CN1195571A - Psa预纯化器 - Google Patents
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Abstract
本发明包括一种用于除去进料气流中存在的杂质的PSA气体预纯化器。本发明的预纯化器有一吸附材料床,包括至少两种不同的吸附剂层,至少一种所述吸附剂相对较强,至少另一种所述吸附剂相对较弱。
Description
本发明一般地涉及变压吸附(PSA)空气分离方法和系统。具体地，涉及PSA空气预纯化。
深冷空气分离设备的操作需要大量预处理过的空气。为防止设备的冷进料端冻结，杂质如CO2和H2O的浓度必须低于1ppm。此外，在深冷液体中溶解度低的那些烃如乙炔和某些C3-C8烃的浓度必须保持非常低，典型地低于1ppb，以消除任何安全性危险。目前在空气预纯化应用中使用变温吸附(TSA)和变压吸附(PSA)。
TSA预纯化器使用相当少量的热吹扫气再生吸附床。典型的吹扫气与进料之比≤10％。它们在从空气进料中除去主要杂质如CO2、H2O和大多数烃方面极有效。进料中所含任何CO和H2一般被带入产品中。如果必须除去CO和H2，则通过催化转化相继进行CO和H2的氧化。由于在解吸期间在TSA预纯化器中可获得大量热驱动力，所以使用强吸附剂如5A或13X沸石。使用这些吸附剂，操作负载和主要杂质的选择性使CO2在乙炔和对深冷空气分离设备的操作有害的其它烃(如C3至C8)之前穿透至产品物流中。
为增加这些吸附剂的能力，通常使进料气冷却。虽然TSA方法有相对低的吹扫气与进料之比，但必须加热吹扫气和冷却进料，均导致设备的投资和操作成本增加。
PSA预纯化器用环境温度的吹扫气再生吸附床。典型的吹扫气与进料之比为40-60％。由于在解吸期间的驱动力较低，所以使用较弱的吸附剂如活性氧化铝。
虽然这些吸附剂的操作负荷比沸石的低，但它们仍是很高的。此外，我们发现使用活性氧化铝时，C2H2在CO2之前穿透至产品物流中。这导致用该预纯化器的产品作为进料的深冷空气分离工艺的操作条件很危险。此外，虽然PSA预纯化器的投资成本低于TSA，但总的能量需求可能较高。特别地，PSA循环在吸附床减压期间泄料需要耗能。这与TSA循环相比是很显著的，因为TSA法每3至6小时循环一次，相反PSA法每15-30分钟循环一次。
基于以上考虑，该领域需要设计一种PSA吸附剂床，其有利于活性氧化铝解吸的特性，还有与吸附较强的沸石相伴的乙炔选择性和负荷。此外，需要使泄料损失最小以降低操作功率。已提出几种可选方案。
Hitachi在DE3045451中公开了一种两床吸附剂系统。第一吸附剂是用于吸附高浓度H2O和CO2的13X，从而抑制氮气的共吸附。第二吸附剂是不很强地共吸附氮气的活性氧化铝，用于完成H2O和CO2的吸附。通过使床中的氮气共吸附最少，也使减压期间的泄料损失最小。
Kumar在US4711645中描述了一种PSA预纯化器，用活性氧化铝吸附H2O和用13X吸附CO2。用活性氧化铝吸附H2O导致进料中的温升比整个床均使用13X的低。这增加了13X区吸附CO2的效能。Kumar建议用于第二区的其它沸石是5A、CaA、CaX和Na-丝光沸石。
Jain在US5232474中也使用活性氧化铝层，然后是13X层。其权利要求书中用活性氧化铝层吸附所有的H2O和大部分CO2。下游13X层的用途是从气流中除去烃和残余的CO2。特别地教导该13X层不用于除去大量CO2。该PSA循环设计用含有较小直径吸附剂球的吸附床操作且没有常规的均压步骤。
鉴于以上情况，本发明的目的之一是提供一种改进的预纯化方法和系统。
本发明的另一目的是提供一种适应性强的PSA预纯化方法和系统，与现有的系统相比可更有效地除去杂质。
本发明的另一目的是提供一种比现有系统需要的能量少的PSA预纯化方法和系统。
本发明的另一目的是提供一种可安全地在本文所述条件下操作的PSA预纯化方法和系统。
本发明包括一种用于除去进料气流中存在的水和其它杂质的PSA气体预纯化器。本发明的预纯化器有一吸附材料床，包括至少两种不同的吸附剂层，对于所述水和其它杂质的吸附而言，至少一种所述吸附剂相对较强，至少另一种所述吸附剂相对较弱。
在优选的实施方案中，相对较强的吸附剂是NaY，相对较弱的吸附剂是活性氧化铝。
由以下优选实施方案的描述和附图，本领域技术人员将想到其它目的、特征和优点，其中：
图1是本发明实施方案的示意图。
本文所述PSA预纯化器的吸附剂床提供增强的性能(例如吸附步骤的时间较长和泄料损失较小)，导致更有效地除去杂质。此外，由于本发明的系统和方法中CO2在C2H2之前穿透吸附床进入产品物流中，因此提供更安全的操作条件。最后，我们的试验表明该方法可适用于宽范围的操作条件(包括吸附压力和进料温度)。本发明可以下面所述的方式进行。
本发明的要素是使用两种分开的有不同性能的吸附剂层，从而获得比所述两种吸附剂之任一分别实现的分离更好和成本更低的性能。基于较强吸附剂的该方法热效应被缓和，从而改善该吸附剂的吸附和解吸性能，使该循环自清洗所需吹扫气量减少。我们应注意术语“自清洗”在本领域一般理解为意指循环期间吸附质被充分吹扫以致它们的平均残余负荷如滞留在吸附剂上的吸附质量不随时间增加的状况。
一般认为NaY与吸附剂如13X、5A、CaA、CaX和Na-丝光沸石相比是弱吸附剂。例如，其对N2、O2和CO2的吸附能力是13X的一半。这意味着NaY将比这些较强吸附剂的泄料损失低，需要较少的吹扫。
然而，与活性氧化铝相比，NaY是强吸附剂。我们的等温穿透试验表明NaY对乙炔的平衡能力为活性氧化铝的约10倍。此外，在PSA预纯化器的进料中的浓度下NaY将优先吸附乙炔优于CO2。这些浓度典型地低于1ppm。
可惜，这些试验也表明为使乙炔有效解吸NaY比活性氧化铝需要更多的吹扫气。在泄料(blowdown)期间发生温度变化的绝热床中增加的吹扫需求甚至更大。
基于上述特性，本发明包括在床内不同层或区中使用相对较强的吸附剂(优选NaY)和相对较弱的吸附剂(优选活性氧化铝颗粒)。在优选实施方案中，所述较强的吸附剂位于床的较热产品端。这通过减少进料步骤期间氮气的共吸附和降低解吸所需吹扫气量缓和PSA方法的热效应。此外，在含有20％NaY的层中，该层状床的穿透能力将大于纯活性氧化铝层的两倍。所有这些特征都对PSA预纯化循环的操作成本有有益影响。
此外，相对较强的吸附剂对所述乙炔或C3-C8烃至少之一而言是自清洗的，比13X所需吹扫气少。
上述实施方案示于图1中。在该图所示的床中，活性氧化铝层用于除去进料气流中的大部分H2O和CO2，较小的NaY层用于除去进料中残余的杂质。流体流动方向由箭头指示。
图1示出本发明的PSA预纯化器的吸附剂床。在图1中，下端板(header)填充惰性陶瓷球7，起流动分布和床支承的作用。不锈钢筛网8支承吸附剂床。该床本身由两层组成。较大的下层是活性氧化铝9；较小的上层是NaY10。上床表面由第二不锈钢筛网11限制，筛网11靠填充上端板的另一层陶瓷球12固定就位。可使端板空间内的陶瓷球12渐次变化以提供改善的分布。
在本发明的操作中，选择合适的吸附剂用于床的产品端是本发明的关键。所选吸附剂必须强吸附乙炔和其它烃，它必须对烃有优于CO2的选择性，以致CO2总是在这些对操作有害的烃(如乙炔)之前穿透该床。此外，在工艺操作条件下它应不是N2或O2的强共吸附剂。如果有，在减压期间不排除冷却，因为吸附产生热量。这将导致解吸步骤期间吸附质更强地保留在吸附剂上，从而需要较多的吹扫气。
在用活性氧化铝除去大部分CO2和H2O的PSA预纯化器的热(产品)端使用适当尺寸的NaY层，显著改善了该循环的经济性。也增加了乙炔在床中的停留时间，确保CO2前沿先穿透。
本发明中，床中所用NaY的量是经济问题。最佳循环将部分取决于相对的能量成本、要除去的烃量、和所用空气分离设备的操作效率。
NaY与活性氧化铝的优选比例在10％NaY/90％活性氧化铝和90％NaY/10％活性氧化铝之间。
更优选的比例在10％NaY/90％活性氧化铝和50％NaY/50％活性氧化铝之间。最优选的比例在10％NaY/90％活性氧化铝和30％NaY/70％活性氧化铝之间。上述比例适用于第一层中活性氧化铝的量与第二层中NaY的量之比。
我们应注意到较强的吸附剂可通过本领域公知的方法重建，产生有NaY性能的吸附剂。这些方法可包括但不限于改变SiO2/Al2O3之比、晶体含量、粘合剂的百分率和残余H2O含量。例如，13X和5A可按上述方法改性产生氮气的共吸附减少和对较强吸附的吸附质(如C2H2、CO2)有充足容量的吸附剂。
当使用NaY作为较强吸附剂时，使用前必须彻底干燥并保持干燥。优选地，NaY上的水负荷应等于或小于4wt％，更优选小于2wt％，最优选小于0.8wt％。在本发明的操作中，可装载活性氧化铝，然后现场干燥。
床中的颗粒分布必须均匀以确保接触所有杂质。要确保适当的性能床中均匀的流动分布和压力特征是必要的。使用颗粒加料器(通常指US5,324,159中所述的)使容器的均匀加料相对简单。控制分布臂的旋转速度将能调节填充密度。
作为实例，设计一种两床PSA空气预纯化器以供应CO2≤0.25ppm、H2O≤0-1ppm和C2H2≤1ppb的产品，有图1中所示构造，该预纯化器将在以下参数下操作，且有以下特征：
进料条件：
进料流＝7,500至16,000SCFH/FT2含有0.33ppm C2H2的空气
温度＝50至120°F
压力＝100至140PSIA
吸附时间＝7至35分钟
再生条件：
吹扫气/进料之比＝40至60％
压力＝大气压
温度＝环境(床)
吹扫时间＝在吸附时间的约1至1.5倍之间。
吸附剂：
LaRouche A-201(7×12球)活性氧化铝
UOP NaY(1/16″挤出物)
床(具体实例)
总床深度＝6.25ft.
活性氧化铝层＝5.00ft.
NaY层＝1.25ft.
优选地，本发明的PSA预纯化器在以下条件下操作；进料温度为约40-120°F、进料压力约30-240psia和再生压力约大气压。操作温度超过100°F和吹扫气与进料之比等于或大于50％时，使用NaY的本发明的性能最优。
本发明的方法不限于图中所提出的单床结构。用于变压吸附循环的有效吸附剂床和这些循环的操作的设计由本领域公知的方法实现。例如，本发明可用一或多个异相操作的床实施。其它实施方案(尽管不优选)包括NaY层可放在床中任何位置的一种实施方案(其中H2O浓度足够低以使C2H2优于CO2选择吸附)，及整个床均为NaY的实施方案。如前所述，NaY最好在床的较热的、较干的产品端。
本发明提供几个优于已知PSA预纯化器的优点。第一，本发明可完全除去空气中的C2H2至低于1ppb。这确保相联的空气分离设备安全操作。
此外，本发明达到CO2吸附前沿的穿透始终在C2H2穿透之前。这提供了相对简单的确保工艺安全的方法，因为预纯化器的进料步骤通常在CO2吸附前沿的穿透开始之前终止。
进一步地，层状PSA床的总操作成本低于单纯氧化铝吸附剂床的操作成本。这大部分是由于吸附步骤的时间较长，因而泄料损失较少。
最后，该系统不需要附加的系统硬件，可在现有容器中完成。
本发明的具体特征示于一或多个附图中仅为方便，因为每个特征都可与本发明的其它特征相结合。本领域技术人员将认识到可选的实施方案，均包括在权利要求的范围内。
Claims (11)
1.一种变压吸附气体纯化器，用于在高吸附压力下吸附进料气流中存在的杂质和在低解吸压力下解吸所述杂质，所述纯化器包括：
一吸附容器，包含能在高吸附压力下选择吸附所述进料气流中存在的所述杂质和在低解吸压力下解吸所述杂质的吸附材料床，所述吸附容器有用于加入所述进料气流的进料端和用于从中回收纯化的进料气的产品端，其中所述吸附材料床包括至少两层吸附剂，对于所述杂质的吸附而言，至少一种所述吸附剂相对较强，至少另一种所述吸附剂相对较弱，其中所述相对较强的吸附剂优先吸附乙炔或C3-C8烃至少之一优于CO2，和其中所述相对较强的吸附剂对所述乙炔或C3-C8烃而言是自清洗的，比13X吸附剂所需吹扫气少。
2.权利要求1的预纯化器，其中所述相对较强的吸附剂是NaY。
3.权利要求1的预纯化器，其中所述相对较弱的吸附剂是活性氧化铝。
4.权利要求1的预纯化器，其中所述相对较弱的吸附剂是活性氧化铝和所述相对较强的吸附剂是NaY，和其中NaY与活性氧化铝之比在10％/90％和90％/10％之间。
5.权利要求1的预纯化器，其中所述相对较弱的吸附剂是活性氧化铝和所述相对较强的吸附剂是NaY，和其中NaY与活性氧化铝之比在10％/90％和50％/50％之间。
6.权利要求1的预纯化器，其中所述相对较弱的吸附剂是活性氧化铝和所述相对较强的吸附剂是NaY，和其中NaY与活性氧化铝之比在10％/90％和30/70％之间。
7.权利要求1的预纯化器，其中所述进料气是空气。
8.权利要求1的预纯化器，其中所述杂质是水、乙炔、CO2和C3-C8烃至少之一。
9.权利要求1的预纯化器，其中所述相对较弱的吸附剂层在所述床的所述进料端和所述相对较强吸附剂层之间。
10.权利要求1的预纯化器，其中所述相对较强的吸附剂选自13X、5A、CaA、CaX或Na-丝光沸石，其中所述吸附剂已由其原形改性。
11.一种纯化气流的方法，所述方法包括使所述气流通过含有能在高吸附压力下选择吸附所述进料气流中存在的所述杂质和在低解吸压力下解吸所述杂质的吸附材料床的变压吸附容器，所述吸附容器包含能在高吸附压力下选择吸附所述进料气流中存在的所述杂质和在低解吸压力下解吸所述杂质的吸附材料床，所述吸附容器有用于加入所述进料气流的进料端和用于从中回收纯化的进料气的产品端，其中所述吸附材料床包括至少两层吸附剂，对于所述杂质的吸附而言，至少一种所述吸附剂相对较强，至少另一种所述吸附剂相对较弱，其中所述相对较强的吸附剂优先吸附乙炔或C3-C8烃至少之一优于CO2，和其中所述相对较强的吸附剂对所述乙炔或C3-C8烃而言是自清洗的，比13X吸附剂所需吹扫气少。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US08/766,443 US5769928A (en) | 1996-12-12 | 1996-12-12 | PSA gas purifier and purification process |
| US766,443 | 1996-12-12 |
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| Publication Number | Publication Date |
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| CN1195571A true CN1195571A (zh) | 1998-10-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN97120839A Pending CN1195571A (zh) | 1996-12-12 | 1997-12-09 | Psa预纯化器 |
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| Country | Link |
|---|---|
| US (1) | US5769928A (zh) |
| EP (1) | EP0847792B1 (zh) |
| KR (1) | KR100322957B1 (zh) |
| CN (1) | CN1195571A (zh) |
| BR (1) | BR9706248A (zh) |
| CA (1) | CA2224471C (zh) |
| DE (1) | DE69729364T2 (zh) |
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| EP4045173A1 (en) | 2019-10-16 | 2022-08-24 | Exxonmobil Upstream Research Company (EMHC-N1-4A-607) | Dehydration processes utilizing cationic zeolite rho |
| CN112142017A (zh) * | 2020-09-30 | 2020-12-29 | 西南石油大学 | 一种基于变压吸附分离技术的氮气制备装置 |
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- 1997-12-09 CA CA002224471A patent/CA2224471C/en not_active Expired - Fee Related
- 1997-12-09 EP EP97121682A patent/EP0847792B1/en not_active Expired - Lifetime
- 1997-12-09 CN CN97120839A patent/CN1195571A/zh active Pending
- 1997-12-09 BR BR9706248A patent/BR9706248A/pt unknown
- 1997-12-09 KR KR1019970066874A patent/KR100322957B1/ko not_active Expired - Fee Related
- 1997-12-09 DE DE69729364T patent/DE69729364T2/de not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100400142C (zh) * | 2005-10-01 | 2008-07-09 | 四川天一科技股份有限公司 | 干气回收c2及c2以上烃类组分的方法 |
| CN104822435A (zh) * | 2012-09-10 | 2015-08-05 | 恩特格林斯公司 | 防止层状净化床装置中微粒与粉尘游移的设备 |
| CN104084123A (zh) * | 2014-07-25 | 2014-10-08 | 株洲高新技术产业开发区壹星科技有限公司 | 吸附式空气干燥机用吸附材料及组合吸附方法 |
| CN109381965A (zh) * | 2017-08-10 | 2019-02-26 | 气体产品与化学公司 | 快速循环变压吸附方法和用于其中的吸附层压板 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP0847792A2 (en) | 1998-06-17 |
| EP0847792A3 (en) | 1998-07-08 |
| KR19980063917A (ko) | 1998-10-07 |
| DE69729364D1 (de) | 2004-07-08 |
| CA2224471C (en) | 2000-10-10 |
| KR100322957B1 (ko) | 2002-03-08 |
| US5769928A (en) | 1998-06-23 |
| BR9706248A (pt) | 1999-08-10 |
| ID19141A (id) | 1998-06-18 |
| EP0847792B1 (en) | 2004-06-02 |
| DE69729364T2 (de) | 2005-06-30 |
| CA2224471A1 (en) | 1998-06-12 |
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