DE821655C - Process for purifying air during its decomposition - Google Patents

Process for purifying air during its decomposition

Info

Publication number
DE821655C
DE821655C DEP41854A DEP0004185A DE821655C DE 821655 C DE821655 C DE 821655C DE P41854 A DEP41854 A DE P41854A DE P0004185 A DEP0004185 A DE P0004185A DE 821655 C DE821655 C DE 821655C
Authority
DE
Germany
Prior art keywords
liquid
pressure column
decomposition
air
impurities
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.)
Expired
Application number
DEP41854A
Other languages
German (de)
Inventor
Philipp Borchardt
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 DEP41854A priority Critical patent/DE821655C/en
Priority to GB29264/49A priority patent/GB663346A/en
Application granted granted Critical
Publication of DE821655C publication Critical patent/DE821655C/en
Expired legal-status Critical Current

Links

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
    • F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
    • F25J3/04242—Cold end purification of the feed air
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—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
    • 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94—Details relating to the withdrawal point
    • 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
    • F25J2205/30—Processes or apparatus using other separation and/or other processing means using a washing, e.g. "scrubbing" or bubble column for purification purposes
    • 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
    • F25J2220/40—Separating high boiling, i.e. less volatile components from air, e.g. CO2, hydrocarbons
    • 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
    • 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
    • F25J2250/42—One 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
    • 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
    • F25J2250/52—One fluid being oxygen enriched compared to air, e.g. "crude oxygen"

Landscapes

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

Description

Es ist durch das Patent 634 202 ein Verfahren bekanntgeworden, wonach durch zweistufige Rektifikation zu zerlegende Luft zwecks vollständiger Ausscheidung leicht kondensierbarer Dämpfe, wie Kohlendioxyd, zwischen Kälteaustauscher und Zerlegungsapparat durch einen Abscheider geführt wird. Die Luft wird zu diesem Zweck durch eine vornehmlich aus flüssigem Sauerstoff bestehende Flüssigkeit geleitet und diese Flüssigkeit darauf von den abgeschiedenen festen Kondensaten durch Filtration getrennt und in die Niederdrucksäule zwecks weiterer Trennung durch Rektifikation eingeführt. Nach der Erfindung wird die in der Drucksäule gewonnene sauerstofffreie Flüssigkeit zu einem kleineren Teil zur Vorwäsche der Luft durch Bullerung oder Berieselung verwendet. Die verunreinigte Waschflüssigkeit wird jedoch nicht durch Filtration gereinigt, sondern direkt oder nach weitgehender Eindampfung abgeführt, während die bei der Eindampfung entwickelten Dämpfe in die Niederdrucksäule eingeführt werden und die Hauptmenge der in der Drucksäule gebildeten Flüssigkeit frei von Verunreinigungen zwecks weiterer Zerlegung direkt in die Niederdrucksäule geführt wird. Der wesentliehe Unterschied gegenüber dem bekannten Verfahren liegt also in der Teilung der Flüssigkeit aus der Drucksäule in einen kleineren Teil, der zur Waschung der eintretenden Luft dient und nach etwaiger Eindampfung abgelassen wird, sowie in einen Hauptteil, der frei von Verunreinigungen direkt auf die Niederdrucksäule zwecks weiterer Rektifikation aufgegeben werden kann. Je nach der Menge der für die Vorwäsche verwendeten Flüssigkeit kann man dieselbe direkt abführen, falls ihr Anteil an der Gesamtflüssigkeit klein ist, oder man kann sie in an sich bekannter Weise, z. B. im Austausch mit kondensierendem Stickstoff, in einem sog. Zusatzkondensator eindampfen, die Dämpfe in die obere Säule einspeisen und den nicht verdampften Rest ins Freie lassen. In diesem Rest sind die Verunreinigungen angesammelt und werden laufend abgeführt. Der Vorteil dieser Anordnung beruht vor allem auf einer Erhöhung der Sicherheit der Anlage, da im Sauerstoff auch öl- und Acetylenspuren angereichert werden, die im Gegensatz zu dem bekannten Verfahren laufend aus dem Apparat entfernt werden und nicht in den eigentlichen Trennungsapparat hineingelangen, so daß dieser ungefährdet betrieben werden kann.A process has become known through patent 634 202, according to which by two-stage rectification Air to be separated for the purpose of complete elimination of easily condensable vapors, such as Carbon dioxide, passed through a separator between the cold exchanger and the decomposition apparatus will. For this purpose, the air is replaced by a predominantly liquid oxygen Liquid passed and this liquid then from the separated solid condensate by filtration separated and introduced into the low pressure column for further separation by rectification. According to the invention, the oxygen-free liquid obtained in the pressure column becomes one A smaller part is used to pre-wash the air by means of bulling or sprinkling. The polluted However, washing liquid is not cleaned by filtration, but directly or after extensive cleaning Evaporation discharged, while the vapors developed during evaporation into the low pressure column are introduced and most of the liquid formed in the pressure column free of Impurities is passed directly into the low-pressure column for the purpose of further decomposition. The essential one The difference compared to the known method lies in the division of the liquid the pressure column into a smaller part, which is used to wash the incoming air, and after any evaporation is drained, as well as in a main part that is free from impurities can be applied directly to the low-pressure column for the purpose of further rectification. Depending on the The amount of liquid used for the prewash can be drained off directly if you Proportion of the total liquid is small, or you can do it in a known manner, for. B. in exchange with condensing nitrogen, evaporate in a so-called additional condenser, the vapors in feed the upper column and let the unevaporated remainder outside. In this rest they are Impurities accumulate and are continuously removed. The advantage of this arrangement is based on above all to increase the safety of the system, since there are also traces of oil and acetylene in the oxygen are enriched, which, in contrast to the known method, are continuously removed from the apparatus and not get into the actual separation apparatus, so that it is safe can be operated.

Die Anordnung sei durch ein Beispiel (s. Abbildung) beschrieben. In Gegenströmern abgekühlte Luft wird in eine Drucksäule 1 bei 32 in einen besonderen Flüssigkeitssammelraum 3 unterhalb eines zweiten Flüssigkeitsraumes 4 eingeführt, wobei sie durch einen Verteiler 5 durch die im Raum 3 befindliche Flüssigkeit geführt oder durch eine Brause 6 mit Flüssigkeit aus dem Raum 4 berieselt wird. Die gewaschene und von Verunreinigungen befreite Luft wird durch das Rohr 8 (mit Schutzdach 7) in die eigentliche Drucksäule 1 eingeführt, wo sie nunmehr einer Vorzerlegung durch Berieselung mit Stickstoff unterzogen wird. Die Hauptmenge der in 4 angesammelten sauerstoffreichen Flüssigkeit wird über das Ventil 9 in die Niederdrucksäule 2 bei 10 entspannt und hier in reinen Sauerstoff und reinen Stickstoff zerlegt. Der Sauerstoff 13 wird bei 12 flüssig oder bei 11 gasförmig entnommen. Der Stickstoff zieht bei 14 gasförmig ab. Die verunreinigte Waschflüssigkeit wird bei 15 aus dem Vorraum 3 entnommen und entweder ins Freie geführt (über Ventil 16) oder über Ventil 17 bei 31 in einen Zusatzkondensator 18 geführt und hier verdampft, wobei die entstehenden Dämpfe im Gleichstrom mit der Restflüssigkeit durch die Rohre 19 strömen, bei 20 entnommen und nach Entspannung über Ventil 21 bei 22 in die obere Säule eingeführt werden. Die nicht verdampfte Flüssigkeit 33,wird über Ventil 23 zusammen mit den darin suspendierten Verunreinigungen abgeführt. Die Verdampfung erfolgt im Austausch mit Stickstoff, der gasförmig unter Druck aus dem Kondensator 24 entnommen und bei 25 in den Zusatzkondensator eingeführt wird. Der gebildete flüssige Stickstoff wird über Ventil 26 entnommen und nach Entspannung und Vereinigung mit der über Ventil 27 bei 28 aus der Drucksäule entnommenen Hauptmenge des flüssigen Stickstoffs bei 29 flüssig zur Berieselung der oberen Säule aufgegeben. Die Dosierung der für die Vorwäsche in Raum 3 aus Raum 4 abgezweigten Flüssigkeit kann über das Ventil 30 erfolgen. Ist dieses geschlossen, wird lediglich die überschüssige Flüssigkeit über den oberen Rand von Durchlaß 8 aus Raum 4 in den Raum 3 abgeführt.The arrangement is described using an example (see figure). Cooled in countercurrents Air is in a pressure column 1 at 32 in a special liquid collecting space 3 below one second liquid space 4 introduced, wherein it is located in space 3 through a distributor 5 through Liquid guided or sprinkled with liquid from space 4 through a shower 6 will. The washed and contaminated air is passed through the pipe 8 (with protective roof 7) is introduced into the actual pressure column 1, where it is now pre-decomposed by sprinkling is subjected to nitrogen. The main amount of the oxygen-rich accumulated in 4 Liquid is expanded through the valve 9 into the low-pressure column 2 at 10 and here in pure oxygen and pure nitrogen are broken down. The oxygen 13 becomes liquid at 12 or gaseous at 11 taken. The nitrogen is withdrawn in gaseous form at 14. The contaminated washing liquid will taken at 15 from the vestibule 3 and either out into the open (via valve 16) or via valve 17 at 31 in an additional capacitor 18 and evaporated here, with the resulting vapors flowing through the tubes in cocurrent with the residual liquid 19 flow, taken at 20 and after relaxation via valve 21 at 22 in the upper column to be introduced. The non-evaporated liquid 33 is via valve 23 together with the therein discharged suspended impurities. The evaporation takes place in exchange with nitrogen, which is taken in gaseous form under pressure from the condenser 24 and at 25 in the additional condenser is introduced. The liquid nitrogen formed is withdrawn via valve 26 and after expansion and union with the main amount withdrawn from the pressure column via valve 27 at 28 abandoned liquid nitrogen at 29 liquid to irrigate the upper column. the Dosing of the liquid diverted from room 4 for the pre-wash in room 3 can be done via the Valve 30 take place. If this is closed, only the excess liquid is over the upper edge of passage 8 discharged from space 4 into space 3.

Claims (1)

PATENTANSPRUCH:PATENT CLAIM: Verfahren zur Reinigung von Luft bei deren Zerlegung durch Tiefkühlung und zweistufige Rektifikation, wobei die Luft zwischen Kälteaustauscher und Zerlegungsapparat zwecks Abscheidung von mitgeführten Verunreinigungen durch einen mit Flüssigkeit aus der Drucksäule gefüllten Abscheider geführt wird, dadurch gekennzeichnet, daß die in der Drucksäule gewonnene sauerstoffreiche Flüssigkeit zu einem kleineren Teil zur Vorwäsche der Luft durch Bullerung oder Berieselung verwendet wird, daß die verunreinigte Waschflüssigkeit direkt oder nach weitgehender Eindampfung abgeführt, dabei entwickelter Dampf in die obere Säule eingeführt wird und daß die Hauptmenge der in der Drucksäule gebildeten Flüssigkeit frei von Verunreinigungen vom Boden der Drucksäule in die Niederdrucksäule zwecks weiterer Zerlegung geführt wird.Process for purifying air during its decomposition by freezing and two-stage Rectification, with the air between the cold exchanger and the decomposition apparatus for the purpose of separation of impurities carried along by a liquid from the pressure column filled separator is performed, characterized in that the obtained in the pressure column oxygen-rich liquid to a smaller extent to pre-wash the air Bullerung or sprinkling is used that the contaminated washing liquid directly or removed after extensive evaporation, with the vapor developed in the process in the upper Column is introduced and that the majority of the liquid formed in the pressure column free of impurities from the bottom of the pressure column in the low pressure column for the purpose further decomposition is carried out.
DEP41854A 1949-05-05 1949-05-05 Process for purifying air during its decomposition Expired DE821655C (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
DEP41854A DE821655C (en) 1949-05-05 1949-05-05 Process for purifying air during its decomposition
GB29264/49A GB663346A (en) 1949-05-05 1949-11-15 Improvements in or relating to the separation of air

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DEP41854A DE821655C (en) 1949-05-05 1949-05-05 Process for purifying air during its decomposition

Publications (1)

Publication Number Publication Date
DE821655C true DE821655C (en) 1951-11-19

Family

ID=6589237

Family Applications (1)

Application Number Title Priority Date Filing Date
DEP41854A Expired DE821655C (en) 1949-05-05 1949-05-05 Process for purifying air during its decomposition

Country Status (2)

Country Link
DE (1) DE821655C (en)
GB (1) GB663346A (en)

Also Published As

Publication number Publication date
GB663346A (en) 1951-12-19

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