CN104411806A - 用于提高从气体混合物除去硫化氢的包含哌嗪水性烷醇胺吸收剂组合物及其使用方法 - Google Patents
用于提高从气体混合物除去硫化氢的包含哌嗪水性烷醇胺吸收剂组合物及其使用方法 Download PDFInfo
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Abstract
本发明涉及从含硫化氢的气体混合物中除去硫化氢的烷醇胺水溶液。所述烷醇胺水溶液包括(i)下式的氨基化合物:R1R2NCH2CH(OH)CH2OH,其中R1和R2独立地表示1至3个碳原子的低级烷基,(ii)哌嗪,和(iii)任选的物理溶剂,其中所述溶液不含强酸。此外,本发明涉及从含有硫化氢和附加的其他酸性气体(如果存在)例如二氧化碳的气体混合物中除去硫化氢的方法,所述方法包括使所述含硫化氢的气体混合物与烷醇胺水溶液接触的步骤,优选其中所述烷醇胺水溶液的温度等于或高于140°F。所述气体混合物的例子包括天然气、合成气、尾气和炼厂气。
Description
技术领域
本发明涉及包含哌嗪和烷醇胺、优选3-(二甲基氨基)-1,2-丙二醇的水溶液的组合物,和利用所述水性组合物从含H2S的气体混合物除去包括H2S的酸性气体的方法。
背景技术
源自于天然气藏、石油或煤炭的流体流经常含有作为杂质的大量酸性气体,例如二氧化碳(CO2)、硫化氢(H2S)、二氧化硫(SO2)、二硫化碳(CS2)、氰化氢(HCN)、硫化羰(COS)或硫醇。所述流体流可以是气体、液体或其混合物,例如诸如天然气、炼厂气、来自页岩热分解的烃气、合成气等气体或诸如液化石油气(LPG)和液化天然气(NGL)的液体。
用于除去酸性气体的各种组合物和方法是已知的并在文献中进行了描述。用胺水溶液处理气体混合物以除去这些酸性气体是公知的。通常,所述胺水溶液在吸收塔中在低温或高压下逆流接触包含所述酸性气体的气体混合物。所述胺水溶液通常含有烷醇胺例如三乙醇胺(TEA)、甲基二乙醇胺(MDEA)、二乙醇胺(DEA)、单乙醇胺(MEA)、二异丙醇胺(DIPA)、或2-(2-氨基乙氧基)乙醇(有时称为二甘醇胺或DGA)。在一些情况下,促进剂与所述烷醇胺组合使用,例如USP4,336,233、4,997,630和6,337,059中公开的哌嗪和MDEA,所述所有文献以其全文通过引用并入本文中。或者,EP 0134948公开了酸与选择的碱性材料例如MDEA混合,以提供提高的酸性气体去除。
叔胺类,例如3-二甲基氨基-1,2-丙二醇(DMAPD),已经显示出对于从气体混合物除去CO2有效,参见USP 5,736,116。此外,在具体的方法、例如Girbotol方法中,叔胺类已经显示对于除去H2S有效,但是显示在升高的温度下能力降低,例如参见“Organic Amines-GirbotolProcess”,Bottoms,R.R.,The Science of Petroleum,第3卷,OxfordUniversity Press,1938年,第1810-1815页。
虽然上述化合物是有效的,但它们各具有有损于它们普遍应用的局限性。特别地,具有包含从气体混合物除去包括H2S的酸性气体的烷醇胺的水性组合物、和/或当在升高的温度、例如超过140°F下使用时,以商业上可行的能力有效除去酸性气体的烷醇胺水溶液,将是理想的。
因此,对于从气体混合物有效除去包括硫化氢的酸性气体、优选在升高的工作温度下除去所述酸性气体的水性吸收剂组合物和使用所述组合物的方法,存在着需要。
发明内容
本发明是烷醇胺水溶液组合物和利用所述烷醇胺水溶液组合物通过与包含硫化氢的气体混合物接触而除去包括硫化氢的酸性气体的方法,优选其中所述烷醇胺水溶液的温度等于或高于140°F,所述组合物包含(i)氨基化合物,优选量从0.1至75重量%,具有以下通式:
R1R2NCH2CH(OH)CH2OH (1)
其中R1和R2独立地表示1至3个碳原子的低级烷基,例如甲基、乙基、丙基和异丙基,更优选R1和R2基团包括甲基和乙基,特别优选的氨基化合物包括其中R1和R2二者都是甲基的3-(二甲基氨基)-1,2-丙二醇、和其中R1和R2二者都是乙基的3-(二乙基氨基)-1,2-丙二醇;(ii)哌嗪,优选以0.1至15重量%的量;和(iii)任选的物理溶剂,优选选自环四亚甲基砜、聚乙二醇的二甲醚、1,3-二甲基-3,4,5,6-四氢-2(1H)嘧啶酮、N-甲酰基吗啉、N-乙酰基吗啉、三乙二醇单甲醚、或其混合物,其中重量百分比基于所述烷醇胺水溶液的总重量,其中所述烷醇胺水溶液不含pKa为8或更低的酸或能够在水介质中形成pKa为8或更低的酸的酸形成材料。
在本发明的一种实施方式中,所述氨基化合物(i)优选是3-(二甲基氨基)-1,2-丙二醇或3-(二乙基氨基)-1,2-丙二醇。
在本发明的一种实施方式中,所述方法还包括汽提所述烷醇胺水溶液的步骤,使得形成贫酸性气体的烷醇胺水溶液,其可以用于所述接触步骤。
附图说明
图1示出了本发明的吸收方法的工艺流程图。
图2是净化气体混合物中的H2S浓度随吸收剂循环速率变化的曲线。
具体实施方式
本发明的烷醇胺水溶液包含氨基化合物和哌嗪。可用于本发明的烷醇胺水溶液的氨基化合物具有以下通式:
R1R2NCH2CH(OH)CH2OH (1)
其中R1和R2独立地表示1至3个碳原子的低级烷基,例如甲基、乙基、丙基和异丙基。更优选R1和R2基团包括甲基和乙基。特别优选的氨基化合物包括其中R1和R2二者都是甲基的3-(二甲基氨基)-1,2-丙二醇、和其中R1和R2二者都是乙基的3-(二乙基氨基)-1,2-丙二醇。
本发明的烷醇胺水溶液含有的烷醇胺的量等于或大于0.1重量%,优选等于或大于5重量%,更优选等于或大于10重量%并且甚至更优选等于或大于20重量%,其中重量%是基于所述溶液的总重量。本发明的烷醇胺水溶液含有的烷醇胺的量等于或小于75重量%,优选等于或小于65重量%,更优选等于或小于55重量%并且甚至更优选等于或小于50重量%,其中重量%是基于所述溶液的总重量。
本发明的烷醇胺水溶液含有的哌嗪的量等于或大于0.1重量%,优选等于或大于1重量%,更优选等于或大于2重量%,其中重量%是基于所述水溶液的总重量。本发明的烷醇胺水溶液含有的哌嗪的量等于或小于20重量%,优选等于或小于15重量%,更优选等于或小于10重量%,并且甚至更优选等于或小于8重量%,其中重量%是基于所述溶液的总重量。
本发明的水性吸收剂组合物可以任选含有一种或多种其他氨基化合物。优选地,所述其他氨基化合物是上文中式(1)未描述的不同的烷醇胺或第二烷醇胺,例如三(2-羟乙基)胺(三乙醇胺,TEA);三(2-羟丙基)胺(三异丙醇);三丁醇胺;双(2-羟乙基)甲胺(甲基二乙醇胺,MDEA);2-二乙基氨基乙醇(二乙基乙醇胺,DEEA);2-二甲基氨基乙醇(二甲基乙醇胺,DMEA);3-二甲基氨基-1-丙醇;3-二乙基氨基-1-丙醇;2-二异丙基氨基乙醇(DIEA);N,N-双(2-羟基丙基)甲胺(甲基二异丙醇胺,MDIPA);N,N’-双(2-羟乙基)哌嗪(二羟乙基哌嗪,DiHEP);二乙醇胺(DEA);2-(叔丁基氨基)乙醇;2-(叔丁基氨基乙氧基)乙醇;或2-氨基-2-甲基丙醇(AMP),2-(2-氨基-乙氧基)乙醇。
优选的其他氨基化合物包含一个或多个叔氨基。
优选所述其他氨基化合物具有一个或多个位阻氨基。包含1-羟乙基-4-吡啶基哌嗪化合物和具有一个或多个位阻氨基的胺的水性吸收组合物尤其适合于除去H2S。
如果存在,则所述烷醇胺水溶液中任选的氨基化合物的量可以等于或大于0.1重量%,优选等于或大于1重量%,更优选等于或大于5重量%,其基于所述溶液的总重量。如果存在,则所述烷醇胺水溶液中任选的氨基化合物的量可以等于或小于75重量%,优选等于或小于50重量%,更优选等于或小于25重量%,其基于所述溶液的总重量。
与待处理气体发生接触的所述烷醇胺水溶液的温度等于或高于120°F,优选等于或高于130°F,更优选等于或高于140°F,并且甚至更优选等于或高于150°F。
除了所述氨基化合物和哌嗪之外,所述烷醇胺水溶液还可以包含根据公知的实践用于流体处理的一种或多种其他化合物。可以任选提供的说明性化合物包括但是不限于,下列一种或多种:消泡剂;物理溶剂,包括二醇以及单-和二-醚或其酯、脂族酸酰胺、N-烷基化吡咯烷酮、砜、亚砜等;抗氧化剂;腐蚀抑制剂;成膜剂;螯合剂例如金属;pH调节剂例如碱化合物;等等。这些任选组分的量不关键,但是可以根据已知的实践以有效量提供。
除了所述氨基化合物、哌嗪和一种或多种用于流体处理的任选的其他化合物之外,所述烷醇胺水溶液还可以包含物理溶剂。优选溶剂例如环四亚甲基砜(可以商品名SULFOLANE得到)、聚乙二醇的二甲醚(可从The Dow Chemical Company以商品名SELEXOL得到)、和三乙二醇单甲醚(TGME或METHOXYTRIGLYCOL,可得自The DowChemical Company)、1,3-二甲基-3,4,5,6-四氢-2(1H)-嘧啶酮、N-甲酰基吗啉、N-乙酰基吗啉、或其混合物。
如果存在,则所述烷醇胺水溶液中物理溶剂的量可以等于或大于1重量%,优选等于或大于5重量%,更优选等于或大于10重量%的量存在,其基于所述溶液的总重量。如果存在,则所述烷醇胺水溶液中物理溶剂的量可以等于或小于75重量%,优选等于或小于65重量%,更优选等于或小于50重量%的量存在,其基于所述溶液的总重量。
本发明的烷醇胺水溶液不含酸或酸形成材料,优选排除的酸或酸形成材料是特征为强酸的那些,其包括pKa为8或更低、优选7或更低、更优选6或更低的任何有机或无机酸。被排除的酸的例子包括磷酸、亚磷酸、盐酸、硫酸、亚硫酸、亚硝酸、焦磷酸、亚碲酸(telurous acid)等等。有机酸例如乙酸、甲酸、己二酸、苯甲酸、正丁酸、氯乙酸、柠檬酸、戊二酸、乳酸、丙二酸、草酸、邻苯二甲酸、琥珀酸、邻甲苯酸等也从本发明的烷醇胺水溶液中排除。另外,在本发明的烷醇胺水溶液中不能存在能够与水接触时形成酸的酸形成材料。
本文中阐述的本发明在石化和能源工业中具有重大的应用。例如,本发明可用于在炼油厂中处理流体流、气体、液体或混合物,处理酸气,处理煤层气体,处理有害的烟囱排放物,处理填埋场气体(land field gas),和一系列新的处理对于人类安全有害的排放物的装置。
待由本发明的方法处理的流体流包含酸性气体混合物,所述混合物包含H2S、并可以包含其它气体例如CO2、N2、CH4、C2H6、C3H8、H2、CO、H2O、COS、HCN、NH3、O2、硫醇等等。通常,这些气体混合物存在于燃烧气、炼厂气、城市煤气、天然气、合成气、尾气、水煤气、丙烷、丙烯、重质烃类气体等中。当所述流体流是例如从页岩油干馏气、煤炭或用空气/蒸汽气化重油或将重质渣油氧气/蒸汽热转化为较低分子量液体和气体、或在制硫装置尾气清理操作中而得到的气体混合物时,本文中的烷醇胺水溶液特别有效。
本发明的方法优选用于从包含H2S和CO2的气体流中,任选在一种或多种其他酸性气体杂质例如N2、CH4、C2H6、C3H8、H2、CO、H2O、COS、HCN、NH3、O2、和/或硫醇存在下,除去H2S和CO2。此外,本发明可以用于从包含H2S、CO2以及SO2、CS2、HCN、COS、和/或硫醇中的一种或多种的气体流中除去H2S、CO2以及N2、CH4、C2H6、C3H8、H2、CO、H2O、COS、HCN、NH3、O2、和/或硫醇中的一种或多种。
本发明的吸收步骤通常包括在任何合适的接触容器中用所述烷醇胺水溶液接触所述流体流,优选气体混合物,例如代表性的吸收方法参见USP 5,736,115和6,337,059,其二者都以它们的全文通过引用并入本文中。在这样的方法中,待从中除去酸性气体的含有H2S和/或其它杂质的流体流可以利用常规手段,例如填充了例如环或具有筛板的塔或容器、或鼓泡反应器,与所述烷醇胺水溶液发生密切接触。
在实施本发明的一个典型方式中,通过将所述流体流进给到吸收塔的下部,同时新鲜的烷醇胺水溶液进给到所述塔的上部区域来进行所述吸收步骤。除去大部分H2S和CO2(如果存在)的流体流从所述塔的上部排出(有时称为处理或净化气体),而所装载的含有吸收的H2S和CO2的烷醇胺水溶液在底部或底部附近离开所述塔。优选地,在所述吸收步骤期间所述吸收剂组合物的进口温度在120°F至210°F的范围内,更优选从140°F至200°F。压力可以大幅变化;所述吸收塔中可接受的压力在5和2,000磅/平方英寸(psi)之间,优选20至1,500psi,并最优选25至1,000psi。所述接触在使得H2S优选被所述溶液吸收的条件下发生。设计吸收条件和设备,从而最小化所述烷醇胺水溶液在所述吸收塔中的停留时间以减少CO2吸收,而同时保持所述流体流与所述水性吸收剂组合物足够的停留时间以吸收最大量的H2S气体。具有低分压的流体流,例如在热转化过程中遇到的那些流体流,与具有较高分压的流体流例如页岩油干馏气相比,在相同的吸收条件下将需要较少的所述烷醇胺水溶液。
所述方法的H2S去除阶段的典型程序包括在含有多个塔盘的塔中,在至少120°F的温度下,和至少0.3英尺/秒(ft/sec,基于“活性”或通气塔盘表面)的气体速度下,通过含有H2S和CO2的气体混合物与所述氨基化合物的烷醇胺水溶液逆流接触来吸收H2S,根据气体的运行压力,所述盘式塔具有少于20个的接触塔盘,例如通常使用4至16个塔盘。
所述流体流与所述烷醇胺水溶液接触之后,所述水溶液被H2S饱和或部分饱和,所述溶液可以至少部分再生,使得其可以再循环回到所述吸收塔。正如吸收那样,所述再生可以在单一液相中进行。通过加热、膨胀、用惰性流体汽提或其组合的常规手段,可以实现所述烷醇胺水溶液的再生或酸性气的脱附,例如将所述溶液减压或将温度提高到闪蒸出所吸收的H2S的温度点,或通过将所述溶液在与吸收步骤中所用的构造相似的容器的上部通入所述容器,并使惰性气体例如空气或氮气或者优选蒸汽向上通过所述容器。再生步骤期间所述溶液的温度应该在120°F至210℃的范围内,并优选从140°F至200°F,以及所述溶液在再生时的压力范围应该从0.5psi至100psi,优选1psi至50psi。所述烷醇胺水溶液在清除至少一部分H2S气体之后,可以再循环回到所述吸收容器中。补充吸收剂可以按需添加。
在一种优选的再生技术中,富含H2S的烷醇胺水溶液被送往所述再生器,其中吸收的组分通过使所述溶液沸腾而产生的蒸汽进行汽提。闪蒸罐和汽提器中的压力通常为1psi至50psi,优选15psi至约30psi,并且温度通常在120°F至340°F的范围内,优选170°F至250°F。当然,汽提器温度和闪蒸温度将取决于汽提器压力;因此脱附期间,在15psi至30psi汽提器压力下,温度将是170°F至250°F。待再生的溶液的加热可以很适合地通过用低压蒸汽间接加热的方式而实现。然而使用蒸汽的直接注入也是可以的。所生成的贫硫化氢的烷醇胺水溶液可以用于接触含H2S的气体混合物。
优选所述清洁的气体含有等于或小于10ppm的H2S,满足一些环境法规,更优选等于或小于4ppm的H2S,满足通常的管道规格。
本发明的优选实施方式包括连续地、或作为连续过程执行本发明的方法。然而,所述方法可以分批地或半连续地进行。所用的方法类型的选择应该通过条件、使用的设备、气体流的类型和量、以及根据本文中的公开内容对本领域普通技术人员显而易见的其它因素来确定。
实施例
实施例1至9是包含烷醇胺、去离子水和任选的第二胺的胺吸收剂水溶液,量基于所述吸收剂组合物的总重量以重量份计。包含含有4.2%H2S、16%CO2和79.8%N2的合成混合物的气体流在中试规模吸收塔中处理以除去H2S和CO2,其中百分比是体积百分比。对于每种胺吸收剂水溶液,所述气体流以三种不同的流率处理。实施例1至9的组成、工艺参数以及残余H2S和CO2水平在表1中列出。在表1中:
“DGA”是98%的2-(2-氨基乙氧基)乙醇,可得自Acros Organics;
“MDEA”是98%的甲基二乙醇胺,可得自The Dow ChemicalCompany;以及
“DMAPD”是98%的3-二甲基氨基-1,2-丙二醇,可得自AKscientific;
“哌嗪”是99%的哌嗪,可得自Aldrich Chemical。
胺吸收剂水溶液经由进料管线5被引入中试规模吸收塔图1的气-液逆流填充床吸收柱2的上部。所述气体流通过进料管线1以10升/分钟的气体流率引入柱2的下部。吸收塔压力调节到238psia。净化的气体(即H2S和CO2的量减少)在吸收柱2的顶部通过管线3排出,并且残余H2S和CO2水平通过气相色谱(GC)分析测定。负载有H2S和CO2的胺水溶液流向所述吸收塔的下部,并通过管线4离开。
管线4中的胺水溶液通过液位控制阀8降低压力并通过管线7流到换热器9,所述换热器加热所述负载的水溶液。所述热的富溶液通过管线10进入再生器12的上部。再生器12配备有实施所述H2S和CO2气体脱附的散堆填料。所述再生器的压力设定在17psia。所述气体通过管线13进入冷凝器14,其中任何残留的水和胺发生冷却和冷凝。所述气体进入分离器15,其中冷凝的液体与蒸气相分离。冷凝的水溶液经由泵22通过管线16泵送到再生器12的上部。冷凝剩余的气体通过管线17除去供最终的收集和/或处置。再生的水溶液向下流过再生器12和紧密连接的再沸器18。配备电加热装置的再沸器18蒸发所述水溶液的一部分以除去任何残余气体。蒸气从所述再沸器产生并返回到再生器12,其与下降的液体混合,然后通过管线13离开以进入所述方法的冷凝阶段。再沸器18的再生水溶液通过管线19离开并在换热器20中冷却,然后经由泵21泵回,通过进料管线5进入吸收柱2。
所述胺吸收剂水溶液的流率通过缓慢向下调节直到纯化气体管线3中H2S的量显示急剧增加来确定。
实施例1至9的结果图示在图2显示的曲线中。H2S水平(以体积百万分率(ppmv)计),相对于胺流率(立方厘米/分钟(cc/min))作图。
表1
实施例 | 1* | 2* | 3* | 4 | 5 | 6 | 7 | 8 | 9 |
吸收剂组成 | |||||||||
DGA | 50 | 50 | 50 | ||||||
DMAPD | 41.3 | 41.3 | 41.3 | ||||||
MDEA | 41.3 | 41.3 | 41.3 | ||||||
哌嗪 | 8.75 | 8.75 | 8.75 | 8.75 | 8.75 | 8.75 | |||
水 | 50 | 50 | 50 | 50 | 50 | 50 | 50 | 50 | 50 |
吸收剂流率,cc/min | 36 | 28.4 | 30 | 26.7 | 23.7 | 25 | 32.5 | 29.9 | 24.8 |
出口气体GC分析 | |||||||||
CO2,ppmv | 150 | 590 | 112 | 31 | 350 | 45 | 40 | 35 | 6000 |
H2S,ppmv | 0.2 | 470 | 16 | 2.5 | 21 | 2.5 | 5 | 2 | 316 |
贫溶液温度,°F | 152 | 152 | 152 | 152 | 152 | 152 | 152 | 152 | 152 |
进口气体温度,°F | 128 | 128 | 128 | 128 | 128 | 128 | 128 | 128 | 128 |
*不是本发明的实施例
Claims (8)
1.用于从含硫化氢的气体混合物中除去包括硫化氢的酸性气体的烷醇胺水溶液,所述溶液包含
(i)下式的氨基化合物:
R1R2NCH2CH(OH)CH2OH (1)
其中R1和R2独立地表示甲基、乙基、丙基或异丙基,
和
(ii)哌嗪,
其中所述烷醇胺水溶液不含pKa为8或更低的酸或能够在水性介质中形成pKa为8或更低的酸的酸形成材料。
2.权利要求1的烷醇胺水溶液,其中
(i)所述氨基化合物的存在量从0.1至75重量%,
和
(ii)所述哌嗪的存在量从0.1至15重量%,
其中重量百分比基于所述烷醇胺水溶液的总重量。
3.权利要求1的烷醇胺水溶液,其中所述氨基化合物(i)是3-(二甲基氨基)-1,2-丙二醇或3-(二乙基氨基)-1,2-丙二醇。
4.权利要求1的烷醇胺水溶液,其还包含
(iii)物理溶剂。
5.权利要求4的烷醇胺水溶液,其中所述物理溶剂(iii)选自环四亚甲基砜、聚乙二醇的二甲醚、1,3-二甲基-3,4,5,6-四氢-2(1H)嘧啶酮、N-甲酰基吗啉、N-乙酰基吗啉、三乙二醇单甲醚、或其混合物。
6.从气体混合物除去酸性气体的方法,所述方法包括使所述气体混合物与权利要求1至3任一项的所述烷醇胺水溶液接触的步骤。
7.权利要求6的方法,其还包括汽提所述烷醇胺水溶液的步骤,使得形成可用于所述接触步骤的贫酸性气体的烷醇胺水溶液。
8.权利要求6的方法,其中所述烷醇胺水溶液的温度等于或高于140°F。
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