CN105865148A - Method for efficient production of high-purity oxygen and high-purity nitrogen - Google Patents

Method for efficient production of high-purity oxygen and high-purity nitrogen Download PDF

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Publication number
CN105865148A
CN105865148A CN201610205678.2A CN201610205678A CN105865148A CN 105865148 A CN105865148 A CN 105865148A CN 201610205678 A CN201610205678 A CN 201610205678A CN 105865148 A CN105865148 A CN 105865148A
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nitrogen
pressure
tower
low
oxygen
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CN105865148B (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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    • 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
    • F25J3/0429—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 of feed air, e.g. used as waste or product air or expanded into an auxiliary column
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing 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
    • F25J3/04054—Providing 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
    • 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
    • F25J3/04048—Providing 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
    • F25J3/0406—Providing 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
    • 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
    • F25J3/04048—Providing 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
    • F25J3/04066—Providing 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
    • 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
    • F25J3/04109—Arrangements of compressors and /or their drivers
    • 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
    • F25J3/04333—Generation 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
    • F25J3/04351—Generation 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
    • F25J3/04357—Generation 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
    • 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
    • F25J3/04436—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 at least a triple pressure main column system
    • 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
    • F25J3/04436—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 at least a triple pressure main column system
    • F25J3/04454—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 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
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/52—Processes 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
    • 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
    • F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
    • F25J2200/54—Processes 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
    • 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
    • F25J2215/00—Processes characterised by the type or other details of the product stream
    • F25J2215/40—Air or oxygen enriched air, i.e. generally less than 30mol% of O2
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2250/00—Details related to the use of reboiler-condensers
    • F25J2250/20—Boiler-condenser with multiple exchanger cores in parallel or with multiple re-boiling or condensing streams

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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

The invention provides a method for efficient production of high-purity oxygen and high-purity nitrogen. A high pressure rectifying tower, a medium pressure rectifying tower and a low pressure rectifying tower are adopted; a reboiler is arranged at the bottom of the medium pressure rectifying tower, and a condensation evaporator is disposed at the bottom of the low pressure rectifying tower; high pressure nitrogen and oxygen-enriched liquid air are obtained through separation of part of air in the high pressure rectifying tower, and the other part of air enters the reboiler of the medium pressure rectifying tower to be condensed into liquid air; the liquid air and the oxygen-enriched liquid air are mixed, then enter a condensation evaporator of the high pressure rectifying tower to be evaporated into a gas state and then enter the medium pressure rectifying tower; and then a high-purity nitrogen product and oxygen-enriched liquid are obtained through separation in the medium pressure rectifying tower, and the oxygen-enriched liquid enters the low pressure rectifying tower to be rectified, so that a high-purity liquid oxygen product is obtained. The high-purity liquid oxygen and the high-purity nitrogen can be produced at the same time; the extraction ratio of the high-purity nitrogen reaches 60%-75%, and the extraction ratio of the high-purity oxygen reaches 70%-72%; and according to the method, air is used as a raw material which is economical and practical, the products are safe and reliable and can be widely applied, and the market prospects are good.

Description

A kind of high pure oxygen of efficient production and the method for High Purity Nitrogen
Technical field
The invention belongs to gas generation field, relate to a kind of method carrying out gas separation by low-temperature liquefaction, particularly relate to a kind of high pure oxygen of efficient production and the method for High Purity Nitrogen.
Background technology
Along with the fast development of the industry such as electronics, chemical industry, high pure nitrogen, high pure oxygen demand being increased dramatically, usual industrial oxygen purity is 99.6%O2, and the high pure oxygen purity ＞ 99.9999%O needed for electronics industry2；In precision electronic industries, high pure oxygen is normally used for the chemical gaseous phase deposition of silicon dioxide, or as oxidation source and the reactant producing high purity water；Or for dry oxidation；Or mix with carbon tetrafluoride, for plasma etching etc..
Current commonly used liquid oxygen is that raw material carries out producing of high pure oxygen, but its extraction ratio is on the low side；And use in krypton xenon raw process flow process, through once, secondarily purified after oxygen, purity reaches 99.5%～99.99%, and it is the splendid raw material of high purity oxygen, it is characterized in that yield is big, purity is high, and krypton xenon rough releasing oxygen source becomes the reason limiting high-purity fluid oxygen yield more at least.
Major gaseous component in air is nitrogen and oxygen, nitrogen and oxygen purity are respectively 78.12% and 20.95%, and air is ubiquitous as low-cost resource, therefore it is directly produced high pure nitrogen by separation air and high purity oxygen gas is the easiest and economic method.Therefore, develop a kind of method isolating high pure oxygen and High Purity Nitrogen from air, become one of study hotspot of current Chemical R & D personnel.
Summary of the invention
It is contemplated that overcome many disadvantages present in above-mentioned prior art, and provide a kind of method isolating high pure oxygen and High Purity Nitrogen efficiently from air, meet the demand using high pure oxygen and High Purity Nitrogen in the field such as precision electronic industries, biological medicine.
Therefore, a first aspect of the present invention, provide a kind of high pure oxygen of efficient production and the method for High Purity Nitrogen, the equipment that the method uses 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, described high-pressure rectification column overhead is provided with condenser/evaporator K1；Being provided with reboiler K2 at the bottom of medium pressure rectifying tower, its tower top is provided with oxygen-rich liquid auxiliary condenser/evaporator K4；Being provided with condenser/evaporator K3 at the bottom of described low-pressure distillation tower tower, its tower top is provided with condenser/evaporator K5；Some valves and pipeline, be used for connecting above each equipment；Described method specifically includes following steps:
Dried for purification air is cooled in fractionating column main heat exchanger E1 saturation, and 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 saturated air is pressed in rectifying column reboiler K2 in entering and is condensed into liquid air；After described liquid air mixes with described oxygen-enriched liquid air, enter in high-pressure rectification tower condenser/evaporator K1 and flash to gaseous state, enter back into middle pressure tower bottom of rectifying tower；The nitrogen separated by high-pressure rectification tower C1 sends into condensation in high-pressure rectification tower condenser/evaporator K1 becomes liquid nitrogen, a part of liquid nitrogen is as high-pressure rectification tower backflow, another part liquid nitrogen, after subcooler E2 is supercool, presses rectifying column C2 top as middle pressure rectifier column reflux liquid in entrance；The oxygen rich air that high-pressure rectification tower condenser/evaporator K1 evaporates respectively enters middle pressure rectifying column C2 and carries out rectification, is separated into medium pressure nitrogen gas and oxygen-rich liquid；
Therefrom extract the described oxygen-rich liquid rich in low boiling hydrocarbon out bottom pressure rectifying column C2, assist condenser/evaporator K4 subsequently into oxygen-rich liquid；In described 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 condenser/evaporator K3, then is condensed into middle hydraulic fluid nitrogen, and a part of medium pressure liquid nitrogen presses rectifying column C2 tower top, as the backflow pressing rectifying column in this in returning；The throttling of another part medium pressure liquid nitrogen to behind 0.01～0.03MPa with the dirty nitrogen heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top and evaporated, low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as high pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3；
Therefrom extract the oxygen-rich liquid without low boiling hydrocarbon out in the middle part of pressure rectifying column C2, after subcooler is supercool, enter the low-pressure distillation tower C3 tower top backflow as this low-pressure distillation tower；The described oxygen-rich liquid without low boiling hydrocarbon after rectification, obtains high-purity fluid oxygen product in this low-pressure distillation tower tower reactor in low-pressure distillation tower C3.
Preferably, the above-mentioned high pure oxygen of efficient production and the method for High Purity Nitrogen, also include the following steps directly producing liquid nitrogen product:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, medium pressure nitrogen enters low-pressure distillation tower condenser/evaporator K3, it is condensed into middle hydraulic fluid nitrogen again, a part of medium pressure liquid nitrogen is divided into two strands: press rectifying column C2 tower top during wherein hydraulic fluid nitrogen returns in one, as pressing the backflow of rectifying column in this, wherein in another stock, hydraulic fluid nitrogen is directly exported as liquid nitrogen product；The throttling of another part medium pressure liquid nitrogen to behind 0.01～0.03MPa with the dirty nitrogen heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top and evaporated, low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as high pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3.
It is further preferred that the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen is further comprising the steps of:
Described low-pressure nitrogen, after subcooler E2, main heat exchanger E1 re-heat, is divided into two strands:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products；
Wherein another gang of low-pressure nitrogen entrance nitrogen compressor CP2 is compressed, cool down again, supercharging is carried out subsequently into turbo-expander ET01 pressurized end Z01, then cool down in water cooler E3, subsequently enter in described fractionating column main heat exchanger E1 and cool down further, then extract out from the middle part of described fractionating column main heat exchanger E1, after entering described turbo-expander ET01 expansion, return described fractionating column main heat exchanger E1 re-heat, be incorporated into described another strand of low-pressure nitrogen afterwards.
Still more preferably, above-mentioned another strand of low-pressure nitrogen is after the middle part of described fractionating column main heat exchanger E1 is extracted out, enter described turbo-expander ET01 and be expanded to 0.01～0.03MPa, return again to described fractionating column main heat exchanger E1 re-heat to room temperature, be incorporated into the suction inlet of described nitrogen compressor CP2 afterwards.
Still more preferably, above-mentioned another strand of low-pressure nitrogen enters nitrogen compressor CP2 and is compressed to 0.80～1.0MPa, it is cooled to less than 40 DEG C, it is pressurized to 1.20～1.40MPa subsequently into turbo-expander ET01 pressurized end Z01, the most water cooled but device E3 is cooled to 40 DEG C, subsequently enter in described fractionating column main heat exchanger E1 and be cooled further to-120 DEG C～-130 DEG C, extract out from the middle part of described fractionating column main heat exchanger E1 again, enter described turbo-expander ET01 and be expanded to 0.020～0.030MPa, return described fractionating column main heat exchanger E1 re-heat to 30～35 DEG C, it is incorporated into described another strand of low-pressure nitrogen afterwards.
Preferably, in the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen, before the dried air of described purification is cooled to saturation in fractionating column main heat exchanger E1, it is divided into two strands:
Wherein the dried air of one purification is directly entered fractionating column main heat exchanger E1；
Wherein another gang of purification dried air entrance turbo-expander ET01 pressurized end Z01 carries out supercharging, then cool down in water cooler E3, subsequently enter in described fractionating column main heat exchanger E1 and cool down further, extract out from the middle part of described fractionating column main heat exchanger E1 again, after entering described turbo-expander ET01 expansion, it is back to described fractionating column main heat exchanger E1 and carries out re-heat；Through the low-pressure air of described fractionating column main heat exchanger E1 output, after air booster supercharging, it is incorporated into the dried air of described purification being divided into before two strands as the air that backflows.
Further preferably, in the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen, the described dried air of another strand of purification enters turbo-expander ET01 pressurized end Z01 and is pressurized to 1.20～1.40MPa, then in water cooler E3,40 DEG C it are cooled to, subsequently enter in described fractionating column main heat exchanger E1 and be cooled further to-120 DEG C～-130 DEG C, extract out from the middle part of described fractionating column main heat exchanger E1 again, enter described turbo-expander ET01 and be expanded to 0.020～0.030MPa, return again to described fractionating column main heat exchanger E1 re-heat to 30～35 DEG C；Through the low-pressure air of described fractionating column main heat exchanger E1 output, after air booster supercharging, it is incorporated into the dried air of described purification being divided into before two strands as the air that backflows.
It is further preferred that the operation pressure of described high-pressure rectification tower C1 is 0.8～1.3MPa, the operation pressure of medium pressure rectifying column C2 is 0.35～0.6MPa, and the operation pressure of described low-pressure distillation tower C3 is 0.02～0.15MPa.In the range of aforesaid operations pressure is preferred, it is 0.5MPa that medium pressure rectifying column C2 most preferably operates pressure.
It is further preferred that described low boiling hydrocarbon be mainly composed of methane.
A second aspect of the present invention, it is provided that high pure oxygen that a kind of method described according to a first aspect of the present invention prepares and/or High Purity Nitrogen, it is characterised in that O in described high pure oxygen2Purity >=99.9999%, N in described High Purity Nitrogen2Purity >=99.999%.Visible, obtained high pure oxygen and/or High Purity Nitrogen have all reached relevant national standard.
Compared with prior art, the invention have the advantages that
(1) Traditional high purity oxygen mainly purifies from industry oxygen (99.5%), it is generally required to 2～3 rectifying columns, remove the high boiling component (methane, krypton, xenon, nitrous oxide etc.) in industry oxygen respectively, then go the argon component in deoxygenation, the present invention at least one equilibrium stage extraction above the middle pressure tower bottom of rectifying tower of High Purity Nitrogen product producing band pressure is substantially free of the oxygen-rich liquid of methane as raw material, the high boiling component content such as methane contained therein, krypton, xenon are ppb level, and the extraction ratio of nitrogen does not reduce simultaneously；
(2) reclaim while the present invention can realize High Purity Nitrogen and high pure oxygen, wherein, the extraction rate reached of High Purity Nitrogen to 60-75%, extraction rate reached 70%-72% of high pure oxygen；
(3) high pure oxygen product is various informative, and the high pure oxygen product of production can be gas, it is possible to for liquid oxygen product, be delivered to liquid storage groove storage；
(4) the low pure liquid oxygen of part is discharged (containing about 50-70% oxygen in medium pressure rectifier bottoms, containing methane about 100-500ppm, surplus is krypton, xenon, nitrous oxide etc.) make the content of hydrocarbon in medium pressure rectifying column reduce, improve the safety of equipment.
(5) the high pure oxygen of efficient production provided by the present invention and the method for High Purity Nitrogen, with air as raw material, economical and practical, and product safety is reliable, the available extensively application of the method, has good market prospect.
Accompanying drawing explanation
Fig. 1 is the technological process method schematic diagram of an embodiment 1 of device of the present invention；
nullWherein: 101 is the dried air of the purification in main line，102、201 is the dried air of the purification in branch road，103 is the saturated air from the output of fractionating column main heat exchanger，104、105 is two parts saturated air from 103 shuntings，106、107 is liquid air，202、203、204 are the air after supercharging，205、206 is the low-pressure air after expanding，300 is high pressure nitrogen，301、302、303 is high-pressure liquid nitrogen，304 is middle hydraulic fluid nitrogen，401、402、404、407 is medium pressure nitrogen gas，403、405、406、410、302b is middle hydraulic fluid nitrogen，411 is low pressure liquid nitrogen，412、413、414 is low-pressure nitrogen，501、502、503 is liquid air，504 is oxygen rich air，601、602 is the oxygen-rich liquid extracted out in the middle part of middle pressure rectifying column，604、605、607、608、609 is dirty nitrogen、The liquid nitrogen fraction that 606 is condensation，603 is the mixture of oxygen-rich liquid 602 and liquid nitrogen fraction 606，701 is high-purity liquid oxygen，901、902、903 is the oxygen-rich liquid that middle pressure tower bottom of rectifying tower is extracted out，904、906 is the oxygen rich air of middle pressure rectifying column auxiliary condenser/evaporator K4 evaporation，E1 is main heat exchanger，E2 is subcooler，E3 is water cooler，K1 is high-pressure rectification tower condenser/evaporator，K2 is middle pressure rectifying column reboiler，K3 is low-pressure distillation tower tower reactor vaporizer，K4 is that oxygen-rich liquid assists condenser/evaporator，K5 is the condenser/evaporator of low-pressure distillation tower C3 tower top，C1 is high-pressure rectification tower，C2 is middle pressure rectifying column，C3 is low-pressure distillation tower，ET01 is turbo-expander，Z01 is the pressurized end connecting turbo-expander，V501、V502、V503、V513、V514、V515 is choke valve.
Fig. 2 is the technological process method schematic diagram of an embodiment 2 of device of the present invention；
nullWherein: 101 is the dried air of the purification in main line，103 is the saturated air from the output of fractionating column main heat exchanger，104、105 is two parts saturated air from 103 shuntings，106、107 is liquid air，207、201 is the nitrogen after nitrogen compressor CP2 compresses，202、203、204 are the nitrogen after supercharging，205、206 is the low-pressure nitrogen after expanding，415 for supplementing the low-pressure nitrogen of nitrogen compressor CP2，300 is high pressure nitrogen，301、302、303 is high-pressure liquid nitrogen，304 is middle hydraulic fluid nitrogen，401、402、404、407 is medium pressure nitrogen gas，403、405、406、410、302b is middle hydraulic fluid nitrogen，411 is low pressure liquid nitrogen，412、413、414 is low-pressure nitrogen，501、502、503 is liquid air，504 is oxygen rich air，601、602 is the oxygen-rich liquid extracted out in the middle part of middle pressure rectifying column，604、605、607、608、609 is dirty nitrogen、The liquid nitrogen fraction that 606 is condensation，603 is the mixture of oxygen-rich liquid 602 and liquid nitrogen fraction 606，701 is high-purity liquid oxygen，901、902、903 is the oxygen-rich liquid that middle pressure tower bottom of rectifying tower is extracted out，904、906 is the oxygen rich air of middle pressure rectifying column auxiliary condenser/evaporator K4 evaporation，E1 is main heat exchanger，E2 is subcooler，E3，E4 is water cooler，K1 is high-pressure rectification tower condenser/evaporator，K2 is middle pressure rectifying column reboiler，K3 is low-pressure distillation tower tower reactor vaporizer，K4 is that oxygen-rich liquid assists condenser/evaporator，K5 is the condenser/evaporator of low-pressure distillation tower C3 tower top，C1 is high-pressure rectification tower，C2 is middle pressure rectifying column，C3 is low-pressure distillation tower，ET01 is turbo-expander，Z01 is the supercharger connecting turbo-expander，CP2 is nitrogen compressor，V501、V502、V503、V513、V514、V515 is choke valve.
Detailed description of the invention
A first aspect of the present invention, it is provided that a kind of high pure oxygen of efficient production and the method for High Purity Nitrogen, specifically includes following steps:
Dried for purification air is cooled in fractionating column main heat exchanger E1 saturation, and 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 saturated air is pressed in rectifying column reboiler K2 in entering and is condensed into liquid air；After described liquid air mixes with described oxygen-enriched liquid air, enter in high-pressure rectification tower condenser/evaporator K1 and flash to gaseous state, enter back into middle pressure tower bottom of rectifying tower；The nitrogen separated by high-pressure rectification tower C1 sends into condensation in high-pressure rectification tower condenser/evaporator K1 becomes liquid nitrogen, a part of liquid nitrogen is as high-pressure rectification tower backflow, another part liquid nitrogen, after subcooler E2 is supercool, presses rectifying column C2 top as middle pressure rectifier column reflux liquid in entrance；The oxygen rich air that high-pressure rectification tower condenser/evaporator K1 evaporates respectively enters middle pressure rectifying column C2 and carries out rectification, is separated into medium pressure nitrogen gas and oxygen-rich liquid；
Therefrom extract the described oxygen-rich liquid rich in low boiling hydrocarbon out bottom pressure rectifying column C2, assist condenser/evaporator K4 subsequently into oxygen-rich liquid；In described 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 condenser/evaporator K3, then is condensed into middle hydraulic fluid nitrogen, and a part of medium pressure liquid nitrogen presses rectifying column C2 tower top, as the backflow pressing rectifying column in this in returning；The throttling of another part medium pressure liquid nitrogen to behind 0.01～0.03MPa with the dirty nitrogen heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top and evaporated, low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as high pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3；
Therefrom extract the oxygen-rich liquid without low boiling hydrocarbon out in the middle part of pressure rectifying column C2, after subcooler is supercool, enter the low-pressure distillation tower C3 tower top backflow as this low-pressure distillation tower；The described oxygen-rich liquid without low boiling hydrocarbon after rectification, obtains high-purity fluid oxygen product in this low-pressure distillation tower tower reactor in low-pressure distillation tower C3.
In a preferred embodiment, the above-mentioned high pure oxygen of efficient production and the method for High Purity Nitrogen, also include the following steps directly producing liquid nitrogen product:
Medium pressure nitrogen is extracted out from medium pressure rectifying column C2 tower top, medium pressure nitrogen enters low-pressure distillation tower condenser/evaporator K3, it is condensed into middle hydraulic fluid nitrogen again, a part of medium pressure liquid nitrogen is divided into two strands: press rectifying column C2 tower top during wherein hydraulic fluid nitrogen returns in one, as pressing the backflow of rectifying column in this, wherein in another stock, hydraulic fluid nitrogen is directly exported as liquid nitrogen product；The throttling of another part medium pressure liquid nitrogen to behind 0.01～0.03MPa with the dirty nitrogen heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top and evaporated, low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, as high pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3.
In a further preferred embodiment, the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen is further comprising the steps of:
Described low-pressure nitrogen, after subcooler E2, main heat exchanger E1 re-heat, is divided into two strands:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products；
Wherein another gang of low-pressure nitrogen entrance nitrogen compressor CP2 is compressed, cool down again, supercharging is carried out subsequently into turbo-expander ET01 pressurized end Z01, then cool down in water cooler E3, subsequently enter in described fractionating column main heat exchanger E1 and cool down further, then extract out from the middle part of described fractionating column main heat exchanger E1, after entering described turbo-expander ET01 expansion, return described fractionating column main heat exchanger E1 re-heat, be incorporated into described another strand of low-pressure nitrogen afterwards.
In one further preferred embodiment, above-mentioned another strand of low-pressure nitrogen is after the middle part of described fractionating column main heat exchanger E1 is extracted out, enter described turbo-expander ET01 and be expanded to 0.01～0.03MPa, return again to described fractionating column main heat exchanger E1 re-heat to room temperature, be incorporated into the suction inlet of described nitrogen compressor CP2 afterwards.
In one further preferred embodiment, above-mentioned another strand of low-pressure nitrogen enters nitrogen compressor CP2 and is compressed to 0.80～1.0MPa, it is cooled to less than 40 DEG C, it is pressurized to 1.20～1.40MPa subsequently into turbo-expander ET01 pressurized end Z01, the most water cooled but device E3 is cooled to 40 DEG C, subsequently enter in described fractionating column main heat exchanger E1 and be cooled further to-120 DEG C～-130 DEG C, extract out from the middle part of described fractionating column main heat exchanger E1 again, enter described turbo-expander ET01 and be expanded to 0.020～0.030MPa, return described fractionating column main heat exchanger E1 re-heat to 30～35 DEG C, it is incorporated into described another strand of low-pressure nitrogen afterwards.
In a preferred embodiment, in the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen, before the dried air of described purification is cooled to saturation in fractionating column main heat exchanger E1, it is divided into two strands:
Wherein the dried air of one purification is directly entered fractionating column main heat exchanger E1；
Wherein another gang of purification dried air entrance turbo-expander ET01 pressurized end Z01 carries out supercharging, then cool down in water cooler E3, subsequently enter in described fractionating column main heat exchanger E1 and cool down further, extract out from the middle part of described fractionating column main heat exchanger E1 again, after entering described turbo-expander ET01 expansion, it is back to described fractionating column main heat exchanger E1 and carries out re-heat；Through the low-pressure air of described fractionating column main heat exchanger E1 output, after air booster supercharging, it is incorporated into the dried air of described purification being divided into before two strands as the air that backflows.
In a further preferred embodiment, in the method for the above-mentioned high pure oxygen of efficient production and High Purity Nitrogen, the described dried air of another strand of purification enters turbo-expander ET01 pressurized end Z01 and is pressurized to 1.20～1.40MPa, then in water cooler E3,40 DEG C it are cooled to, subsequently enter in described fractionating column main heat exchanger E1 and be cooled further to-120 DEG C～-130 DEG C, extract out from the middle part of described fractionating column main heat exchanger E1 again, enter described turbo-expander ET01 and be expanded to 0.020～0.030MPa, return again to described fractionating column main heat exchanger E1 re-heat to 30～35 DEG C；Through the low-pressure air of described fractionating column main heat exchanger E1 output, after air booster supercharging, it is incorporated into the dried air of described purification being divided into before two strands as the air that backflows.
In one further preferred embodiment, the operation pressure of described high-pressure rectification tower C1 is 0.8～1.3MPa, and the operation pressure of medium pressure rectifying column C2 is 0.35～0.6MPa, and the operation pressure of described low-pressure distillation tower C3 is 0.02～0.15MPa.
In one further preferred embodiment, described low boiling hydrocarbon be mainly composed of methane.
A second aspect of the present invention, it is provided that high pure oxygen that a kind of method described according to a first aspect of the present invention prepares and/or High Purity Nitrogen, it is characterised in that O in described high pure oxygen2Purity >=99.9999%, N in described High Purity Nitrogen2Purity >=99.999%.
Below in conjunction with detailed description of the invention, the present invention is further elaborated, but the present invention is not limited to following example.Each step in described method is conventional steps if no special instructions；Described equipment the most all can be either commercially available from open.
Embodiment 1
The technological process method as shown in Figure 1 of employing produces high pure oxygen and High Purity Nitrogen:
By dried for purification air 101 (3350NM3/ h, 0.96MPa) air 206 merges with backflowing, and after merging, described purification dried air total flow is 7750NM3/ h, and before being cooled to saturation in fractionating column main heat exchanger E1, it is divided into two strands:
Wherein one 102 is directly entered fractionating column main heat exchanger E1；
Wherein another stock 201 (4400NM3/ h, 0.96MPa) enter after turbo-expander ET01 pressurized end Z01 is pressurized to 1.32MPa and obtain 202, the most water cooled but device E3 is cooled to 40 DEG C, subsequently enter fractionating column main heat exchanger E1 and be cooled to-122 DEG C, in the middle part of main heat exchanger, extract 204 out, and enter described turbo-expander ET01 and be expanded to 0.025MPa, obtain 205, return again to described fractionating column main heat exchanger E1 re-heat to 32 DEG C, obtain 206；Wherein, the cold that described turbo-expander produces maintains device cold balancing.Through the low-pressure air 206 of described fractionating column main heat exchanger E1 output, after air booster is pressurized to 0.96MPa, being incorporated into the Trunk Line of the dried air of purification 101 as the air that backflows, 101 on this Trunk Line are not also divided into two strands；
Above-mentioned 102 (3350NM3/ h, 0.96MPa) in fractionating column main heat exchanger E1, it is cooled to saturation 103；Then, 103 saturated air 104 and saturated air 105 two parts are split into, wherein:
Saturated air 104 (2950NM3/ h) enter high-pressure rectification tower C1 tower reactor, in this high-pressure rectification tower C1, it is separated into high pressure nitrogen 300 and oxygen-enriched liquid air 501；
Saturated air 105 (400NM3/ h) enter in press in rectifying column reboiler K2 and be condensed into liquid air 106；
After described liquid air 106 mixes with the described oxygen-enriched liquid air 501 from high-pressure rectification tower, obtain 503, flash to gaseous state 504 subsequently in high-pressure rectification tower condenser/evaporator K1, enter back into middle pressure rectifying column C2 tower reactor；The nitrogen 404 that high-pressure rectification tower C1 separates being sent into condensation in high-pressure rectification tower condenser/evaporator K1 and becomes liquid nitrogen 405, a part of liquid nitrogen is as high-pressure rectification tower backflow, another part liquid nitrogen (1000NM3/ h) cross through subcooler E2 and to be cooled to-181 DEG C, entrance is pressed rectifying column C2 top as middle pressure rectifier column reflux liquid；The oxygen rich air 504 that high-pressure tower condenser/evaporator K1 evaporates respectively enters middle pressure rectifying column C2 and carries out rectification, and wherein, the operation pressure pressing rectifying column C2 in this is 0.5MPa, is separated into medium pressure nitrogen gas 401 and oxygen-rich liquid 901.
Press from this bottom rectifying column C2 and extract the described oxygen-rich liquid 901 (160NM rich in low boiling hydrocarbon out3/ h), assist condenser/evaporator K4 subsequently into oxygen-rich liquid；In described oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air 904, exports 906 after re-heat；
Therefrom pressure rectifying column C2 tower top extracts medium pressure nitrogen 401 (2840NM out3/ h), medium pressure nitrogen enters low-pressure distillation tower condenser/evaporator K3, then is condensed into middle hydraulic fluid nitrogen 405, and a part of medium pressure liquid nitrogen 405 presses rectifying column C2 tower top, as the backflow pressing rectifying column in this in returning；Another part medium pressure liquid nitrogen (1880NM3/ h) throttling to after 0.03MPa with the dirty nitrogen heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top and evaporated, low-pressure nitrogen after evaporation is after subcooler E2, main heat exchanger E1 re-heat, exporting as high pure nitrogen product 414, i.e. low-pressure nitrogen 414, its yield is 1880NM3/ h, wherein as the O of foreign gas2Content≤3pppm, pressure 0.01MPa；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3；
Therefrom extract the oxygen-rich liquid (1300NM without low boiling hydrocarbon out in the middle part of pressure rectifying column C23/ h), after subcooler is supercool, enter the low-pressure distillation tower C3 tower top backflow 603 as this low-pressure distillation tower；The described oxygen-rich liquid without low boiling hydrocarbon after rectification, obtains O in this low-pressure distillation tower tower reactor in low-pressure distillation tower C32The high-purity fluid oxygen product 701 (500NM of purity >=99.9999%3/h)。
Embodiment 2
The technological process method as shown in Figure 2 of employing produces high pure oxygen and High Purity Nitrogen:
By dried for purification air 101 (3350NM3/ h, 0.96MPa) in fractionating column main heat exchanger E1, it is cooled to saturation 103, a part of saturated air 104 (2950NM3/ h) enter high-pressure rectification tower C1 tower reactor, high-pressure rectification tower C1 is separated into high pressure nitrogen 300 and oxygen-enriched liquid air 501；Another part saturated air 105 (400NM3/ h) enter in press in rectifying column reboiler K2 and be condensed into liquid air 106, liquid air 106 mix with the oxygen-enriched liquid air 501 of high pressure tower reactor after 503, entrance high-pressure rectification tower condenser/evaporator K1 flashes to gaseous state 504, enters back into middle pressure tower bottom of rectifying tower；The nitrogen 404 that high-pressure rectification tower C1 separates being sent into high-pressure rectification tower condenser/evaporator K1 condensation and becomes liquid nitrogen 405, a part of liquid nitrogen therein is as high-pressure rectification tower backflow；Another branch liquid nitrogen (1000NM therein3/ h) cross through subcooler E2 and to be cooled to-181 DEG C, entrance is pressed rectifying column C2 top as middle pressure rectifier column reflux liquid, the oxygen rich air 504 that high-pressure rectification tower condenser/evaporator K1 evaporates respectively enters middle pressure rectifying column C2 and carries out rectification, wherein, the operation pressure pressing rectifying column C2 in this is 0.5MPa, is separated into medium pressure nitrogen gas 401 and oxygen-rich liquid 901.
Therefrom extract the described oxygen-rich liquid 901 (160NM rich in low boiling hydrocarbon out bottom pressure rectifying column C23/ h), assist condenser/evaporator K4 subsequently into oxygen-rich liquid；In described oxygen-rich liquid auxiliary condenser/evaporator K4, oxygen-rich liquid is evaporated into oxygen rich air 904, exports 906 after re-heat；
Therefrom pressure rectifying column C2 tower top extracts medium pressure nitrogen 401 (2840NM out3/ h), medium pressure nitrogen enters low-pressure distillation tower condenser/evaporator K3, then is condensed into middle hydraulic fluid nitrogen 404, and a portion medium pressure liquid nitrogen presses rectifying column C2 tower top, as the backflow pressing rectifying column in this in returning；Wherein hydraulic fluid nitrogen 405 (1880NM in another part3/ h) throttle to 0.01MPa, evaporating with dirty nitrogen 609 heat exchange in the condenser/evaporator K5 of low-pressure distillation tower C3 tower top, the low-pressure nitrogen after evaporation, after subcooler E2, main heat exchanger E1 re-heat, exports as high pure nitrogen product 414, i.e. low-pressure nitrogen 414, its yield is 1880NM3/ h, wherein as the O of foreign gas2Content≤3pppm, pressure 0.01MPa；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower C3；
Therefrom extract the oxygen-rich liquid 601 (1300NM without low boiling hydrocarbon out in the middle part of pressure rectifying column C23/ h), after subcooler is supercool, enter the low-pressure distillation tower C3 tower top backflow 603 as this low-pressure distillation tower；The described oxygen-rich liquid without low boiling hydrocarbon after rectification, obtains O in this low-pressure distillation tower tower reactor in low-pressure distillation tower C32The high-purity fluid oxygen product 701 (500NM of purity >=99.9999%3/h)。
Additionally, the low-pressure nitrogen 414 from main heat exchanger E1 output is divided into two strands, wherein one is as it has been described above, directly as high pure nitrogen output of products；And another strand of low-pressure nitrogen 414 mixes with 206, obtain 207 (4100NM3/ h, 0.01MPa, 32 DEG C), enter nitrogen compressor CP2, be compressed to 0.96MPa, the most water cooled but device E3 is cooled to less than 40 DEG C, pressurized end Z01 subsequently into turbo-expander ET01 is pressurized to 1.32MPa, obtains 202, is cooled to 40 DEG C afterwards, subsequently enter described fractionating column main heat exchanger E1 and be cooled to-122 DEG C, obtain 204；Extracting out from the middle part of main heat exchanger E1, enter turbo-expander ET01 and be expanded to 0.025MPa, obtain 205, be then back to described fractionating column main heat exchanger E1 re-heat to 32 DEG C, obtain 206, this 206 is incorporated into described another strand of low-pressure nitrogen；Wherein, the cold that decompressor produces maintains device cold balancing.
Being described in detail the specific embodiment of the present invention above, but it is intended only as example, the present invention is not restricted to particular embodiments described above.To those skilled in the art, any equivalent modifications carrying out the present invention and replacement are the most all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.

Claims (10)

1. the high pure oxygen of efficient production and the method for High Purity Nitrogen, it is characterised in that comprise the steps:
Dried for purification air is cooled to saturation in fractionating column main heat exchanger (E1), a part Saturated air enters high-pressure rectification tower (C1) tower reactor, is separated into high pressure nitrogen in high-pressure rectification tower (C1) And oxygen-enriched liquid air；Another part saturated air is pressed in rectifying column reboiler (K2) in entering and is condensed into liquid air； After described liquid air mixes with described oxygen-enriched liquid air, enter in high-pressure rectification tower condenser/evaporator (K1) and flash to Gaseous state, enters back into middle pressure tower bottom of rectifying tower；The nitrogen separated by high-pressure rectification tower (C1) sends into high pressure Condensation becomes liquid nitrogen in rectifying column condenser/evaporator (K1), a part of liquid nitrogen as high-pressure rectification tower backflow, Another part liquid nitrogen, after subcooler (E2) is supercool, presses rectifying column (C2) top as middle pressure essence in entrance Evaporate tower backflow；The oxygen rich air that high-pressure rectification tower condenser/evaporator (K1) evaporates respectively enters middle pressure rectification Tower (C2) carries out rectification, is separated into medium pressure nitrogen gas and oxygen-rich liquid；
Rectifying column (C2) bottom is therefrom pressed to extract the described oxygen-rich liquid rich in low boiling hydrocarbon out, subsequently into oxygen-enriched Liquid auxiliary condenser/evaporator (K4)；In described oxygen-rich liquid auxiliary condenser/evaporator (K4), oxygen-rich liquid is steamed Send out into oxygen rich air, export after re-heat；
Therefrom pressing rectifying column (C2) tower top to extract medium pressure nitrogen out, medium pressure nitrogen enters low-pressure distillation Tower condenser/evaporator (K3), then it is condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen presses rectifying column in returning (C2) tower top, as the backflow pressing rectifying column in this；Another part medium pressure liquid nitrogen throttles extremely Change with the dirty nitrogen in the condenser/evaporator (K5) of low-pressure distillation tower (C3) tower top after 0.01～0.03MPa Heat and evaporated, the low-pressure nitrogen after evaporation after subcooler (E2), main heat exchanger (E1) re-heat, as High pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower (C3)；
Rectifying column (C2) middle part is therefrom pressed to extract the oxygen-rich liquid without low boiling hydrocarbon out, after subcooler is supercool, Enter low-pressure distillation tower (C3) tower top backflow as this low-pressure distillation tower；Described without low boiling hydrocarbon Oxygen-rich liquid after rectification, obtains high-purity fluid oxygen product in this low-pressure distillation tower tower reactor in low-pressure distillation tower (C3).
Method the most according to claim 1, it is characterised in that also include directly producing below liquid nitrogen product Step:
Extracting medium pressure nitrogen out from medium pressure rectifying column (C2) tower top, medium pressure nitrogen enters low pressure Rectifying column condenser/evaporator (K3), then it is condensed into middle hydraulic fluid nitrogen, a part of medium pressure liquid nitrogen is divided into two strands: Rectifying column (C2) tower top is pressed during wherein hydraulic fluid nitrogen returns in one, as this presses the backflow of rectifying column, Wherein in another stock, hydraulic fluid nitrogen is directly exported as liquid nitrogen product；Another part medium pressure liquid nitrogen throttles extremely Change with the dirty nitrogen in the condenser/evaporator (K5) of low-pressure distillation tower (C3) tower top after 0.01～0.03MPa Heat and evaporated, the low-pressure nitrogen after evaporation after subcooler (E2), main heat exchanger (E1) re-heat, as High pure nitrogen output of products；And the liquid nitrogen fraction condensed is as the backflow of low-pressure distillation tower (C3).
Method the most according to claim 1 and 2, it is characterised in that further comprising the steps of:
Described low-pressure nitrogen, after subcooler (E2), main heat exchanger (E1) re-heat, is divided into two strands:
Wherein one low-pressure nitrogen is directly as high pure nitrogen output of products；
Wherein another burst of low-pressure nitrogen entrance nitrogen compressor (CP2) is compressed, then cools down, then Enter turbo-expander (ET01) pressurized end (Z01) and carry out supercharging, then in water cooler (E3) Cooling, subsequently enters in described fractionating column main heat exchanger (E1) and cools down further, then from described fractionating column master The middle part of heat exchanger (E1) is extracted out, after entering described turbo-expander (ET01) expansion, returns described point Evaporate tower main heat exchanger (E1) re-heat, be incorporated into described another strand of low-pressure nitrogen afterwards.
Method the most according to claim 3, it is characterised in that described another strand of low-pressure nitrogen is from described fractional distillation After the middle part of tower main heat exchanger (E1) is extracted out, enter described turbo-expander (ET01) and be expanded to 0.01～0.03MPa, return again to the re-heat of described fractionating column main heat exchanger (E1) to room temperature, be incorporated into institute afterwards State the suction inlet of nitrogen compressor (CP2).
Method the most according to claim 3, it is characterised in that described another strand of low-pressure nitrogen enters nitrogen pressure Contracting machine (CP2) is compressed to 0.80～1.0MPa, is cooled to less than 40 DEG C, subsequently into turbo-expander (ET01) pressurized end (Z01) is pressurized to 1.20～1.40MPa, and the most water cooled but device (E3) is cooled to 40 DEG C, subsequently enter in described fractionating column main heat exchanger (E1) and be cooled further to-120 DEG C～-130 DEG C, then Extract out from the middle part of described fractionating column main heat exchanger (E1), enter described turbo-expander (ET01) and expand To 0.020～0.030MPa, return the re-heat of described fractionating column main heat exchanger (E1) to 30～35 DEG C, afterwards It is incorporated into described another strand of low-pressure nitrogen.
Method the most according to claim 1, it is characterised in that the dried air of described purification is at fractionating column Before main heat exchanger (E1) is cooled to saturation, it is divided into two strands:
Wherein the dried air of one purification is directly entered fractionating column main heat exchanger (E1)；
Wherein another burst of purification dried air entrance turbo-expander (ET01) pressurized end (Z01) is carried out Supercharging, then cooling in water cooler (E3), subsequently enter in described fractionating column main heat exchanger (E1) Cooling further, then extract out from the middle part of described fractionating column main heat exchanger (E1), enter described turbine expansion After machine (ET01) expands, it is back to described fractionating column main heat exchanger (E1) and carries out re-heat；Through described fractional distillation The low-pressure air that tower main heat exchanger (E1) exports, after air booster supercharging, as backflowing air also Enter to the dried air of described purification being divided into before two strands.
Method the most according to claim 6, it is characterised in that the described dried sky of another strand of purification Gas enters turbo-expander (ET01) pressurized end (Z01) and is pressurized to 1.20～1.40MPa, then in water-cooled But device (E3) is cooled to 40 DEG C, subsequently enters in described fractionating column main heat exchanger (E1) and cool down further To-120 DEG C～-130 DEG C, then extract out from the middle part of described fractionating column main heat exchanger (E1), enter described turbine Decompressor (ET01) is expanded to 0.020～0.030MPa, returns again to described fractionating column main heat exchanger (E1) Re-heat is to 30～35 DEG C；Through the low-pressure air that described fractionating column main heat exchanger (E1) exports, increase through air After press supercharging, it is incorporated into the dried air of described purification being divided into before two strands as the air that backflows.
8. according to the method according to any one of claim 1,2,6,7, it is characterised in that described high-pressure rectification The operation pressure of tower (C1) is 0.8～1.3MPa, and the operation pressure of medium pressure rectifying column (C2) is 0.35～0.6MPa, the operation pressure of described low-pressure distillation tower (C3) is 0.02～0.15MPa.
9. according to the method according to any one of claim 1,2,6,7, it is characterised in that described low boiling hydrocarbon Be mainly composed of methane.
10. the high pure oxygen prepared according to the method described in any of the above-described claim and/or a High Purity Nitrogen, it is special Levy and be, O in described high pure oxygen2Purity >=99.9999%, N in described High Purity Nitrogen2Purity >=99.999%.
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CN107062800A (en) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 The method and its device of a kind of superpure nitrogen dehydrogenation
CN107270655A (en) * 2017-08-04 2017-10-20 杭州特盈能源技术发展有限公司 A kind of single column nitrogen halfload operating mode volume increase liquid nitrogen device for making and method
CN109323533A (en) * 2018-11-06 2019-02-12 杭州杭氧股份有限公司 Pressure rectifying column reduces space division energy consuming process and device in a kind of use
CN109357475A (en) * 2018-08-30 2019-02-19 华中科技大学 A kind of system that cascade utilization LNG cold energy produces liquid oxygen liquid nitrogen
CN111412724A (en) * 2020-04-29 2020-07-14 杭州特盈能源技术发展有限公司 Novel low-energy-consumption pressure oxygen enrichment preparation process for kiln
CN113465292A (en) * 2021-07-05 2021-10-01 乔治洛德方法研究和开发液化空气有限公司 Method for increasing yield of krypton/xenon in air rectification device

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Publication number Priority date Publication date Assignee Title
CN107062800A (en) * 2017-04-21 2017-08-18 上海启元特种气体发展有限公司 The method and its device of a kind of superpure nitrogen dehydrogenation
CN107270655A (en) * 2017-08-04 2017-10-20 杭州特盈能源技术发展有限公司 A kind of single column nitrogen halfload operating mode volume increase liquid nitrogen device for making and method
CN107270655B (en) * 2017-08-04 2022-07-15 杭州特盈能源技术发展有限公司 Single-tower nitrogen-making half-load working condition yield-increasing liquid nitrogen making device and method
CN109357475A (en) * 2018-08-30 2019-02-19 华中科技大学 A kind of system that cascade utilization LNG cold energy produces liquid oxygen liquid nitrogen
CN109323533A (en) * 2018-11-06 2019-02-12 杭州杭氧股份有限公司 Pressure rectifying column reduces space division energy consuming process and device in a kind of use
CN109323533B (en) * 2018-11-06 2023-10-20 杭氧集团股份有限公司 Method and device for reducing space division energy consumption by using medium-pressure rectifying tower
CN111412724A (en) * 2020-04-29 2020-07-14 杭州特盈能源技术发展有限公司 Novel low-energy-consumption pressure oxygen enrichment preparation process for kiln
CN111412724B (en) * 2020-04-29 2021-06-04 杭州特盈能源技术发展有限公司 Novel low-energy-consumption pressure oxygen enrichment preparation process for kiln
CN113465292A (en) * 2021-07-05 2021-10-01 乔治洛德方法研究和开发液化空气有限公司 Method for increasing yield of krypton/xenon in air rectification device

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