EP1001236A2 - Procédé de production d'azote à ultra haute pureté - Google Patents

Procédé de production d'azote à ultra haute pureté Download PDF

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Publication number: EP1001236A2
Authority: EP; European Patent Office
Prior art keywords: column; free; nitrogen; pressure column; low
Prior art date: 1998-11-11
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.): Granted

Application number

EP99122146A

Other languages

German (de)

English (en)

Other versions

EP1001236B1 (fr

EP1001236A3 (fr

Inventor

Dietrich Dipl.-Ing. Rottmann

Christian Dipl.-Ing. Kunz

Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)

Linde GmbH

Original Assignee

Linde GmbH

Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)

1998-11-11

Filing date

1999-11-05

Publication date

2000-05-17

1999-11-05 Application filed by Linde GmbH filed Critical Linde GmbH

2000-05-17 Publication of EP1001236A2 publication Critical patent/EP1001236A2/fr

2000-11-08 Publication of EP1001236A3 publication Critical patent/EP1001236A3/fr

2004-09-29 Application granted granted Critical

2004-09-29 Publication of EP1001236B1 publication Critical patent/EP1001236B1/fr

2019-11-05 Anticipated expiration legal-status Critical

Status Expired - Lifetime legal-status Critical Current

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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04187—Cooling of the purified feed air by recuperative heat-exchange; Heat-exchange with product streams
- F25J3/04218—Parallel arrangement of the main heat exchange line in cores having different functions, e.g. in low pressure and high pressure cores
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
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- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
- F25J3/04078—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression
- F25J3/04084—Providing pressurised feed air or process streams within or from the air fractionation unit providing pressurized products by liquid compression and vaporisation with cold recovery, i.e. so-called internal compression of nitrogen
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- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
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- F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
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- F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
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- F25J3/04436—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using at least a triple pressure main column system
- F25J3/04454—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using at least a triple pressure main column system a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
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- F25J3/04763—Start-up or control of the process; Details of the apparatus used
- F25J3/04866—Construction and layout of air fractionation equipments, e.g. valves, machines
- F25J3/04951—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network
- F25J3/04963—Arrangements of multiple air fractionation units or multiple equipments fulfilling the same process step, e.g. multiple trains in a network and inter-connecting equipment within or downstream of the fractionation unit(s)
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
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- F25J2200/10—Processes or apparatus using separation by rectification in a quadruple, or more, column or pressure system
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- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
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- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
- F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
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- F25J2220/42—Separating low boiling, i.e. more volatile components from nitrogen, e.g. He, H2, Ne
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- F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
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- F25J2250/00—Details related to the use of reboiler-condensers
- F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams
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- F25J2270/00—Refrigeration techniques used
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- F25J2290/00—Other details not covered by groups F25J2200/00 - F25J2280/00
- F25J2290/62—Details of storing a fluid in a tank
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S62/00—Refrigeration
- Y10S62/92—Carbon monoxide

Definitions

the invention relates to a process for the production of ultra-pure nitrogen by Cryogenic air separation in a rectification system with at least one Rectification column, whereby compressed and cleaned feed air into a pressure column led, an oxygen-free pressure nitrogen fraction obtained from the pressure column, in a low pressure column and in the low pressure column carbon monoxide free Low pressure nitrogen is obtained as a top gas.
the object of the invention is therefore to avoid this disadvantage and Reduce energy consumption.
Another object of the invention is to demonstrate a method which either with a liquid pressure nitrogen fraction directly from the pressure column or is operated from a tank with liquid pressure column nitrogen.
the oxygen-free pressurized nitrogen fraction is either withdrawn in liquid form from an upper region of the pressure column or is provided from a liquid tank with stored oxygen-free nitrogen and that the oxygen-free pressurized nitrogen fraction is expanded into the low-pressure column heated in its sump, steam rising in the low-pressure column formed and freed of carbon monoxide with the aid of a reflux at the top of the low-pressure column with ultra-pure nitrogen, drawn off at the top of the low-pressure column as carbon monoxide-free head gas and partially liquefied after a pressure increase and the liquefied part in a He-Ne-H 2 - heated in its sump
the column is relaxed, from which the ultra-pure nitrogen is removed in liquid form.
the ultra pure nitrogen is obtained in liquid form and is easier to transport in this form and therefore easier to distribute to customers become.
the process can also be used universally. Because it can with Connection to an air separation plant (with or without liquid nitrogen tank) or only on a liquid nitrogen tank (with spatial separation from the air separation plant) be used. On an air separation plant with a liquid nitrogen tank also the ultra pure liquid nitrogen can be obtained without the Air separation plant is in operation.
the carbon monoxide-free head gas and a head gas of the He-Ne-H 2 column can be combined to form a cold gas stream free of carbon monoxide.
the carbon monoxide-free overhead gas can be partially liquefied in a condenser / evaporator against a liquid refrigerant, which is evaporated in the process, and a gas stream resulting from the evaporation of the liquid refrigerant and a top gas from the He-Ne-H 2 column can cold to a carbon monoxide-free Gas flow can be summarized.
the carbon monoxide-free cold gas stream is advantageously warmed in a heat exchanger, compressed and cooled in countercurrent in the same heat exchanger and then partly in the low-pressure column and partly in the He-Ne-H 2 column for heating the Used sump and liquefied except gaseous residual streams and fed as the liquid refrigerant to the condenser / evaporator.
the flows liquefied during the heating of the He-Ne-H 2 column and the low-pressure column can be fed to the He-Ne-H 2 column as a return.
the flows liquefied during the heating of the He-Ne-H 2 column and the low pressure column in the evaporator / condenser of the low pressure column can liquefy the carbon monoxide-free overhead gas of the low pressure column to a residual flow and are at least partially fed as reflux to the He-Ne-H 2 column.
the disadvantage of an additional investment for the condenser / evaporator is then offset by the advantage, which should not be underestimated, that in the event of air leakage during the compression of the carbon monoxide-free gas stream, the ultrapure liquid nitrogen cannot be contaminated.
Ultrapure nitrogen can be drawn off liquid from the He-Ne-H 2 column and can be obtained partly as the return of the low-pressure column and partly as a liquid ultra-pure nitrogen product.
the ultra pure liquid nitrogen product can be fed to a product tank.
the ultra pure liquid nitrogen product can be pressurized with a pump, under Use of the cold content in the production of oxygen-free Compressed nitrogen fraction evaporates, warmed up and as a gaseous pressure product Use can be supplied.
the process for producing ultra pure Liquid nitrogen product also made and ultra-pure nitrogen gas product the cold of the original liquid product is used sensibly become.
FIG. 1 shows schematically an embodiment of the method according to the invention for the production of ultra-pure nitrogen. Except for a residual content in the range of a few mol ppm of oxygen-free liquid pressure nitrogen fraction 1 is expanded into a heated low pressure column 2, which is operated at a pressure between 4.5 and 5.5 bar. In the low-pressure column 2, rising steam is released from the He-Ne-H 2 column 4 of carbon monoxide and thus also of impurities boiling heavier than carbon monoxide, such as argon and the residual oxygen content, depending on the purity requirement, by means of ultrapure nitrogen 3 which is applied at the top as a return line exempted a few mol-ppb.
the carbon monoxide-free head gas 5 and a head gas 6 of the He-Ne-H 2 column are combined to form a carbon monoxide-free cold gas stream 7, heated in a heat exchanger 8 and cooled again after compression 9 in the same heat exchanger 8.
the cooled gas stream 10 is used to a part 11 in the low pressure column 2 and to another part 12 in the He-Ne-H 2 column 4 for heating 13, 14 of the sump and liquefied except for gaseous residual streams 15, 16.
the liquefied streams 17, 18 are fed to the He-Ne-H 2 column 4 as a return.
FIG. 2 shows schematically the production of the ultra-pure liquid nitrogen product 20 as in FIG. 1.
the liquid nitrogen fraction 1 used as the insert is different from in the embodiment according to FIG. 1 of a pressure column 25 of a rectification system removed and fed into the low pressure column 2 via a heat exchanger 24.
the ultra pure liquid nitrogen product 20 is pressurized by a pump 26 in counterflow to the liquid nitrogen fraction 1 via the heat exchanger 24 passed and using the cold content in a condenser 27 and in one Heat exchanger 28 in the extraction of the oxygen-free pressure nitrogen fraction used, evaporated, warmed and as a gaseous ultra-pure printed product 29 fed for further use.
FIG. 3 schematically shows an embodiment of the method according to the invention using a condenser / evaporator 30.
the carbon monoxide-free top gas 5 of the low-pressure column 2 (against one by combining the liquefied streams 17, 18 formed liquid coolant 31, which evaporates here) liquefied in the condenser / evaporator 30 except for a gaseous residual stream 32 and used in the He-Ne-H 2 column 4 as the return 33.
a gas stream 5 ′ formed during the evaporation of the liquid refrigerant and the top gas 6 of the He-Ne-H 2 column 4 are combined to form the cold carbon monoxide-free gas stream 7.
Figure 4 schematically shows an embodiment of the method according to the invention in FIG. 2, but carried out with the condenser / evaporator 30 as in FIG. 3.
FIG. 5 shows schematically that the inventive method on a existing rectification system can be used.
Condenser 27 is added and the heat exchanger 8 receives two additional ones Passages for the use of the cold of the ultra pure nitrogen 20 'to be heated the cooling and liquefaction of a partial flow 34 of the air 35 for the Rectification system.
the ultrapure heated in this case in the heat exchanger 8 Nitrogen is used as a gaseous ultrapure printed product 29 for further use fed.
a common feature of the design of the method according to the invention according to Figures 1 to 5 is that all residual gas flows (15, 16, 36 in Figure 1, 2, 5 and 15, 16, 32, 36 in Figure 3, 4) to a cold residual gas stream 37 summarized heated in the heat exchanger 8 and as an impure gas 38 to the Atmosphere.
m 3 means: m 3 in the normal state at 0 ° C and 1.0133 bar; ie 1m 3 corresponds to 1.25 kg.

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Engineering & Computer Science (AREA)
Physics & Mathematics (AREA)
Mechanical Engineering (AREA)
Thermal Sciences (AREA)
General Engineering & Computer Science (AREA)
Separation By Low-Temperature Treatments (AREA)
Arrangement Of Elements, Cooling, Sealing, Or The Like Of Lighting Devices (AREA)
Crystals, And After-Treatments Of Crystals (AREA)
Removal Of Specific Substances (AREA)

EP99122146A 1998-11-11 1999-11-05 Procédé de production d'azote à ultra haute pureté Expired - Lifetime EP1001236B1 (fr)

Applications Claiming Priority (4)

Application Number	Priority Date	Filing Date	Title
DE19852019		1998-11-11
DE19852019		1998-11-11
DE19924375		1999-05-27
DE19924375		1999-05-27

Publications (3)

Publication Number	Publication Date
EP1001236A2 true EP1001236A2 (fr)	2000-05-17
EP1001236A3 EP1001236A3 (fr)	2000-11-08
EP1001236B1 EP1001236B1 (fr)	2004-09-29

Family

ID=26050074

Family Applications (1)

Application Number	Title	Priority Date	Filing Date
EP99122146A Expired - Lifetime EP1001236B1 (fr)	1998-11-11	1999-11-05	Procédé de production d'azote à ultra haute pureté

Country Status (11)

Country	Link
US (1)	US6276172B1 (fr)
EP (1)	EP1001236B1 (fr)
JP (1)	JP2000180051A (fr)
KR (1)	KR20000035406A (fr)
CN (1)	CN1134640C (fr)
AT (1)	ATE278166T1 (fr)
CA (1)	CA2289173A1 (fr)
DE (2)	DE19929798A1 (fr)
ES (1)	ES2229608T3 (fr)
SG (1)	SG74755A1 (fr)
TW (1)	TW432191B (fr)

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* Cited by examiner, † Cited by third party
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DE10158327A1 (de) *	2001-11-28	2003-06-18	Linde Ag	Verfahren und Vorrichtung zur Herstellung hoch reinen Stickstoffs aus weniger reinem Stickstoff
DE10205094A1 (de) *	2002-02-07	2003-08-21	Linde Ag	Verfahren und Vorrichtung zur Erzeugung hoch reinen Stickstoffs
CN102959352B (zh) *	2009-07-24	2016-07-06	英国备选能源国际有限公司	二氧化碳和氢气的分离
CN102797974A (zh) *	2012-07-31	2012-11-28	张立永	氢脉
CN114165989A (zh) *	2021-11-22	2022-03-11	四川空分设备(集团)有限责任公司	制取中压氮气的装置及方法

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US4464188A (en) *	1983-09-27	1984-08-07	Air Products And Chemicals, Inc.	Process and apparatus for the separation of air
US5123947A (en) *	1991-01-03	1992-06-23	Air Products And Chemicals, Inc.	Cryogenic process for the separation of air to produce ultra high purity nitrogen
US5167125A (en) *	1991-04-08	1992-12-01	Air Products And Chemicals, Inc.	Recovery of dissolved light gases from a liquid stream
US5170630A (en) *	1991-06-24	1992-12-15	The Boc Group, Inc.	Process and apparatus for producing nitrogen of ultra-high purity
JP3306517B2 (ja) *	1992-05-08	2002-07-24	日本酸素株式会社	空気液化分離装置及び方法
US5351492A (en) *	1992-09-23	1994-10-04	Air Products And Chemicals, Inc.	Distillation strategies for the production of carbon monoxide-free nitrogen
FR2696821B1 (fr) *	1992-10-09	1994-11-10	Air Liquide	Procédé et installation de production d'azote ultra-pur sous pression.
JP3447437B2 (ja) *	1995-07-26	2003-09-16	日本エア・リキード株式会社	高純度窒素ガス製造装置
DE19640711A1 (de) *	1996-10-02	1998-04-09	Linde Ag	Verfahren und Vorrichtung zur Gewinnung von hochreinem Stickstoff
DE19806576A1 (de) *	1998-02-17	1998-08-06	Linde Ag	Verfahren und Vorrichtung zur Gewinnung von CO-freiem Stickstoff
US5906113A (en) *	1998-04-08	1999-05-25	Praxair Technology, Inc.	Serial column cryogenic rectification system for producing high purity nitrogen

1999
- 1999-06-29 DE DE19929798A patent/DE19929798A1/de not_active Withdrawn
- 1999-10-29 TW TW088118824A patent/TW432191B/zh not_active IP Right Cessation
- 1999-11-05 DE DE59910646T patent/DE59910646D1/de not_active Expired - Fee Related
- 1999-11-05 EP EP99122146A patent/EP1001236B1/fr not_active Expired - Lifetime
- 1999-11-05 ES ES99122146T patent/ES2229608T3/es not_active Expired - Lifetime
- 1999-11-05 AT AT99122146T patent/ATE278166T1/de not_active IP Right Cessation
- 1999-11-09 CA CA002289173A patent/CA2289173A1/fr not_active Abandoned
- 1999-11-10 JP JP11319519A patent/JP2000180051A/ja active Pending
- 1999-11-10 SG SG1999005577A patent/SG74755A1/en unknown
- 1999-11-10 US US09/437,263 patent/US6276172B1/en not_active Expired - Fee Related
- 1999-11-11 KR KR1019990049862A patent/KR20000035406A/ko not_active Ceased
- 1999-11-11 CN CNB991238044A patent/CN1134640C/zh not_active Expired - Fee Related

Also Published As

Publication number	Publication date
ES2229608T3 (es)	2005-04-16
EP1001236B1 (fr)	2004-09-29
ATE278166T1 (de)	2004-10-15
CN1255619A (zh)	2000-06-07
CN1134640C (zh)	2004-01-14
DE19929798A1 (de)	2000-05-25
DE59910646D1 (de)	2004-11-04
KR20000035406A (ko)	2000-06-26
SG74755A1 (en)	2000-08-22
TW432191B (en)	2001-05-01
EP1001236A3 (fr)	2000-11-08
US6276172B1 (en)	2001-08-21
JP2000180051A (ja)	2000-06-30
CA2289173A1 (fr)	2000-05-11

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