US3500651A - Production of high pressure gaseous oxygen by low temperature rectification of air - Google Patents

Production of high pressure gaseous oxygen by low temperature rectification of air Download PDF

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US3500651A
US3500651A US609208A US3500651DA US3500651A US 3500651 A US3500651 A US 3500651A US 609208 A US609208 A US 609208A US 3500651D A US3500651D A US 3500651DA US 3500651 A US3500651 A US 3500651A
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air
oxygen
column
pressure
high pressure
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Rudolf Becker
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Linde GmbH
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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
    • 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
    • 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
    • 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
    • F25J3/04006—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
    • F25J3/0409—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 oxygen
    • 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
    • F25J3/04224—Cores associated with a liquefaction or refrigeration cycle
    • 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
    • F25J3/04309—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 of nitrogen
    • 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
    • F25J3/04309—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 of nitrogen
    • F25J3/04315—Lowest pressure or impure nitrogen, so-called waste nitrogen expansion
    • 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
    • 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
    • F25J3/04406—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 dual pressure main column system
    • F25J3/04412—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 dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure 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
    • F25J2200/20—Processes or apparatus using separation by rectification in an elevated pressure multiple column system wherein the lowest pressure column is at a pressure well above the minimum pressure needed to overcome pressure drop to reject the products to atmosphere
    • 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
    • F25J2200/70—Refluxing the column with a condensed part of the feed stream, i.e. fractionator top is stripped or self-rectified
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/24—Processes or apparatus using other separation and/or other processing means using regenerators, cold accumulators or reversible heat exchangers
    • 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
    • F25J2230/00—Processes or apparatus involving steps for increasing the pressure of gaseous process streams
    • F25J2230/42—Processes or apparatus involving steps for increasing the pressure of gaseous process streams the fluid being nitrogen
    • 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
    • F25J2245/00—Processes or apparatus involving steps for recycling of process streams
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
    • 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
    • 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

Definitions

  • This invention relates to the low temperature rectification of air, and in particular, to a process and apparatus for the production of gaseous high pressure oxygen, wherein the air is cooled and cleansed in regenerators and fed to a fractionating column; nitrogen is withdrawn at the head of the fractionating column and warmed in the regenerators countercurrently to the air; and liquid oxygen is pumped to the desired pressure and then vaporized countercurrently to a gaseous process stream.
  • German Patent No. 1,103,363 discloses a process wherein the liquid oxygen is withdrawn from the low pressure section of a double column and heated,by being pumped through a heat exchanger countercurrently to a stream which had been previously withdrawn from the bottom portion of the high pressure section of the column, and was reheated in regenerators (said stream having substantially the same composition as air).
  • regenerators said stream having substantially the same composition as air.
  • Processes are also known wherein the gaseous oxygen is produced under normal pressure and then compressed in the gaseous phase to the desired pressure in piston compressors.
  • An object of this invention is to provide a more economical system for the production of high pressure oxygen gas.
  • FIGURE 1 is a schematic illustration of a preferred embodiment of this invention wherein the rectification column is in the form of a single column.
  • FIGURE 2 is a schematic illustration of a preferred embodiment of this invention wherein the rectification column is in the form of a double column.
  • a system wherein (a) the air is compressed to such a pressure that it is liquefied in the sump of a single column rectification column in heat exchange with boiling low pressure oxygen; (b) a portion, about 20 to 30%, of the cleansed and cooled air from the regenerators is passed countercurrently and reheated in the regenerators, and is then employed for vaporizing compressed liquid oxygen; and (c) the refrigeration is provided by engine expansion of the enriched nitrogen stream from the top of the column.
  • engine expansion refers to expansion with the production of external work.
  • this invention also embraces the use of a double column.
  • the nitrogen enriched fraction obtained from the air is liquefied in heat exchange with evaporating oxygen.
  • it can also be advantageous to pass, instead of said portion of cleansed and cooled air, a corresponding partial amount of a separation product countercurrently through the regenerators, warming the same in this manner, and then employing the heated separation product for vaporizing the high pressure oxygen.
  • This invention is thus characterized by the utilization of a low pressure air separation step in cooperation with steps for the production of high pressure gaseous 0 without requiring a high compression of either the air to be separated or the by-product nitrogen stream.
  • the raw air is generally compressed to from 6 to 20, preferably 9 to 12 atmospheres absolute.
  • the air separation step for a single column rectification column is generally conducted at a pressure of 2 to 9, preferably 3 to 4 atmospheres absolute, and for a double column, a pressure of generally 6 to 20, preferably 9 to 12 atmospheres absolute in the high pressure section, and generally a pressure of 1.6 to 7, preferably 2.5 to 3.5 atmospheres absolute in the low pressure section.
  • the pressure of the high pressure oxygen product it is generally at least about 40 to 300, and preferably in the range of about 50 to atmospheres absolute.
  • the expansion of the nitrogen leaving the head of a single column rectifier is advantageously conducted in a turbine which is continuously under full load.
  • the nitrogen exit temperature at the regenerators can be regulated by adjusting the throttle valve for that portion of cooled and cleansed air branched off the main air stream and recycled countercurrently through the regenerators, which throttle valve is located upstream of the rectification column.
  • the pressure of the air or the separation product used for heating, or for vaporizing and heating the oxygen it is basically possible for either the pressure of the air or the separation product used for heating, or for vaporizing and heating the oxygen, to be much below the pressure of the high pressure oxygen.
  • the pressure of the heating gas is generally about 6 to 20 atmospheres absolute, whereas the air is compressed to the lower pressure of the said range.
  • the refrigeration energy and thusthe purity of the oxygen can be controlled by expanding the nitrogen in the turbine, by either manually or automatically adjusting the suction throttle valve of a bypass line or the turbine guide vanes.
  • the output capacity of the oxygen pump can be regulated when operating with a variable air feed by simply controlling the liquid level of oxygen in the rectification column.
  • the nitrogen withdrawn from the head of the rectifier is used, before 3 eing expanded, for cooling the main air stream and the ecycle air stream.
  • a major advantage of this invention resides in the relaive simplicity and inexpensiveness of the apparatus that an be employed to carry out the process.
  • air at a rate f 11,000 Nmfi/h. is compressed in compressor 1' and utroduced into cyclically switchable regenerators 1 at a emperature of 300 K. and a pressure of 10 atmospheres bsolute.
  • This air is cooled therein to 107.5 K., thereby reezing out H and CO to form cleansed air.
  • Downtream of the regenerator outlet the cleansed air stream 5 branched at 2, one portion about 76.5% passing through :onduit 3 to the sump of the rectification column 5, while be other portion is recycled via the branch conduit 4, nto the regenerators 1, wherein said other portion is releated to 290 K.
  • the air in the coil 6 is ndirectly heat exchanged with the liquid fractionated vxygen product. Thereafter, the air is expanded in exansion valve 7 to the column pressure of 3.3 atmosiheres absolute.
  • the column is operated so that the liquid oxygen c01- ects in the bottom (sump) While the nitrogen-enriched tream is withdrawn as overhead.
  • This nitrogen stream is lsed for subcooling the air in a countercurrent heat ex- :hanger 8, and is then passed to the expansion turbine 16 'ia conduit 14.
  • the nirogen stream is passed through countercurrent heat ex- -.hanger 15 for cooling the cleansed air before the latter s passed through the sump of the column 5.
  • the nitrogen enters the turbine 16 at 105 K. and 3 itmospheres absolute and is expanded to 1.2 atmospheres tbsolute, whereby it is cooled to 86 K. Thereupon, the nitrogen is passed through the regenerators countercurently to the air to be cooled and cleansed, and leaves he regenerators at a temperature of 290 K.
  • a turbine by- )ass line 17 having a valve 18 positioned therein.
  • the liquid oxygen From the sump of column 5, the liquid oxygen, unler a pressure of 3.3 atmospheres absolute, flows through he conduit 19 to a pump 20 which compresses the oxygen 0 preferably 50-250 atmospheres absolute.
  • the degree of iurity of the oxygen is determined by adjusting the re- :rigeration output of the turbine.
  • the liquid level of the xygen in the sump of the column 5 can be varied by by- )ass line 22 provided with a valve 21. This line is branched )if the pressure side of the pump 20 and terminates in he sump of the column.
  • the oxygen being under a pressure of 50 atmospheres absolute downstream of the pump 20, is passed through I countercurrent heat exchanger heated by warm air.
  • the temperature of the oxygen is thereby increased from [02 K. to 276 K. From 11,000 Nm. /h. of air, there are hus obtained 1,325 Nm. /h. of high pressure gaseous )xygen.
  • the nitrogen is hereby liquefied and passed by conduits 11' and 31 by way of the countercurrent heat exchanger 8 and expansion device 7 as a reflux to the head of the low pressure column. Another part of the reflux is achieved from the head of the high pressure column by way of a control valve 32 through the line 31.
  • FIGURE 2 The other details of FIGURE 2 are analogous to FIG- URE 'l.
  • a second compressor 9 may be inserted in conduit 9 of FIGURE 1 or in conduit 9' of FIGURE 2, respectively.
  • a low temperature air rectification process for the production of high pressure gaseous oxygen which comprises passing raw air through regenerators; passing resultant cooled and cleaned air to a fractionating column; withdrawing nitrogen enriched stream from the head of the fractionating column; passing the withdrawn nitrogen through the regenerators countercurrently to the passage of the raw air; pumping liquid oxygen from the fractionating column to a higher pressure, and vaporizing resultant higher pressure liquid oxygen countercurrently to a gaseous process stream,
  • the improvement which comprises compressing said raw air to such a pressure in the range of 6-20 atmospheres absolute that said resultant cooled and cleansed air is liquefied in'indirect heat exchange as the heat source in the sump of a single column rectification column operating as said fractionating column at 2-9 atmospheres absolute, and branching a portion of the cleansed and cooled air from the regenerators countercurrently back through the regenerators to reheat said cooled and cleansed air, and employing resultant reheated air at 6-20 atmospheres absolute as said gaseous process stream to vaporize the higher pressure liquid oxygen, said higher pressure being about 40-300 atmospheres absolute.
  • the improvement which comprises passing a gaseous process stream, at 6-20 atmospheres absolute, said stream being selected from the group consisting of (a) branched, cleansed and cooled air from the regenerators, and (b) fractionation product from said fractionating column, countercurrently through the regenerators to reheat said gaseous process stream, and employing resultant reheated gaseous process stream at 6-20 atmospheres absolute to vaporize by indirect heat exchange contact the higher pressure liquid oxygen, said higher pressure being 40300 atmospheres absolute.
  • fractionating column is a double column
  • nitrogen enriched gas from the high pressure stage of the double column after being reheated is at least partly liquefied in heat exchange relationship with evaporating oxygen.
  • Apparatus for producing high pressure gaseous oxygen comprising reversible regenerators (1) including means for alternate charging thereof with air and fractionation products;
  • a compressor for compressing raw air to between 6 and 20 atmospheres absolute
  • a second conduit (4) communicative with each of said first conduits (3) downstream of said regenerators (1) and carrying a portion of said cleansed and cooled air back through said regenerators (1);
  • a heat exchanger communicative with said second conduit (4) through a third conduit (9) and with said column (5) by means of an air exit conduit (11) having an expansion valve (13) therein, said heat exchanger (10) further having countercurrent passages therein communicative with a source of higher pressure oxygen to be heated, said source including a pump (20) communicative with the sump of said fractionating column (5) for pumping liquid therefrom to a pressure of between 40 and 300 atmospheres absolute.
  • expansion valves (3, 7) disposed in said exit conduit (11) and said first conduits (3) between said countercurrent heat exchanger (8) and said column (5) for expanding fluids passing therethrough to the pressure of said column (5).
  • a process as defined by claim 1 wherein the branched portion comprises 2030% of the entire cooled and cleansed raw air.

Description

3,500,651 LOW March 17, 1970 R. BECKER PRODUCTION OF HIGH PRESSURE GASEOUS OXYGEN BY TEMPERATURE BECTIFICATION OF AIR 2 Sheets-Sheet 1 Filed Jan. 13, 1967 INVENTOR RUDOLF BECKER B '0 ATTORNEY March 17, 1970 R. BECKER 3,500,651
PRODUCTION OF HIGH PRESSURE GASEOUS OXYGEN BY Low TEMPERATURE RECTIFICATION OF AIR Filed Jan. 13,. 1967 2 Sheets-Sheet z INVENTOR RUDOLF BECKER ATTORNEY United States Patent 2,58 Int. Cl. F25j 3/04, 5/00 U.S. Cl. 62-13 21 Claims ABSTRACT OF THE DISCLOSURE System for producing high pressure gaseous oxygen by using a liquid pump to elevate pressure of oxygen, and by using such inlet raw gas pressure in conjunction with either air reheat or separation product reheat that relatively low pressure gaseous process streams can be employed to vaporize high pressure liquid oxygen.
This invention relates to the low temperature rectification of air, and in particular, to a process and apparatus for the production of gaseous high pressure oxygen, wherein the air is cooled and cleansed in regenerators and fed to a fractionating column; nitrogen is withdrawn at the head of the fractionating column and warmed in the regenerators countercurrently to the air; and liquid oxygen is pumped to the desired pressure and then vaporized countercurrently to a gaseous process stream.
There are several known processes for the production of gaseous high pressure oxygen. Thus, German Patent No. 1,103,363, for example, discloses a process wherein the liquid oxygen is withdrawn from the low pressure section of a double column and heated,by being pumped through a heat exchanger countercurrently to a stream which had been previously withdrawn from the bottom portion of the high pressure section of the column, and was reheated in regenerators (said stream having substantially the same composition as air). Processes are also known wherein the gaseous oxygen is produced under normal pressure and then compressed in the gaseous phase to the desired pressure in piston compressors.
Known processes have the disadvantage that they require either the use of expensive high pressure compressors for compressing the gaseous oxygen or, as in the apparatus according to the above-mentioned German patent, the employment of an additional high pressure cycle for the direct or indirect heating and vaporization of liquid oxygen pumped to an increased pressure.
An object of this invention, therefore, is to provide a more economical system for the production of high pressure oxygen gas.
Upon further study of the specification and claims, other objects and advantages of the present invention will become apparent.
In the drawings:
FIGURE 1 is a schematic illustration of a preferred embodiment of this invention wherein the rectification column is in the form of a single column.
FIGURE 2 is a schematic illustration of a preferred embodiment of this invention wherein the rectification column is in the form of a double column.
To attain the objects of this invention, a system is provided wherein (a) the air is compressed to such a pressure that it is liquefied in the sump of a single column rectification column in heat exchange with boiling low pressure oxygen; (b) a portion, about 20 to 30%, of the cleansed and cooled air from the regenerators is passed countercurrently and reheated in the regenerators, and is then employed for vaporizing compressed liquid oxygen; and (c) the refrigeration is provided by engine expansion of the enriched nitrogen stream from the top of the column. (In this connection, the term engine expansion refers to expansion with the production of external work.) Each of steps (a), (b) and (c) contributes to the over-all successful operation of the process, and each one separately leads to an improvement in process economics.
Alternatively, this invention also embraces the use of a double column. In this case, the nitrogen enriched fraction obtained from the air is liquefied in heat exchange with evaporating oxygen. In such a system, it can also be advantageous to pass, instead of said portion of cleansed and cooled air, a corresponding partial amount of a separation product countercurrently through the regenerators, warming the same in this manner, and then employing the heated separation product for vaporizing the high pressure oxygen.
This invention is thus characterized by the utilization of a low pressure air separation step in cooperation with steps for the production of high pressure gaseous 0 without requiring a high compression of either the air to be separated or the by-product nitrogen stream. In this connection, for the purposes of this invention, the raw air is generally compressed to from 6 to 20, preferably 9 to 12 atmospheres absolute. The air separation step for a single column rectification column is generally conducted at a pressure of 2 to 9, preferably 3 to 4 atmospheres absolute, and for a double column, a pressure of generally 6 to 20, preferably 9 to 12 atmospheres absolute in the high pressure section, and generally a pressure of 1.6 to 7, preferably 2.5 to 3.5 atmospheres absolute in the low pressure section. As for the pressure of the high pressure oxygen product, it is generally at least about 40 to 300, and preferably in the range of about 50 to atmospheres absolute.
The expansion of the nitrogen leaving the head of a single column rectifier is advantageously conducted in a turbine which is continuously under full load. The nitrogen exit temperature at the regenerators can be regulated by adjusting the throttle valve for that portion of cooled and cleansed air branched off the main air stream and recycled countercurrently through the regenerators, which throttle valve is located upstream of the rectification column.
By the present invention, it is basically possible for either the pressure of the air or the separation product used for heating, or for vaporizing and heating the oxygen, to be much below the pressure of the high pressure oxygen. In those cases, however, wherein the oxygen is to be heated to a relatively high temperature, e.g., 350 to 400 K., additional compression of the heating gas before heat exchange with the high pressure oxygen has been proven to be advantageous. In the latter case, the pressure of the heating gas is generally about 6 to 20 atmospheres absolute, whereas the air is compressed to the lower pressure of the said range.
As another feature of this invention, it has proved advantageous, for regulating the oxygen withdrawal rate, to provide a recycle line into the sump of the rectifier downstream of the pressure-elevating liquid oxygen pump.
The refrigeration energy and thusthe purity of the oxygen can be controlled by expanding the nitrogen in the turbine, by either manually or automatically adjusting the suction throttle valve of a bypass line or the turbine guide vanes. The output capacity of the oxygen pump can be regulated when operating with a variable air feed by simply controlling the liquid level of oxygen in the rectification column.
In still another feature of this invention, the nitrogen withdrawn from the head of the rectifier is used, before 3 eing expanded, for cooling the main air stream and the ecycle air stream.
A major advantage of this invention resides in the relaive simplicity and inexpensiveness of the apparatus that an be employed to carry out the process.
Referring now to the drawings in detail, air at a rate f 11,000 Nmfi/h. is compressed in compressor 1' and utroduced into cyclically switchable regenerators 1 at a emperature of 300 K. and a pressure of 10 atmospheres bsolute. This air is cooled therein to 107.5 K., thereby reezing out H and CO to form cleansed air. Downtream of the regenerator outlet, the cleansed air stream 5 branched at 2, one portion about 76.5% passing through :onduit 3 to the sump of the rectification column 5, while be other portion is recycled via the branch conduit 4, nto the regenerators 1, wherein said other portion is releated to 290 K.
In the sump of the column 5, the air in the coil 6 is ndirectly heat exchanged with the liquid fractionated vxygen product. Thereafter, the air is expanded in exansion valve 7 to the column pressure of 3.3 atmosiheres absolute.
The column is operated so that the liquid oxygen c01- ects in the bottom (sump) While the nitrogen-enriched tream is withdrawn as overhead. This nitrogen stream is lsed for subcooling the air in a countercurrent heat ex- :hanger 8, and is then passed to the expansion turbine 16 'ia conduit 14. Before entering the turbine 16, the nirogen stream is passed through countercurrent heat ex- -.hanger 15 for cooling the cleansed air before the latter s passed through the sump of the column 5.
The nitrogen enters the turbine 16 at 105 K. and 3 itmospheres absolute and is expanded to 1.2 atmospheres tbsolute, whereby it is cooled to 86 K. Thereupon, the nitrogen is passed through the regenerators countercurently to the air to be cooled and cleansed, and leaves he regenerators at a temperature of 290 K. For adusting the entrance temperature of the nitrogen before :ntering the regenerators, there is provided a turbine by- )ass line 17 having a valve 18 positioned therein.
From the sump of column 5, the liquid oxygen, unler a pressure of 3.3 atmospheres absolute, flows through he conduit 19 to a pump 20 which compresses the oxygen 0 preferably 50-250 atmospheres absolute. The degree of iurity of the oxygen is determined by adjusting the re- :rigeration output of the turbine. The liquid level of the xygen in the sump of the column 5 can be varied by by- )ass line 22 provided with a valve 21. This line is branched )if the pressure side of the pump 20 and terminates in he sump of the column.
The oxygen, being under a pressure of 50 atmospheres absolute downstream of the pump 20, is passed through I countercurrent heat exchanger heated by warm air. The temperature of the oxygen is thereby increased from [02 K. to 276 K. From 11,000 Nm. /h. of air, there are hus obtained 1,325 Nm. /h. of high pressure gaseous )xygen.
For vaporizing the oxygen in the heat exchanger 10, 2,580 Nmfi/h. of air are branched off at the cold end of the regenerators 1, at 2, warmed countercurrently to the air entering the regenerators to a temperature of 290 K., and passed to the heat exchanger 10 via conduit 9.
The air, at a pressure of 9.6 atmospheres absolute, is
cooled to 106.4" K. in the heat exchanger 10, leaves the heat exchanger 10 through conduit 11, and is liquefied in a coil 12 in the sump of the column by indirect heat exchange with liquid oxygen, where it is cooled to a temperature of l04.9 K. After further cooling in the countercurrent heat exchanger 8 by gaseous nitrogen, the air is expanded in expansion valve 13 before entering column 5.
I and warm the liquid oxygen from the low pressure colof the high pressure column is reheated in the group of regenerators 1 and used by way of line 9 to evaporate umn 5' after compression by the pump 20 to the desired pressure.
The nitrogen is hereby liquefied and passed by conduits 11' and 31 by way of the countercurrent heat exchanger 8 and expansion device 7 as a reflux to the head of the low pressure column. Another part of the reflux is achieved from the head of the high pressure column by way of a control valve 32 through the line 31.
The other details of FIGURE 2 are analogous to FIG- URE 'l.
Wherein the airis liquefied in the conduits 6 and 12 by evaporating oxygen in the sump of the single column.
If it is desired to produce relatively warm oxygen at a temperature of 350-400 K., a second compressor 9 may be inserted in conduit 9 of FIGURE 1 or in conduit 9' of FIGURE 2, respectively.
From the foregoing description, one skilled in the art can easily ascertain the essential characteristics of this invention, and without departing. from the spirit and scope thereof, can make various changes and modifications of the invention to adapt it to various usages and conditions. Consequently, such changes and modifications are properly, equitably, and intended to be, within the full range of equivalence of the following claims.
What is claimed is:
1. In a low temperature air rectification process for the production of high pressure gaseous oxygen which comprises passing raw air through regenerators; passing resultant cooled and cleaned air to a fractionating column; withdrawing nitrogen enriched stream from the head of the fractionating column; passing the withdrawn nitrogen through the regenerators countercurrently to the passage of the raw air; pumping liquid oxygen from the fractionating column to a higher pressure, and vaporizing resultant higher pressure liquid oxygen countercurrently to a gaseous process stream,
the improvement which comprises compressing said raw air to such a pressure in the range of 6-20 atmospheres absolute that said resultant cooled and cleansed air is liquefied in'indirect heat exchange as the heat source in the sump of a single column rectification column operating as said fractionating column at 2-9 atmospheres absolute, and branching a portion of the cleansed and cooled air from the regenerators countercurrently back through the regenerators to reheat said cooled and cleansed air, and employing resultant reheated air at 6-20 atmospheres absolute as said gaseous process stream to vaporize the higher pressure liquid oxygen, said higher pressure being about 40-300 atmospheres absolute. 2. A process as defined by claim 1 wherein refrigeration losses are compensated for by engine expanding said nitrogen enrich stream from the said fractionating column.
3. A process as defined by claim 1, wherein the reheated air employed for heating the higher pressure oxygen is additionally compressed within the range of 6-20 atmospheres absolute before heat exchange with the oxygen.
4. A process as defined by claim 1, wherein a portion of oxygen withdrawn from the sump of the fractionating column is branched otf downstream of the pumping zone, and .is recycled into said fractionating column.
5. A process as defined by claim 2, Wherein the nitrogen enriched stream withdrawn from the head of said fractionating column, before being engine expanded, is passed in countercurrent heat exchange relationship with air being passed to said fractionating column from the regenerators.
6. A process as defined by claim 2, wherein the nitrogen enriched stream Withdrawn from the head of said fractionating column, before being engine expanded, is passed in countercurrent heat exchange relationship with reheated air after said reheated air is employed for vaporizing the higher pressure oxygen.
7. A process as defined by claim 2, wherein the nitrogen enriched stream from the head of said fractionating column, before being engine expanded, is passed in countercurrent heat exchange relationship with (a) air being passed fro mthe regenerators to said fractionating column, and (b) reheated air after said reheated air is employed for vaporizing the high pressure oxygen.
8. In a low temperature air rectification process for the production of high pressure gaseous oxygen which comprises passing raw air through regenerators, passing resultant cooled and cleansed air to a fractionating column; withdrawing nitrogen enriched stream from the head of the fractionating column; passing the withdrawn nitrogen through the regenerators countercurrentiy to the passage of the raw air; pumping liquid oxygen from the fractionating column to a higher pressure, and vaporizing resultant higher pressure liquid oxygen countercurrently to a gaseous process stream,
the improvement which comprises passing a gaseous process stream, at 6-20 atmospheres absolute, said stream being selected from the group consisting of (a) branched, cleansed and cooled air from the regenerators, and (b) fractionation product from said fractionating column, countercurrently through the regenerators to reheat said gaseous process stream, and employing resultant reheated gaseous process stream at 6-20 atmospheres absolute to vaporize by indirect heat exchange contact the higher pressure liquid oxygen, said higher pressure being 40300 atmospheres absolute.
9. A process as defined by claim 8, wherein the fractionating column is a double column, and nitrogen enriched gas from the high pressure stage of the double column after being reheated is at least partly liquefied in heat exchange relationship with evaporating oxygen.
10. Apparatus for producing high pressure gaseous oxygen comprising reversible regenerators (1) including means for alternate charging thereof with air and fractionation products;
a compressor for compressing raw air to between 6 and 20 atmospheres absolute;
a fractionating column (5);
first conduits (3) communicating cleansed and cooled air from said regenerator (1) to said column (5);
a second conduit (4) communicative with each of said first conduits (3) downstream of said regenerators (1) and carrying a portion of said cleansed and cooled air back through said regenerators (1);
a heat exchanger communicative with said second conduit (4) through a third conduit (9) and with said column (5) by means of an air exit conduit (11) having an expansion valve (13) therein, said heat exchanger (10) further having countercurrent passages therein communicative with a source of higher pressure oxygen to be heated, said source including a pump (20) communicative with the sump of said fractionating column (5) for pumping liquid therefrom to a pressure of between 40 and 300 atmospheres absolute.
11. An apparatus in accordance with claim 10, further comprising a countercurrent heat exchanger (8), said first conduits (3) and said air exit conduit (11) passing through said countercurrent heat exchanger (8); and
expansion valves (3, 7) disposed in said exit conduit (11) and said first conduits (3) between said countercurrent heat exchanger (8) and said column (5) for expanding fluids passing therethrough to the pressure of said column (5).
12. A process as defined by claim 1 wherein said raw air is compressed to a pressure of 9l2 atmospheres absolute.
13. A process as defined by claim 1 wherein said higher pressure is 50200 atmospheres absolute.
14. A process as defined by claim 12 wherein said higher pressure is 50-200 atmospheres absolute.
15. A process as defined by claim 1 wherein said column is operated at 3-4 atmospheres absolute.
16. A process as defined by claim 14 wherein said column is operated at 3-4 atmospheres absolute.
17. A process as defined by claim 1 wherein the branched portion comprises 2030% of the entire cooled and cleansed raw air.
18. A process as defined by claim 8 wherein said process stream is at 9-12 atmospheres absolute.
19. A process as defined by claim 1 wherein said higher pressure is50200 atmospheres absolute.
20. A process as defined by claim 18 wherein said higher pressure is 50200 atmospheres absolute.
21. A process as defined by claim 8 wherein a portion of oxygen withdrawn from the sump of the fractionating column is branched off downstream of the pumping Zone, and is recycled into said fractionating column.
References Cited UNITED STATES PATENTS 2,802,349 8/1957 Skaperdas 62l8 XR 2,824,428 2/ 1958 Yendall 6241 XR 2,918,802 12/ 1959 Grunberg 6241 XR 3,034,306 5/1962 Schuftan et al. 6241 XR 3,070,966 1/ 1963 Ruhemann et a1. 6239 XR 3,086,371 4/1963 Schilling 6241 XR 3,222,878 12/1965 Becker 6241 XR 3,257,814 6/ 1966 Carbonell 6239 XR FOREIGN PATENTS 752,439 1/1953 Germany.
WHrBUR BASCOMB, JR., Primary Examiner U.S. Cl. X.R. 6229, 39, 41
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US4775399A (en) * 1987-11-17 1988-10-04 Erickson Donald C Air fractionation improvements for nitrogen production
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US4756731A (en) * 1986-02-20 1988-07-12 Erickson Donald C Oxygen and argon by back-pressured distillation
US4775399A (en) * 1987-11-17 1988-10-04 Erickson Donald C Air fractionation improvements for nitrogen production
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US5123946A (en) * 1990-08-22 1992-06-23 Liquid Air Engineering Corporation Cryogenic nitrogen generator with bottom reboiler and nitrogen expander
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US5379598A (en) * 1993-08-23 1995-01-10 The Boc Group, Inc. Cryogenic rectification process and apparatus for vaporizing a pumped liquid product
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