EP0343065A1 - Stickstoffgasherstellungsverfahren - Google Patents

Stickstoffgasherstellungsverfahren Download PDF

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Publication number
EP0343065A1
EP0343065A1 EP89401358A EP89401358A EP0343065A1 EP 0343065 A1 EP0343065 A1 EP 0343065A1 EP 89401358 A EP89401358 A EP 89401358A EP 89401358 A EP89401358 A EP 89401358A EP 0343065 A1 EP0343065 A1 EP 0343065A1
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EP
European Patent Office
Prior art keywords
heat exchanger
main heat
nitrogen gas
gas
oxygen
Prior art date
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
EP89401358A
Other languages
English (en)
French (fr)
Other versions
EP0343065B1 (de
Inventor
Harumitsu L'air Liquide Takagi
Takashi L'air Liquide Nagamura
Takao L'air Liquide Yamamoto
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.)
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
Air Liquide SA
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
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Publication date
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Application filed by Air Liquide SA, LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical Air Liquide SA
Publication of EP0343065A1 publication Critical patent/EP0343065A1/de
Application granted granted Critical
Publication of EP0343065B1 publication Critical patent/EP0343065B1/de
Expired legal-status Critical Current

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Classifications

    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • 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
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • 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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • 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
    • F25J3/044—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 a single pressure main column system only
    • 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
    • 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
    • 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
    • F25J2200/00—Processes or apparatus using separation by rectification
    • F25J2200/74—Refluxing the column with at least a part of the partially condensed overhead gas
    • 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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen

Definitions

  • the present invention relates to a method of producing nitrogen gas from compressed air by utilizing a single frac­tionating tower.
  • oxygen-rich liquid having a large nitrogen content is collected in a sump at the bottom of the fractionating tower.
  • the oxygen-rich liquid in the sump is taken out as it is and led to a condenser in the top of the fractionating tower to be used as a coolant therein.
  • This liquid is vaporized into oxygen-rich air through heat ex­change in the condenser, which air is thereafter used as a coolant in the main heat exchanger and is then released as exhaust gas.
  • the oxygen-rich gas is released as exhaust gas as noted above without its effective use being attained to the full extent although it is possible to make effective use of the oxygen-rich gas.
  • the present invention has been made having regard to the above state of the art, and its object is to provide a method of producing nitrogen gas with improved yield and with low manufacturing cost per unit amount, which is achieved by making effective use of the oxygen-rich gas which has been disposed of as exhaust gas as noted above.
  • a method of producing nitrogen gas according to the present invention comprises the steps of removing impurities such as moisture and carbon dioxide from a raw material consisting of compressed air, feeding the impurity-free raw material, after cooling the same to a temperature close to a liquefying point through a main heat exchanger, to a lower position of a fractionating tower for fractionating the raw material, withdrawing nitrogen gas from a top position of the fractionating tower and leading the nitrogen gas to the main heat exchanger for use as a coolant, and heating the nitrogen gas to room temperature by heat exchange therein to obtain nitrogen gas product, characterized in that oxygen-rich liquid is taken out of a bottom position of the fractionating tower and, while being expanded, is fed to a condenser disposed in a top position of the fractionating tower for use as a coolant therein, said liquid being vaporized in said condenser into oxygen-rich gas, said gas is taken out of said condenser and led to said main heat exchanger for use as a coolant therein, said gas being heated to room temperature
  • the cold energy of the oxygen-rich gas taken out of the condenser is first used as a cold source in the main heat exchanger, whereby the oxygen-rich gas is heated to room temperature. At least part of this oxygen-rich gas is compressed and returned to the main heat exchanger where it is cooled, and is thereafter fed to the bottom of the fractionating tower (to a reboiler disposed therein, for example). Then a heat exchange takes place in the bottom of the fractionating tower between the compressed oxygen-rich gas and the oxygen-rich liquid. The oxygen-rich liquid is thereby heated and the compressed oxygen-rich gas is liquefied.
  • the gas evaporated as the oxygen-rich liquid is heated ascends in counter current contact with a recircu­lation liquid (liquid nitrogen, for example) descending through the fractionating tower. Fractionation is thereby effected with oxygen becoming liquefied and descending, and nitrogen-rich gas ascending.
  • the oxygen-­rich liquid collected in the bottom of the fractionating tower is taken out of the bottom, expanded and fed to the condenser to act as a coolant.
  • the oxygen-­rich liquid is fed to the top of the fractionating tower to produce the recirculation liquid necessary for separating the nitrogen content from the raw material air by liquefying the nitrogen gas ascending through the fractionating tower.
  • the oxygen-rich gas taken out of the condenser is used as a coolant in the main heat exchanger, and thereafter compress­ed, cooled and fed to the bottom of the fractionating tower for heating the oxygen-rich liquid in the bottom of the fractionating tower.
  • the oxygen-rich liquid in the bottom of the fractionating tower is used as a cold source for producing the recirculation liquid.
  • raw material air GA stripped of dust by an air filter (not shown) is compressed by a com­pressor 1 to a nitrogen gas product pressure and pressure necessary for operating an air separator (9.5kg/cm2G, for example).
  • the compressed raw material air GA is fed through a piping P1 to a drying and carbon removing unit 2.
  • the compressed raw mate­rial air GA is fed to one of two molecularceive towers where moisture and carbon dioxide are removed from the raw mate­rial air GA through adsorption.
  • oxygen-rich gas GW having passed through a main heat exchanger 3 to be described later is fed to the other molecularceive tower to regenerate this tower.
  • the raw material air GA stripped of moisture and carbon dioxide at the drying and carbon removing unit 2 is fed through a piping P2 to the main heat exchanger 3 to be cool­ed to a temperature close to the liquefying point.
  • This fractionating tower 4 receives liquid nitrogen LN, which is one example of cold source, delivered through a piping P4 to an upper position thereof.
  • the raw material air GA ascending from below and the liquid nitrogen (recircula­tion liquid) descending from above contact each other in counter current, whereby oxygen in the raw material air GA is liquefied to fractionate and separate nitrogen gas GN.
  • the nitrogen gas GN taken out of the top of the frac­tionating tower 4 is fed through a piping P5 to the main heat exchanger 3 so that the cold energy of nitrogen gas GN is used as a coolant in the main heat exchanger 3 and that the nitrogen gas GN is heated to room temperature.
  • the nitrogen gas GN at room temperature taken out of the main heat exchanger 3 through a piping P7 is supplied as a nitro­gen gas product having an appropriate pressure (9.0kg/cm2G, for example).
  • Oxygen-rich liquid LW is collected in the bottom of the fractionating tower 4. This liquid LW is taken out of the bottom and is led through a piping P6 having an expansion valve 5 to a condenser 10 disposed in the top position of the fractionating tower 4. The liquid LW is expanded by the expansion valve 5 to an appropriate pressure (3.5kg/cm2G, for example) and is led into the condenser 10 to be used as a coolant therein. In the condenser 10 the liquid LW is vaporized into oxygen-rich gas GW.
  • the oxygen-rich gas GW after being taken out of the condenser 10, is led through a piping P8 to the main heat exchanger 3 to be used as a coolant therein.
  • This gas GW is heated to room temperature at the main heat exchanger 3, and is thereafter led through a piping P9 to the drying and carbon removing unit 2 and a compressor 6.
  • Part of the gas GW is released as exhaust gas GW after being used for regen­erating the drying and carbon removing unit 2 as described hereinbefore.
  • the remainder is compressed by the compressor 6 (to a pressure of 3.5kg/cm2G to 10.0kg/cm2G, for example), and returned through a piping P10 to the main heat exchanger 3.
  • the gas GW is cooled through heat exchange in the main heat exchanger 3.
  • the cooled gas GW is led through a piping P11 to a reboiler 7 disposed in the bottom of the fraction­ating tower 4 to give off heat. Then the gas GW is cooled therein and expanded to a pressure of 3.5kg/cm2G, for exam­ple, through a piping P12 having an expansion valve 8 at an intermediate position thereof. Thereafter expanded gas GW is led to the compressor 10 disposed in the top position of the fractionating tower 4 to join the oxygen-rich gas GW.
  • the oxygen-rich gas GW taken out of the condenser 10 is used as a coolant in the main heat exchanger 3. After being taken out of the main heat exchanger 3, the gas GW is compressed, cooled and fed to the reboiler 7 for heating the oxygen-rich liquid LW collected in the bottom of the fractionating tower 4. More­over, the oxygen-rich liquid LW which has been liquefied in the reboiler 7 is used as a cold source in the condenser 10 for producing the recirculation liquid.
  • effective use is made of the oxygen-rich gas GW, whereby the yield of nitrogen gas is improved to about 88% compared with less than 50% of nitrogen gas heretofore obtained from nitrogen contained in the air.
  • part of the oxygen-rich gas taken out of the condenser 10 and heated to room temper­ature by the main heat exchanger 3 is utilized for regener­ating the drying and carbon removing unit 2. This feature promotes the effective use of the oxygen-rich gas.
  • the oxygen-rich gas GW taken out of the compressor 10 may be taken out at an intermediate posi­tion of the main heat exchanger 3 through a piping P13.
  • Part of the gas GW is adiabatically expanded by an expansion turbine 11 and returned through a piping P14 to the main heat exchanger 3 to be used as a coolant in the main heat exchanger 3.
  • the gas GW used as a coolant may be taken out of the main heat exchanger 3 and led through a piping P15 to the drying and carbon removing unit 2 for regenerating this unit 2.
  • the gas GW led through the piping P9 need not be used as the regenerating gas. This method pro­vides an even more effective use of the oxygen-enriched gas GW.
  • the oxygen-rich gas GW returned to the main heat exchanger 3 may be led through a piping 16 directly to the bottom of the fractionating tower 4 after being cooled by the main heat exchanger 3 to a temperature adjacent the liquefying point.

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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)
EP19890401358 1988-05-19 1989-05-17 Stickstoffgasherstellungsverfahren Expired EP0343065B1 (de)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP122681/88 1988-05-19
JP63122681A JP2755953B2 (ja) 1988-05-19 1988-05-19 窒素ガス製造方法

Publications (2)

Publication Number Publication Date
EP0343065A1 true EP0343065A1 (de) 1989-11-23
EP0343065B1 EP0343065B1 (de) 1991-11-27

Family

ID=14841992

Family Applications (1)

Application Number Title Priority Date Filing Date
EP19890401358 Expired EP0343065B1 (de) 1988-05-19 1989-05-17 Stickstoffgasherstellungsverfahren

Country Status (3)

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EP (1) EP0343065B1 (de)
JP (1) JP2755953B2 (de)
DE (1) DE68900471D1 (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0412793A1 (de) * 1989-08-11 1991-02-13 The Boc Group, Inc. Verfahren und Vorrichtung zur Herstellung von Stickstoff aus Luft
US5303556A (en) * 1993-01-21 1994-04-19 Praxair Technology, Inc. Single column cryogenic rectification system for producing nitrogen gas at elevated pressure and high purity
EP0816784A1 (de) * 1996-06-26 1998-01-07 Crio & Eng S.r.l. Vorrichtung zur Fraktionierung von Luft oder Sauerstoffstickstoff Gasgemischen zur Gewinnung von Stickstoff und Sauerstoff oder von Stickstoff

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2225705A1 (de) * 1973-04-13 1974-11-08 Cryoplants Ltd
EP0241817A2 (de) * 1986-04-02 1987-10-21 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von Stickstoff

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0627621B2 (ja) * 1986-11-19 1994-04-13 株式会社日立製作所 高純度窒素ガス製造装置

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2225705A1 (de) * 1973-04-13 1974-11-08 Cryoplants Ltd
EP0241817A2 (de) * 1986-04-02 1987-10-21 Linde Aktiengesellschaft Verfahren und Vorrichtung zur Erzeugung von Stickstoff

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0412793A1 (de) * 1989-08-11 1991-02-13 The Boc Group, Inc. Verfahren und Vorrichtung zur Herstellung von Stickstoff aus Luft
US5303556A (en) * 1993-01-21 1994-04-19 Praxair Technology, Inc. Single column cryogenic rectification system for producing nitrogen gas at elevated pressure and high purity
EP0816784A1 (de) * 1996-06-26 1998-01-07 Crio & Eng S.r.l. Vorrichtung zur Fraktionierung von Luft oder Sauerstoffstickstoff Gasgemischen zur Gewinnung von Stickstoff und Sauerstoff oder von Stickstoff

Also Published As

Publication number Publication date
JP2755953B2 (ja) 1998-05-25
DE68900471D1 (de) 1992-01-09
JPH01296076A (ja) 1989-11-29
EP0343065B1 (de) 1991-11-27

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