CN1123753C - 生产超高纯氮和超高纯氧的低温精馏系统 - Google Patents
生产超高纯氮和超高纯氧的低温精馏系统 Download PDFInfo
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Abstract
本发明涉及一种通过进料空气的低温精馏生产超高纯氮和超高纯氧的方法,其中进料空气分为第一进料空气和第二进料空气,该方法包括:在主塔中低温精馏第一进料空气,分离成主塔富氧流和主塔富氮流;在辅塔中低温精馏第二进料空气,分离成辅塔富氧流和辅塔富氧流;使辅塔富氮流进入主塔;使主塔或辅塔富氧流进入汽提塔;在其下部产生超高纯氧流;使部分汽提塔超高纯氧流与主塔富氧流间接热交换,蒸发成上流蒸汽;将另一部分汽提塔超高纯氧流回收;将主塔富氮流回收。本发明还涉及用于上述方法的装置。其可在高回收率下同时生产超高纯氮和超高纯氧。
Description
本发明一般涉及进料空气的低温精馏以生产氮和氧,更具体地,本发明涉及如电子工业所需要的超高纯产品。
在对杂质非常敏感的制造工艺中,如生产半导体和其他的电子器件,需要超高纯氮,尤其是高压的。通过进料空气的低温精馏可有效地进行超高纯氮的生产。近来在所述制造工艺中,除了超高纯氮以外,还出现了使用超高纯氧化的要求。超高纯氧可以使用生产超高纯氮的惯用低温精馏装置进行生产,但是这样的系统与供产任何指定数量氮的常规超高纯氮的装置相比,降低了超高纯氮的回收从而导致能源消耗的增加。
由此,本发明的目的在于提供一种低温精馏系统,该系统在使用至今已知系统的经验减小氮回收和能源消耗损失的同时,还能生产超高纯氮和超高纯氧。
本发明可以达到上述和其他目的,这些对所属技术领域的技术人员来说,在阅读本说明书的公开之后将是明显的,本发明的一个方面是:
一种通过进料空气的低温精馏生产超高纯氮和超高纯氧的方法,其中进料空气分为第一进料空气和第二进料空气,该方法包括:
(A)第一进料空气进入主塔并且该第一进料空气在该主塔内通过低温精馏分离成主塔富氧流体和主塔富氮流体;
(B)第二进料空气进入辅塔并且该第二进料空气在该辅塔内通过低温精馏分离成辅塔富氮流体和辅富氧流体;
(C)辅塔富氮流体从辅塔流入主塔的上部;
(D)主塔富氧流体或辅塔富氧流体进入汽提塔上部再迎着上充蒸汽向下流过汽提塔以便在该汽提塔的下部产生超高纯氧流体;
(E)在上述汽提塔内通过与主塔富氧流体的间接热交换蒸发一部分超高纯氧流体以产生所述上流蒸汽;
(F)回收作为产品超高纯氧的另一部分来自上述汽提塔的超高纯氧流体;和
(G)回收作为产品超高纯氮的主塔富氮流体。
本发明的另一方面是:
通过进料空气的低温精馏生产超高纯氮和超高纯氧的设备,包括:
(A)具有顶部冷凝器的主塔和进料空气进入塔用的装置;
(B)具有顶部冷凝器的辅塔和进料空气进入辅塔用的装置;
(C)具有塔底再沸器的汽提塔;
(D)用于流体从主塔下部进入主塔顶部冷凝器和从主塔顶部冷凝器进入汽提塔塔底再沸器的装置;
(E)用于流体从辅塔的上部进入辅塔顶部冷凝器和从辅塔顶部冷凝器进入主塔上部的装置;
(F)用于流体从主塔或辅塔进入汽提塔上部的装置;和
(G)用于从汽提塔下部回收超高纯氧的装置,和用于从主塔的上部回收超高纯氮的装置。
当用于本发明是,术语“塔”指的是蒸馏或分馏塔或区,即接触塔或区,其中液相和气相通过在一系列重复放置的塔盘或装在塔内的塔板和/或填料元件如结构填料或无规填料上逆流接触以进行流体混合物的分离。为进一步讨论蒸馏塔,可参见化学工程师手册,第五版,R.H.佩里和C.H.奇尔顿编,麦格劳-希尔图书公司,纽约,第13章,连续蒸馏工艺过程(See the Chemical Engineer’s Handbook,fifthedition,edited by R.H.Perry and C.H.Chilton,McGraw-HillBook Company,New York,Section 13,The ContimuousDistillation Process)。
气液接触分离工艺过程取决于各成分蒸汽压的差别。高蒸汽压(或更易挥发或低沸点),成分倾向在气相中浓集而低蒸汽压(或不易挥发或高沸点)的成分倾向在液相中浓集。部分冷凝是一种分离过程,借此蒸汽混合物的冷却可用于浓集可挥发成分(一种或多种)于气相中和由此减少液相中的可挥发成分(一种或多种)。精馏,或连续蒸馏,是一种通过逆流处于是气液相时所获得的连续部分蒸发和冷凝结合起来的分离过程。气液相的逆流接触通常是绝热的并且包括积分(分级)或微分(连续)相间的接触。利用精馏原理分离混合物的分离过程装置常常被可互换地称作精馏塔、蒸馏塔或分馏塔。低温精馏是一种至少部分温度在150度或低于150度开氏温度(K)下进行的精馏过程。
当用于本发明中时,术语“间接热交换”意指使两股流体进行热交换但无任何物理接触或流体彼此之间的混合。
当用于本发明中时,术语“顶部冷凝器”意指能从塔的蒸汽产生塔的下流液体的热交换装置。
当用于本发明中时,术语“塔底再沸器”意指能从塔的液体产生塔的上流蒸汽的热交换装置。
当用于本发明中时,术语“涡轮膨胀”和“涡轮膨胀机”分别指高压气体流经涡轮机以降低气体的压力和温度并由此产生致冷效果的方法和设备。
当用于本发明中时,术语“上部”和“下部”意指塔中点以上和以下相应塔的部分。
当用于本发明中时,术语“汽提塔”意指相对于液体下流有足够的蒸汽上流的情况下操作的塔,以便能实现从液体中把可挥发性成分分离成为可挥发性成分逐渐向上富集的蒸汽。
当用于本发明中时,术语“超高纯氮”意指氮浓度至少为99.99摩尔%和氧浓度低于百万分之一(ppm),优选低于0.1ppm的流体。
当用于本发明中时,术语“超高纯氧”意指氧浓度至少为99.99摩尔%的流体。
图1是本发明低温精馏系统一个最佳实施方案的示意图。
图2是本发明低温精馏系统另一个最佳实施方案的示意图。
图3是本发明低温精馏系统又一个最佳实施方案的示意图。
附图中的数字就通用元件而言是相同的。
在实施本发明时,在低于主塔压力下操作的辅塔是与超高纯氧汽提塔公开操作的,因为汽提塔是通过来自主塔的流体再沸的。这一点能使辅塔在更低的压力下也能操作,因此改善了来自主塔,总的来说最终是来自本系统的氮回收。下文将参照附图对本发明作更详细地描述。
现见附图1,进料空气1被分成第一进料空气流2和第二进料空气流3。第一进料空气流2通过在一次热交换器4中与返回流体的间接热交换被冷却,所得到的冷却第一进料空气流5进入主塔的下部。第二进料空气流3通过流经压缩机7压缩,压缩过的第二进料空气流8通过部分经过一次热交换器4冷却。冷却压缩过的第二进料空气流9通过流经涡轮膨胀机10而涡轮膨胀,所得到的涡轮膨胀过的第二进料空气流11进入辅塔12的下部。
主塔6在95-180磅/英寸2绝对压力(psia)范围内的压力下运行。在主塔6内,第一进料空气通过低温精馏被分离成富氧流体和更富氮流体。富氧流体作为液体13从主塔6的下部排出再通过部分流经一次热交换器4被过冷。所得到的过冷富氧的液体14再流入主塔顶部冷凝器15的沸腾侧。更富氮流体作为气流16从主塔6的上部排出而其部分17进入顶部冷凝器15的冷凝侧,其中它通过与部分蒸发的富氧液体的间接热交换被冷凝。所得到的更富氮液体以流体18作为回流液进入主塔6的上部。所得到的富氧蒸汽,以流体19从主塔顶部冷凝器15排出且其部分20流入辅塔12的下部。
辅塔12在低于主塔6的压力下操作且压力范围为45-65psia。在辅塔12内进入该塔的进料通过低温精馏被分离成富氮流体和更富氧流体。更富氧流体作为液体21由辅塔12的下部排出并进入辅塔顶部冷凝器22的沸腾侧。富氧液体以流体23从顶部冷凝器15同样进入顶部冷凝器22的沸腾侧。作为在下面将进一步讨论的,取自超高纯汽提塔塔底再沸器的第三流体24,也进入顶部冷凝器22的沸腾侧。
富氮流体作为气流25从辅塔12的上部进入辅塔顶部冷凝器22的冷凝侧,它在其中通过与流入顶部冷凝器22沸腾侧的流体间接热交换被冷凝。所得到的富集氮液体作为流体26从顶部冷凝器22排出其部分27作为回流液返回辅塔12。富氮液体的第二部分28通过流经泵29用泵压高到较高的压力,所得到的加压富氮液体30作为附加回流液进入主塔6的上部。如需要,部分富集氮液体31可作为产品液氮回收。
把来自辅塔的富氮液体加至主塔6液体回流液的数量和质量,所以能在主塔内生产出高回收和超高纯度的更富氮流体。更富氮蒸汽16的部分32通过流经一次热交换器4加热再作为产品超高纯氮流体33回收。
部分更富氧流体以液流34从辅塔12的下部排出作为汽提塔的进料进入汽提塔35的上部,优选顶部。进入汽提塔35的进料不应当含有任何量大的杂质,即较氧挥发性低的成分,如甲烷、氪、氙,以避免这类大量杂质在超高纯氧产品42中出现。达到这一点可以通过从辅塔的中间部位排放进料,例如进料空气入口高度以上。汽提塔进料迎着上流蒸汽向下流过汽提塔35,工艺过程中汽提塔进料内较易挥发的成分,如氮和氩,由下流液体中出来进入上流蒸汽,最终在汽提塔35的下部产生超高纯氧流体,和从汽提塔35出来的废气流36。气流36与来自辅塔顶部冷凝器22的气流37合并形成废气流38,通过流经一次热交换器4加热后以气流39排出系统。
来自主塔顶部冷凝器15的富集氧蒸汽19的部分40进入汽提塔塔底再沸器41,它在那里通过与超高纯氧液体的间接热交换冷凝在汽提塔35的下部。部分超高纯氧液体蒸发在汽提塔35中形成前述上流蒸汽。如前所述所得到的冷凝富氧液体从塔底再沸器41以液流24流入顶部冷凝器22。剩余的超高纯氧流体部分作为产品超高纯氧从汽提塔35的下部回收,回收时可呈气态和/或液态。用图1所说明的本发明实施方案表明超高纯氧产品是作为液流42回收的。
图2和3说明本发明其他优选的实施方案。图2和3中的数字对于通用元件是相同的且对这些部分不再详细描述。
现看图2,进入汽提塔35的含氧进料取自主塔6的下部进料空气入口高度以上,而不像图1所说明的实施方案那样从辅塔12取用。在图2说明的实施方案中,富氧流体以液流50从主塔6的下部排出再作为汽提塔的进料进入汽提塔35的上部。
在图3说明的本发明实施方案中,富氧流体作为附加进料流体51从主塔6出来进入辅塔12,而来自辅塔的更富氧液体作为液流34,如同图1所说明的实施方案,由辅塔12出来作为汽提塔进料进入汽提塔35。
就实施本发明而言,可在高回收率下同时生产超高纯氮和超高纯氧。尽管参照某些优选实施方案对本发明进行了详细地说明,但本领域技术人员将会认识到在权利要求书的精神和范围内还存在着本发明其他的实施方案。
Claims (8)
1.一种通过进料空气的低温精馏生产超高纯氮和超高纯氧的方法,其中进料空气分为第一进料空气和第二进料空气,该方法包括:
(A)第一进料空气进入主塔,且该第一进料空气在该主塔内通过低温精馏分离成主塔富氧流体和主塔富氮流体;
(B)第二进料空气进入辅塔,且该第二进料空气在该辅塔内通过低温精馏分离成辅塔富氮流体和辅塔富氧流体;
(C)来自辅塔的辅塔富氮流体进入主塔的上部;
(D)主塔富氧流体或辅塔富氧流体流入汽提塔的上部,并且迎着上流蒸汽向下流过汽提塔以便在汽提塔的下部产生超高纯氧流体;
(E)在上述汽提塔内通过与主塔富氧流体的间接热交换蒸发部分超高纯氧流体以便产生所述的上流蒸汽;
(F)回收作为产品超高纯氧的另一部分来自上述汽提塔的超高纯氧流体;和
(G)回收作为产品提高纯氮的主塔富氮流体。
2.按权利要求1所述的方法,进一步包括主塔富氧流体从主塔进入辅塔。
3.按权利要求1所述的方法,进一步包括由辅塔回收部分辅塔富氮流体。
4.一种用于通过进料空气的低温精馏生产超高纯氮和超高纯氧的设备,包括:
(A)具有顶部冷凝器的主塔和进料空气进入塔用的装置;
(B)具有顶部冷凝器的辅塔和进料空气进入辅塔用的装置;
(C)具有塔底再沸器的汽提塔;
(D)用于流体从主塔下部进入主塔顶部冷凝器和从主塔顶部冷凝器进入汽提塔塔底再沸器的装置;
(E)用于流体从辅塔的上部进入辅塔顶部冷凝器和从辅塔顶部冷凝器进入主塔上部的装置;
(F)用于流体从主塔或辅塔进入汽提塔上部的装置;和
(G)用于从汽提塔下部回收超高纯氧的装置,和用于从主塔的上部回收超高纯氮的装置。
5.按权利要求4所述的设备,其中用于流体从辅塔顶部冷凝器进入主塔上部的装置包括液体泵。
6.按权利要求4所述的设备,进一步包括用于流体从主塔的下部进入辅塔下部的装置。
7.按权利要求4所述的设备,进一步包括用于流体从主塔顶部冷凝器进入辅塔下部的装置。
8.按权利要求4所述的设备,其中用于进料空气进入辅塔的装置包括涡轮膨胀机。
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US09/024196 | 1998-02-17 | ||
US09/024,196 | 1998-02-17 | ||
US09/024,196 US5918482A (en) | 1998-02-17 | 1998-02-17 | Cryogenic rectification system for producing ultra-high purity nitrogen and ultra-high purity oxygen |
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CN1226673A CN1226673A (zh) | 1999-08-25 |
CN1123753C true CN1123753C (zh) | 2003-10-08 |
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US (1) | US5918482A (zh) |
EP (1) | EP0936429B1 (zh) |
JP (1) | JP3545629B2 (zh) |
KR (1) | KR100407184B1 (zh) |
CN (1) | CN1123753C (zh) |
BR (1) | BR9900646A (zh) |
CA (1) | CA2262238A1 (zh) |
DE (1) | DE69910272T2 (zh) |
ES (1) | ES2200417T3 (zh) |
ID (1) | ID23302A (zh) |
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US5934104A (en) * | 1998-06-02 | 1999-08-10 | Air Products And Chemicals, Inc. | Multiple column nitrogen generators with oxygen coproduction |
US6173586B1 (en) | 1999-08-31 | 2001-01-16 | Praxair Technology, Inc. | Cryogenic rectification system for producing very high purity oxygen |
US6327873B1 (en) | 2000-06-14 | 2001-12-11 | Praxair Technology Inc. | Cryogenic rectification system for producing ultra high purity oxygen |
US6397631B1 (en) | 2001-06-12 | 2002-06-04 | Air Products And Chemicals, Inc. | Air separation process |
US6460373B1 (en) | 2001-12-04 | 2002-10-08 | Praxair Technology, Inc. | Cryogenic rectification system for producing high purity oxygen |
US7284395B2 (en) * | 2004-09-02 | 2007-10-23 | Praxair Technology, Inc. | Cryogenic air separation plant with reduced liquid drain loss |
US20080127676A1 (en) * | 2006-11-30 | 2008-06-05 | Amcscorporation | Method and apparatus for production of high-pressure nitrogen from air by cryogenic distillation |
US9103587B2 (en) * | 2009-12-17 | 2015-08-11 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procedes Georges Claude | Process and apparatus for the separation of air by cryogenic distillation |
JP5205436B2 (ja) * | 2010-10-29 | 2013-06-05 | 株式会社シマノ | 自転車用モータ制御システム |
US9097459B2 (en) * | 2011-08-17 | 2015-08-04 | Air Liquide Process & Construction, Inc. | Production of high-pressure gaseous nitrogen |
CN102506559A (zh) * | 2011-09-28 | 2012-06-20 | 开封东京空分集团有限公司 | 多段精馏制取高纯氮气空分工艺 |
CN104048478B (zh) * | 2014-06-23 | 2016-03-30 | 浙江大川空分设备有限公司 | 高提取率和低能耗污氮气提纯氮气的设备及其提取方法 |
CN113566495B (zh) * | 2021-07-28 | 2022-04-26 | 杭州特盈能源技术发展有限公司 | 一种玻璃窑炉用低能耗氮氧制取工艺 |
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DE2535489C3 (de) * | 1975-08-08 | 1978-05-24 | Linde Ag, 6200 Wiesbaden | Verfahren und Vorrichtung zur Zerlegung eines tiefsiedenden Gasgemisches |
US4560397A (en) * | 1984-08-16 | 1985-12-24 | Union Carbide Corporation | Process to produce ultrahigh purity oxygen |
US4780118A (en) * | 1987-07-28 | 1988-10-25 | Union Carbide Corporation | Process and apparatus to produce ultra high purity oxygen from a liquid feed |
US4755202A (en) * | 1987-07-28 | 1988-07-05 | Union Carbide Corporation | Process and apparatus to produce ultra high purity oxygen from a gaseous feed |
US4902321A (en) * | 1989-03-16 | 1990-02-20 | Union Carbide Corporation | Cryogenic rectification process for producing ultra high purity nitrogen |
US5049173A (en) * | 1990-03-06 | 1991-09-17 | Air Products And Chemicals, Inc. | Production of ultra-high purity oxygen from cryogenic air separation plants |
US5098457A (en) * | 1991-01-22 | 1992-03-24 | Union Carbide Industrial Gases Technology Corporation | Method and apparatus for producing elevated pressure nitrogen |
US5195324A (en) * | 1992-03-19 | 1993-03-23 | Prazair Technology, Inc. | Cryogenic rectification system for producing nitrogen and ultra high purity oxygen |
JP2966999B2 (ja) * | 1992-04-13 | 1999-10-25 | 日本エア・リキード株式会社 | 超高純度窒素・酸素製造装置 |
US5528906A (en) * | 1995-06-26 | 1996-06-25 | The Boc Group, Inc. | Method and apparatus for producing ultra-high purity oxygen |
US5582032A (en) * | 1995-08-11 | 1996-12-10 | Liquid Air Engineering Corporation | Ultra-high purity oxygen production |
US5590543A (en) * | 1995-08-29 | 1997-01-07 | Air Products And Chemicals, Inc. | Production of ultra-high purity oxygen from cryogenic air separation plants |
-
1998
- 1998-02-17 US US09/024,196 patent/US5918482A/en not_active Expired - Lifetime
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1999
- 1999-02-04 ID IDP990080D patent/ID23302A/id unknown
- 1999-02-12 BR BR9900646-4A patent/BR9900646A/pt not_active Application Discontinuation
- 1999-02-12 KR KR10-1999-0004996A patent/KR100407184B1/ko not_active IP Right Cessation
- 1999-02-14 CN CN99102216A patent/CN1123753C/zh not_active Expired - Fee Related
- 1999-02-16 ES ES99103064T patent/ES2200417T3/es not_active Expired - Lifetime
- 1999-02-16 CA CA002262238A patent/CA2262238A1/en not_active Abandoned
- 1999-02-16 EP EP99103064A patent/EP0936429B1/en not_active Expired - Lifetime
- 1999-02-16 JP JP03717799A patent/JP3545629B2/ja not_active Expired - Fee Related
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CA2262238A1 (en) | 1999-08-17 |
EP0936429B1 (en) | 2003-08-13 |
KR100407184B1 (ko) | 2003-11-28 |
DE69910272D1 (de) | 2003-09-18 |
JP3545629B2 (ja) | 2004-07-21 |
EP0936429A3 (en) | 1999-11-24 |
BR9900646A (pt) | 1999-12-28 |
ID23302A (id) | 2000-04-05 |
JPH11316080A (ja) | 1999-11-16 |
EP0936429A2 (en) | 1999-08-18 |
ES2200417T3 (es) | 2004-03-01 |
CN1226673A (zh) | 1999-08-25 |
US5918482A (en) | 1999-07-06 |
DE69910272T2 (de) | 2004-06-17 |
KR19990072641A (ko) | 1999-09-27 |
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