV电极525可以用作用于将气态烃510引入至液体燃料504的入口。具体而言,气体入口518连接到管状HV电极525的内腔,以将气态烃510输送到产生大气压辉光放电508的位置处的液体燃料504中,以提高转换效率。
在另一个实施方案中,可以按如图9所示实施采用大气压辉光放电508的PLS 500。在该实施方案中,使用多个HV电极525以在液体燃料504中的多个位置处产生大气压辉光放电508。每个HV电极525也可实施为管状电极,其与气体入口518相连,从而将气态烃510经由HV电极525供给到等离子体放电产生的位置处的液体燃料504中。接地电极514可以实施为金属网。多个HV电极525可以为直立方向并且可以彼此平行。多个HV电极525中的每一个的尖端贴近电极514以产生大气压辉光放电508。
如图所示,图9的实施方案还包括气态烃再循环520以收集和再循环离开液体燃料504的未反应的气态烃510。未反应的气态烃510可以通过气体入口518和管状HV电极525再循环回到液体燃料504中。
在另一个实施方案中,如图10所示,PLS 500可以采用大体水平方向的多个HV电极525,以产生多个大气压辉光放电508,其中HV电极525也可以彼此平行。接地电极514再一次贴近HV电极525的尖端。在该实施方案中,HV电极525也是管状电极,并且连接到用于气态烃510的气体入口518。大气压辉光放电508在HV电极525的每个尖端516处产生。该实施方案还包括将未反应的气态烃再循环520,以收集离开液体燃料504的未反应的气态烃510,并将收集的未反应的气态烃510通过气体入口518和高压电极525再循环回到液体燃料504。
本发明的一个优点是,与现有技术方法相比,其需要显著更少的能量,因为本发明不会断裂气态烃中的化学键,而断裂化学键需要显著更多的能量。本发明中甲烷并入的理论能量消耗不应超过0.3eV/mol(7kcal/mole),其对应于每1m3并入的天然气的0.3kW-h的OPEX(运营支出)成本,或每桶产生的额外的液体燃料约30美元的成本。这比使用Fisher-Tropsch合成的常规天然气液化工艺的能量消耗低约四倍。在实践中,使用本发明的甲烷并入的能量消耗为0.3-0.5eV/mol,对应于产生的液体燃料约30-50美元/桶。相比之下,据估计,使用E/N比为约300-1000Td的电场的US 2011/0190565的方法的能量消耗约为10-20eV/mol。此外,据估计,进行US 2012/0297665(也使用非常高的减弱的电场)的方法的能量消耗在20-30eV/mol的水平。
本发明使用非热等离子体对气态烃(例如甲烷)进行振动激发,随后进行表面化学吸附并将其并入到液体燃料中的液态烃中。该方法激发气态烃并入液态烃的放热和热中性过程。如在等离子体动力学计算中证明的,该方法允许甲烷以约0.3eV/mol的能量消耗并入。最后应该提到的是,许多研究人员试图使用等离子体解离方法通过中间体如H2、CH自由基和其他活性物质将CH4转化成液态烃。这个方法经证明是非常耗能的,在工业应用中是经济上不可行的。
以商业规模运营本发明的资本成本为:OPEX为30美元/桶产生的液体燃料(约1美元/加仑)和CAPEX(资本性支出)为2,100美元/桶/天。假设设备寿命为20年(和约1000天维护),OPEX和CAPEX总和为30美元/桶(约1美元/加仑)。为了比较,基于Fischer-Tropsch合成的方法的OPEX为15美元/桶(0.5美元/加仑),CAPEX为100,000美元/桶/天。假设设备寿命为20年(和约1000天维护),OPEX和CAPEX总和为120美元/桶(约4美元/加仑)。因此,与基于Fischer-Tropsch合成的方法相比,本发明便宜约四倍。
本文描述的装置适于模块化、可扩展和便携化,因此能够运输到并用在那些难以到达的区域,例如海上钻井平台和环境敏感区域。这些装置能够将天然气转化成稳定的燃料,例如柴油、汽油、轻质合成油、煤油和其他烃燃料,这些燃料可以在普通燃料运输工具中经过道路、海道或铁路运输。
实施例
以下实施例是对本发明的方法和组合物的解释而非限制。对本领域技术人员而言显而易见的、在本领域中通常遇到的对各种条件和参数进行的其他合适的修改和适应也在本发明的范围内。
实施例1
在可行性研究中,将0.5L的甲醇使用滑动电弧等离子体发生器处理9分钟。将等离子体发生器的喷嘴浸没在甲醇中。等离子体功率为约200W。等离子体气体为具有10%的CH4的N2。气相色谱分析表明,在处理过程中,约25%的CH4消失了。同时,通过分光光度法进行的对液体甲醇的分析显示在液体中未经确认的(可能是液态烃)化合物的量增加(参见图6A和6B)。图6A示出了在使用N2+CH4混合物进行滑动电弧处理期间液体组成的变化,图6B是使用仅含N2的等离子体进行的对照处理。
实施例2
在该实施例中,使用等离子体来激发甲烷直接液化为30%甲基萘(芳族化合物)和70%十六烷(脂肪族化合物)的液体混合物。这两种化合物用作柴油中通常发现的烃类化合物的替代物。该实施例的目的是确定(i)等离子体激发的甲烷并入芳族化合物和脂族化合物的选择性,(ii)芳环饱和程度。
在天然气存在下,通过两种类型的放电即介质阻挡放电(DBD)和大气压辉光放电(APGD)来处理液体混合物。使用核磁共振光谱(NMR)分析经处理的液体混合物(具有并入的甲烷)。图11A-11B的NMR光谱显示了未处理的液体混合物与使用DBD处理的液体混合物的前后比较。图12A-12B的NMR光谱示出了未处理的液体混合物与使用APG放电处理的液体混合物的前后比较。
基于这些NMR光谱,在DBD和APGD处理之后,约90%的甲烷通过芳环的饱和被并入到芳族化合物中,仅约10%的甲烷通过脂族化合物的聚合作用被并入到脂族化合物中。约85-90%的芳环饱和是由甲基萘的第一个环的饱和引起的。约10-15%的甲基萘被转化为脂族化合物。因此,相对于脂族化合物,等离子体诱导的甲烷液化显示优先并入芳族化合物。这与如上所述的事实一致,即由于放热特性,芳环被甲烷饱和的过程是节能的过程,而脂族化合物的聚合需要大量的能量,因为它是吸热过程。
实施例3
液体甲基萘(C11H10)在CH4存在下分别用DBD和APGD放电处理1小时。通过傅里叶变换红外光谱(FTIR)分析经处理的液体的样品。绘制了等离子体处理前后的FTIR光谱之间的差异,以显示等离子体处理的效果。图13A显示APGD处理后的甲基萘的差异,图13B显示DBD处理后的甲基萘的差异。图13A-13B表明,作为两种等离子体处理的结果,甲基萘中的饱和度(以新的C-H键计)增加,苯环数量减少。
基于光谱分析,DBD和APGD处理均显著增加了饱和度并降低了甲基萘的芳香度。总体上,APGD和DBD等离子体处理1小时后的甲基萘减少总量分别为~1.7%和~2.6%。
实施例4
在该实施例中,在根据图8的等离子体***中通过APGD处理50g的低硫柴油。在该实施例中采用2.4kV的电压和0.62mA的电流。引入柴油的气体是约2.7L/min的CH4和0.27L/min的N2的两种气流的混合物。在处理期间使用气相色谱法以1分钟的间隔分析反应混合物的组成。结果如表1所示:
表1.反应混合物的各种组分的气相色谱分析(浓度)
基于恒定的N2流速根据体积重新计算的反应混合物的组成示于表2中。
表2.在柴油的APGD等离子体处理期间气体混合物体积(以L计)的变化
观察到,在APGD处理仅5分钟之后,甲烷的体积减少了约0.4L。这种甲烷体积的减少不能通过甲烷分解产生H2、C2H2和C2H6来解释,因为这些组分的检测量太低而不足以对甲烷减少的量进行解释。因此,甲烷减少是由于将甲烷并入液态柴油而引起的。
然而,应当理解,即使在前面的描述中已经阐述了本发明的许多特征和优点,以及本发明的结构和功能的细节,本发明仅是说明性的,并且可以在发明的原理下在表达所附权利要求书的措辞的广泛一般含义所表明的全部范围内对细节进行改变,特别是部件的形状、尺寸和布置方面的改变。
Claims (23)
1.将气态烃并入液态烃中的方法,其包括以下步骤:
将所述气态烃暴露于使用E/N比在10Td至30Td范围内的减弱的电场产生的非热等离子体,以提供活化的气态烃,其中E/N比是减弱的电场的量度,其中E是单位为V/cm的电场,N是中性粒子的浓度或数量密度;和
使所述活化的气态烃与所述液态烃接触以将所述气态烃并入到所述液态烃中。
2.根据权利要求1所述的方法,其中所述减弱的电场的E/N比在12Td至28Td的范围内。
3.根据权利要求1或2所述的方法,其中所述减弱的电场产生在0.2eV至2eV范围内的电子能量。
4.根据权利要求1所述的方法,其中所述减弱的电场通过选自高气体流动滑动电弧放电、微波放电、电晕放电、大气压辉光放电和介质阻挡放电的放电产生。
5.根据权利要求4所述的方法,其中所述放电是大气压辉光放电。
6.根据权利要求5所述的方法,其中使用1kV至5kV的电压产生所述大气压辉光放电。
7.根据权利要求5或6所述的方法,其中使用在0.2mA至10mA的范围内的电流产生所述大气压辉光放电。
8.根据权利要求5或6所述的方法,其中,使用频率在1kHz至500kHz的范围内的交流电产生所述大气压辉光放电。
9.根据权利要求1、2和4-6中任一项所述的方法,其中所述气态烃选自甲烷、乙烷、丙烷、正丁烷、异丁烷、叔丁烷及其组合。
10.根据权利要求1、2和4-6中任一项所述的方法,其中所述气态烃是天然气中的甲烷。
11.根据权利要求1、2和4-6中任一项所述的方法,其中所述液态烃选自具有C5-C28烃基的烃。
12.根据权利要求1、2和4-6中任一项所述的方法,其中所述液态烃选自C5-C20烷烃、烯烃、炔烃、它们的异构形式及其组合。
13.根据权利要求1、2和4-6中任一项所述的方法,其中所述液态烃是液体燃料的组分,所述液体燃料选自原油、汽油、煤油、石脑油、柴油、瓦斯油、加热油、残余油和其他由原油制得的石油产品。
14.根据权利要求1、2和4-6中任一项所述的方法,其中所述液态烃是液体燃料的组分,所述液体燃料选自低级液体燃料和衍生自煤、页岩油、沥青砂和焦油砂的合成燃料。
15.根据权利要求1、2和4-6中任一项所述的方法,其中所述接触步骤包括将液体燃料减小为平均直径范围1微米至30微米的液滴,其中所述液态烃是所述液体燃料的组分。
16.根据权利要求15所述的方法,其中使用气动喷嘴或雾化器产生所述液滴。
17.根据权利要求1、2和4-6中任一项所述的方法,其中在所述接触步骤中,所述气态烃与所述液态烃之间的摩尔比在1:20至1:2的范围内。
18.根据权利要求1、2和4-6中任一项所述的方法,其中在所述接触步骤期间存在催化剂。
19.根据权利要求18所述的方法,其中所述催化剂是含过渡金属的化合物。
20.根据权利要求19所述的方法,其中所述过渡金属选自周期表的第V、VI和VIII族元素。
21.根据权利要求18所述的方法,其中所述催化剂是金属环烷酸盐、硫酸乙酯或多价金属阴离子的铵盐。
22.根据权利要求18所述的方法,其中所述催化剂为微丸、颗粒、线、网筛、多孔板、棒和条带的形式。
23.根据权利要求1所述的方法,其中将未反应的气态烃再循环回到所述暴露步骤。
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US20180171249A1 (en) | 2018-06-21 |
US10308885B2 (en) | 2019-06-04 |
EA037733B1 (ru) | 2021-05-14 |
ZA201703865B (en) | 2019-07-31 |
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JP2018506597A (ja) | 2018-03-08 |
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