CN1467014A - 使用复合吸附剂的气流纯化 - Google Patents
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Abstract
描述了空气、合成气或天然气的进料气流中至少水分和二氧化碳的去除工艺,包含下列步骤:使该进料气流接触一种包含硅石和金属氧化物的复合吸附剂,其中该复合吸附剂含有至少50wt%硅石,形成一种第一纯化气流,和使该复合吸附剂在0~200℃的温度再生。该工艺任选地进一步包含使该第一纯化气流接触一种二氧化碳吸附剂和/或一种氧化亚氮或烃吸附剂。
Description
技术领域
本发明涉及一种进料气流中至少水分和二氧化碳的去除工艺。
背景技术
空气的低温纯化需要一个预纯化步骤来脱除高沸点和危险的物质。主要高沸点空气成分包括水和二氧化碳。如果环境空气中这些杂质的脱除没有达到,则水和二氧化碳将在该分离装置的冷段(例如热交换器和液氧泵)中凝固出来,引起压力降低以及流动和操作问题。各种危险物质包括乙炔及其它烃类也需要脱除。高沸点烃类是一个问题,因为它们浓缩在该分离装置的液氧段,导致一种潜在***危险。目前空气的预纯化是用吸附法实现的。吸附***包括温度转换吸附(见US-A-4541851和US-A-5137548)和压力转换吸附(见US-A-5232474)***。这些***通常是为完全脱除环境空气中的水分和二氧化碳而设计的。对水分和二氧化碳选择性的吸附剂是这些***所需要的。
温度转换吸附工艺典型地使用一种层叠式床思路,其中,进料空气首先接触一种水选择性吸附剂例如氧化铝或硅胶。然后,干燥、含二氧化碳的空气接触一种沸石吸附剂,使二氧化碳去除到非常低水平。
已经有很多出版物涉及改善的二氧化碳选择性吸附剂。US-A-4249915公开了13X(NaX)或5A沸石。US-A-3885927公开了含有至少90%钡离子的X沸石可用于脱除含有不多于1000ppm二氧化碳的气流中的二氧化碳。US-A-5531808公开了硅/铝比不大于1.15的X沸石可用于气流中低水平二氧化碳的去除。
反之,只有少数出版物涉及改善的干燥剂材料。最近的一份专利(US 6,379,430)公开了含有少量硅石和金属氧化物的活性氧化铝用于空气中水分和二氧化碳同时去除的用途。US-A-5779767公开了复合氧化铝/沸石吸附剂用于低温蒸馏前空气中水分和二氧化碳脱除的用途。
总而言之,关于生产氧气或氮气的低温蒸馏之前空气预纯化吸附***,有很多专利公开。这些***需要干燥剂来去除进料空气流中的环境水分。先有技术上公开的干燥剂包括氧化铝、硅胶和沸石。
发明内容
本发明涉及空气、合成气或天然气的进料气流中至少水分和二氧化碳的去除工艺,包含下列步骤:
使该进料气流接触一种包含硅石和金属氧化物的复合吸附剂,其中该复合吸附剂含有至少50wt%硅石,形成一种第一纯化气流,和
使该复合吸附剂在0~200℃的温度再生。
这里使用的“复合”系指颗粒状材料,其中,每个颗粒都在该颗粒内部各分立部分含有硅石和金属氧化物。该硅石和金属氧化物并非在显著程度上化学结合的。
较好,该复合吸附剂含有0.1~10wt%金属氧化物。较好,该金属氧化物包含铝、铁、锌、钒和钛中至少一种的氧化物。更好,该金属氧化物是氧化铝。
较好,该工艺进一步包含以下步骤:
使第一纯化气流接触一种包含氧化铝、浸渍氧化铝、A沸石、或X沸石中一种或多种的二氧化碳吸附剂,形成一种第二纯化气流。更好,该工艺进一步包含该二氧化碳吸附剂的再生步骤。该工艺可进一步包含以下步骤:
使该第二纯化气流接触一种包含CaX、NaX、和BaX沸石中一种或多种的氧化亚氮或烃吸附剂,形成一种第三纯化气流。
在这种情况下,本发明较好进一步包含该氧化亚氮或烃吸附剂的再生步骤。该氧化亚氮或烃吸附剂可以是与该二氧化碳吸附剂相同的材料。
较好,该进料气流处于0~50℃的温度。
较好,该进料气流处于2~20大气压的绝对压力。
较好,该复合吸附剂是在0.1~20大气压的绝对压力再生的。
较好,由氧、氮、甲烷、氢、氩或者其中两种或更多种的混合物组成的再生气体,在再生期间从该复合吸附剂上通过。
附图说明
图1显示本发明的一个较好实施方案中使用的装置的示意图。
图2显示高表面积硅胶、氧化铝/硅石复合物、低表面积硅胶和氧化铝在25℃吸附的水对相对湿度的作图(水等温线)。
图3显示氧化铝和氧化铝/硅石复合物的水穿透时间对床接触时间的作图。
具体实施方式
空气预纯化的很多工艺方案使用低再生温度(例如US-A-5614000)。使用这些低再生温度是为了降低装置动力消耗。在使用低再生温度的情况下,我们已经认识到该干燥剂的再生能力对于使吸附床规模最小化以减少装置基本费用来说是重要的。
通常用来脱除空气中水分的干燥剂是沸石、氧化铝和硅胶。沸石吸附水分非常强烈,其吸附热为大约18kcal/mole(75kJ/mole),因此,需要高再生能量,因而,沸石只能用于高温TSA工艺,其中,再生热脉冲彻底惯穿该吸附床。氧化铝有大约14kcal/mole(59kJ/mole)的较低水吸附热,而且也脱除二氧化碳。然而,氧化铝在吸附循环期间蒙受不可逆水热老化。这个主要是氧化铝向氢氧化铝转化的结果的老化过程减少了该氧化铝的表面积并降低了其水容量。硅胶有大约12kcal/mole(50kJ/mole)的低水吸附热。然而,达到高水容量所需要的高表面积硅胶当暴露于液体水时就破裂开。在吸附性干燥过程期间对液体水的暴露总是可能的,因此,高表面积硅胶无法用于空气预纯化过程。
因此,目前仍然需要更适用于进料气流的、有再生能力的干燥剂。本发明提供这样一种干燥剂。
在本发明的一个较好实施方案中,该复合吸附剂是Engelhard公司的Sorbead WS。适用的氧化铝/硅石复合物可以用以下所述任意一种工艺制造。
在第一种工艺中,将硅酸钠或活性硅酸凝胶、铝酸钠和氢氧化钠混合,生成一种硅铝酸钠,后者在85~200℃的温度、在大气压或水热条件下均化和结晶,形成一种P型沸石。该沸石洗涤并遭遇到一种酸处理以除去钠成分,从而赋予该沸石以无定形。该酸处理可以使用一种较好呈水溶液的无机酸或有机酸例如盐酸、硫酸、硝酸或磷酸进行。为了执行酸处理,形成该P型沸石的一种水浆状物并向该浆状物中加酸。该酸处理较好在20~100℃的温度进行,该浆状物中沸石颗粒的浓度较好是5~30wt%。该酸处理可以分一个阶段或者两个或更多个阶段进行,任选地由一个干燥或焙烧和热处理阶段分隔开。
所得到的氧化铝/硅石颗粒用水洗涤、干燥和焙烧,得到一种最终产品。
在第二种工艺中,一种醇(例如乙醇)、水、一种烷氧化硅(例如四乙氧化硅)和一种酸(例如盐酸)在能防止二氧化硅凝胶化或沉淀的条件下混合。添加一种铝化合物的酸性溶液、添加一种凝胶化剂、回收一种凝胶并用水和一种有机液体洗涤、然后使该凝胶干燥直至得到一种粉末,并焙烧该粉末。这种工艺的一个实例见US-A-5849852
实施例3。
这种复合吸附剂可以替而代之地包含除氧化铝外的金属氧化物,例如氧化铁。
如同图1中所示,要纯化的空气从进气口12供给一个主空气压缩机***10,其中,在用水通过热交换冷却之间和之后用一台多级压缩机使之压缩。任选地,压缩的空气进料在冷却器8中进行亚冷却。冷却的压缩空气供给一个含有进气控制阀16和18的进气多支管14,该多支管上连接一对含有容器20和22的吸附剂床。该多支管在控制阀16和18下游跨接一个含有排气阀26和28的排气多支管24,这些排气阀用来关闭和打开各吸附剂容器20和22的上游端经由消音器32与排气口30之间的连接。这两个吸附剂床20和22中每一个都含有两种吸附剂。各该吸附剂床的下部分别用数字34、34′表示,上部分别用数字36、36′表示。34、34′部含有用以上所述工艺制造的、吸附水和二氧化碳的第一复合吸附剂,而36、36′部含有吸附二氧化碳的第二吸附剂(例如沸石)。
在一种替代实施方案中,每个吸附剂床都可以含有三种独立的吸附剂-吸附氧化亚氮或烃类的第三吸附剂。吸附剂可以是分层排列的,例如,吸附剂可以是径向层叠的。应当理解的是,容器20和22,如果希望,每个都可以分隔成串联排列的较小容器,而且以上吸附剂“层”的提法包括各独立吸附剂置于串联式排列的各独立容器中的配置。
该装置有一个出气口38经由一个含有出气控制阀42、44的出气多支管40连接到这两个吸附剂容器20、22的下游端。该出气口连接到一个空气分离单元(ASU)上。该出气多支管40跨接一个含有再生气控制阀48和50的再生气多支管46。在再生气多支管46的上游,也有一条含有控制阀54的管线跨接在出气多支管40上。
在56处提供一个再生气出口,它是经由控制阀58连接的,以通过加热器62连接到再生气多支管46上。这些阀门的操作可以用业内已知的适用可编程定时和阀门开启手段(图上未显示)控制。
在操作上,空气是在主压缩机***10中压缩并进料到进气多支管14,然后通过两个含有吸附剂的容器之一。从空气通过开启的阀门16到达吸附剂容器20、和通过开启的阀门42到达出气品38和空气分离单元的态势开始,进气多支管上的阀门18将正好已经关闭,从而切断容器22的纯化用空气进料。阀门44也正好已经关闭。在这一阶段,阀门46、50、54、26和28全都关闭。因此,床20是在线的,而床22是要再生的。
为了开始床22的降压,使阀门28开启,一旦容器22中的压力下降到所希望的水平,就让阀门28保持开启同时使阀门50开启以开始再生气体的流动。该再生气体将典型地是一种从所示装置中纯化的空气送达的、可能含有少量氩气、氧气及其它气体的空气分离单元低温箱得到的、干燥、无二氧化碳的氮气流、阀门58是开启的,使得该再生气体在通入容器22之前能加热到例如100℃的温度。出口吹扫气体来自处于冷却状态的排气口30。
在所分配的再生期结束时,可以将阀门58关闭以结束再生气体的流动,而且可以将阀门54开启,以置换来自吸附剂的氮气,并在阀门28关闭之后用纯化空气使容器22再加压。然后,可以使阀门54关闭、而且可以使阀门18和44开启,以使容器22回到工艺线上。然后,可以以类似方式使容器20再生,而且在阶段操作周期中继续执行整套顺序:使该容器在线、降压、再生、再加压、和回到工艺线上。
要知道的是,尽管本发明已经参照较好实施方案加以描述,但其很多变异和改良在本发明范围内是可能的。
实施例
实施例1
对活性氧化铝(Alcan AA-300TM,320m2/g)、高表面积硅胶(Davison Bead GelTM,750m2/g,99.6%硅石)、氧化铝/硅胶复合物(Engelhard Sorbead WSTM,650m2/g,3%氧化铝/97%硅石)和低表面硅肢(Davison Grade 55TM,300m2/g,99.6%硅石),测定了水吸附等温线。这些水等温线显示于图2中。
图2中的结果指出,高表面(HSA)硅胶显示出所试验材料中最高的水容量。然而,当HSA硅肢置于液体水中时它会破裂开。氧化铝/硅石复合吸附剂有稍低的水容量,但它在液体水中是稳定的。因此,氧化铝/硅石复合吸附剂兼备TSA和PSA干燥器所要求的高水容量和对液体水的所需稳定性。低表面积硅胶对液体水是稳定的,但它有非常低的水容量。
实施例2
对实施例1中使用的活性氧化铝和氧化铝/硅石复合物样品测定了水穿透曲线。这些穿透曲线是在25℃用水饱和空气进行的。进料压力是135psig(9.31kPa),流量率是55lbmoles/hr/ft2(2.7×105moles/hr/m2),吸附剂的粒度平均为3.6mm,塔是6英尺(1.8m)长和1英寸(2.5cm)直径。水穿透是用一种露点探针确定的,用-45℃的出口露点来定义水穿透。穿透试验的结果显示于图3中。
图3显示在不同的总床吸附剂接触时间上让水穿透-45℃露点需要多长时间。对于相对穿透时间为4的脱水床来说,图3显示氧化铝接触时间是3.9秒。对于氧化铝/硅胶复合物来说,接触时间是2.2秒。由于在相同进料条件(温度、压力和流量率)下测试了这两种吸附剂,因而,接触时间与床体积直接相关。因此,这些结果显示,与氧化铝相比,用氧化铝/硅胶复合物脱水可以使用少44%的床体积。
实施例3
进行了PSA实验,以比较碱处理氧化铝(如US-A-5656064中所述)与氧化铝/硅胶复合物(20vol%)随后碱氧化铝(80vol%)的层叠床的性能。该PSA是在25℃用水饱和空气、进料流量率为30lbmoles/hr/ft2(1.5×105moles/hr/m2)、进料压力为30psig(2.1kPa)、吹扫气/空气摩尔比为0.55进行的。吹扫是用氮气、以8psig(0.55kPa)和25℃进行的,所使用的设备如实施例2中所述。PSA试验的结果列于表1中。
表1
吸附剂 | 脱水用相对床体积 | 脱二氧化碳用相对床体积 | 复合氧化铝/硅石层中脱除的水% |
碱处理氧化铝 | 1.0 | 1.0 | N/A |
氧化铝/硅石复合物和碱处理氧化铝 | 0.43 | 0.62 | 99% |
表1中的结果显示,使用氧化铝/硅石复合物作为PSA中的干燥剂,对脱水和脱二氧化碳来说,都减少了所需要的床体积。在PSA入口处使用氧化铝/硅石复合物,使脱水所需床体积减少57%。在PSA进料端该复合物的使用,也使脱二氧化碳用总床体积减少38%。这清楚地显示氧化铝/硅石复合物干燥剂改善环境空气中至少水分和二氧化碳的脱除用的PSA干燥器和预纯化PSA两者的性能的效用。
实施例4
表2中列出纯硅胶(99.6%硅石)、活性氧化铝和氧化铝/硅石复合物的抗碎强度。所测试材料的平均粒度是3.6mm。
表2
吸附剂 | 堆积密度(lb/ft3) | 抗碎强度(lb) |
硅石 | 47(750kg/m2) | 3.6(1.6kg) |
氧化铝(3%)/硅石(97%) | 44(710kg/m2) | 34.3(15.5kg) |
氧化铝 | 54(860kg/m2) | 35.3(16.0kg) |
表2中的数据显示,三种干燥剂全都有非常类似的堆积密度。然而,硅石有比其它两种吸附剂低得多的抗碎强度。十分令人意外的是,氧化铝/硅石复合物有与氧化铝相同的抗碎强度,尽管有两倍表面积(650m2/g比320m2/g)。
实施例5
商品干燥剂的另一种重要性质是水热稳定性。在长时期内,水和水蒸汽会通过使氧化物转化成氢氧化物而有效地使干燥剂老化。这种缓慢化学转化导致该干燥剂表面积的损失和水吸附容量的损失。希望的是拥有一种对水热老化的敏感性尽可能小的干燥剂。
为了测试一些干燥剂的水热稳定性,将这些材料以不同水蒸汽压力蒸16小时,然后在30℃测定水吸附等温线,并与新鲜材料的水等温线比较、蒸水蒸汽实验的结果列于表3中。
表3
吸附剂 | 进货时在23%RH的水容量 | 在23%RH、1.7bar水蒸汽时的水容量 | 在23%RH、3.0bar水蒸汽时的水容量 |
硅石 | 11.0wt% | 5.9wt% | 5.6wt% |
氧化铝/硅石 | 7.9wt% | 7.4wt% | 7.0wt% |
氧化铝 | 8.8wt% | 5.8wt% | 5.4wt% |
表3中的结果显示,在23%RH时,氧化铝和硅石都有比氧化铝/硅石复合物更高的水容量。然而,在这些材料以1.7bar水蒸汽蒸16小时之后,氧化铝/硅石复合物只损失其水容量的6%。事实上,在以1.7bar水蒸汽蒸之后,氧化铝/硅石复合物有在23%RH测试的干燥剂中最高的水容量。在以3.0bar水蒸汽蒸之后,看到了同样的趋势。这清楚地显示氧化铝/硅石复合物有比氧化铝和硅石改善的水热稳定性。
实施例6
用温度转换吸附工艺测试了氧化铝/硅石复合物的效用。这种两床工艺是用6英寸直径(15cm)×6英尺(1.8m)长的容器进行的。在35℃用水饱和的、有400ppm二氧化碳的进料空气以7.3bar和135Nm3/hr空气流量进行处理。再生温度是65℃,吹扫气/空气摩尔比是0.45。在一个试验中,这些TSA容器在该床的进料端含有75vol%像US-A-5656064中那样的浸渍氧化铝,并在产品端含有25vol%13X沸石。在第二个试验中,该床进行重新构型,以便从进料到出口依次包括25vol%氧化铝/硅石复合物、50vol%同上的浸渍氧化铝和25vol%13X沸石。试验结果显示,有本发明氧化铝/硅石复合物的床构型,对于与无该复合物的床构型相同的容器体积来说,多加工20%进行空气。
实施例7
对于氧化铝、硅石和氧化铝/硅石复合物,在25℃、7.8bar、用含有400ppm二氧化碳的进料空气,测定了二氧化碳穿透曲线。穿透试验的结果列于表4中。
表4
吸附剂 | 二氧化碳容量(mmole/g) |
氧化铝 | 0.11 |
氧化硅 | 0.004 |
氧化铝/氧化硅 | 0.013 |
表4中的结果显示,与硅石或氧化铝/硅石复合物相比,氧化铝有显著较高的二氧化碳容量。这就是为什么氧化铝典型地是当同时要求脱水和脱二氧化碳时使用的较好干燥剂。给出了上述结果,令人惊讶的是,在同时要求脱水和脱二氧化碳的工艺中,像氧化铝/硅石复合物这样的干燥剂可以表现得比纯氧化铝出色。氧化铝/硅石复合物优于纯硅石的另一个优点是该复合材料有大约3倍的二氧化碳容量。
Claims (13)
1.空气、合成气或天然气的进料气流中至少水分和二氧化碳的去除工艺,包含下列步骤:
使该进料气流接触一种包含硅石和金属氧化物的复合吸附剂,其中该复合吸附剂含有至少50wt%硅石,形成一种第一纯化气流,和
使该复合吸附剂在0~200℃的温度再生。
2.按照权利要求1的工艺,其中,该复合吸附剂含有0.1~10wt%金属氧化物。
3.按照权利要求1的工艺,其中,该金属氧化物包含铝、铁、锌、钒和钛中至少一种的氧化物。
4.按照权利要求3的工艺,其中,该金属氧化物是氧化铝。
5.按照权利要求1的工艺,进一步包含以下步骤:
使第一纯化气流接触一种包含氧化铝、浸渍氧化铝、A沸石、或X沸石中一种或多种的二氧化碳吸附剂,形成一种第二纯化气流。
6.按照权利要求5的工艺,进一步包含该二氧化碳吸附剂的再生步骤。
7.按照权利要求5的工艺,进一步包含以下步骤:
使第二纯化气流接触一种包含CaX、NaX和BaX沸石中一种或多种的氧化亚氮或烃吸附剂,形成一种第三纯化气流。
8.按照权利要求7的工艺,进一步包含该氧化亚氮或烃吸附剂的再生步骤。
9.按照权利要求8的工艺,其中,该氧化亚氮或烃吸附剂是与二氧化碳吸附剂相同的材料。
10.按照权利要求1的工艺,其中,该进料气流处于0~50℃的温度。
11.按照权利要求1的工艺,其中,该进料气流处于2~20大气压的绝对压力。
12.按照权利要求1的工艺,其中,该复合吸附剂是在0.1~20大气压的绝对压力再生的。
13.按照权利要求1的工艺,其中,让一种由氧气、氮气、甲烷、氢气、氩气或者其中两种或更多种的混合物组成的再生气体在再生期间从该复合吸附剂上通过。
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CN102626579A (zh) * | 2012-04-13 | 2012-08-08 | 苏州市兴鲁空分设备科技发展有限公司 | 多组分吸附装置及工艺 |
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CN104140085A (zh) * | 2014-07-28 | 2014-11-12 | 中昊光明化工研究设计院有限公司 | 一种深度脱除氧化亚氮中水和二氧化碳的装置与方法 |
CN104140085B (zh) * | 2014-07-28 | 2016-06-22 | 中昊光明化工研究设计院有限公司 | 一种深度脱除氧化亚氮中水和二氧化碳的装置与方法 |
CN110662594A (zh) * | 2017-05-24 | 2020-01-07 | 巴斯夫公司 | 采用吸附剂/干燥剂混合床进行的气体脱水 |
CN110090616A (zh) * | 2018-01-30 | 2019-08-06 | 北京航天试验技术研究所 | 一种低温液体吸附除水材料的制备 |
CN108273359A (zh) * | 2018-01-31 | 2018-07-13 | 天津大学 | 一种低温沼气纯化装置 |
Also Published As
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US20040045434A1 (en) | 2004-03-11 |
EP1366794A1 (en) | 2003-12-03 |
JP2004000975A (ja) | 2004-01-08 |
US20030221555A1 (en) | 2003-12-04 |
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