CN105865148B - A method of efficiently producing high pure oxygen and High Purity Nitrogen - Google Patents

A method of efficiently producing high pure oxygen and High Purity Nitrogen Download PDF

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Publication number
CN105865148B
CN105865148B CN201610205678.2A CN201610205678A CN105865148B CN 105865148 B CN105865148 B CN 105865148B CN 201610205678 A CN201610205678 A CN 201610205678A CN 105865148 B CN105865148 B CN 105865148B
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pressure
nitrogen
tower
low
air
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CN105865148A (en
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周大荣
俞建
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SHANGHAI QIYUAN GAS DEVELOPMENT Co.,Ltd.
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SHANGHAI QIYUAN AIR SEPARATION TECHNOLOGY DEVELOPMENT Co Ltd
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    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/0429Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/04054Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of air
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/0406Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of nitrogen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
    • F25J3/04066Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams of oxygen
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04006Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04109Arrangements of compressors and /or their drivers
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04248Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04351Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
    • F25J3/04357Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen and comprising a gas work expansion loop
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04436Processes 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 at least a triple pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02Processes 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
    • F25J3/04Processes 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
    • F25J3/04436Processes 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 at least a triple pressure main column system
    • F25J3/04454Processes 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 at least a triple pressure main column system a main column system not otherwise provided, e.g. serially coupling of columns or more than three pressure levels
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the high pressure column of a double pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2200/00Processes or apparatus using separation by rectification
    • F25J2200/50Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column in the low pressure column of a double pressure main column system
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2215/00Processes characterised by the type or other details of the product stream
    • F25J2215/40Air or oxygen enriched air, i.e. generally less than 30mol% of O2
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25JLIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00Details related to the use of reboiler-condensers
    • F25J2250/20Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams

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

Abstract

The present invention provides a kind of method for efficiently producing high pure oxygen and High Purity Nitrogen, using high, medium and low voltage rectifying column, in and, the tower bottom of low-pressure distillation tower reboiler and condenser/evaporator is respectively set, portion of air is separated into high pressure nitrogen and oxygen-enriched liquid air in high-pressure rectification tower, and pressure rectifying tower reboiler is condensed into liquid air in the entrance of another part air;The liquid air and the oxygen-enriched liquid air, which are mixed into high-pressure rectification tower condenser/evaporator, flashes to gaseous state, enters back into middle pressure rectifying column;Therefrom pressure rectifying column isolates high pure nitrogen product and oxygen-rich liquid later, which enters low-pressure distillation tower, and high-purity liquid oxygen product is obtained after rectifying.High-purity liquid oxygen, high pure nitrogen can produce simultaneously;The recovery rate of High Purity Nitrogen reaches 60-75%, and the recovery rate of high pure oxygen reaches 70%-72%;This method is economical and practical using air as raw material, and product safety is reliable, can be widely applied, and has good market prospects.

Description

A method of efficiently producing high pure oxygen and High Purity Nitrogen
Technical field
The invention belongs to gas generation fields, are related to a kind of method for carrying out gas separation by low-temperature liquefaction, especially relate to A kind of and method for efficiently producing high pure oxygen and High Purity Nitrogen.
Background technique
With the fast development of the industries such as electronics, chemical industry, high pure nitrogen, high pure oxygen demand increased dramatically, usual work Industry oxygen purity is 99.6%O2, and high-purity oxygen purity > 99.9999%O needed for electronics industry2;In precision electronic industries, High pure oxygen is normally used for the chemical vapor deposition of silica, or the reactant as oxidation source and generation high purity water;Or Person is used for dry oxidation;Or mixed with carbon tetrafluoride, for plasma etching etc..
Generalling use liquid oxygen at present is that raw material carries out producing for high pure oxygen, however its recovery rate is relatively low;And use krypton xenon thick In process flow processed, oxygen after primary, secondarily purified, purity reaches 99.5%~99.99%, is high purity oxygen Splendid raw material, its main feature is that yield is big, purity is high, and the crude release oxygen sources of krypton xenon are relatively few then becomes the high-purity liquid oxygen of limitation The reason of yield.
Major gaseous component in air is nitrogen and oxygen, and nitrogen and oxygen purity are respectively 78.12% He 20.95%, and air is ubiquitous as low-cost resource, therefore directly produces high pure nitrogen and high pure oxygen by separation air Gas is method the easiest and economic.Therefore, a kind of method that high pure oxygen and High Purity Nitrogen are isolated from air is developed, at For one of the research hotspot of current Chemical R & D personnel.
Summary of the invention
The present invention is directed to overcome above-mentioned many disadvantages existing in the prior art, and one kind is provided and is efficiently divided from air The method for separating out high pure oxygen and High Purity Nitrogen meets and uses high pure oxygen and High Purity Nitrogen in the fields such as precision electronic industries, biological medicine Demand.
Therefore, the first aspect of the present invention, provides a kind of method for efficiently producing high pure oxygen and High Purity Nitrogen, and this method is adopted Equipment mainly includes fractionating column main heat exchanger E1, subcooler E2, high-pressure rectification tower C1, middle pressure rectifying column C2, low-pressure distillation Tower C3, wherein the high-pressure rectification column overhead is provided with condenser/evaporator K1;Medium pressure rectifying tower bottom is provided with reboiler K2, tower top are provided with oxygen-rich liquid auxiliary condenser/evaporator K4;The low-pressure distillation tower tower bottom is provided with condenser/evaporator K3, Tower top is provided with condenser/evaporator K5;Several valves and pipeline, for connecting above each equipment;The method specifically includes as follows Step:
Will purifying it is dry after air be cooled to saturation state in fractionating column main heat exchanger E1, a part of saturated air into Enter high-pressure rectification tower C1 tower reactor, is separated into high pressure nitrogen and oxygen-enriched liquid air in high-pressure rectification tower C1;Another part saturated air It is pressed in rectifying tower reboiler K2 in and is condensed into liquid air;After the liquid air is mixed with the oxygen-enriched liquid air, into high-pressure rectification Gaseous state is flashed in tower condenser/evaporator K1, enters back into middle pressure tower bottom of rectifying tower;The nitrogen that high-pressure rectification tower C1 is separated Being sent into condensation in high-pressure rectification tower condenser/evaporator K1 becomes liquid nitrogen, and a part of liquid nitrogen is another as high-pressure rectification tower phegma Part liquid nitrogen presses in being used as at the top of rectifying column C2 in after subcooler E2 supercooling and presses rectifier column reflux liquid;High-pressure rectification tower The oxygen rich air that condenser/evaporator K1 is evaporated respectively enters middle pressure rectifying column C2 and carries out rectifying, is separated into medium pressure nitrogen gas and oxygen-enriched Liquid;
Therefrom the extraction of the pressure bottom rectifying column C2 is rich in the oxygen-rich liquid of low boiling hydrocarbon, assists condensing subsequently into oxygen-rich liquid Evaporator K4;In oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air, exports after re-heat;
Therefrom pressure rectifying column C2 tower top extracts medium pressure nitrogen out, and medium pressure nitrogen enters low-pressure distillation tower condensation evaporation Device K3, then be condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen return in press rectifying column C2 tower top, as pressing rectifying column in this Phegma;Another part medium pressure liquid nitrogen steams after throttling to 0.01~0.03MPa with the condensation of low-pressure distillation tower C3 tower top Hair device K5 in dirty nitrogen heat exchange and be evaporated, the low-pressure nitrogen after evaporation after subcooler E2, main heat exchanger E1 re-heat, as High pure nitrogen output of products;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower C3;
Therefrom oxygen-rich liquid of the extraction without low boiling hydrocarbon in the middle part of pressure rectifying column C2, after subcooler is subcooled, into low pressure essence Evaporate phegma of the tower C3 tower top as the low-pressure distillation tower;The oxygen-rich liquid without low boiling hydrocarbon is smart in low-pressure distillation tower C3 After evaporating, high-purity liquid oxygen product is obtained in the low-pressure distillation tower tower reactor.
Preferably, the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen further includes directly produce liquid nitrogen product following Step:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, and medium pressure nitrogen enters low-pressure distillation tower condensation Evaporator K3, then it is condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen is divided into two strands: during wherein hydraulic fluid nitrogen returns in one Rectifying column C2 tower top is pressed, as the phegma for pressing rectifying column in this, wherein hydraulic fluid nitrogen is by direct as liquid nitrogen product in another stock Output;Condenser/evaporator with low-pressure distillation tower C3 tower top after another part medium pressure liquid nitrogen throttles to 0.01~0.03MPa Dirty nitrogen in K5 exchanges heat and is evaporated, and the low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as high-purity Nitrogen product output;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower C3.
High pure oxygen is efficiently produced and the method for High Purity Nitrogen is further comprising the steps of it is further preferred that above-mentioned:
The low-pressure nitrogen is divided into two strands after subcooler E2, main heat exchanger E1 re-heat:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products;
Wherein another strand of low-pressure nitrogen enters nitrogen compressor CP2 and is compressed, then is cooled down, swollen subsequently into turbine Swollen machine ET01 pressurized end Z01 is pressurized, then cooling in water cooler E3, subsequently enters the fractionating column main heat exchanger E1 In further cool down, then from the middle part of the fractionating column main heat exchanger E1 extract out, into the turbo-expander ET01 expansion after, The fractionating column main heat exchanger E1 re-heat is returned, is incorporated into another strand of low-pressure nitrogen later.
It is further preferred that above-mentioned another strand of low-pressure nitrogen extracts it out from the middle part of the fractionating column main heat exchanger E1 Afterwards, it is expanded to 0.01~0.03MPa into the turbo-expander ET01, returns again to the fractionating column main heat exchanger E1 re-heat extremely Room temperature is incorporated into the suction inlet of the nitrogen compressor CP2 later.
It is further preferred that above-mentioned another strand of low-pressure nitrogen enters nitrogen compressor CP2 and is compressed to 0.80~1.0MPa, 40 DEG C are cooled to hereinafter, 1.20~1.40MPa is pressurized to subsequently into turbo-expander ET01 pressurized end Z01, then through water Cooler E3 is cooled to 40 DEG C, subsequently enters in the fractionating column main heat exchanger E1 and is cooled further to -120 DEG C~-130 DEG C, It is extracted out again from the middle part of the fractionating column main heat exchanger E1,0.020 is expanded into the turbo-expander ET01~ 0.030MPa returns to the fractionating column main heat exchanger E1 re-heat to 30~35 DEG C, is incorporated into another strand of low-pressure nitrogen later.
Preferably, in the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen, the air after the purifying is dry is dividing It evaporates and is cooled to before saturation state in tower main heat exchanger E1, be divided into two strands:
Air after wherein one purifying is dry is directly entered fractionating column main heat exchanger E1;
Air after wherein another burst of purifying is dry enters turbo-expander ET01 pressurized end Z01 and is pressurized, and then exists It is cooling in water cooler E3, it subsequently enters and is further cooled down in the fractionating column main heat exchanger E1, then changed from the fractionating column master The middle part of hot device E1 is extracted out, into after turbo-expander ET01 expansion, is back to the fractionating column main heat exchanger E1 and is carried out Re-heat;The low-pressure air exported through the fractionating column main heat exchanger E1, after air booster is pressurized, as the air that backflows Air after being incorporated into the purifying drying before being divided into two strands.
It is further preferred that in the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen, another burst of purifying drying Air afterwards enters turbo-expander ET01 pressurized end Z01 and is pressurized to 1.20~1.40MPa, then cooling in water cooler E3 It to 40 DEG C, subsequently enters and is cooled further to -120 DEG C~-130 DEG C in the fractionating column main heat exchanger E1, then from the fractionation The middle part of tower main heat exchanger E1 is extracted out, is expanded to 0.020~0.030MPa into the turbo-expander ET01, is returned again to institute Fractionating column main heat exchanger E1 re-heat is stated to 30~35 DEG C;The low-pressure air exported through the fractionating column main heat exchanger E1, by sky After the pressurization of gas supercharger, the air after the drying of the purifying before being divided into two strands is incorporated into as the air that backflows.
It is further preferred that the operating pressure of the high-pressure rectification tower C1 is 0.8~1.3MPa, medium pressure rectifying column The operating pressure of C2 is 0.35~0.6MPa, and the operating pressure of the low-pressure distillation tower C3 is 0.02~0.15MPa.In above-mentioned behaviour Make in pressure preferred scope, the most preferred operating pressure of medium pressure rectifying column C2 is 0.5MPa.
It is further preferred that the main component of the low boiling hydrocarbon is methane.
The second aspect of the present invention provides high pure oxygen made from a kind of method according to a first aspect of the present invention And/or High Purity Nitrogen, which is characterized in that O in the high pure oxygen2Purity >=99.9999%, N in the High Purity Nitrogen2Purity >= 99.999%.As it can be seen that obtained high pure oxygen and/or High Purity Nitrogen have reached relevant national standard.
Compared with prior art, the invention has the following advantages that
(1) Traditional high purity oxygen is mainly purified from industrial oxygen (99.5%), generally requires 2~3 rectifying columns, point Not Qu Chu high boiling component (methane, krypton, xenon, nitrous oxide etc.) in industrial oxygen, then go the argon component in deoxygenation, the present invention The extraction of at least one equilibrium stage is substantially free of methane above the middle pressure tower bottom of rectifying tower for producing the High Purity Nitrogen product with pressure Oxygen-rich liquid is as raw material, and the high boiling components content such as methane contained therein, krypton, xenon is ppb grades, while the recovery rate of nitrogen Do not reduce;
(2) present invention can be achieved to recycle while High Purity Nitrogen and high pure oxygen, wherein the recovery rate of High Purity Nitrogen reaches 60- 75%, the recovery rate of high pure oxygen reaches 70%-72%;
(3) high pure oxygen product is various informative, and the high pure oxygen product of production can be gas, can also be liquid oxygen product, conveying It is stored to liquid storage groove;
(4) the low pure liquid oxygen of medium pressure rectifier bottoms discharge part (containing about 50-70% oxygen, the about 100- containing methane 500ppm, surplus are krypton, xenon, nitrous oxide etc.) content of hydrocarbon in medium pressure rectifying column is reduced, improve the safety of equipment Property.
(5) method provided by the present invention for efficiently producing high pure oxygen and High Purity Nitrogen, it is economical and practical using air as raw material, Product safety is reliable, and this method can be widely applied, and has good market prospects.
Detailed description of the invention
Fig. 1 is the process flow method schematic diagram of one embodiment 1 of device of the present invention;
Wherein: 101 air for the purifying in main line after dry, 102,201 air for the purifying in branch after dry, 103 be the saturated air exported from fractionating column main heat exchanger, 104,105 two parts saturated air to shunt from 103,106, 107 be liquid air, and 202,203,204 be pressurized air, and 205,206 be the low-pressure air after expansion, and 300 be elevated pressure nitrogen Gas, 301,302,303 be high-pressure liquid nitrogen, 304 be middle hydraulic fluid nitrogen, 401,402,404,407 be medium pressure nitrogen gas, 403,405,406, 410,302b is middle hydraulic fluid nitrogen, and 411 be low pressure liquid nitrogen, and 412,413,414 be low-pressure nitrogen, and 501,502,503 be liquid air, 504 For oxygen rich air, 601,602 oxygen-rich liquids to extract out in the middle part of middle pressure rectifying column 604,605,607,608,609 be dirt nitrogen, 606 are The liquid nitrogen fraction of condensation, 603 be the mixture of oxygen-rich liquid 602 and liquid nitrogen fraction 606, and 701 be high-purity liquid oxygen, and 901,902,903 are The oxygen-rich liquid of tower bottom of rectifying tower extraction is pressed, 904,906 assist the oxygen rich air of condenser/evaporator K4 evaporation for middle pressure rectifying column, and E1 is Main heat exchanger, E2 are subcooler, and E3 is water cooler, and K1 is high-pressure rectification tower condenser/evaporator, and K2 is that middle pressure rectifying column boils again Device, K3 are low-pressure distillation tower tower reactor evaporator, and K4 is that oxygen-rich liquid assists condenser/evaporator, and K5 is the cold of low-pressure distillation tower C3 tower top Solidifying evaporator, C1 are high-pressure rectification tower, and C2 is middle pressure rectifying column, and C3 is low-pressure distillation tower, and ET01 is turbo-expander, and Z01 is The pressurized end of turbo-expander is connected, V501, V502, V503, V513, V514, V515 are throttle valve.
Fig. 2 is the process flow method schematic diagram of one embodiment 2 of device of the present invention;
Wherein: 101 air for the purifying in main line after dry, 103 be the saturation sky exported from fractionating column main heat exchanger Gas, 104,105 two parts saturated air to shunt from 103,106,107 be liquid air, and 207,201 is through nitrogen compressor CP2 Compressed nitrogen, 202,203,204 be pressurized nitrogen, and 205,206 be the low-pressure nitrogen after expansion, and 415 be supplement The low-pressure nitrogen of nitrogen compressor CP2,300 be high pressure nitrogen, and 301,302,303 be high-pressure liquid nitrogen, and 304 be middle hydraulic fluid nitrogen, 401,402,404,407 be medium pressure nitrogen gas, 403,405,406,410,302b be middle hydraulic fluid nitrogen, 411 be low pressure liquid nitrogen, 412, 413,414 be low-pressure nitrogen, and 501,502,503 be liquid air, and 504 be oxygen rich air, and 601,602 press rectifying column middle part to extract out to be middle Oxygen-rich liquid 604,605,607,608,609 is dirty nitrogen, 606 is the liquid nitrogen fraction of condensation, and 603 be oxygen-rich liquid 602 and liquid nitrogen fraction 606 Mixture, 701 be high-purity liquid oxygen, 901,902,903 for it is middle pressure tower bottom of rectifying tower extraction oxygen-rich liquids, 904,906 be middle pressure Rectifying column assists the oxygen rich air of condenser/evaporator K4 evaporation, and E1 is main heat exchanger, and E2 is subcooler, and E3, E4 are water cooler, K1 For high-pressure rectification tower condenser/evaporator, K2 is middle pressure rectifying tower reboiler, and K3 is low-pressure distillation tower tower reactor evaporator, and K4 is oxygen-enriched Liquid assists condenser/evaporator, and K5 is the condenser/evaporator of low-pressure distillation tower C3 tower top, and C1 is high-pressure rectification tower, and C2 is middle pressure rectifying Tower, C3 are low-pressure distillation tower, and ET01 is turbo-expander, and Z01 is the supercharger for connecting turbo-expander, and CP2 is nitrogen compression Machine, V501, V502, V503, V513, V514, V515 are throttle valve.
Specific embodiment
The first aspect of the present invention provides a kind of method for efficiently producing high pure oxygen and High Purity Nitrogen, specifically includes as follows Step:
Will purifying it is dry after air be cooled to saturation state in fractionating column main heat exchanger E1, a part of saturated air into Enter high-pressure rectification tower C1 tower reactor, is separated into high pressure nitrogen and oxygen-enriched liquid air in high-pressure rectification tower C1;Another part saturated air It is pressed in rectifying tower reboiler K2 in and is condensed into liquid air;After the liquid air is mixed with the oxygen-enriched liquid air, into high-pressure rectification Gaseous state is flashed in tower condenser/evaporator K1, enters back into middle pressure tower bottom of rectifying tower;The nitrogen that high-pressure rectification tower C1 is separated Being sent into condensation in high-pressure rectification tower condenser/evaporator K1 becomes liquid nitrogen, and a part of liquid nitrogen is another as high-pressure rectification tower phegma Part liquid nitrogen presses in being used as at the top of rectifying column C2 in after subcooler E2 supercooling and presses rectifier column reflux liquid;High-pressure rectification tower The oxygen rich air that condenser/evaporator K1 is evaporated respectively enters middle pressure rectifying column C2 and carries out rectifying, is separated into medium pressure nitrogen gas and oxygen-enriched Liquid;
Therefrom the extraction of the pressure bottom rectifying column C2 is rich in the oxygen-rich liquid of low boiling hydrocarbon, assists condensing subsequently into oxygen-rich liquid Evaporator K4;In oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air, exports after re-heat;
Therefrom pressure rectifying column C2 tower top extracts medium pressure nitrogen out, and medium pressure nitrogen enters low-pressure distillation tower condensation evaporation Device K3, then be condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen return in press rectifying column C2 tower top, as pressing rectifying column in this Phegma;Another part medium pressure liquid nitrogen steams after throttling to 0.01~0.03MPa with the condensation of low-pressure distillation tower C3 tower top Hair device K5 in dirty nitrogen heat exchange and be evaporated, the low-pressure nitrogen after evaporation after subcooler E2, main heat exchanger E1 re-heat, as High pure nitrogen output of products;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower C3;
Therefrom oxygen-rich liquid of the extraction without low boiling hydrocarbon in the middle part of pressure rectifying column C2, after subcooler is subcooled, into low pressure essence Evaporate phegma of the tower C3 tower top as the low-pressure distillation tower;The oxygen-rich liquid without low boiling hydrocarbon is smart in low-pressure distillation tower C3 After evaporating, high-purity liquid oxygen product is obtained in the low-pressure distillation tower tower reactor.
In a preferred embodiment, the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen, further includes directly producing liquid The following steps of nitrogen product:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, and medium pressure nitrogen enters low-pressure distillation tower condensation Evaporator K3, then it is condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen is divided into two strands: wherein pressing in return of hydraulic fluid nitrogen in one Rectifying column C2 tower top, as the phegma for pressing rectifying column in this, wherein hydraulic fluid nitrogen is by directly defeated as liquid nitrogen product in another stock Out;Condenser/evaporator K5 with low-pressure distillation tower C3 tower top after another part medium pressure liquid nitrogen throttles to 0.01~0.03MPa In dirty nitrogen heat exchange and be evaporated, the low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as High Purity Nitrogen Gas output of products;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower C3.
In a further preferred embodiment, the above-mentioned high pure oxygen and the method for High Purity Nitrogen of efficiently producing further includes following Step:
The low-pressure nitrogen is divided into two strands after subcooler E2, main heat exchanger E1 re-heat:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products;
Wherein another strand of low-pressure nitrogen enters nitrogen compressor CP2 and is compressed, then is cooled down, swollen subsequently into turbine Swollen machine ET01 pressurized end Z01 is pressurized, then cooling in water cooler E3, subsequently enters the fractionating column main heat exchanger E1 In further cool down, then from the middle part of the fractionating column main heat exchanger E1 extract out, into the turbo-expander ET01 expansion after, The fractionating column main heat exchanger E1 re-heat is returned, is incorporated into another strand of low-pressure nitrogen later.
In an embodiment still more preferably, above-mentioned another strand of low-pressure nitrogen is from the fractionating column main heat exchanger E1 Middle part extraction after, be expanded to 0.01~0.03MPa into the turbo-expander ET01, return again to the fractionating column master and change Hot device E1 re-heat is incorporated into the suction inlet of the nitrogen compressor CP2 to room temperature later.
In an embodiment still more preferably, above-mentioned another strand of low-pressure nitrogen enters nitrogen compressor CP2 compression To 0.80~1.0MPa, be cooled to 40 DEG C hereinafter, be pressurized to 1.20 subsequently into turbo-expander ET01 pressurized end Z01~ Then 1.40MPa is cooled by water device E3 and is cooled to 40 DEG C, subsequently enter and further cool down in the fractionating column main heat exchanger E1 It is extracted out to -120 DEG C~-130 DEG C, then from the middle part of the fractionating column main heat exchanger E1, it is swollen into the turbo-expander ET01 It is swollen to 0.020~0.030MPa, return to the fractionating column main heat exchanger E1 re-heat to 30~35 DEG C, be incorporated into later described another Stock low-pressure nitrogen.
In a preferred embodiment, in the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen, the purifying drying Before air afterwards is cooled to saturation state in fractionating column main heat exchanger E1, it is divided into two strands:
Air after wherein one purifying is dry is directly entered fractionating column main heat exchanger E1;
Air after wherein another burst of purifying is dry enters turbo-expander ET01 pressurized end Z01 and is pressurized, and then exists It is cooling in water cooler E3, it subsequently enters and is further cooled down in the fractionating column main heat exchanger E1, then changed from the fractionating column master The middle part of hot device E1 is extracted out, into after turbo-expander ET01 expansion, is back to the fractionating column main heat exchanger E1 and is carried out Re-heat;The low-pressure air exported through the fractionating column main heat exchanger E1, after air booster is pressurized, as backflowing air simultaneously Air after entering the purifying drying to before being divided into two strands.
It is described in the above-mentioned method for efficiently producing high pure oxygen and High Purity Nitrogen in a further preferred embodiment Air after another burst of purifying is dry enters turbo-expander ET01 pressurized end Z01 and is pressurized to 1.20~1.40MPa, then in water It is cooled to 40 DEG C in cooler E3, subsequently enters in the fractionating column main heat exchanger E1 and is cooled further to -120 DEG C~-130 DEG C, then it is extracted out from the middle part of the fractionating column main heat exchanger E1,0.020 is expanded into the turbo-expander ET01~ 0.030MPa is returned again to the fractionating column main heat exchanger E1 re-heat to 30~35 DEG C;It is defeated through the fractionating column main heat exchanger E1 It is dry to be incorporated into the purifying before being divided into two strands as the air that backflows after air booster is pressurized for low-pressure air out Air after dry.
In an embodiment still more preferably, the operating pressure of the high-pressure rectification tower C1 is 0.8~1.3MPa, The operating pressure of medium pressure rectifying column C2 is 0.35~0.6MPa, the operating pressure of the low-pressure distillation tower C3 is 0.02~ 0.15MPa。
In an embodiment still more preferably, the main component of the low boiling hydrocarbon is methane.
The second aspect of the present invention provides high pure oxygen made from a kind of method according to a first aspect of the present invention And/or High Purity Nitrogen, which is characterized in that O in the high pure oxygen2Purity >=99.9999%, N in the High Purity Nitrogen2Purity >= 99.999%.
The present invention is further elaborated With reference to embodiment, but the present invention is not limited to following embodiments. Each step in the method is conventional steps unless otherwise specified;The equipment unless otherwise specified can be from open business Approach obtains.
Embodiment 1
High pure oxygen and High Purity Nitrogen are produced using process flow method as shown in Figure 1:
By air 101 (3350NM of the purifying after dry3/ h, 0.96MPa) air 206 merges with backflowing, and it is described after merging Air total flow after purifying is dry is 7750NM3/ h, and before being cooled to saturation state in fractionating column main heat exchanger E1, point It is two strands:
Wherein one 102 is directly entered fractionating column main heat exchanger E1;
Wherein another 201 (4400NM of stock3/ h, 0.96MPa) it is pressurized into turbo-expander ET01 pressurized end Z01 202 are obtained after 1.32MPa, then is cooled by water device E3 and is cooled to 40 DEG C, are subsequently entered fractionating column main heat exchanger E1 and are cooled to -122 DEG C, Extraction 204 in the middle part of from main heat exchanger, and it is expanded to 0.025MPa into the turbo-expander ET01,205 are obtained, institute is returned again to Fractionating column main heat exchanger E1 and re-heat are stated to 32 DEG C, obtains 206;Wherein, the cooling capacity that the turbo-expander generates maintains device Cold balancing.The low-pressure air 206 exported through the fractionating column main heat exchanger E1, is pressurized to 0.96MPa by air booster Afterwards, the Trunk Line of the air 101 after purifying drying is incorporated into as the air that backflows, 101 on the Trunk Line are not divided into two strands also;
Above-mentioned 102 (3350NM3/ h, 0.96MPa) in fractionating column main heat exchanger E1 it is cooled to saturation state 103;Then, 103 split into 105 two parts of saturated air 104 and saturated air, in which:
104 (2950NM of saturated air3/ h) enter high-pressure rectification tower C1 tower reactor, height is separated into high-pressure rectification tower C1 Press nitrogen 300 and oxygen-enriched liquid air 501;
105 (400NM of saturated air3/ h) enter in press rectifying tower reboiler K2 in be condensed into liquid air 106;
After the liquid air 106 is mixed with the oxygen-enriched liquid air 501 from high-pressure rectification tower, 503 are obtained, subsequently into high pressure Gaseous state 504 is flashed in rectifying column condenser/evaporator K1, enters back into middle pressure rectifying column C2 tower reactor;High-pressure rectification tower C1 is isolated The nitrogen 404 come, which is sent into condensation in high-pressure rectification tower condenser/evaporator K1, becomes liquid nitrogen 405, and a part of liquid nitrogen is as high-pressure rectification Tower phegma, another part liquid nitrogen (1000NM3/ h) it is crossed through subcooler E2 and is cooled to -181 DEG C, it presses in and makees at the top of rectifying column C2 For middle pressure rectifier column reflux liquid;The oxygen rich air 504 that high-pressure tower condenser/evaporator K1 is evaporated respectively enter middle pressure rectifying column C2 into Row rectifying, wherein the operating pressure that rectifying column C2 is pressed in this is 0.5MPa, is separated into medium pressure nitrogen gas 401 and oxygen-rich liquid 901。
From the 901 (160NM of the oxygen-rich liquid for pressing the extraction of the bottom rectifying column C2 to be rich in low boiling hydrocarbon in this3/ h), then into Enter oxygen-rich liquid auxiliary condenser/evaporator K4;In oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air 904,906 are exported after re-heat;
Therefrom pressure rectifying column C2 tower top extracts 401 (2840NM of medium pressure nitrogen out3/ h), medium pressure nitrogen enters low pressure Rectifying column condenser/evaporator K3, then it is condensed into middle hydraulic fluid nitrogen 405, rectifying column C2 is pressed in a part of return of medium pressure liquid nitrogen 405 Tower top, as the phegma for pressing rectifying column in this;Another part medium pressure liquid nitrogen (1880NM3/ h) it throttles to 0.03MPa It exchanges heat and is evaporated with the dirty nitrogen in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top, the low-pressure nitrogen after evaporation is through being subcooled After device E2, main heat exchanger E1 re-heat, exported as high pure nitrogen product 414, i.e. low-pressure nitrogen 414, yield 1880NM3/ H, wherein the O as foreign gas2Content≤3pppm, pressure 0.01MPa;And the liquid nitrogen fraction condensed is as low-pressure distillation tower C3 Phegma;
Therefrom oxygen-rich liquid (1300NM of the extraction without low boiling hydrocarbon in the middle part of pressure rectifying column C23/ h), it is subcooled by subcooler Enter phegma 603 of the low-pressure distillation tower C3 tower top as the low-pressure distillation tower afterwards;The oxygen-rich liquid without low boiling hydrocarbon exists In low-pressure distillation tower C3 after rectifying, O is obtained in the low-pressure distillation tower tower reactor2High-purity liquid oxygen product 701 of purity >=99.9999% (500NM3/h)。
Embodiment 2
High pure oxygen and High Purity Nitrogen are produced using process flow method as shown in Figure 2:
By air 101 (3350NM of the purifying after dry3/ h, 0.96MPa) be cooled in fractionating column main heat exchanger E1 it is full With state 103, a part of 104 (2950NM of saturated air3/ h) enter high-pressure rectification tower C1 tower reactor, divide in high-pressure rectification tower C1 From at high pressure nitrogen 300 and oxygen-enriched liquid air 501;105 (400NM of another part saturated air3/ h) enter in pressure rectifying column boil again Be condensed into liquid air 106 in device K2, liquid air 106 mixed with the oxygen-enriched liquid air 501 of high pressure tower reactor after 503, it is cold into high-pressure rectification tower Gaseous state 504 is flashed in solidifying evaporator K1, enters back into middle pressure tower bottom of rectifying tower;The nitrogen that high-pressure rectification tower C1 is separated 404, which are sent into high-pressure rectification tower condenser/evaporator K1 condensation, becomes liquid nitrogen 405, and a part of liquid nitrogen therein is returned as high-pressure rectification tower Flow liquid;Another branch's liquid nitrogen (1000NM therein3/ h) it is crossed through subcooler E2 and is cooled to -181 DEG C, it is pressed at the top of rectifying column C2 in As middle pressure rectifier column reflux liquid, the oxygen rich air 504 that high-pressure rectification tower condenser/evaporator K1 is evaporated respectively enters middle pressure rectifying Tower C2 carries out rectifying, wherein the operating pressure that rectifying column C2 is pressed in this is 0.5MPa, is separated into medium pressure nitrogen gas 401 and oxygen-rich liquid 901。
Therefrom the extraction of the pressure bottom rectifying column C2 is rich in the 901 (160NM of the oxygen-rich liquid of low boiling hydrocarbon3/ h), subsequently into Oxygen-rich liquid assists condenser/evaporator K4;In oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air 904,906 are exported after re-heat;
Therefrom pressure rectifying column C2 tower top extracts 401 (2840NM of medium pressure nitrogen out3/ h), medium pressure nitrogen enters low pressure Rectifying column condenser/evaporator K3, then it is condensed into middle hydraulic fluid nitrogen 404, rectifying column C2 is pressed in the return of a portion medium pressure liquid nitrogen Tower top, as the phegma for pressing rectifying column in this;Wherein 405 (1880NM of hydraulic fluid nitrogen in another part3/ h) it throttles to 0.01MPa Afterwards, it exchanges heat and evaporates with the dirty nitrogen 609 in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top, the low-pressure nitrogen warp after evaporation After subcooler E2, main heat exchanger E1 re-heat, exported as high pure nitrogen product 414, i.e., low-pressure nitrogen 414, yield are 1880NM3/ h, wherein the O as foreign gas2Content≤3pppm, pressure 0.01MPa;And the liquid nitrogen fraction condensed is as low pressure essence Evaporate the phegma of tower C3;
Therefrom oxygen-rich liquid 601 (1300NM of the extraction without low boiling hydrocarbon in the middle part of pressure rectifying column C23/ h), it is subcooled through subcooler Afterwards, the phegma 603 into low-pressure distillation tower C3 tower top as the low-pressure distillation tower;The oxygen-rich liquid without low boiling hydrocarbon exists In low-pressure distillation tower C3 after rectifying, O is obtained in the low-pressure distillation tower tower reactor2High-purity liquid oxygen product 701 of purity >=99.9999% (500NM3/h)。
In addition, to be divided to be two strands to the low-pressure nitrogen 414 exported from main heat exchanger E1, wherein one as described above, directly as High pure nitrogen output of products;And another strand of low-pressure nitrogen 414 and 206 is mixed, and 207 (4100NM are obtained3/ h, 0.01MPa, 32 DEG C), into nitrogen compressor CP2, it is compressed to 0.96MPa, then be cooled by water device E3 and be cooled to 40 DEG C hereinafter, subsequently into turbine The pressurized end Z01 of expanding machine ET01 is pressurized to 1.32MPa, obtains 202, is cooled to 40 DEG C later, subsequently enters the fractionating column master Heat exchanger E1 is cooled to -122 DEG C, obtains 204;It extracts out from the middle part of main heat exchanger E1, is expanded into turbo-expander ET01 again 0.025MPa, obtains 205, then returns to the fractionating column main heat exchanger E1 re-heat to 32 DEG C, obtains 206, this 206 be incorporated into it is described another One low-pressure nitrogen;Wherein, the cooling capacity that expanding machine generates maintains device cold balancing.
Specific embodiments of the present invention are described in detail above, but it is merely an example, the present invention is simultaneously unlimited It is formed on particular embodiments described above.To those skilled in the art, any couple of present invention carries out equivalent modifications and Substitution is also all among scope of the invention.Therefore, without departing from the spirit and scope of the invention made by equal transformation and Modification, all should be contained within the scope of the invention.

Claims (9)

1. the method that one kind efficiently produces high pure oxygen and High Purity Nitrogen, which comprises the steps of:
Air of the purifying after dry is cooled to saturation state in fractionating column main heat exchanger (E1), a part of saturated air enters High-pressure rectification tower (C1) tower reactor, is separated into high pressure nitrogen and oxygen-enriched liquid air in high-pressure rectification tower (C1);Another part saturation is empty It is pressed in rectifying tower reboiler (K2) in gas entrance and is condensed into liquid air;After the liquid air is mixed with the oxygen-enriched liquid air, into high pressure Gaseous state oxygen rich air is flashed in rectifying column condenser/evaporator (K1), enters back into middle pressure tower bottom of rectifying tower;By high-pressure rectification tower (C1) The nitrogen separated, which is sent into condensation in high-pressure rectification tower condenser/evaporator (K1), becomes liquid nitrogen, and a part of liquid nitrogen is as high pressure essence Tower phegma is evaporated, another part liquid nitrogen presses in being used as at the top of rectifying column (C2) in after subcooler (E2) supercooling and presses rectifying Tower phegma;The gaseous state oxygen rich air that high-pressure rectification tower condenser/evaporator (K1) evaporates presses rectifying column (C2) to carry out in entering Rectifying is separated into medium pressure nitrogen gas and oxygen-rich liquid;
Therefrom the extraction of the pressure rectifying column bottom (C2) is rich in the oxygen-rich liquid of low boiling hydrocarbon, assists condensation to steam subsequently into oxygen-rich liquid It sends out device (K4);In oxygen-rich liquid auxiliary condenser/evaporator (K4), oxygen-rich liquid is evaporated into oxygen rich air, defeated after re-heat Out;
Therefrom pressure rectifying column (C2) tower top extracts medium pressure nitrogen out, and medium pressure nitrogen enters low-pressure distillation tower condenser/evaporator (K3), then be condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen return in press rectifying column (C2) tower top, as pressing rectifying in this The phegma of tower;Another part medium pressure liquid nitrogen is cold with low-pressure distillation tower (C3) tower top after throttling to 0.01~0.03MPa Dirty nitrogen in solidifying evaporator (K5) exchanges heat and is evaporated, and the low-pressure nitrogen after evaporation is through subcooler (E2), main heat exchanger (E1) After re-heat, as high pure nitrogen output of products;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower (C3);
Therefrom oxygen-rich liquid of the extraction without low boiling hydrocarbon in the middle part of pressure rectifying column (C2), after subcooler is subcooled, into low-pressure distillation Phegma of tower (C3) tower top as the low-pressure distillation tower;The oxygen-rich liquid without low boiling hydrocarbon is in low-pressure distillation tower (C3) After rectifying, high-purity liquid oxygen product is obtained in the low-pressure distillation tower tower reactor.
2. the method according to claim 1, wherein further including the following steps for directly producing liquid nitrogen product:
Medium pressure nitrogen is extracted out from medium pressure rectifying column (C2) tower top, and medium pressure nitrogen enters low-pressure distillation tower condensation and steams It sends out device (K3), then is condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen is divided into two strands: wherein being pressed in return of hydraulic fluid nitrogen in one Rectifying column (C2) tower top, as the phegma for pressing rectifying column in this, wherein hydraulic fluid nitrogen is by direct as liquid nitrogen product in another stock Output;Condensation evaporation with low-pressure distillation tower (C3) tower top after another part medium pressure liquid nitrogen throttles to 0.01~0.03MPa In device (K5) dirty nitrogen heat exchange and be evaporated, the low-pressure nitrogen after evaporation after subcooler (E2), main heat exchanger (E1) re-heat, As high pure nitrogen output of products;And phegma of the liquid nitrogen fraction condensed as low-pressure distillation tower (C3).
3. method according to claim 1 or 2, which is characterized in that further comprising the steps of:
The low-pressure nitrogen is divided into two strands after subcooler (E2), main heat exchanger (E1) re-heat:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products;
Wherein another strand of low-pressure nitrogen enters nitrogen compressor (CP2) and is compressed, then is cooled down, subsequently into turbine expansion Machine (ET01) pressurized end (Z01) is pressurized, then cooling in water cooler (E3), subsequently enters the fractionating column main heat exchange It further cools down in device (E1), then is extracted out from the middle part of the fractionating column main heat exchanger (E1), into the turbo-expander (ET01) after expanding, fractionating column main heat exchanger (E1) re-heat is returned, is incorporated into another strand of low-pressure nitrogen later.
4. according to the method described in claim 3, it is characterized in that, another strand of low-pressure nitrogen is from the fractionating column main heat exchange After the middle part extraction of device (E1), it is expanded to 0.01~0.03MPa into the turbo-expander (ET01), returns again to described point (E1) re-heat of tower main heat exchanger is evaporated to room temperature, is incorporated into the suction inlet of the nitrogen compressor (CP2) later.
5. according to the method described in claim 3, it is characterized in that, another strand of low-pressure nitrogen enters nitrogen compressor (CP2) it is compressed to 0.80~1.0MPa, is cooled to 40 DEG C hereinafter, subsequently into turbo-expander (ET01) pressurized end (Z01) It is pressurized to 1.20~1.40MPa, device (E3) is then cooled by water and is cooled to 40 DEG C, subsequently enter the fractionating column main heat exchanger (E1) it is cooled further to -120 DEG C~-130 DEG C in, then is extracted out from the middle part of the fractionating column main heat exchanger (E1), into institute State turbo-expander (ET01) and be expanded to 0.020~0.030MPa, return fractionating column main heat exchanger (E1) re-heat to 30~ 35 DEG C, it is incorporated into another strand of low-pressure nitrogen later.
6. the method according to claim 1, wherein the air after the purifying is dry is in fractionating column main heat exchanger (E1) it is cooled to before saturation state in, is divided into two strands:
Air after wherein one purifying is dry is directly entered fractionating column main heat exchanger (E1);
Air after wherein another burst of purifying is dry enters turbo-expander (ET01) pressurized end (Z01) and is pressurized, and then exists It is cooling in water cooler (E3), it subsequently enters and is further cooled down in the fractionating column main heat exchanger (E1), then from the fractionating column The middle part of main heat exchanger (E1) is extracted out, into after the turbo-expander (ET01) expansion, is back to the fractionating column main heat exchange Device (E1) carries out re-heat;The low-pressure air exported through the fractionating column main heat exchanger (E1) is made after air booster is pressurized The air after the drying of the purifying before being divided into two strands is incorporated into for the air that backflows.
7. according to the method described in claim 6, it is characterized in that, the air after another burst of purifying is dry to enter turbine swollen Swollen machine (ET01) pressurized end (Z01) is pressurized to 1.20~1.40MPa, is then cooled to 40 DEG C in water cooler (E3), then Into being cooled further to -120 DEG C~-130 DEG C in the fractionating column main heat exchanger (E1), then from the fractionating column main heat exchanger (E1) middle part extraction, is expanded to 0.020~0.030MPa into the turbo-expander (ET01), returns again to the fractionation (E1) re-heat of tower main heat exchanger is to 30~35 DEG C;The low-pressure air exported through the fractionating column main heat exchanger (E1), by air After supercharger pressurization, the air after the drying of the purifying before being divided into two strands is incorporated into as the air that backflows.
8. according to claim 1, method described in any one of 2,6,7, which is characterized in that the behaviour of the high-pressure rectification tower (C1) Making pressure is 0.8~1.3MPa, and the operating pressure of medium pressure rectifying column (C2) is 0.35~0.6MPa, the low-pressure distillation tower (C3) operating pressure is 0.02~0.15MPa.
9. according to claim 1, method described in any one of 2,6,7, which is characterized in that the main component of the low boiling hydrocarbon For methane.
CN201610205678.2A 2016-04-01 2016-04-01 A method of efficiently producing high pure oxygen and High Purity Nitrogen Active CN105865148B (en)

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