US1967718A - Apparatus for purifying liquefied gases - Google Patents

Apparatus for purifying liquefied gases Download PDF

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Publication number
US1967718A
US1967718A US672191A US67219133A US1967718A US 1967718 A US1967718 A US 1967718A US 672191 A US672191 A US 672191A US 67219133 A US67219133 A US 67219133A US 1967718 A US1967718 A US 1967718A
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US
United States
Prior art keywords
condenser
column
liquid
gas
chamber
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 - Lifetime
Application number
US672191A
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English (en)
Inventor
Walter F Moeller
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 Air Products Co
Original Assignee
Linde Air Products Co
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
Priority to FR754118D priority Critical patent/FR754118A/fr
Priority claimed from US607032A external-priority patent/US1967717A/en
Priority to GB6554/33A priority patent/GB416051A/en
Application filed by Linde Air Products Co filed Critical Linde Air Products Co
Priority to US672191A priority patent/US1967718A/en
Application granted granted Critical
Publication of US1967718A publication Critical patent/US1967718A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures

Definitions

  • This invention relates to a process and appafor carrying out the process of the present ratus for purifying liquefied gases, for example, invention;' and liquid oxygen, nitrogen, and the like, which are Fig. 2 is a view mainly in vertical section produced in a manufacturing cycle, where they showing a gas production apparatus incorpo 5 are generally contaminated with undesirable rating purifying apparatus arranged for the 55 impurities and has for its main object an impractice of the present invention. proved procedure whereby such impurities are In the commercial production of a purified readily and expeditiously removed.
  • the invention relates to the are substantially completely removed, the puriprovision of suitable steps for concentrating unfi n may e accompli h d with the Xp n- 60 desired impurities occurring in the production i re of relat v ly li le ner y y taking the of liquefied gases of the character indicated in gas m a i e qu d phase d treating it a manner in the cycle of production such that y the p of Partial evaporation to produce the impurities may be separated readily by metWO p s a d t en p at the P chanlcal means, whereby a gas product i fithis process being generically set forth in the o5 nally obtained in the liquid phase from which appending pp io fil d in h n m f substantially all impurities afe practically com- Lawrence J Bowditch O April 1932, Serial pletely removed
  • Another object is to produce a liquefied gas i those impurities which occur in relatively small a purified condition with an expenditure of a amounts in liq d ga uch a liquid r, 70 relatively small amount of additional energy and Oxygen, Carbon d n the like, th e at relatively little additional cost, tration being such that they do not materially still another object is to separate the desired change the il p i f the liquefied gas, liquefied gas from the undesired impurity by but are otherwise objectionable and impair the 25 the step either of partial evaporation or partial Commercial q t es o t e gas p od 75 condensation and thereafter causing the gas e e a e ce t type of impurities 00mmaterial to revert to the liquid phasewith an mohly i p a d W the gas material, on expenditure of a relatively small amount of account of the source from which the gas
  • the invention accordingly com rises the sevm er l con inin the un ired impuri y in so eral steps and the relation of one or more of a single phase by the step of fractional evaps h steps with respect to each of th thers, oration or condensation under conditions of a d th apparatus embodying features of m temperature and pressure where the vapor presstruction, combinations of elements and aru e o t p y is of a negligible va ue.
  • A denotes generally apart of the apparatus into which the gas material in liquid phase that is to be purified is passed and caused to evaporate partially by the application of heat
  • B denotes a second part serving to condense the vapor produced in part A, which is conducted thereto and recondensed by bringing it into thermal contact with a fluid of lower temperature than the condensing temperature of the gasimaterial being purified.
  • the vaporizing portion of part A consists of a vessel 10 having an inlet conduit 11 for the liquefied gas, an outlet conduit 12 for the vapor, and a drain conduit 13 with a control valve 13.
  • a suitable heating means for example a coil 14 provided with inlet and outlet connections adapted to be supplied with a heating agent.
  • This agent may be any convenient vehicle that will pass without difiiculty at the low operating temperatures here employed, for example, compressed air.
  • the vapor outlet conduit 12 surrounds the inlet conduit 11 in order to effect heat exchange and separation of the liquid from the gas phase; the vapor thus separated being led.
  • the condenser shown in connection with part B consists of an upper header 15 and a lower header 16 connected by condenser tubes 17.
  • the conduit 12 is here shown as discharging the vapor to be condensed into the upper header 15, while a conduit 18 is connected to the lower header to withdraw the reliquefied gas.
  • the condenser is disposed within a chamber 19 having inlet and outlet conduits 20' and 21, respectively, for the purpose of circulating a cooling medium, for example, liquefied oxygen, or a cold gaseous material that may be a by-product drawn from another part of the manufacturing cycle; the cooling medium carrying away the heat from the condenser so that re-liquefaction is readily accomplished in the condenser.
  • a cooling medium for example, liquefied oxygen, or a cold gaseous material that may be a by-product drawn from another part of the manufacturing cycle
  • the vapor is conducted through conduit 12 into the condenser at its upper header 15 whence it passes into the tubes 17 and is condensed because it loses heat through the tube walls to the fluid of lower temperature surrounding the tubes.
  • the liquefied gas collects in the lower header 16 from which it is withdrawn through conduit 18 in a purified state.
  • a heat interchanger for the manufacture of liquefied oxygen is modified and arranged to separate out the impurities which have relatively high boiling points and are in general inflammable, and then recondense the purified oxygen in order to supply it in the liquid phase.
  • a conduit 25 provided with an expansion valve 26 is arranged to supply compressed air drawn from a suitable high pressure source to the rectifying column shown generally at 27.
  • This rectifying column is provided with a kettle or evaporator 28 at its. lower end and a condenser 29 at its upper end.
  • a conduit 30 provided with an expansion valve 31 and distributor 32 is arranged to draw liquid from the evaporator 28 and'to discharge it into the upv per portion of a second rectifying column 33 disposed above the column 27 and arranged to be in heat exchanging relation with the condenser 29.
  • Each of these columns is provided with suitable counter-current contact cooling means, for example, a series of perforated trays,
  • the evaporator 28 associated with the column 27 is provided with suitable heating means, for example, a heating coil as.
  • a tray 27" arranged to collect the condensate which drips from the condenser 29 and to convey the same to a conduit 34 having a controlling valve 35 and a distributor 36 discharging into the top of the column 33, the distributor 36 being preferably disposed above the distributor 32.
  • a gas withdrawal'conduit 3'? which is arranged for withdrawing non-corrdensible vapors, while a liquid withdrawal conduit 38 is arranged to withdraw liquid from the base of the column 33 from about the condenser 29.
  • liquid collecting in the vaporator 28 Gas or vapor rising through the column 27 passes into the condenser 29 where the less volatile portion is recondensed to produce a'refiux in the column 27.
  • Liquid nitrogen collects in the tray 27'-, whereas the liquid in the evaporator 28 comprises a relatively large percentage of liquid oxygen. Any non-condensible vapor that is more volatile than liquid nitrogen or oxygen is withdrawn through the conduit 37; Liquefied gas comprising mainly liquid oxygen and the impurities of relatively high melting point are withdrawn through the conduit 30 and introduced into the column 33 through the distributor 32.
  • a second condenser shown generally at 4,0 is incorporated at a convenientpoint in the column 33.
  • This condenser comprises upper and lower portions 41 and 42, connected by an intermediate portion 43.
  • One or more passages or fiues 44 are associated with the condenser in order to establish communication between the space above the condenser with the space below; a
  • the chamber for this condenser being preferably provided in the column by means of a partition 45 disposed transversely in the column below the condenser and a second partition 46, which The partition 46 is provided with one or more passages 47 that permits communication with the flues 44 so as to establish communication in the column 33 for the space on the two sides of the condenser chamber containing condenser 40.
  • the partition 46 is also provided with one or more liquid drains 48 which allow liquid to drain from the partition into the chamber about the condenser 40.
  • Gaseous oxygen to be recondensed and which has been evaporated by the condenser 29 is led from a point near the lower end of the column 33 from the chamber about the condenser 29 by means of a conduit 50 and passed into the portion 41 of condenser 40.
  • liquid oxygen collects in a purified state and is withdrawn from the lower portion 42 through a conduit 51.
  • the heat absorbed from the condenser 29 in effecting refrigeration for the column 27 vaporizes a portion of the liquid which is now a high concentrate of liquid oxygen contaminated with the impurities of relatively high melting point.
  • the oxygen vaporized in this chamber is substantially pure oxygen gas which is withdrawn through the conduit 50 and passed into the condenser 41, where it is recondensed by the heat abstracted by the liquid in the chamber about the condenser 41.
  • liquefied oxygen in the purified state desired collects in the portion 42 and is withdrawn by the conduit 51.
  • the liquid which collects in the chamber about the condenser 41 is seen to comprise a mixture of oxygen and nitrogen in the liquid phases, together with any substances that may be present either as solids or in solution.
  • the vaporization which takes place in this chamber is of a fractional nature, the more volatile nitrogen being boiled oil and passed up through the fiues 47 into the upper portion of the column 33.
  • This liquid nitrogen is seen to be supplied to the column ma nly from the conduit 34; thus the cooling of the condenser 41 is seen to be accomplished by means of a cooling agent that is withdrawn from another portion of the cycle of production.
  • the vaporized nitrogen is seen to pass from the top of the column 33 in the usual manner.
  • the agents here used for heating the liquid in the evaporators and for extracting heat from the vapor in the condensers, in order to conserve energy, are thus with advantage both taken from some other portions of the cycle of production, and since no change has occurred therein other than a change in the quantity of absorbed heat, they may be returned, if desired, to the cycle substantially without loss.
  • a rectification column having an inlet by which gas material in the liquid phase is introduced and an evaporator adjacent the lower end, of counter-current gas and liquid contactmeans in said column between said inlet and said evaporator, said rectificaton column being provided with a chamber to which a refrigerating agent is admitted from another part of the system, a condenser disposed in said chamber and spaced from the walls thereof, means for supplying a gas fraction drawn from said evaporator to said condenser, and means for withdrawing the con densation product directly from said condenser to a point on the exterior of said column.
  • a rectification column having an inlet by which gas material substantially in the liquid phase is introduced, an evaporator at its lower end and a condenser at its upper end, of a second rectification column having its lower end connected to be in heat exchanging relation with the fiuid in said con denser, a connection leading from said first rectification column and discharging into the second near the upper end thereof, an auxiliary condenser located within said second rectification column exposed to a refrigerating agent and spaced from the column walls, a connection arranged to supply a gas fraction withdrawn from said second rectification column to said auxiliary condenser which is distilled off by the heat of said first condenser, and a withdrawal connection for withdrawing the condensate from said auxiliary condenser.
  • a rectification column having an inlet by which gas material substantially in the liquid phase is introduced, an evaporator at its lower end and a condenser at its upper end, of a second rectification column having its lower end connected to be in heat exchanging relation with said condenser and a connection for receiving liquid at its upper end which is withdrawn from said evaporator, said second rectification column being formed with a chamber at a point intermediately of its ends, a second condenser disposed within and spaced from the walls of said chamber, means for supplying a refrigerating agent to said chamber, means for supplying a gas fraction distilled from said second rectification column to said second condenser whereby a purified liquefied gas is collected in said second condenser, and means for directly withdrawing the collected condensate from said second condenser.
  • a rectification column having an inlet by which gas material in the liquid phase is introduced near the upper end and an evaporator adjacent the lower end, of countercurrent contact means in said column between said inlet and said evaporator, perforated partitions located so as to interrupt the regular occurrence of said counter-current contact means at an intermediate point and providing a chamber within said rectification column, a condenser disposed within and spaced from the walls of said chamber, the perforations in said partitions being arranged for admitting a refrigerating agent to said chamber, means for supplying a gas fraction drawn from said evaporator to said condenser, and means for withdrawing the condensation product from said condenser.
  • a rectification column having an inlet by which gas material in the liquid phase is introduced near the upper end and an evaporator adjacent the lower end, of countercurrent contact means in said column between said inlet and said evaporator, perforated partitions interrupting said counter-current contact means at an intermediate point to provide a chamber within said rectification column, a condenser within and spaced from the walls of said chamber, pipe connections for leading a gas fraction directly from said evaporator to said condenser, means for withdrawing the condensation product from said condenser, the perforations in said partitions admitting the passage of liquefied gas material drawn from an upper part of the column as the refrigerating agent to said chamber, and means for withdrawing said gas material when the refrigerating efiect is spent and returning the same to another part of said rectification column.

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • Thermal Sciences (AREA)
  • General Engineering & Computer Science (AREA)
  • Separation By Low-Temperature Treatments (AREA)
US672191A 1932-04-23 1933-05-22 Apparatus for purifying liquefied gases Expired - Lifetime US1967718A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
FR754118D FR754118A (fr) 1932-04-23
GB6554/33A GB416051A (en) 1932-04-23 1933-03-03 Improvements in or relating to processes of and apparatus for purifying liquefied gases
US672191A US1967718A (en) 1932-04-23 1933-05-22 Apparatus for purifying liquefied gases

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US607032A US1967717A (en) 1932-04-23 1932-04-23 Process for purifying liquefied gases
US672191A US1967718A (en) 1932-04-23 1933-05-22 Apparatus for purifying liquefied gases

Publications (1)

Publication Number Publication Date
US1967718A true US1967718A (en) 1934-07-24

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US672191A Expired - Lifetime US1967718A (en) 1932-04-23 1933-05-22 Apparatus for purifying liquefied gases

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US (1) US1967718A (fr)
FR (1) FR754118A (fr)
GB (1) GB416051A (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3484233A (en) * 1966-10-14 1969-12-16 Chlormetals Inc Process and apparatus for separating metals by distillation
CN114057252A (zh) * 2021-12-07 2022-02-18 天华化工机械及自动化研究设计院有限公司 改善精对苯二甲酸装置脱水塔水质的系统及其方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3484233A (en) * 1966-10-14 1969-12-16 Chlormetals Inc Process and apparatus for separating metals by distillation
CN114057252A (zh) * 2021-12-07 2022-02-18 天华化工机械及自动化研究设计院有限公司 改善精对苯二甲酸装置脱水塔水质的系统及其方法
CN114057252B (zh) * 2021-12-07 2024-05-03 天华化工机械及自动化研究设计院有限公司 改善精对苯二甲酸装置脱水塔水质的系统及其方法

Also Published As

Publication number Publication date
FR754118A (fr) 1933-10-31
GB416051A (en) 1934-09-03

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