CN103988037B - Air separating method and device - Google Patents

Air separating method and device Download PDF

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Publication number
CN103988037B
CN103988037B CN201280059867.3A CN201280059867A CN103988037B CN 103988037 B CN103988037 B CN 103988037B CN 201280059867 A CN201280059867 A CN 201280059867A CN 103988037 B CN103988037 B CN 103988037B
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Prior art keywords
stream
oxygen
distillation column
liquid
nitrogen
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CN103988037A (en
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H.E.霍瓦尔德
M.R.怀特
T.J.伯格曼
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Praxair Technology Inc
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Praxair Technology Inc
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Priority claimed from US13/311,038 external-priority patent/US20130139546A1/en
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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
    • F25J3/04006—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
    • F25J3/04006—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
    • F25J3/04103—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 using solely hydrostatic liquid head
    • 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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • 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
    • F25J3/04193—Division of the main heat exchange line in consecutive sections having different functions
    • F25J3/04206—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product
    • F25J3/04212—Division of the main heat exchange line in consecutive sections having different functions including a so-called "auxiliary vaporiser" for vaporising and producing a gaseous product and simultaneously condensing vapor from a column serving as reflux within the or another 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
    • F25J3/04151—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
    • F25J3/0423—Subcooling of liquid process streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—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
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • 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.
    • F25J3/04884—Arrangement of reboiler-condensers
    • 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
    • F25J2205/00—Processes or apparatus using other separation and/or other processing means
    • F25J2205/02—Processes or apparatus using other separation and/or other processing means using simple phase separation in a vessel or drum
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/42—Nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/50—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
    • F25J2240/00—Processes or apparatus involving steps for expanding of process streams
    • F25J2240/40—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval
    • F25J2240/44—Expansion without extracting work, i.e. isenthalpic throttling, e.g. JT valve, regulating valve or venturi, or isentropic nozzle, e.g. Laval 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
    • 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
    • F25J2270/00—Refrigeration techniques used
    • F25J2270/02—Internal refrigeration with liquid vaporising loop

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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)

Abstract

A kind of method and apparatus producing oxygen and nitrogen joint product, wherein by the compressed and air stream cooling of purification, completely or partially compresses, then carries out rectification in main distillation column to form nitrogen rich vapor overhead and thick liquid oxygen.Thick liquid oxygen stream is reduced pressure, then strips to produce oxygen enriched liquid to thick liquid oxygen stream with stripping gas in auxiliary distillation column.In the future the nitrogen rich vapor overhead of autonomous distillation column be used for being formed nitrogen product and make thick liquid oxygen partial gasification to produce stripping gas, by remaining oxygen enriched liquid and liquid nitrogen reflux to main distillation column.By providing heat exchange duty in the condensation of the air stream of compressed and purification or by being concentrated in the nitrogen rich vapor used in the backflow of main distillation column, and formed oxygen product by remaining oxygen enriched liquid.

Description

Air separating method and device
Invention field
The present invention relates to a kind of method and apparatus for separating air, wherein produce nitrogen product by compressed and purification air being carried out rectification in main distillation column, and produce oxygen product by the thick liquid oxygen formed in main distillation column being stripped in auxiliary distillation column, thus produce the oxygen product as joint product (co-products) and nitrogen product.
Background of invention
Generally, by frequently with the low temp air fractionation system of simple distillation tower from air separating off nitrogen, and obtain nitrogen with high-purity.In such a device, then air compression is removed higher impurity to produce the air stream of compressed and purification.Then inside main heat exchanger, compressed and purification air stream is cooled to be suitable for the temperature of its cryogenic rectification, is then introduced under about 3 bars or higher pressure the single distillation column of operation.Rectification is carried out, to produce nitrogen rich vapor overhead and to be referred to as the oxygen enriched liquid bottoms of thick liquid oxygen or still liquid at the air within distillation column.Oxygen enriched liquid is reduced pressure by expansion valve, is then introduced into heat exchanger so that the condensation of nitrogen rich vapor column overhead stream, thus produces the liquid nitrogen refluxed in a distillation column.The oxygen enriched liquid being partially vaporized may be used for being formed the refrigeration for equipment, or alternatively by liquid nitrogen being added to king-tower or making stream entrance main heat exchanger can provide refrigeration to equipment.
Generally, from this single column nitrogen equipment, oxygen is not reclaimed.But, there is also the interest reclaiming oxygen from this equipment.Such as, float glass typically requires flow-rate ratio and is of about nitrogen and the low purity oxygen of 2:1.Utilize oxygen to improve the response rate and the low-purity typically requiring between 90 and 95% and the oxygen of the pressure between 10 and 20 psig in glass furnace.Although single Vacuum pressure swing adsorption equipment can be utilized or by making the evaporation of the situ liquid of conveying provide this oxygen, but the expense increased is irrational.It should be pointed out that, can typically have high-pressure tower and the double-tower air separation equipment of lower pressure column and produce oxygen and nitrogen to utilize in the way of operationally relevant to heat transfer relation.But, due to requirement and the higher initial capital cost (such as producing float glass) of product compression, thus this equipment is uneconomic.Amendment to the increase of the little single column nitrogen equipment for exporting nitrogen and oxygen product can meet the requirement of technique economically, such as float glass, wherein needs to provide nitrogen and oxygen product with (nitrogen of e.g., less than 100 standard cubic foots/hour (kcfh)) under the flow of appropriateness under stress.
In the prior art, exist and be modified and the example of the single column nitrogen equipment of coproduction nitrogen and oxygen product.Such as, at US In 4,783,210, in the heat exchanger of stream condensation for making produced nitrogen rich vapor overhead in a distillation column, thick liquid oxygen tower base stream part is made to evaporate.The nitrogen-rich liquid formed is for refluxing in a distillation column.Then, the stream of the gained liquid phase produced by thick liquid oxygen partial gasification is carried out stripping to produce rich oxygen containing bottoms in two grades or auxiliary distillation column, oxygen product at the bottom of this tower, can not be taken as.Making auxiliary distillation column reboiling by another nitrogen enriched vapor stream, this nitrogen enriched vapor stream condenses and can be taken as liquid nitrogen product in reboiling and is also used for refluxing in a distillation column.
US Disclosing a kind of single column nitrogen-making device in 5,074,898, auxiliary distillation column produces oxygen product.In this patent, in auxiliary distillation column, thick liquid oxygen stream produced in main distillation column is stripped.The stream utilizing the nitrogen rich vapor overhead produced in main distillation column makes auxiliary distillation column reboiling.Thus make nitrogen rich vapor condensation thus be formed at the backflow in main distillation column.The remaining liq produced in auxiliary distillation column can be taken as fluid product together with the condensed nitrogen steam of part.
In above-mentioned two patent, it is used for bottoms making nitrogen condense, it is necessary under the pressure less than nitrogen, complete nitrogen condensation.As a result, oxygen product is also at low-pressure state.Additionally, because the bottoms of part is taken as product, so the less tower bottom liquid for making nitrogen condense will be there is.Therefore, nitrogen yield is restricted.As being discussed below, the present invention provides a kind of for producing nitrogen and the method and apparatus of oxygen joint product, except further advantage, the method and device allow to produce at an elevated pressure oxygen product.In another aspect of this invention, stand-by still substrate through stage evaporation it is thus possible to obtain bigger oxygen mark with the energy consumption less than technique employed in prior art.
Summary of the invention
The present invention provides a kind of and separates to produce oxygen and the method for nitrogen co-product by air.According to this method, carry out cooling down and rectification by compressed and purification the aeriferous stream of bag, to produce nitrogen rich vapor overhead and thick liquid oxygen inside main distillation column.By at least in part the thick liquid oxygen stream being made up of thick liquid oxygen being reduced pressure, with the stripping gas risen, thick liquid oxygen stream is stripped inside auxiliary distillation column, and make oxygen enriched liquid part evaporate by carrying out indirect heat exchange with the nitrogen enriched vapor stream being made up of nitrogen rich vapor overhead, and inside auxiliary distillation column, produce oxygen enriched liquid and the auxiliary overhead containing the oxygen not less than 5.0 volume %.As a result, liquid nitrogen stream, stripping gas and remaining oxygen enriched liquid are thus produced.Reflux in main distillation column with at least part of liquid nitrogen stream.The phrase " at least in part " used with claim herein represents and can be for further processing produce oxygen enriched liquid and assist overhead inside auxiliary distillation column.As described hereinafter, although stand-by still can be used only for stripping thick liquid oxygen stream, but it can be used for by nitrogenous produced by above-mentioned stripping and oxygen steam carry out rectification with improve oxygen reclaim.
Make remaining oxygen-rich liquid stream by partial gasification by the gaseous flow exchanged heat indirectly of remaining oxygen-rich liquid stream with the nitrogen concentration with the nitrogen concentration not less than air, and formed oxygen-rich steam fraction by remaining oxygen enriched liquid.Formed oxygen product stream by vapor fraction, nitrogen rich vapor form nitrogen product stream, the auxiliary overhead of auxiliary distillation column form waste stream.Oxygen product stream, nitrogen product stream and waste stream and compressed and purification stream is made to carry out indirect heat exchange.
As may be appreciated from be discussed above, because of by correspondingly being formed oxygen product stream by vapor fraction produced by remaining oxygen enriched liquid, so the production of oxygen product no longer with for main distillation column backflow nitrogen production occur directly contact, because the nitrogen rich vapor that remaining oxygen enriched liquid is not used for making autonomous distillation column condenses.As a result, the nitrogen backflow that the removal of remaining oxygen enriched liquid does not reduce to main distillation column does not the most reduce nitrogen yield, such as situation of the prior art.
It addition, because remaining oxygen enriched liquid is not used for making nitrogen condense, it is possible to produce this liquid at elevated pressures.
As set forth above, it is possible to only produce auxiliary overhead by thick liquid oxygen stream being stripped inside auxiliary distillation column.Alternatively, reflux in main distillation column with the liquid nitrogen stream of part.In the latter case, inside auxiliary distillation exhausting section of column, thick liquid oxygen stream is stripped and strips generation containing nitrogen and the steam stream of oxygen.Reflux in rectifying section by the steam conductance containing nitrogen and oxygen being entered rectifying section and the therefore use another part liquid nitrogen stream that refluxes in auxiliary distillation column, and inside the auxiliary distillation column in being positioned at the rectifying section of the auxiliary distillation column above stripping section, the steam stream containing nitrogen and oxygen is carried out rectification.This effect be by effectively fetter the oxygen within the waste stream that otherwise will escape out stand-by still improve within remaining oxygen enriched liquid oxygen reclaim.
In either case, oxygen enriched liquid can be collected in the inside of auxiliary distillation column.Oxygen enriched liquid part is made to evaporate by once-through heat exchanger by making oxygen-rich liquid stream and nitrogen enriched vapor stream to form stripping gas and the remaining oxygen enriched liquid collected as the bottoms of auxiliary distillation column.
Gaseous flow can be compressed and purification stream.Compressed and purification stream is partly condensed within the condenser and is collected in separation container by remaining oxygen-rich liquid stream.The liquid phase stream being made up of the liquid phase produced inside separation container imported condenser and makes liquid phase stream part evaporate within the condenser by carrying out indirect heat exchange with the stream of compressed and purification, thus being produced two phase flow by liquid phase stream.This two phase flow is imported separation container and inside separation container, makes liquid phase and the vapor phase separation of two phase flow, to form oxygen-rich steam fraction and the liquid phase stream together with the residue oxygen enriched liquid being collected in separation container.Then, by discharging the stream of oxygen-rich steam fraction from separation container, and oxygen product stream is formed.
In above-mentioned embodiment of the present invention, condenser may be located at the air making condensation in main distillation column bottom zone and mixes with the liquid phase by declining produced by rectification, thus produces the thick liquid oxygen as bottoms in main distillation column.Furthermore, it is possible to reflux in main distillation column with the liquid nitrogen stream of part, and waste stream and thick liquid oxygen stream exchanged heat indirectly are so that before depressurizing by thick liquid oxygen stream sub-cooled.
As being formed the replacement of gaseous flow by compressed and purification stream, gaseous flow can be made up of nitrogen rich vapor overhead.In this embodiment, by will be enriched in the stream decompression of liquid oxygen and making in the inside of thermosyphon reboiler remaining oxygen-rich liquid stream and gaseous flow carry out indirect heat exchange, and between remaining oxygen-rich liquid stream and gaseous flow exchanged heat indirectly.Produce vapor fraction from there through the part evaporation of residue oxygen-rich liquid stream and produce condensation liquid stream by the condensation of gas stream.This condensed fluid conductance is become owner of distillation column as the backflow together with liquid nitrogen stream.
In the above-described embodiment, before being reduced pressure by thick liquid oxygen stream, waste stream can be with thick liquid oxygen stream generation indirect heat exchange so that by thick liquid oxygen stream sub-cooled.
In any embodiment of the present invention, can be by the pressurization of remaining oxygen-rich liquid stream also oxygen product stream to be pressurizeed.Additionally, liquid nitrogen refrigerating conductance is become owner of distillation column to freeze.
The present invention also provides for a kind of for separating air to produce oxygen and the device of nitrogen joint product.This device includes main heat exchanger, main distillation column and auxiliary distillation column.Main heat exchanger is configured to be cooled down compressed and purification the aeriferous stream of bag；Main distillation column is configured to compressed and purification stream carry out rectification to produce nitrogen rich vapor overhead and thick liquid oxygen.Auxiliary distillation column is connected to main distillation column, and it is configured to inside auxiliary distillation column with the stripping gas risen, the thick liquid oxygen stream being made up of thick liquid oxygen be stripped, and at least partially due to the stripping of thick liquid oxygen stream is produced oxygen enriched liquid and the auxiliary overhead containing the oxygen not less than 5.0 volume %.Expansion valve is between main distillation column and auxiliary distillation column, in order to reduced pressure by thick liquid oxygen stream before importing auxiliary distillation column.
Provide a mean for and carried out indirect heat exchange by the formed nitrogen enriched vapor stream of nitrogen rich vapor overhead and make oxygen enriched liquid part evaporate, thus producing liquid nitrogen stream, stripping gas and the device of remaining oxygen enriched liquid.Oxygen enriched liquid part vaporising device is connected to main distillation column, in order to reflux in main distillation column with at least part of liquid nitrogen stream.Main heat exchanger is connected to main distillation column and auxiliary distillation column so that the nitrogen product stream formed by nitrogen rich vapor and by the auxiliary waste stream that formed of overhead of auxiliary distillation column and the compressed and air stream exchanged heat indirectly of purification.Also provide for between remaining oxygen-rich liquid stream and the gaseous flow of the nitrogen concentration with the nitrogen concentration not less than air indirectly exchanged heat to make the device that remaining oxygen-rich liquid stream part is evaporated.Further it is provided that for the device being formed oxygen-rich steam fraction after part evaporation by remaining oxygen-rich liquid stream.Main heat exchanger is connected to oxygen-rich steam fraction and forms device, main distillation column and auxiliary distillation column, in order to the nitrogen product stream by the oxygen product stream of oxygen-rich steam fractional composition, being made up of nitrogen rich vapor overhead inside main heat exchanger and the waste stream being made up of the auxiliary overhead of auxiliary distillation column and the compressed and stream generation indirect heat exchange of purification.
Stand-by still can only possess thick liquid oxygen stream is carried out steam stripped stripping section.As a replacement, stand-by still can possess stripping section and be positioned at the rectifying section above stripping section.In the latter case, in auxiliary distillation exhausting section of column, carry out the stripping of thick liquid oxygen stream and in stripping section, produce the steam stream entering the nitrogenous and oxygen for the rectifying section that the steam stream of nitrogenous and oxygen is carried out rectification.Thering is provided this rectification, the oxygen thus increased in residue oxygen enriched liquid reclaims.Oxygen enriched liquid part vaporising device is connected to main distillation column, to reflux in main distillation column with the liquid nitrogen stream of part, oxygen enriched liquid part vaporising device is also connected to assist distillation column to make auxiliary distillation column therefore reflux in rectifying section with the liquid nitrogen stream of another part.Another expansion valve is between oxygen enriched liquid part vaporising device and auxiliary distillation column, in order to the pressure drop of the liquid nitrogen stream of another part as little as assists the pressure of distillation column.
In any embodiment of the present invention, auxiliary distillation column can possess the device for collecting oxygen enriched liquid.Oxygen enriched liquid part vaporising device is once-through heat exchanger, this heat exchanger be connected to assist distillation column and oxygen enriched liquid collection device with will pass through make the oxygen-rich liquid stream being made up of oxygen enriched liquid by and make oxygen enriched liquid part evaporate inside once-through heat exchanger, and remain oxygen enriched liquid and collect as assisting distillation column bottoms.Main distillation column is connected to once-through heat exchanger, in order to nitrogen enriched vapor stream condensed inside once-through heat exchanger.
Gaseous flow can be compressed and purification air stream.In this case, remaining oxygen-rich liquid stream heat-exchange device and oxygen-rich steam fraction form device is condenser and separation container.Condenser is connected to main heat exchanger so that by compressed and purification stream partial condensation.Separation container is connected to assist distillation column so that remaining oxygen-rich liquid stream collects in separation container.Separation container is connected to condenser, in order to the two phase flow being imported in separation container with generation by the liquid phase stream part evaporation formed in internal the produced liquid phase of separation container within the condenser.Making the liquid phase of two phase flow and vapor phase separation to form oxygen-rich steam fraction and liquid phase inside separation container, main heat exchanger is connected to separation container to be formed oxygen product stream by oxygen-rich steam fraction.
In the embodiment of the invention described above, condenser may be located in the bottom zone of main distillation column in case the air of condensation with by the stream of compressed and purification being carried out the liquid mixing of the produced decline of rectification, using generation as the thick liquid oxygen of the bottoms in main distillation column.Additionally, once-through heat exchanger may be coupled to main distillation column, in order to reflux in main distillation column with the liquid nitrogen stream of part.Sub-cooled heat exchanger is connected to once-through heat exchanger, auxiliary distillation column and expansion valve, in order in internal waste stream and the thick liquid oxygen stream exchanged heat indirectly of sub-cooled heat exchanger, and by thick liquid oxygen stream sub-cooled before by expansion valve.
As a replacement, gaseous flow can be made up of nitrogen rich vapor.In this case, residue oxygen-rich liquid stream heat-exchange device and oxygen-rich steam fraction form device is to be made up of the thermosyphon reboiler with housing.Housing is connected to stand-by still to receive remaining oxygen-rich liquid stream, another expansion valve between housing and stand-by still so that remaining oxygen-rich liquid stream is reduced pressure.Thermosyphon reboiler is connected to main distillation column to receive gaseous flow, from there through carrying out indirect heat exchange with residue oxygen-rich liquid stream, gaseous flow is condensed, thus form oxygen-rich steam fraction and using condensation liquid stream as the reflux withdrawal together with liquid nitrogen stream to main distillation column in enclosure interior.Main heat exchanger is connected to housing, main distillation column and auxiliary distillation column, so as the oxygen product stream formed by vapor fraction, the nitrogen product stream formed by nitrogen rich vapor overhead, the auxiliary overhead produced in the middle of auxiliary distillation column the waste stream formed is all in the inside of main heat exchanger and the compressed and stream generation indirect heat exchange of purification.
In the above-described embodiment, sub-cooled heat exchanger is at auxiliary distillation column, between main distillation column and main heat exchanger, in order to waste stream and thick liquid oxygen stream generation indirect heat exchange before the waste stream before the decompression of thick liquid oxygen stream and in heating main heat exchanger.
In any embodiment of the present invention, main distillation column can possess for importing liquid nitrogen refrigerating stream to give the top inlet of refrigeration.
Accompanying drawing is sketched
Although the present invention is with it is manifestly intended that applicant is considered the claim of the theme of its invention for terminating, it is generally understood that be better understood with the present invention when read in conjunction with the accompanying drawings, wherein:
Fig. 1 is the schematic diagram for implementing the air separation equipment according to the inventive method.
Fig. 2 is the schematic diagram of an alternate embodiments for implementing the air separation equipment according to the inventive method.
Fig. 3 is the schematic diagram of another alternate embodiments for implementing the air separation equipment according to the inventive method.
Describe in detail
With reference to Fig. 1, it is shown that can coproduction oxygen and nitrogen product (" N2" and " O2") air separation equipment 1.
Saturated or approximate saturated in the case of compressed and purification air stream 10 is cooled to be suitable in main heat exchanger 12 temperature of its rectification.As will be appreciated, air separation equipment 1 can be the part needing compressed-air actuated device, therefore can be formed compressed and purification air stream 10 by partial air produced in this device.Alternatively, then this stream can be formed to being purified at the air of cryogenic temperature solidification or the higher impurity (such as carbon dioxide, steam and hydro carbons) concentrated by air being compressed to usual pressure between 70 psia to 90 psia.Main heat exchanger 12 can have the brazed aluminum plate fin structure of routine.As will be appreciated by one of skill in the art, main heat exchanger 12 can be made up of multiple unit of parallel work-flow.
After cooled, compressed and purification air stream 10 is imported the condenser 14 in the base area 16 being positioned at main distillation column 18.Distillation column 18 is containing mass transfer contact elements, and such as column plate, structured packing, random packing or the combination of this element, these elements generally represent with reference number 20.Preferably, partly condensing to produce vapor fraction 22 by the air of entrance inside condenser 14, this vapor fraction 22 ascends into mass transfer contact elements 20 and contacts with the liquid phase of the decline producing nitrogen rich vapor overhead 23.Nitrogen rich vapor overhead 23 is typically the purest nitrogen.The partial condensation of air produces liquid distillate 24, and this liquid distillate constitutes the entrance air of about 20% and collects together with as the liquid declined inside the contact element 20 in the base area 16 of main distillation column 18 of thick liquid oxygen 26.
It should be pointed out that, for making the substituted device of the air setting of entrance that condenser 14 will be made to be positioned at the outside of main distillation column 18.Together with this device, can individually by liquid distillate 24 and the liquid mixing that declined inside distillation column 20 to form thick liquid oxygen 26 or can be by they sub-cooled and be added separately in tower 34.In another this device, compressed and purification air stream can be introduced directly into main distillation column housing.Air will be allowed to and the steam within tower and carry out the recirculation steam 22 of condenser 14 and mix.In such configuration, condenser will not have condensation side house steward, the most only makes gas inflow heat exchanger by condensation.Substitute as another, the cooled air stream 10 of a part can be guided the housing to tower 18, and utilize pipeline that portion of air stream 10 is directly delivered to condenser 14.This structure will allow to be adjusted product oxygen stream and nitrogen stream.But, this structure will may require that extra valve and controls device.Another device will use the independent air stream that can be further compressed.If this single air stream is further compressed, will be separated at fire end, if or be not compressed, separated at cold end.Then, it will by this air stream total condensation inside condenser 14.It is then passed through suitable pipeline and condensed air is imported the intersegmental position of main distillation column 18.Condensed air will not be collected in the storage tank of this tower, but is joined several sections from the bottom up of main distillation column 14 by liquefied air.
Then, preferably in the inside of sub-cooled heat exchanger 30, the thick liquid oxygen stream 28 being made up of thick liquid oxygen 26 is carried out sub-cooled, thick liquid oxygen stream 28 is decompressed to the pressure of preferably 15 to 25 psia by the expansion valve 32 between main distillation column 18 and stand-by still 34.Then, thick liquid oxygen stream 28 is stripped inside auxiliary distillation column 34 by making this stream contact in mass transfer contact elements 36 with the stripping air-flow 52 of rising；Mass transfer contact elements 36 can be column plate, structured packing, random packing or the combination of this element.Stripping produces auxiliary overhead 38, and this distillation 38 usually contains the residue oxygen enriched liquid 56 of the nitrogen between 80 volume % to 90 volume % and the oxygen usually containing 85 volume % to 98 volume %.
Oxygen enriched liquid 40 can be collected in inside or the similar device of collecting column plate 42, wherein collect the liquid quilt of decline and allow the steam risen pass through and enter mass transfer contact elements 36.By carrying out indirect heat exchange with by the formed nitrogen enriched vapor stream of nitrogen rich vapor 23 46 within once-through heat exchanger 48, and make the stream part evaporation of the oxygen enriched liquid 44 being made up of oxygen enriched liquid 40.As the result of indirect heat exchange, produce liquid nitrogen stream 50.Making the evaporation of oxygen-rich liquid stream 44 part to produce stripping gas 52 and remaining gas liquid stream 54, remaining gas liquid stream 54 collects in the bottom of auxiliary distillation column 34 as remaining oxygen enriched liquid 56.It should be noted that, in an alternative embodiment, the two phase flow of the boiling lateral of once-through heat exchanger can be extracted from from auxiliary distillation column 34, and this two phase flow is guided to a single phase separator to produce remaining stream of oxygen-enriched liquid 68, then utilizes pipeline to be delivered to vapor phase assist distillation column 34 to form stripping gas 52.Although being not preferred, but this embodiment would be equivalent to the embodiment shown in accompanying drawing.
As once-through heat exchanger 48 and the substituted device of collection column plate 42, it is possible to use the thermosyphon reboiler being positioned at stand-by still 34 base portion makes the evaporation of oxygen enriched liquid 40 part drop to the base portion of stand-by still 34 from mass transfer contact elements 36.The core of this reboiler will be located in remaining the inside of oxygen enriched liquid, and produces stripping gas by making oxygen enriched liquid 40 evaporate.But, this will be not preferred, it is contemplated that this heat exchanger will not utilize the temperature difference of once-through heat exchanger to operate；The air of entrance must be compressed to elevated pressures subsequently.
As it can be seen, liquid nitrogen stream 50 (its whole or its part) can be imported main distillation column 18 as backflow stream 58.By auxiliary the formed remainder of overhead 38, liquid nitrogen stream 60 (being depressurized by valve 63) and waste stream 62 as other, sub-cooled heat exchanger 30 can be first introduced into and carry out indirect heat exchange with thick liquid oxygen stream 28 thus by its sub-cooled, then carry out indirect heat exchange with compressed and purification the air stream 10 entered thus contribute to being cooled to inside main heat exchanger 12.Alternatively, stream 60 can be mixed and heated with stream 62.After heated, will discharge from main heat exchanger 12 as gaseous nitrogen joint product (" N2") other liquid nitrogen stream 60, and can be used for waste stream 62 making being used for the air entered is carried out the regeneration of adsorbent that uses in the pre-purification unit of prepurification and being used for air separation equipment 1.In addition it is also possible to by being recompressed and it being mixed with the air entered, and make all or part of this stream recirculation.It should be pointed out that, the application of stream 60 is optional, the purpose of the evaporation of liquid nitrogen stream 60 is to provide extra sub-cooled to stream 28 and therefore, it is possible to realize bigger oxygen yield.
It should be pointed out that, liquid nitrogen reflux stream 60 can be extracted from the intersegmental position of tower 20 before by valve 63.
It should also be noted that, the sub-cooled heat exchanger 30 or 30' being discussed can be combined with main heat exchanger 12.It is also possible that do not using this sub-cooled heat exchanger 30 or 30 ' in the case of constitute an embodiment of the invention.Under any circumstance, in this embodiment illustrated, other liquid nitrogen stream 60 before by sub-cooled heat exchanger 30 and main heat exchanger 12, can be made in expansion valve 63 to reduce pressure.
Heat, by carrying out indirect heat exchange in main heat exchanger 12 inside with the compressed and purified air stream 10 entered, the nitrogen product stream 64 being made up of nitrogen rich vapor overhead 23 thus obtain nitrogen joint product, also contribute to cool down air stream 10 simultaneously.As it can be seen, by the nitrogen enriched vapor stream 66 taken out from main distillation column 18 top is separated into aforesaid two streams, and produce nitrogen product stream 64 and nitrogen enriched vapor stream 46.However, it is possible to take out nitrogen product stream 64 and nitrogen enriched vapor stream 46 individually from main distillation column 18.It should be pointed out that, because whole liquid nitrogen stream 50 can be imported main distillation column 18 as backflow, it is possible to only formed nitrogen joint product by heated nitrogen product stream 64.
By taking out the residue oxygen-rich liquid stream 68 being made up of residue oxygen enriched liquid 56 and this conductance being entered separation container 70, and produce oxygen joint product.Make liquid phase stream 72 part being made up of liquid phase 74 evaporation produce two phase flow 76 so that the compressed and purified air stream 10 that will pass through and enter carries out indirect heat exchange in condenser 14, thus compressed and purification air stream 10 is partly condensed.The liquid distillate making two phase flow 76 inside separation container separates with vapor fraction, to form vapor fraction and the liquid phase 74 produced by separating and remain the interpolation of oxygen enriched liquid 68 with stream.Available control valve (not shown) regulates the operation pressure of container 70.The vapor phase flow 80 being made up of vapor fraction 78 forms oxygen product stream.Can optionally will be collected as fluid product (or discharging vaporizer as pollutant) by the discharge stream 82 of valve 84.Alternatively, the stream 68 that can extract a part as fluid product and is transported to suitable storage facility.
It should be pointed out that, the auxiliary distillation column 34 of the position being positioned beyond main distillation column 18 height can be utilized to be pressurizeed by remaining oxygen-rich liquid stream 68.It is consequently formed pressurized oxygen product.Another substitutes and is by mean of mechanical pump or the use of pump and combines head of liquid produced by the top by auxiliary distillation column 34 is positioned at main distillation column 18, is pressurizeed by remaining oxygen-rich liquid stream.
As it can be seen, condenser 14 plays the effect of thermal siphon.As the substituted device for forming oxygen product, separation container 70 can be built into receiving condenser 14.In this case, two phase flow enters the inside of separation container 70 by leaving condenser.But, it is considered that, this embodiment illustrated has more cost benefit than above-mentioned layout.If it addition, will be greater than the oxygen product of about 20% as fluid product by discharging stream 82, then condenser 14 can be reconstructed once-through heat exchanger and save power consumption the most further.In this arrangement, utilize pipeline that remaining oxygen-rich liquid stream 68 is fed directly to condenser 14.Then, in phase separation container, the product of part evaporation is separated and there will be no backflow stream, such as, be imported into the oxygen-rich liquid stream in condenser 14.
With reference to Fig. 2, it is shown that one alternate embodiments of the present invention is as air separation equipment 2.It should be pointed out that, the element shown in Fig. 2 by tool and is discussed identical description above with reference to Fig. 1, this element shown in Fig. 2 will use the reference number identical with Fig. 1；Will not be discussed further for brevity.Air separation equipment 2 is specifically designed to allow the nitrogen using contained in bigger mark air to be reclaimed as product.This is to be realized to the liquid nitrogen reflux of main distillation column 18 by increase.
In air separation equipment 2, after being cooled inside main heat exchanger 12, compressed and purification air stream 10 is imported main distillation column 20 and carries out rectification, to produce nitrogen rich vapor overhead 23 and thick liquid oxygen bottoms 26'.After being depressurized inside expansion valve 32, can optionally strip by thick liquid oxygen stream 28 ' sub-cooled and inside auxiliary distillation column 34 in sub-cooled unit 30'.In the way of described in air separation equipment 1, condense to produce the first liquid nitrogen stream 50 and remaining oxygen enriched liquid 56 by the first nitrogen enriched vapor stream 46 in once-through heat exchanger 48.After being depressurized in expansion valve 90, the gained residue oxygen-rich liquid stream 68 produced in auxiliary distillation column 34 is imported in thermosyphon reboiler 86.By carrying out indirect heat exchange with gaseous flow 92, and residue oxygen-rich liquid stream 68 part can be evaporated, described gaseous flow 92 can be made up of the nitrogen rich vapor overhead 23 of main distillation column 18.Gaseous flow 92 is passed through the core 94 being positioned within thermosyphon reboiler 86 housing 96, to complete heat exchange.Gaseous flow 92 is condensed and condenses the liquid stream 98 part as the backflow being used in above-mentioned tower using what generation was imported in main distillation column 18.The whole liquid nitrogen streams 50 produced in once-through heat exchanger 48 are imported main distillation column 18 reflux as tower.The segmentation condensation of this nitrogen rich vapor overhead will increase liquid nitrogen reflux, therefore increase air separation equipment 2 and produce the ability of nitrogen product.
As will be appreciated, if discharging stream 106 there is enough flows, then other device (including once-through heat exchanger) replacing thermosyphon reboiler 86 can be used.Although additionally, not shown, replace nitrogen rich vapor, the conductance with the nitrogen concentration of the nitrogen concentration not less than air can be entered the core 94 of thermosyphon reboiler 86.For example, it is possible to air stream is compressed and makes this flow liquid in main heat exchanger 12.Hereafter, the centre position of main distillation column 18 can be conducted into.Then, there is the gaseous flow with this roughly the same composition of liquid stream to enter the core 94 of thermosyphon reboiler 86 and be condensed.Gained condensed fluid conductance being become owner of the position of distillation column, in this position, the composition of the tower liquid of decline is identical with above-mentioned condensed fluid or approximately the same, or enters to assist distillation column 34 by this condensed fluid conductance to carry out the production of stripping and oxygen joint product.
The part evaporation of residue oxygen-rich liquid stream 68 forms vapor fraction and liquid distillate, and this vapor fraction and liquid distillate collect in the housing as vapor fraction 100 and liquid phase 102.Inside main heat exchanger 12, there is indirect heat exchange with compressed and purification the air stream 10 entered in the vapor phase flow 104 being made up of vapor fraction 100, in order to heating steam flows 100 mutually, thus produces oxygen product (" O2") and contribute to cooling down compressed and purification air stream 10.The discharge stream 106 being made up of liquid phase 102 can be depressurized in valve 108 and be collected as liquid oxygen product.In this embodiment, optionally, waste stream 62 can and thick liquid oxygen stream 28' generation indirect heat exchange internal at sub-cooled heat exchanger 30'.Subsequently, also there is indirect heat exchange with compressed and purification air stream 10 at main heat exchanger 12 internal waste stream 62, to heat waste stream 62 and to help to cool down compressed and purification air stream 10.Waste stream 62 can be recycled in the air entered.Complete after this can heat by directly mixing with the air entered in exchanger 12 or after compression further.As the situation in air separation equipment 1, by there is indirect heat exchange with the compressed and purified air stream 10 entered, and heated by the nitrogen product stream 64 being made up of nitrogen rich vapor overhead 23 inside main heat exchanger 12, thus also contribute to cool down compressed and purified air stream 10.
See figures.1.and.2, freeze to air separation equipment 1 or air separation equipment 2 by means of liquid nitrogen stream 110；Liquid nitrogen stream 110 is then directed to be positioned at the top inlet 114 at the top of main distillation column 18 by flow control valve 112.Liquid nitrogen stream 110 can be obtained from on-the-spot basin and liquid nitrogen stream 110 can have high pressure or low pressure.Adding of liquid nitrogen stream 110 compensates the warm end losses that ambient heat leaks and caused due to the operation of main heat exchanger 12.It should be pointed out that, in steam stream liquid stream 110 can being introduced directly in the steam stream of entrance heat exchanger 30' or 12.As will be appreciated, before importing main distillation column 18, the entrance air of a part can be made to expand.In this respect, compressed and purification the air stream of a part can be made after main heat exchanger 12 interior section cools down to expand, then mix with waste gas stream 62.Alternatively possible would is that applies back pressure to the distillation column system of main distillation column 18 and can expand in turbo-expander and in the internal further heating of main heat exchanger 12 by auxiliary distillation column 34 and the heating of waste stream 62 part inside main heat exchanger 12.The use of turbo-expander can provide the probability taking out fluid product from Tower System.A part of liquid nitrogen obtained in condenser 48 or 96 can be delivered to suitable storage facility.Another replacement is liquid oxygen stream can to import remaining oxygen-rich liquid stream 68 or mix with this liquid stream 68, is then introduced in the housing 96 of thermosyphon reboiler 86.
With reference to Fig. 3, it is shown that the air separation equipment 1' of the alternate embodiments of air separation equipment 1 shown in pie graph 1.In air separation equipment 1, it is illustrated that stand-by still 34 ' possess stripping section 36a, this stripping section 36a can possess as above with reference to mass transfer contact elements 36 described by Fig. 1.Inside this stripping section 36a, thick liquid oxygen stream 28 stripped as mentioned above rather than directly produce auxiliary overhead, but producing nitrogenous and oxygen steam.It is for the steam of this nitrogenous and oxygen is carried out rectification, thus recovery section oxygen that stand-by still 34a is also equipped with the rectifying section 36b being positioned at above stripping section 36a, this rectifying section 36b, and these oxygen are the most just discharged from equipment in waste stream 62.The liquid nitrogen stream 60' being imported into stand-by still 34' top with valve 63' after reducing pressure is utilized to reflux in this rectifying section.As will be appreciated, the equipment shown in Fig. 2 can be made identical amendment.In this case, in the way of being similar to shown in Fig. 3, stand-by still will be revised.In the case of the embodiment of Fig. 2, the condensation liquid stream 98 of part is used in stand-by still 34' backflow.
As will be appreciated, all of expection is the oxygen of the part otherwise can lost in refuse to be reclaimed increase oxygen reclaim.However, it is necessary to break the oxygen recovery of increase and from the balance being otherwise used in main distillation column in the liquid nitrogen of backflow between the fact that take out liquid nitrogen and therefore produce nitrogen.Any bigger rectification will be with the flow increase of liquid nitrogen stream 60' therefore with the decline of available product nitrogen 64, because in order to maintain product nitrogen impurity must maintain the reflux ratio of king-tower.More specifically mode in stating this restriction is the performance of rectifying section 36b, when combining the performance of stripping section 36a, and should be containing the oxygen not less than 5.0 volume % at the auxiliary overhead 38 within stand-by still 36.In order to reach this purpose, the flow-rate ratio (summation of stream 60 and 64) of usual liquid nitrogen stream 60' and the total available nitrogen stream from tower 18 should be between 0.1 and 0.4, and the liquid/vapor ratio in rectifying section 36b is 0.23 or less.
Although describing the present invention with reference to preferred implementation, but as will be appreciated by one of skill in the art, can in without departing substantially from claims, on the premise of stated spirit and scope of the invention, many changes may be made, add and omit.

Claims (11)

1. separating air to produce oxygen and a method for nitrogen joint product, described method includes:
Cool down compressed and purification the aeriferous stream of bag；
The described compressed and stream of purification is partly condensed in the condenser being positioned at main distillation column bottom zone；
Inside main distillation column, the vapor fraction of the stream of the described compressed and purification partly condensed is carried out rectification, to produce nitrogen rich vapor overhead, and the air wherein condensed is with by the liquid mixing declined produced by the described rectification in main distillation column, thus produces the thick liquid oxygen bottoms in described main distillation column；
Inside auxiliary distillation column, oxygen enriched liquid and the auxiliary overhead containing the oxygen not less than 5.0 volume % is produced by being reduced pressure by the thick liquid oxygen stream being made up of thick liquid oxygen bottoms at least in part, with the stripping gas risen described thick liquid oxygen stream stripped inside described auxiliary distillation column and make described oxygen enriched liquid part evaporate by carrying out indirect heat exchange with the nitrogen enriched vapor stream being made up of described nitrogen rich vapor overhead, thus producing liquid nitrogen stream, stripping gas and remaining oxygen enriched liquid；
Reflux in described main distillation column with at least part of described liquid nitrogen stream；
At oxygen enriched liquid described in described auxiliary distillation column internal gathering；
By making the oxygen-rich liquid stream being made up of described oxygen enriched liquid and described nitrogen enriched vapor stream be made described oxygen enriched liquid partly evaporate by once-through heat exchanger, in order to form described stripping gas and the described remaining oxygen enriched liquid collected as the bottoms of described auxiliary distillation column；
Described remaining oxygen-rich liquid stream is collected in separation container；
The liquid phase stream being made up of the liquid phase produced inside described separation container is imported described condenser, and make described liquid phase stream partly evaporate by carrying out indirect heat exchange with the stream of described compressed and purification in described condenser, from described liquid phase stream, thus produce two phase flow；
The liquid phase by the described two phase flow described separation container of importing and making described two phase flow in the inside of described separation container and vapor phase separation are to form oxygen-rich steam fraction, and described liquid phase are collected in described separation container together with described remaining oxygen-rich liquid stream；
By giving off the stream of described oxygen-rich steam fraction from described separation container, and form oxygen product stream；
Nitrogen product stream is formed by described nitrogen rich vapor overhead；Waste stream is formed by described auxiliary overhead；With
Described oxygen product stream, described nitrogen product stream and described waste stream and described compressed and purification stream is made to carry out indirect heat exchange.
2. the method for claim 1, wherein said auxiliary overhead is merely by stripping described thick liquid oxygen stream inside auxiliary distillation column and producing.
3. the method for claim 1, wherein refluxes in described main distillation column with the described liquid nitrogen stream of part；
The stripping of described thick liquid oxygen stream is carried out in the inside of auxiliary distillation exhausting section of column；
Inside described auxiliary distillation column, described thick liquid oxygen stream is carried out stripping and produces the nitrogenous and steam stream of oxygen；With
By the described steam conductance containing nitrogen and oxygen enters to assist the inside of the rectifying section of distillation column and the described auxiliary distillation column in being positioned at the rectifying section of the described auxiliary distillation column above described stripping section described nitrogenous and oxygen steam stream carries out rectification, and therefore reflux in described rectifying section in described auxiliary distillation column with the described liquid nitrogen stream of another part, thus improve and reclaim at the oxygen within described residue oxygen enriched liquid.
4. the method for claim 1, wherein:
Reflux in described main distillation column with the described liquid nitrogen stream of part；With
Described waste stream and described thick liquid oxygen stream exchanged heat indirectly so that before depressurizing by described thick liquid oxygen stream sub-cooled.
5. the method for claim 1, wherein by the pressurization of described remaining oxygen-rich liquid stream also to be pressurizeed by described oxygen product stream.
6. the method for claim 1, wherein enters described main distillation column to freeze by liquid nitrogen refrigerating conductance.
7., for separating air to produce oxygen and a device for nitrogen joint product, described device includes:
Main heat exchanger, it is configured to cool down compressed and purification the aeriferous stream of bag；
Condenser, it is positioned in the bottom zone of main distillation column, is configured to partly condense the described compressed and stream of purification；
Main distillation column, its vapor fraction being configured to the stream to the described compressed and purification partly condensed carries out rectification to produce nitrogen rich vapor overhead, the air wherein condensed, with by the liquid mixing declined produced by the described rectification in main distillation column, thus produces thick liquid oxygen bottoms；
Auxiliary distillation column, it is connected to described main distillation column and the thick liquid oxygen stream being made up of described thick liquid oxygen bottoms is stripped by the stripping gas that is configured to rise in the inside of described auxiliary distillation column, and at least partially due to the stripping of described thick liquid oxygen stream produces oxygen enriched liquid and the auxiliary overhead containing oxygen not less than 5.0 volume %；
Expansion valve, it is at described main distillation column and assists between distillation column to be reduced pressure before being imported into described auxiliary distillation column by described thick liquid oxygen stream；
Device, it makes described oxygen enriched liquid part evaporate by carrying out indirect heat exchange with the nitrogen enriched vapor stream being made up of described nitrogen rich vapor overhead, thus produces liquid nitrogen stream, stripping gas and residue oxygen enriched liquid；
Oxygen enriched liquid part vaporising device, it is connected to described main distillation column so that reflux in described main distillation column with at least part of described liquid nitrogen stream；
Described main heat exchanger is connected to described main distillation column and described auxiliary distillation column, in order to the nitrogen product stream being made up of described nitrogen rich vapor overhead and the waste stream formed by the auxiliary overhead of described auxiliary distillation column and the described compressed and air stream exchanged heat indirectly of purification；
Described auxiliary distillation column has the device for collecting described oxygen enriched liquid；
Described oxygen enriched liquid part vaporising device is once-through heat exchanger, described once-through heat exchanger be connected to assist distillation column and described oxygen enriched liquid collection device with will pass through the oxygen-rich liquid stream that is made up of described oxygen enriched liquid by and make described oxygen enriched liquid evaporate at described once-through heat exchanger interior section, and described remaining oxygen enriched liquid is collected as the bottoms of described auxiliary distillation column；
Described main distillation column is connected to described once-through heat exchanger, in order to described nitrogen enriched vapor stream condensed inside described once-through heat exchanger；
Described remaining oxygen enriched liquid heat-exchange device is condenser, and described oxygen-rich steam fraction formation device is separation container；
Described separation container is connected to described auxiliary distillation column, in order to described remaining oxygen-rich liquid stream collects in described separation container；
Described separation container is connected to described condenser, with will pass through carry out indirect heat exchange with described compressed and purification stream and make in described condenser by inside described separation container produce liquid phase formed liquid phase stream part evaporation, it is imported into the two phase flow in described separation container to produce, makes in the inside of described separation container the liquid phase of described two phase flow and vapor phase separation to form described oxygen-rich steam fraction and described liquid phase；With
Described main heat exchanger is connected to described separation container, described main distillation column and described auxiliary distillation column so that the nitrogen product stream that by the oxygen product stream of described oxygen-rich steam fractional composition, is made up of described nitrogen rich vapor overhead and the waste stream that is made up of the auxiliary overhead of described auxiliary distillation column inside described main heat exchanger by and carry out indirect heat exchange with described compressed and purification stream.
8. device as claimed in claim 7, wherein said stand-by still only possesses and wherein described thick liquid oxygen stream is carried out steam stripped stripping section.
9. device as claimed in claim 7, wherein:
Described stand-by still has stripping section and is positioned at the rectifying section above described stripping section；
The stripping of described thick liquid oxygen stream is carried out in the inside of auxiliary distillation exhausting section of column, and in described stripping section, produce nitrogenous and oxygen steam stream, the steam stream of described nitrogenous and oxygen enters described rectifying section so that described nitrogenous and oxygen steam stream is carried out rectification, thus improves in the oxygen recovery described residue oxygen enriched liquid within；
Described oxygen enriched liquid part vaporising device is connected to described main distillation column, to reflux in described main distillation column with the described liquid nitrogen stream of part, and it is also connected to described auxiliary distillation column therefore to reflux in described rectifying section in described auxiliary distillation column with the described liquid nitrogen stream of another part；With
Another expansion valve is between described oxygen enriched liquid part vaporising device and described auxiliary distillation column, in order to the pressure of the liquid nitrogen stream of described another part is reduced to the pressure of described auxiliary distillation column.
10. device as claimed in claim 7, wherein:
Described once-through heat exchanger is connected to described main distillation column to reflux in described main distillation column with the described liquid nitrogen stream of part；With
Sub-cooled heat exchanger is connected to described once-through heat exchanger, described auxiliary distillation column and described expansion valve, so that described waste stream and described thick liquid oxygen stream are in the inside exchanged heat indirectly of described sub-cooled heat exchanger, and by described thick liquid oxygen stream sub-cooled before by described expansion valve.
11. devices as claimed in claim 7, wherein said main distillation column has for importing liquid nitrogen refrigerating stream to give the top inlet of refrigeration.
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Publication number Priority date Publication date Assignee Title
CN103277981B (en) * 2013-06-14 2015-05-06 济钢集团有限公司 Device and method for increasing nitrogen-to-oxygen ratio of air separation unit
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4560397A (en) * 1984-08-16 1985-12-24 Union Carbide Corporation Process to produce ultrahigh purity oxygen
US4755202A (en) * 1987-07-28 1988-07-05 Union Carbide Corporation Process and apparatus to produce ultra high purity oxygen from a gaseous feed
CN1198524A (en) * 1997-03-19 1998-11-11 普拉塞尔技术有限公司 Process for producing ammonia and recovering argon using low purity oxygen
CN1236087A (en) * 1998-05-18 1999-11-24 普拉塞尔技术有限公司 Cryogenic rectification system with integral product boiler
CN101886871A (en) * 2010-08-04 2010-11-17 四川空分设备(集团)有限责任公司 Method and device for producing pressure oxygen by air separation

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4783210A (en) 1987-12-14 1988-11-08 Air Products And Chemicals, Inc. Air separation process with modified single distillation column nitrogen generator
EP0383994A3 (en) * 1989-02-23 1990-11-07 Linde Aktiengesellschaft Air rectification process and apparatus
US5074898A (en) * 1990-04-03 1991-12-24 Union Carbide Industrial Gases Technology Corporation Cryogenic air separation method for the production of oxygen and medium pressure nitrogen
US5195324A (en) * 1992-03-19 1993-03-23 Prazair Technology, Inc. Cryogenic rectification system for producing nitrogen and ultra high purity oxygen
US5546767A (en) * 1995-09-29 1996-08-20 Praxair Technology, Inc. Cryogenic rectification system for producing dual purity oxygen
US5592832A (en) * 1995-10-03 1997-01-14 Air Products And Chemicals, Inc. Process and apparatus for the production of moderate purity oxygen
US6079223A (en) * 1999-05-04 2000-06-27 Praxair Technology, Inc. Cryogenic air separation system for producing moderate purity oxygen and moderate purity nitrogen

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4560397A (en) * 1984-08-16 1985-12-24 Union Carbide Corporation Process to produce ultrahigh purity oxygen
US4755202A (en) * 1987-07-28 1988-07-05 Union Carbide Corporation Process and apparatus to produce ultra high purity oxygen from a gaseous feed
CN1198524A (en) * 1997-03-19 1998-11-11 普拉塞尔技术有限公司 Process for producing ammonia and recovering argon using low purity oxygen
CN1236087A (en) * 1998-05-18 1999-11-24 普拉塞尔技术有限公司 Cryogenic rectification system with integral product boiler
CN101886871A (en) * 2010-08-04 2010-11-17 四川空分设备(集团)有限责任公司 Method and device for producing pressure oxygen by air separation

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