DE1033689B - Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process - Google Patents

Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process

Info

Publication number
DE1033689B
DE1033689B DEG21735A DEG0021735A DE1033689B DE 1033689 B DE1033689 B DE 1033689B DE G21735 A DEG21735 A DE G21735A DE G0021735 A DEG0021735 A DE G0021735A DE 1033689 B DE1033689 B DE 1033689B
Authority
DE
Germany
Prior art keywords
liquid
oxygen
evaporator
evaporated
hydrocarbon
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.)
Pending
Application number
DEG21735A
Other languages
German (de)
Inventor
Dr-Ing Ernst Karwat
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
Gesellschaft fuer Lindes Eismaschinen AG
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.)
Filing date
Publication date
Application filed by Gesellschaft fuer Lindes Eismaschinen AG filed Critical Gesellschaft fuer Lindes Eismaschinen AG
Priority to DEG21735A priority Critical patent/DE1033689B/en
Priority to DEG21772A priority patent/DE1039079B/en
Priority to US721492A priority patent/US2975606A/en
Priority to GB8972/58A priority patent/GB851619A/en
Publication of DE1033689B publication Critical patent/DE1033689B/en
Pending 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
    • F25J3/04763—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
    • F25J3/04872—Vertical layout of cold equipments within in the cold box, e.g. columns, heat exchangers etc.
    • F25J3/04878—Side by side arrangement of multiple vessels in a main column system, wherein the vessels are normally mounted one upon the other or forming different sections of the same 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
    • 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
    • F25J3/044—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
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • 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
    • F25J3/04763—Start-up or control of the process; Details of the apparatus used
    • F25J3/04769—Operation, control and regulation of the process; Instrumentation within the process
    • F25J3/04854—Safety aspects of operation
    • F25J3/0486—Safety aspects of operation of vaporisers for oxygen enriched liquids, e.g. purging of liquids
    • 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
    • F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
    • 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
    • F25J2220/00—Processes or apparatus involving steps for the removal of impurities
    • F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/50—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/02—Bath type boiler-condenser using thermo-siphon effect, e.g. with natural or forced circulation or pool boiling, i.e. core-in-kettle heat exchanger
    • 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
    • F25J2250/04—Down-flowing type boiler-condenser, i.e. with evaporation of a falling liquid film
    • 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
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/40—One fluid being 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
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/30—External or auxiliary boiler-condenser in general, e.g. without a specified fluid or one fluid is not a primary air component or an intermediate fluid
    • F25J2250/50—One fluid being oxygen
    • 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
    • Y10S62/902—Apparatus
    • Y10S62/908—Filter or absorber

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Health & Medical Sciences (AREA)
  • Emergency Medicine (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Description

DEUTSCHESGERMAN

Luftzerlegungsapparate, in denen Luft durch Verflüssigung und Rektifikation in Stickstoff und. Sauerstoff zerlegt wird, sind durch die unvermeidbare Anwesenheit von Kohlenwasserstoffen in der Luft, wie Acetylen oder Propylen, bekanntlich gefährdet. Eine der besten bekannten Maßnahmen zur Verhütung größerer Ansammlungen solcher Kohlenwasserstoffe in dem am Fuß der Zerlegungssäule den Hauptkondensator umspülenden Bad von flüssigem Sauerstoff besteht darin, die zu produzierende Sauerstoffmenge flüssig dem Bad zu entnehmen und außerhalb des Bades im Gleichstrom mit den entstehenden Dämpfen in einem Zusatzverdampfer in die Gasform überzuführen. Dieser Zusatzverdampfer besteht aus einer Reihe parallel geschalteter Rohre, die außen von unter Druck befindlichem Gas, Luft oder Stickstoff umgeben sind. Dieses Gas kondensiert und gibt dabei die zur Verdampfung des flüssigen Sauerstoffes innerhalb der Rohre notwendige Wärme ab. Die im Sauerstoff befindlichen Kohlenwasserstoffe haben weit kleinere Dampfdrücke als der Sauerstoff. Sie reichern sich demzufolge in der flüssigen Phase während des Verdampfungsvorganges an. Die Anreicherung kann so weit gehen, daß die Löslichkeit der Kohlenwasserstoffe in der Flüssigkeit überschritten wird. Dann treten Festabscheidungen auf. Doch gerade in dieser Form fester Ausscheidung haben die Kohlenwasserstoffe die höchste Explosivkraft. Für den Betrieb des Zusatzverdampfers pflegt man deshalb vorzuschreiben, daß ein kleiner Bruchteil der zu verdampfenden Flüssigkeit am unteren Ende des Zusatzverdampfers flüssig in Form einer ungesättigten Lösung entnommen wird. Sie fällt in einem dem Verdampfer nachgeO'rdneten Abscheider an, wo sie sich vom Gas trennt. Sie muß ins Freie abgeführt werden. Das bedeutet einen Verlust an Sauerstoffproduktion. Ein Verlust von 2% Sauerstoff in flüssiger Phase ist schon untragbar, weil er einen Verlust von 10% des gesamten Kälteaufwandes mit sich bringt. Der Entnahme von Flüssigkeit sind also sehr enge Grenzen (0,1 bis 1% der Sauerstoffproduktion) gesetzt. Leider ist damit die Gefährdung des Zusatzverdampfers noch nicht in allen Fällen beseitigt. Gelegentlich verlegt sich das eine oder andere der parallel geschalteten Rohre mit Wassereis oder Kohlensäureeis. Anschließend in ein solches Rohr eindringender flüssiger Sauerstoff wird in ihm total verdampft, und Kohlenwasserstoffe häufen sich in fester Form in diesem Rohr. Die Folge kann sein, daß es durch eine Kohlenwasserstoffexplosion zerstört wird und dann ständig Stickstoff in den Sauerstoff eindringt.Air separation apparatus in which air is liquefied and rectification in nitrogen and. Oxygen is broken down by its inevitable presence is known to be at risk from hydrocarbons in the air, such as acetylene or propylene. One of the best known measures to prevent the accumulation of such hydrocarbons in the bath of liquid oxygen around the main condenser at the foot of the decomposition column consists in taking the amount of oxygen to be produced in liquid form from the bath and outside of the bath in cocurrent with the resulting vapors in an additional evaporator into the gaseous form convict. This additional evaporator consists of a series of pipes connected in parallel, which are connected to the outside of surrounded by pressurized gas, air or nitrogen. This gas condenses and gives the heat necessary for the evaporation of the liquid oxygen within the tubes. The in Hydrocarbons in oxygen have far lower vapor pressures than oxygen. You enrich consequently in the liquid phase during the evaporation process. The enrichment can go so far that the solubility of the hydrocarbons in the liquid is exceeded. then solid deposits occur. But it is precisely in this form of solid excretion that the hydrocarbons have the highest explosive power. For the operation of the additional evaporator it is therefore customary to prescribe that a small fraction of the liquid to be evaporated at the lower end of the additional evaporator liquid is taken in the form of an unsaturated solution. It falls in a downstream of the evaporator Separator where it separates from the gas. It must be taken outside. That means a loss of oxygen production. A Loss of 2% oxygen in the liquid phase is already intolerable because it causes a loss of 10% of the entails the entire cooling effort. There are therefore very narrow limits to the withdrawal of liquid (0.1 to 1% of oxygen production). Unfortunately, this puts the additional evaporator at risk not yet eliminated in all cases. Occasionally one or the other of those connected in parallel is misplaced Pipes with water ice or carbonated ice. Subsequently, liquid penetrating into such a pipe Oxygen is totally evaporated in it, and hydrocarbons accumulate in solid form in it Pipe. The consequence can be that it is caused by a hydrocarbon explosion is destroyed and then nitrogen constantly penetrates the oxygen.

Die Erfindung hat zum Ziel, die Sicherheit der Handhabung des Zusatzverdampfers zu erhöhen und den Ausfall an Produktion von Sauerstoff einzu-Verfahren zum Eindampfen
kohlenwasserstoffhaltigen, flüssigenThe aim of the invention is to increase the safety of the handling of the additional evaporator and to reduce the production of oxygen by using the method for evaporation
hydrocarbon-containing, liquid

Sauerstoffes und Einrichtung
zur Durchführung des VerfahrensOxygen and establishment
to carry out the procedure

Anmelder:Applicant:

Gesellschaft für Linde's EismaschinenSociety for Linde's ice machines

Aktienges ells chaf t,
Höllriegelskreuth bei MünchenAktiengesellschaft,
Höllriegelskreuth near Munich

Dr.-Ing. Ernst Karwat, Pullach bei München,
ist als Erfinder genannt wordenDr.-Ing. Ernst Karwat, Pullach near Munich,
has been named as the inventor

schränken. Das Verfahren der Erfindung zum Eindampfen von durch Rektifikation von kohlenwasserstoffverunreinigter Luft in einer Rektifikationssäule gewonnenem kohlenwasserstoffhaltigem flüssigem Sauerstoff in einem aus einem Bündel parallel geschalteter Rohre bestehenden Verdampfer durch Wärmeaustausch mit einem außen an dem Rohrbündel kondensierenden Gas besteht darin, daß dem Verdampfer mehr flüssiger Sauerstoff zugeführt als verdampft wird und der entstehende gasförmige Sauerstoff im Gleichstrom mit der verdampfenden Flüssigkeit fließt und der nicht verdampfte Teil in das Bad von flüssigem Sauerstoff am Fuß der Rektifikationssäule zurückgeführt wird. restrict. The process of the invention for evaporating hydrocarbon contaminated by rectification Hydrocarbon-containing liquid obtained from air in a rectification column Oxygen in an evaporator consisting of a bundle of tubes connected in parallel Heat exchange with a gas condensing on the outside of the tube bundle is that of the evaporator more liquid oxygen is supplied than is evaporated and the resulting gaseous oxygen flows in cocurrent with the evaporating liquid and the non-evaporated part into the bath of liquid oxygen is returned at the foot of the rectification column.

Es ist zwar auch bekannt, mehr flüssigen Sauerstoff in einen Kondensatorverdampfer einzuleiten und den nicht verdampften Teil in das Bad von flüssigem Sauerstoff am Fuß der Rektifikationssäule zurückzuführen; hierbei werden jedoch im Kondensatorverdampfer der gasförmige und der flüssige Sauerstoff im Gegenstrom geführt.It is also known to introduce more liquid oxygen into a condenser evaporator and returning the unevaporated part to the bath of liquid oxygen at the foot of the rectification column; here, however, the gaseous and liquid oxygen in the condenser evaporator guided in countercurrent.

Im Zusatzverdampfer werden der flüssige und der gasförmige Sauerstoff im Gleichstrom bevorzugt von oben nach unten geführt. In Sonderfällen kann auch die Richtung des gleichsinnigen Stromes von verdampfender Flüssigkeit und entstehenden Dämpfen umgekehrt sein; flüssiger Sauerstoff und gasförmigerIn the additional evaporator, the liquid and gaseous oxygen are preferred in cocurrent guided up and down. In special cases, the direction of the flow in the same direction from the evaporating Liquid and resulting vapors be reversed; liquid oxygen and gaseous

Sauerstoff strömen gemeinsam von unten nach oben. Hier, am oberen Ende des Zusatzverdampfers, wird die überschüssige Flüssigkeit vom entstandenen Gas getrennt, dk Flüssigkeit zum Bad des flüssigen Sauerstoffes im Hauptkondensator zurückgeführt, derOxygen flow together from the bottom to the top. Here, at the top of the additional evaporator, is the excess liquid is separated from the resulting gas, dk liquid to the bath of the liquid Oxygen returned in the main condenser, the

809 560/147809 560/147

3 43 4

gasförmige Sauerstoff zum Wärmeaustauscher und in . soll. Die Flüssigkeit durchläuft das aus einer größeren Sonderfällen ein Teilstrom in die Gasphase über dem Zahl parallel geschalteter Rohre bestehende Rohr-Sumpf der Trennsäule. bündel 10 und wird im Abwärtsströmen von der Im stetigen Betrieb des Lufttrenners wird ihm mit außen am Rohrbündel kondensierten Luft verdampft, der Luft ständig eine gewisse Menge von Kohlen- 5 wobei die Dämpfe im Gleichstrom mit der Flüssigwasserstoffen zugeführt. Im Beharrungszustand muß keit stehen. Ein nicht verdampfter Überschuß von IG die gleiche Menge von Kohlenwasserstoffen aus dem bis 30% der Flüssigkeit trennt sich im Abscheider 14 Trenner heraus z. B. mit dem gasförmigen Sauerstoff von dem bei 15 abziehenden gasförmigen Sauerstoff, abgeführt werden. Damit die im Beharrungszustand verläßt bei 16 den Abscheider 14 und wird von der nötige Konzentration eines Kohlenwasserstoffes im io Pumpe 17 über den mit Silicagel gefüllten Adsorber abziehenden gasförmigen Sauerstoff erreicht werden 18 bei 19 zur Hauptmenge des flüssigen Sauerstoffes kann, muß in der mit der Gasphase im Gleichgewicht im Bad 3 zurückgeführt. Während des Verdampf ens stehenden Flüssigkeit der Kohlenwasserstoff min- im Rohrbündel 10 geht ein Teil der in der Flüssigkeit destens die Gleichgewichtskonzentration annehmen. enthaltenen Kohlenwasserstoffe in die Gasphase, und Bei jedem Kohlenwasserstoff besteht ein für ihn 15 der Gehalt der Flüssigkeit an Kohlenwasserstoffen charakteristisches Verhältnis seiner Konzentration in steigt während des Eindampfens an, wobei in erster der flüssigen Phase im Gleichgewicht zur Konzen- Annäherung bezüglich des'Verhältnisses der Konzentration in der Gasphase. Bei einem schwer verdampf- tration des Kohlenwasserstoffes in der Gasphase zur baren Kohlenwasserstoff, z. B. Propylen, ist diese Konzentration des Kohlenwasserstoffes in der flüs-Verhältniszahl sehr hoch. Der Beharrungszustand 20 sigen Phase Gleichgewicht angestrebt wird. Im würde erst erreicht, wenn im flüssigen Sauerstoff des Adsorber 18 werden die in der Flüssigkeit angerei-Bades und des Verdampferkreislaufes der Kohlen- cherten Kohlenwasserstoffe durch Adsorption an wasserstoff auf eine sehr hohe Konzentration ange- Silicagel gebunden. Nach dem Verlassen des reichert würde.. Dies kann aus Gründen der Sicherheit Adsorbers enthält die rückkehrende Flüssigkeit nur unerwünscht sein. Daher wird nach einem weiteren 25 noch Spuren von Kohlenwasserstoffen. Der Adsorber Erfindungsschritt der dem Zusatzverdampfer entnom- 18 wird zweckmäßig, wenn er beladen ist, durch Ermene Überschuß von Flüssigkeit mit einem Adsorp- wärmen unter gleichzeitigem Durchspülen von bei 20 tionsmittel von Kohlenwasserstoffen befreit, ehe er in zugeführtem und bei 21 abgeführtem trockenen Gas, den Hauptkondensator zurückgeführt wird. Als z. B. Stickstoff, von den aufgenommenen Kohlen-Adsorptionsmittel eignet sich z. B. Silicagel. 30 Wasserstoffen befreit. Während dieser Zeit geht die Der Anhäufung eines Kohlenwasserstoffes kann Flüssigkeit bei geschlossenen Ventilen 24 und 25 von auch dadurch entgegengewirkt werden, daß in an sich der Pumpe 17 über den Umgang 22 bei 19 zum Bad 3. bekannter Weise eine sehr kleine Menge des verun- Am Abscheider 14 kann bei 16 eine kleine Menge reinigten Sauerstoffes flüssig aus dem Abscheider kohlenwasserstoffreiche Flüssigkeit über Ventil 23 nach außen abgeführt wird. Im Maße, in dem solche 35 ins Freie abgelassen werden, um die Reinigung des Schritte der Reinigung des Kreislaufes wirksam sind, Kreislaufes zu unterstützen.gaseous oxygen to the heat exchanger and in. target. The liquid passes through this from a larger one Special cases a partial flow into the gas phase over the number of parallel connected pipes existing pipe sump the separation column. bundle 10 and is in the downward flow of the In continuous operation of the air separator is evaporated with the air condensed on the outside of the tube bundle, the air constantly contains a certain amount of carbon, the vapors being in cocurrent with the liquid hydrogen fed. There must be speed in a steady state. An unevaporated excess of IG the same amount of hydrocarbons from which up to 30% of the liquid separates in the separator 14 Separator out z. B. with the gaseous oxygen from the gaseous oxygen withdrawn at 15, be discharged. So that the steady-state leaves the separator 14 at 16 and is of the necessary concentration of a hydrocarbon in pump 17 via the adsorber filled with silica gel withdrawing gaseous oxygen can be achieved 18 at 19 to the main amount of liquid oxygen can, must be returned to the bath 3 in equilibrium with the gas phase. During evaporation Standing liquid of the hydrocarbon min- in the tube bundle 10 is part of the in the liquid at least assume the equilibrium concentration. hydrocarbons contained in the gas phase, and For every hydrocarbon there is what is for it the hydrocarbon content of the liquid characteristic ratio of its concentration in increases during evaporation, being in the first place the liquid phase in equilibrium with the concentration approximation with respect to the ratio of the concentration in the gas phase. In the case of difficult evaporation of the hydrocarbon in the gas phase to cash hydrocarbon, e.g. B. propylene, this concentration of the hydrocarbon is in the flüs ratio very high. The steady state 20 sigen phase equilibrium is sought. in the would only be achieved when the liquid oxygen of the adsorber 18 is in the liquid anerei bath and the evaporation circuit of the carbon-based hydrocarbons by adsorption Hydrogen bound to a very high concentration of silica gel. After exiting the would enrich .. This may be for safety reasons the adsorber only contains the returning liquid be undesirable. Therefore, after another 25, there will still be traces of hydrocarbons. The adsorber Invention step which is taken from the additional evaporator 18 is expedient, if it is loaded, by Ermene Excess of liquid with an adsorption heating with simultaneous flushing of at 20 hydrocarbons are removed from the medium before it is converted into dry gas that is fed in and discharged at 21, the main capacitor is fed back. As z. B. nitrogen, from the absorbed carbon adsorbent is suitable e.g. B. silica gel. 30 hydrogen liberated. During this time the The accumulation of a hydrocarbon can remove liquid with valves 24 and 25 closed can also be counteracted by the fact that in per se the pump 17 via the bypass 22 at 19 to the bath 3. As is known, a very small amount of the contaminated At the separator 14 can be a small amount at 16 purified liquid oxygen from the separator, hydrocarbon-rich liquid via valve 23 is discharged to the outside. To the extent that such 35 are drained into the open in order to clean the Circulatory purification steps are effective to support circulatory system.

braucht der gasförmige Sauerstoff dann nur noch In der Fig. 2 ist ein Gleichstromverdampfer geeinen Teil der mit der Luft eingeführten Kohlen- zeigt, welcher von dem zu verdampfenden Sauerstoff Wasserstoffe abzuführen. Bei der Ausführung des von unten nach oben durchströmt wird. In der Figur Verfahrens der Erfindung kann natürlich auch von 40- bezeichnen gleiche Zahlen die gleichen Teile und Mitteln Gebrauch gemacht werden, welche in der gleiche Funktionen der Apparatur wie in der Fig. 1. Technik bereits üblich sind, um die in der Luft ent- Es wird daher davon abgesehen, ihre Bedeutung nochhaltenen Kohlenwasserstoffe von der Hauptrektifi- mais zu beschreiben. Abweichend von dem bei Fig. 1 kationssäule fernzuhalten, z. B. selbstreinigende geschilderten Verfahren wird hier bei 30 aus dem Regeneratoren für die Kühlung und Reinigung der 45 Bad des Hauptkondensators mit der Pumpe 31 eintretenden Luft oder Silicageladsorber im Weg der flüssiger Sauerstoff in einer den zu verdampfenden flüssigen Luft von der Drucksäule zur Niederdruck- Sauerstoff übersteigenden Menge entnommen, dem säule eines Doppelsäulenrektifikators. senkrecht stehenden Rohrbündel 32 des Zusatzver-the gaseous oxygen then only needs. In FIG. 2, a direct-current evaporator is used Part of the coal introduced with the air shows which of the oxygen to be evaporated Discharge hydrogen. In the execution of the flow from bottom to top. In the figure The method of the invention can of course also from 40- denote the same numbers the same parts and Means are used, which in the same functions of the apparatus as in Fig. 1. Technology are already common to those in the air. It is therefore refrained from maintaining their importance Describe hydrocarbons from the main rectific maize. Deviating from that in FIG. 1 keep away cation column, z. B. self-cleaning described method is here at 30 from the Regenerators for cooling and cleaning the 45 bath of the main condenser with the pump 31 incoming air or silica gel adsorber in the way of the liquid oxygen in one of the to be evaporated liquid air taken from the pressure column to the low pressure oxygen excess amount, the column of a double column rectifier. vertical tube bundle 32 of the additional

Das Verfahren wird im folgenden an Beispielen dampfers 33 von unten zugeführt und dort ein der und den Fig. 1 und 2 erläutert. Die im nicht gezeigten 50 produzierten Sauerstoff menge gleicher Teil durch die Wärmeaustausch mit ihren Zerlegungsprodukten Kondensation von Luft verdampft, welche bei 34 in Sauerstoff und Stickstoff abgekühlte kohlenwasser- den Zusatzverdampfer gasförmig eintritt, bei 26 total stoffhaltige Luft tritt bei 1 vor die Zerlegungsappa- verflüssigt den Zusatzverdampfer verläßt und mit ratur und teilt sich dort in zwei Ströme, deren einer Ventil 27 in die obere Säule 2 entspannt wird, in der Rohrschlange 4 des am Fuß der Rektifikations- 55 Die produzierte Menge gasförmigen Sauerstoffes säule 2 befindlichen Verdampferkondensators 3 kon- verläßt den Zusatzverdampfer 33 bei 38 über das densiert, vom Ventil 5 aus auf den Kopf der Säule 2 Ventil 39. Der unverdampfte Überschuß an flüssigem entspannt und auf den Böden 6 der Rektifikations- Sauerstoff verläßt den Zusatzverdampfer 33 und geht säule in flüssigen Sauerstoff im Bad 3 und gasförmig über das Ventil 35 durch den Adsorber 36, um dann am Kopf der Säule bei 7 abziehenden Stickstoff zer- 60 gereinigt bei 37 in das Bad des flüssigen Sauerstoffes legt wird. Etwa der fünfte Teil der kohlenwasserstoff- im Hauptkondensator 3 zurückzukehren. Bezüglich haltigen Luft wird bei 8 abgezweigt und dem Zusatz- der Reinigung, die im Adsorber 36 eintritt, gilt das verdampfer 9 zugeführt, wo er sich an der Außenseite gleiche wie an Hand der Fig. 1 vom Adsorber ausdes von flüssigem Sauerstoff durchströmten Rohr- gesagte und ebenso für die in der Fig. 2 am Adsorber bündeis 10 verflüssigt, bei 11 entnommen und über 65 36 nicht dargestellten Maßnahmen zur Desorption des das Ventil 12 auf den Kopf der Säule 2 entspannt Adsorbers.In the following, the process is carried out using examples steamer 33 from below and one of the there and Figs. 1 and 2 explained. The amount of oxygen produced in not shown 50 by the same part Heat exchange with their decomposition products evaporates condensation of air, which at 34 in Oxygen and nitrogen cooled hydrocarbons enter the additional evaporator in gaseous form, at 26 total Substantial air occurs at 1 before the decomposition apparatus liquefies it leaves the additional evaporator and with it temperature and divides there into two streams, one of which is a valve 27 in the upper column 2, in the coil 4 of the at the foot of the rectification 55 The amount of gaseous oxygen produced column 2 located evaporator condenser 3 kon- leaves the additional evaporator 33 at 38 via the condensed, from valve 5 to the top of column 2 valve 39. The unevaporated excess of liquid relaxed and on the bottoms 6 of the rectification oxygen leaves the additional evaporator 33 and goes column in liquid oxygen in the bath 3 and gaseous via the valve 35 through the adsorber 36 to then At the top of the column at 7 nitrogen is removed, 60 purified at 37 in the bath of liquid oxygen is laying. About the fifth part of the hydrocarbon return in the main condenser 3. In terms of Containing air is branched off at 8 and the additional cleaning that occurs in the adsorber 36 applies Evaporator 9 supplied, where it is the same on the outside as shown in FIG. 1 from the adsorber ausdes the pipe through which liquid oxygen flows, and also for those in FIG. 2 on the adsorber Bündeis 10 liquefied, removed at 11 and over 65 36 measures not shown for desorption of the the valve 12 on the head of the column 2 relaxes adsorber.

wird. Dem Bad von flüssigem Sauerstoff im Haupt- Die Zusatzverdampfer gemäß den Figuren könnenwill. The bath of liquid oxygen in the main The additional evaporator according to the figures can

kondensator 3 wird bei 13 ein z. B. um 10 bis 50% auch so betrieben werden, daß in ihnen mehr als die oder noch größeres Gewicht an flüssigem Sauerstoff ent- produzierte Sauerstoff menge vergast wird, im Grenznommen, als gasförmiger Sauerstoff erzeugt werden 70 fall so, daß zusammen mit der zu erzeugenden auchCapacitor 3 is at 13 a z. B. be operated by 10 to 50% so that in them more than that or even greater weight of liquid oxygen, the amount of oxygen produced is gasified, in the limit, can be generated as gaseous oxygen 70 in such a way that together with the oxygen to be generated as well

die zur Rektifikation erforderliche Sauer stoff menge entsteht. Der Überschuß des Vergasten über die Produktion wird dann im Fall der Fig. 2 über das Ventil 40 bei 41 in die Rektifikationssäule 2 eingeführt. Unter solchen Bedingungen muß die bei 30 entnommene Menge flüssigen Sauerstoffes nicht nur um den unverdampft gebliebenen Teil der Flüssigkeit größer sein als die Menge des produzierten Sauerstoffes, sondern auch um den Betrag an gasförmigem Sauerstoffweicher bei 41 in die Rektifikationssäule zurückgeführt wird. Tn den in dem Beispiel genannten Zahlen soll keine Beschränkung für den Flüssigkeitsüberschuß mitgesprochen sein. Es steht im Rahmen des Erfindunggedankens jedem frei, auch kleineren oder größeren Überschuß an Flüssigkeit zirkulieren zu lassen, z. B. das Dreifache der Sauerstoffproduktion.the amount of oxygen required for rectification arises. The excess of gasification over production is then in the case of FIG. 2 via the valve 40 introduced into rectification column 2 at 41. Under such conditions, the one removed at 30 must The amount of liquid oxygen is not only larger by the part of the liquid that has not evaporated be softer than the amount of oxygen produced, but also by the amount of gaseous oxygen at 41 is returned to the rectification column. Tn the numbers given in the example no restriction for the excess of liquid should be included. It is part of the According to the invention, everyone can circulate freely, even a smaller or larger excess of liquid let, e.g. B. three times the oxygen production.

Üblicherweise wird Luft in einer Drucksäule vorzerlegt und in einer mit Drucksäulenstickstoff beheizten Niederdrucksäule zu Ende rektifiziert. Wird der Erfindungsgedanke in einem solchen System angewendet, so werden die Zusatzverdampfer 9 bzw. 33 ebenso wie das Bad des flüssigen Sauerstoffes in 3 nicht mit Luft, sondern mit kondensierendem Drucksäulenstickstoff beheizt.Usually air is pre-separated in a pressure column and heated in one with pressure column nitrogen Low pressure column rectified to the end. If the idea of the invention is applied in such a system, the additional evaporators 9 and 33 as well as the bath of liquid oxygen in FIG heated not with air, but with condensing pressure column nitrogen.

Der technische Fortschritt des neuen Verfahrens liegt in der erhöhten Sicherheit von Rektifiziersäule und Zusatzverdampfer durch die kräftigere Durchspülung des Verdampfers mit flüssigem Sauerstoff und durch die reinigende Wirkung des Adsorbers im Verdampferkreislauf.The technical progress of the new process lies in the increased safety of rectifying columns and additional vaporizer by flushing the vaporizer more vigorously with liquid oxygen and the cleaning effect of the adsorber in the evaporator circuit.

Claims (5)

Patentansprüche:Patent claims: 1. Verfahren zum Eindampfen von durch Rektifikation mit kohlenwasserstoffverunreinigter Luft in einer Rektifikationssäule gewonnenem kohlenwasserstoffhaltigem flüssigem Sauerstoff in einem aus einem Bündel parallel geschalteter Rohre bestehenden Verdampfer durch Wärmeaustausch mit einem außen an dem Rohrbündel kondensierenden Gas, dadurch gekennzeichnet, daß dem Verdampfer mehr flüssiger Sauerstoff zugeführt als verdampft wird und der entstehende gasförmige Sauerstoff im Gleichstrom mit der verdampfenden Flüssigkeit fließt und der nicht verdampfte Teil in das Bad von flüssigem Sauerstoff am Fuß der Rektifikationssäule zurückgeführt wird.1. Process for the evaporation of air polluted by rectification with hydrocarbons Hydrocarbon-containing liquid oxygen obtained in a rectification column in one consisting of a bundle of tubes connected in parallel by exchanging heat with the evaporator a gas condensing on the outside of the tube bundle, characterized in that the evaporator more liquid oxygen is supplied than is evaporated and the resulting gaseous oxygen flows in cocurrent with the evaporating liquid and the non-evaporated part flows into the Bath of liquid oxygen is returned at the foot of the rectification column. 2. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß während des Emdampfens flüssiger und gasförmiger Sauerstoff von oben nach unten fließen.2. The method according to claim 1, characterized in that liquid during the vaporization and gaseous oxygen flow from top to bottom. 3. Verfahren nach Anspruch 1, dadurch gekennzeichnet, daß während des Emdampfens flüssiger und gasförmiger Sauerstoff von unten nach oben fließen.3. The method according to claim 1, characterized in that liquid during the vaporization and gaseous oxygen flow from bottom to top. 4. Verfahren nach Anspruch 1 bis 3, dadurch gekennzeichnet, daß der nicht verdampfte Teil mit einem Adsorptionsmittel von Kohlenwasserstoffen befreit wird, ehe er in den Kondensatorverdampfer der Rektifikationssäule zurückgeführt wird.4. The method according to claim 1 to 3, characterized in that the non-evaporated part with an adsorbent is freed from hydrocarbons before entering the condenser evaporator the rectification column is returned. 5. Einrichtung zur Durchführung des Verfahrens nach Anspruch 1 bis 4 mit Zusatzgleichstromverdampfer für den produzierten Sauerstoff mit angeschlossenem Abscheider zum Trennen von gasförmigem Sauerstoff und unverdampfter Flüssigkeit, gekennzeichnet durch eine Pumpe, die den Flüssigkeitsrest dem Abscheider entnimmt und zur Rektifikationssäule drückt, und einen Adsorber zum Reinigen des Flüssigkeitsrestes.5. Device for performing the method according to claim 1 to 4 with an additional direct current evaporator for the oxygen produced with a connected separator to separate gaseous oxygen and non-evaporated liquid, characterized by a pump that removes the liquid residue from the separator and to the rectification column presses, and an adsorber for cleaning the liquid residue. Hierzu 1 Blatt Zeichnungen1 sheet of drawings © 809 560/147 7.58© 809 560/147 7.58
DEG21735A 1957-03-20 1957-03-20 Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process Pending DE1033689B (en)

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DEG21735A DE1033689B (en) 1957-03-20 1957-03-20 Process for evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process
DEG21772A DE1039079B (en) 1957-03-20 1957-03-26 Process for the evaporation of hydrocarbon-containing liquid oxygen and device for carrying out the process
US721492A US2975606A (en) 1957-03-20 1958-03-14 Procedure for the vaporization of liquid oxygen which contains hydrocarbons
GB8972/58A GB851619A (en) 1957-03-20 1958-03-20 Improvements in or relating to the rectification of air

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