WO2011010630A1 - 空気液化分離方法及び装置 - Google Patents
空気液化分離方法及び装置 Download PDFInfo
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- WO2011010630A1 WO2011010630A1 PCT/JP2010/062158 JP2010062158W WO2011010630A1 WO 2011010630 A1 WO2011010630 A1 WO 2011010630A1 JP 2010062158 W JP2010062158 W JP 2010062158W WO 2011010630 A1 WO2011010630 A1 WO 2011010630A1
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
- F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
- F25J3/04024—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of purified feed air, so-called boosted air
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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
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
- F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
- F25J3/04175—Hot end purification of the feed air by adsorption of the impurities at a pressure of substantially more than the highest pressure column
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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
- F25J3/04296—Claude expansion, i.e. expanded into the main or high pressure column
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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
- F25J3/04333—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
- F25J3/04339—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 air
- F25J3/04345—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 air and comprising a gas work expansion loop
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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
- F25J3/04375—Details relating to the work expansion, e.g. process parameter etc.
- F25J3/04393—Details relating to the work expansion, e.g. process parameter etc. using multiple or multistage gas work expansion
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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
- F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
- F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
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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
- F25J3/04642—Recovering noble gases from air
- F25J3/04648—Recovering noble gases from air argon
- F25J3/04654—Producing crude argon in a crude argon column
- F25J3/04666—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system
- F25J3/04672—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser
- F25J3/04678—Producing crude argon in a crude argon column as a parallel working rectification column of the low pressure column in a dual pressure main column system having a top condenser cooled by oxygen enriched liquid from high pressure column bottoms
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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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream being air
Definitions
- the present invention relates to an air liquefaction separation method and apparatus, and more particularly, to an air liquefaction separation method for collecting at least liquid oxygen as a product by subjecting compressed, purified and cooled raw material air to cryogenic separation in an intermediate pressure tower and a low pressure tower. And an apparatus.
- the production is generally carried out by a so-called deep-cooling type air liquefaction separation apparatus which uses air as a raw material and separates it by a double rectification column comprising an intermediate pressure column and a low pressure column. is there.
- this cryogenic air liquefaction separation apparatus about 5% of the product can be produced as liquid oxygen, liquid nitrogen, or liquid argon.
- additional liquefaction processes are required to produce more liquid products.
- the liquefaction process is a process in which raw air, nitrogen gas, etc. are compressed, circulated, and adiabatic expansion to obtain the cooling required for the process, and many techniques have been disclosed for each process (for example, see Patent Document 1). .)
- the circulating fluid is supplied to the distillation tower in a partially liquefied state, and a liquid product that is thermally suitable is collected.
- the air circulation liquefaction process that compresses a part of higher-pressure raw material air and uses it as a circulating fluid This is a fundamentally advantageous process that requires less power to compress the fluid.
- the air circulation liquefaction process increases the liquefaction rate of the raw material air supplied to the intermediate pressure tower, and the distillation conditions of the intermediate pressure tower decrease, making it difficult to cope with it. Become.
- liquid nitrogen suitable for the liquid product is supplied to the intermediate pressure tower, and even when the amount of the product liquid is large, the distillation conditions of the intermediate pressure tower are not lowered. That is, when the amount of product liquid is relatively small, an air circulation liquefaction process with less power consumption is superior, but when the amount of product liquid is relatively large, only the nitrogen circulation liquefaction process can be handled.
- the raw material air is pressurized to 460 kPa (gauge pressure, hereinafter referred to as kPaG) with a compressor and purified, and then introduced into the circulating air compressor together with a part of the circulating air processed by the expansion turbine.
- the pressure is increased to a suitable pressure.
- These circulating air is cooled to a predetermined temperature by a heat exchanger and then introduced into an expansion turbine to generate the necessary cooling for the apparatus.
- a part of the circulating air treated by the expansion turbine is introduced into the intermediate pressure tower, and the rest is introduced into the circulating compressor together with the raw air.
- the operation pressure of the intermediate pressure tower is about 480 kPaG, which is approximately the same as the expansion turbine discharge pressure and the pretreatment device operation pressure.
- an object of the present invention is to provide an air liquefaction separation method and apparatus capable of reducing the apparatus cost in an air circulation liquefaction process for collecting at least liquid oxygen as a product.
- a first configuration of the present invention is an air liquefaction separation method in which at least liquid oxygen is collected as a product by low-temperature distillation of compressed, purified, and cooled raw material air in a medium-pressure tower and a low-pressure tower.
- a raw material air compression step in which the total amount of the raw material air is increased to a first set pressure higher than the operation pressure of the intermediate pressure tower to obtain the pressurized raw material air;
- the second configuration of the present invention is an air liquefaction separation method for collecting at least liquid oxygen as a product by low-temperature distillation of compressed, purified, and cooled raw material air in an intermediate pressure column and a low pressure column,
- a raw material air compression step in which the total amount of air is boosted to a first set pressure higher than the operation pressure of the intermediate pressure tower to form pressurized raw material air, and adsorption purification by adsorbing and removing impurities from the pressurized raw material air
- a step a circulating air merging step in which the pressure-purified air and the pressure-returned return air, which will be described later, are merged to form circulating air, and the first shunt air that has been circulated in three minutes is cooled to the first set temperature to the medium pressure
- the second split air is cooled to a second set temperature higher than the first set temperature to form cold expansion air
- the third split air is set to a third set temperature higher than the second set temperature.
- a cooling step a first expansion step in which the cold expansion air is adiabatically expanded to a second set pressure lower than the first set pressure to form a first low-temperature air, and the warm expansion air is used as the second set pressure.
- a second expansion step of adiabatic expansion into the second low-temperature air having a temperature higher than the first set temperature, a step of introducing a part of the first low-temperature air into the intermediate pressure tower, and the first low temperature A temperature raising step of recovering the temperature of the remaining air and the second low-temperature air to obtain return air, a circulation compression step of raising the feedback air to obtain the boosted feedback air, and the intermediate pressure tower introduction air to And a step of introducing into the intermediate pressure tower.
- a circulating air pressurizing step is provided for boosting the circulating air to a pressure higher than the first set pressure.
- the third configuration of the present invention is an air liquefaction separation apparatus that collects at least liquid oxygen as a product by low-temperature distillation of compressed, purified, and cooled raw material air in a medium-pressure tower and a low-pressure tower,
- a raw material air compressor that boosts the total amount of air to a first set pressure that is higher than the operating pressure of the intermediate pressure tower to obtain pressurized raw material air
- an adsorption device that adsorbs and removes impurities from the pressurized raw material air to obtain pressurized purified air
- a circulating air merging pipe that joins the pressure-purified air and pressure-returning return air, which will be described later, to form a circulating air, and a first divided air that has been divided into two by circulating the circulating air to a first preset temperature
- a main heat exchanger that is a tower introduction air, cools the second shunt air to a second set temperature higher than the first set temperature, and makes the expansion air; and a second heat lower
- Adiabatic expansion to the set pressure results in low-temperature air Circulation of the expansion turbine, piping for introducing a part of the low-temperature air into the intermediate pressure tower, and the return air whose temperature is recovered by the main heat exchanger for the rest of the low-temperature air to be the boosted feedback air
- a compressor and a pipe for introducing the intermediate-pressure tower introduction air into the intermediate-pressure tower are provided.
- the fourth configuration of the present invention is an air liquefaction separation apparatus for collecting at least liquid oxygen as a product by low-temperature distillation of compressed, purified, and cooled raw material air in an intermediate pressure column and a low pressure column
- a raw material air compressor that boosts the total amount of air to a first set pressure that is higher than the operating pressure of the intermediate pressure tower to obtain pressurized raw material air
- an adsorption device that adsorbs and removes impurities from the pressurized raw material air to obtain pressurized purified air
- a circulating air merging pipe that circulates the pressurized purified air and the boosted return air, which will be described later, to form circulating air, and the first divided air that has been circulated into the circulating air for 3 minutes is cooled to the first set temperature to the medium pressure
- the second split air is cooled to a second set temperature higher than the first set temperature to form cold expansion air
- the third split air is set to a third set temperature higher than the second set temperature.
- An exchanger Mainly cooled and used as air for thermal expansion
- a cold expansion turbine that adiabatically expands the cold expansion air to a second set pressure lower than the first set pressure to form first low-temperature air
- the thermal expansion air is insulated to the second set pressure
- the main expansion of the thermal expansion turbine to be expanded into the second low-temperature air
- the piping for introducing a part of the first low-temperature air into the intermediate pressure tower, the remainder of the first low-temperature air and the second low-temperature air.
- a circulating compressor is used to pressurize the return air whose temperature has been recovered by a heat exchanger to obtain the boosted feedback air, and a pipe for introducing the intermediate pressure tower introduction air into the intermediate pressure tower.
- a circulating air compressor that boosts the circulating air to a pressure higher than the first set pressure
- the circulating air booster includes the expansion An expansion turbine braking blower provided in the turbine, and the expansion turbine is braked by any of a blower, a generator, and a hydraulic pump.
- the total amount of the raw material air that has been conventionally increased to a pressure corresponding to the operation pressure of the intermediate pressure tower is set to a first set pressure higher than the operation pressure of the intermediate pressure tower, for example, the operation pressure of the intermediate pressure tower.
- the pressure is increased to at least about 1.5 times, and impurities such as water vapor and carbon dioxide contained in the raw material air are adsorbed and removed in that state.
- the adsorption device and the surrounding piping can be reduced in size.
- the partial pressure of water vapor contained in the raw air becomes relatively low, it is possible to reduce the necessary amount of adsorbent for adsorbing and removing moisture, and to reduce the energy required for regeneration of the adsorbent. Therefore, the device price and the like can be reduced with the same power consumption as in the conventional case.
- FIG. 1 is a system diagram of an air liquefaction separation apparatus showing a first embodiment of the present invention. It is a principal part systematic diagram of the air liquefaction separation apparatus which shows the 2nd form example of this invention. It is a principal part systematic diagram of the air liquefaction separation apparatus which shows the 3rd example of this invention. It is a principal part systematic diagram of the air liquefaction separation apparatus which shows the 4th example of this invention. It is a principal part systematic diagram of the air liquefaction separation apparatus which shows the 5th example of this invention. It is a principal part systematic diagram of the air liquefaction separation apparatus which shows the 6th form example of this invention.
- the air liquefaction / separation apparatus shown in the first embodiment of FIG. 1 is obtained by subjecting raw material air that has been compressed, purified, and cooled to low temperature distillation in a medium pressure tower 11 and a low pressure tower 12, thereby producing liquid oxygen LO 2 and liquid as liquid products.
- the crude argon LAr and the liquid nitrogen LN 2 are collected, and the oxygen gas GO 2 and the nitrogen gas GN 2 are collected as gas products.
- the raw material air compressor 13, the adsorption device 14, and the circulating compressor 15 are collected.
- a main heat exchanger 16 an expansion turbine 17, a main condenser 18, a crude argon tower 19, an argon condenser 20, and a supercooler 21.
- the total amount of the raw material air is introduced into the raw material air compression process in which the raw material air compressor 13 boosts the pressure to the first set pressure higher than the operation pressure of the intermediate pressure tower 11 to obtain the boosted raw material air.
- the pressurized raw material air is cooled by a cooler 13a, separated from condensed water by a drain separator 13b, and then introduced into an adsorption device 14 that performs an adsorption purification process.
- impurities such as water vapor and carbon dioxide contained in the raw material air are adsorbed and removed by the adsorbent, and the pressurized raw material air is purified to become pressurized purified air.
- the pressure-purified air is cooled by the cooler 14a, passes through one pipe 51a constituting the circulating air confluence pipe 51, and is discharged from the circulation compressor 15 to the pipe 51b that is the other confluence pipe.
- a circulating air merging step is performed by merging with the return air to become circulating air flowing through the pipe 51c.
- the circulating air in the pipe 51 c is introduced into the main heat exchanger 16 that performs the cooling process after being divided into two parts, the first divided air in the pipe 52 and the second divided air in the pipe 53.
- the first diverted air is cooled to the first set temperature by the main heat exchanger 16, led out from the cold end of the main heat exchanger 16 to the pipe 54, and becomes intermediate pressure tower introduction air.
- This intermediate pressure tower introduction air is depressurized by the valve 31 to a pressure corresponding to the operation pressure of the intermediate pressure tower 11, and is mostly introduced into the lower part of the intermediate pressure tower 11 from the pipe 55 in a liquefied state.
- the second shunt air of the pipe 53 is cooled to the second set temperature higher than the first set temperature in the cooling process in the main heat exchanger 16 and is piped before reaching the cold end of the main heat exchanger 16.
- the air is extracted into the expansion air 56 and introduced into the expansion turbine 17.
- the expansion air is subjected to an expansion process in which the expansion turbine 17 adiabatically expands to a second set pressure lower than the first set pressure, and becomes low-temperature air in the pipe 57.
- This low-temperature air is divided into the pipe 58 and the pipe 59 from the pipe 57, and the low-temperature air divided into the pipe 59 is introduced as a rising gas from the pipe 60 to the lower part of the intermediate pressure tower 11 through the valve 32.
- the remaining portion of the low-temperature air that has been diverted to the pipe 58 is introduced into the cold end of the main heat exchanger 16 to perform a temperature raising step, and heat exchange is performed with the first and second diverted air to exchange each diverted air.
- the temperature While cooling to a predetermined temperature, the temperature itself recovers to near normal temperature and becomes return air of the pipe 61.
- the return air is sucked into the circulation compressor 15 and subjected to a circulation compression process.
- the compressed air is discharged to the pipe 51b and joined to the pressurized purified air in the pipe 51a. Then, it becomes the circulating air of the pipe 51c.
- the raw material air introduced into the lower part of the intermediate pressure tower 11 from the pipe 55 and the pipe 60 is subjected to distillation operation in the intermediate pressure tower 11 so that the medium pressure nitrogen-enriched gas at the top of the intermediate pressure tower and the oxygen enrichment at the bottom of the intermediate pressure tower. Separated from the chemical solution.
- the oxygen-enriched liquid is extracted from the bottom of the intermediate pressure tower to the pipe 62 and cooled by the supercooler 21, and then is divided into the pipe 63 and the pipe 64.
- the oxygen-enriched liquid in the pipe 64 is After being reduced to a pressure corresponding to the operating pressure of the low-pressure column 12, it is introduced as a reflux liquid into the intermediate portion of the low-pressure column 12 through the pipe 65.
- the oxygen-enriched liquid flowing through the pipe 63 is decompressed by the valve 34 and then introduced into the argon condenser 20 provided at the upper part of the crude argon tower 19.
- the oxygen-enriched gas vaporized in the argon condenser 20 is introduced as an ascending gas into the intermediate portion of the low-pressure column 12 through the pipe 66.
- the oxygen content in the oxygen-enriched liquid and oxygen-enriched gas introduced into the low-pressure column 12 is concentrated at the bottom of the low-pressure column by distillation operation in the low-pressure column 12 to become low-pressure liquid oxygen.
- a part of this low-pressure liquid oxygen is extracted to the pipe 67 and cooled by the supercooler 21 and then collected from the pipe 68 as product liquid oxygen.
- the medium-pressure nitrogen-enriched gas at the top of the intermediate-pressure tower is introduced into the main condenser 18 disposed at the bottom of the low-pressure tower through the pipe 69, and indirectly heat exchanges with the low-pressure liquid oxygen to vaporize the low-pressure liquid oxygen.
- the gas is liquefied into liquid nitrogen.
- the liquid nitrogen is partially returned to the upper portion of the intermediate pressure tower 11 through the pipe 70 as a reflux liquid, and the remainder of the liquid nitrogen is cooled by the supercooler 21 through the pipe 71 and then partially.
- the product is diverted to the pipe 72 and collected as product liquid nitrogen.
- Most of the liquid nitrogen is depressurized to a pressure corresponding to the operating pressure of the low-pressure column 12 by the valve 35, and then introduced into the upper portion of the low-pressure column 12 through the pipe 73 as a reflux liquid.
- a gas fluid rich in argon is extracted from the intermediate portion of the low-pressure column 12 into the pipe 74 and introduced into the lower portion of the crude argon column 19.
- a crude argon gas enriched with argon is separated at the top of the column, and a liquid having a reduced argon concentration is separated at the bottom of the crude argon column.
- the liquid having a reduced argon concentration is extracted from the bottom of the crude argon tower to the pipe 75 and returned to the intermediate part of the low-pressure tower 12 as a descending liquid.
- the crude argon gas at the top of the crude argon column is introduced into the argon condenser 20 through the pipe 76, and is liquefied by heat exchange with the oxygen-enriched liquid in the argon condenser 20 to become liquid crude argon.
- a part of the liquid crude argon is collected from the pipe 77 as the liquid crude argon of the product, and the remaining liquid crude argon is introduced as a reflux liquid through the pipe 78 into the upper portion of the crude argon tower 19.
- the low-pressure nitrogen gas concentrated at the top of the low-pressure column by the distillation operation in the low-pressure column 12 is extracted into the pipe 79 and introduced into the supercooler 21 and used as a cooling source for the liquids. And then introduced into the cold end of the main heat exchanger 16. A part of the low-pressure oxygen gas vaporized in the main condenser 18 is extracted into the pipe 81 and introduced into the cold end of the main heat exchanger 16, and most of the remaining low-pressure oxygen gas is supplied to the low-pressure column 12. Ascending gas.
- a part of the gas rising in the low-pressure column 12 is extracted from the upper part of the low-pressure column 12 to the pipe 82 as waste gas WG and becomes a cooling source for the supercooler 21, and then the main heat exchanger 16 introduced at the cold end.
- the first set pressure of the pressurized feed air obtained by boosting the feed air with the feed air compressor 13 is set to a pressure higher than the operation pressure of the intermediate pressure tower 11.
- the operation pressure of the intermediate pressure column 11 in the double rectification column having the intermediate pressure column 11, the low pressure column 12 and the main condenser 18 is about 500 kPaG, and is introduced into the lower part of the intermediate pressure column 11 from the pipe 60.
- the pressure of the low-temperature air is about the same, and the return air flowing through the pipe 61 is about 500 kPaG, which is about the same as the operation pressure of the intermediate pressure tower 11, so that the compression ratio of the circulating compressor 15 for boosting the circulating air is 1 .5 to 1.8, the pressure of the pressurized raw material air having a pressure equal to the discharge pressure of the circulating compressor 15, that is, the first set pressure is about 750 kPaG (500 kPaG ⁇ 1.5) to 900 kPaG (500 kPaG ⁇ 1. 8).
- the operating pressure of the adsorption device 14 that removes impurities from the raw air is about 1.5 times that in the case of a conventional ordinary air liquefaction separation device. It is possible to reduce the size of the main body and the surrounding piping, and to reduce the device price. That is, compared with the conventional adsorption apparatus, the diameter of the adsorption cylinder of the adsorption apparatus 14 can be reduced, so that the price of the adsorption cylinder material is reduced and the amount of water vapor entrained in the raw material air is reduced. Since the amount of alumina gel necessary for the adsorption device can be reduced, the equipment cost of the entire adsorption device can be greatly reduced. Further, since the amount of water vapor contained in the raw air is reduced, it is not necessary to cool the raw air to a low temperature, and the cost required for the cooling equipment can be reduced.
- the circulating compressor 15 is a multistage compressor having a first compression stage 15a and a second compression stage 15b, and the boosted feedback air discharged from the first compression stage 15a. And the pressurized purified air are combined to form a circulating air, and the circulating air is further pressurized to a high-pressure circulating air by performing a circulating air pressurizing step in the second compression stage 15b of the circulating compressor 15, and then the expansion turbine. By performing the second circulating air pressurizing step with 17 brake blowers 22, the pressure is further increased to a high pressure.
- the pressure-purified air obtained by refining the raw material air whose total amount has been increased to the first set pressure by the raw material air compressor 13 by the adsorption device 14 passes through the pipe 51a of the circulating air merging pipe line 51 and passes through the first compression stage 15a.
- the pressurized feedback air of the pipe 51b discharged and cooled by the aftercooler merges with the pipe 51c, and is pressurized to a pressure higher than the first set pressure by the second compression stage 15b to become high-pressure circulating air.
- a part of the high-pressure circulating air discharged from the circulation compressor 15 is divided into the pipe 52 and, as described above, is introduced into the main heat exchanger 16 and cooled to the first set temperature. Then, it is introduced into the lower part of the intermediate pressure tower 11 in a state where most of the liquid is liquefied through the pipe 55.
- the remainder of the high-pressure circulating air that has been diverted to the pipe 53 is introduced into the brake blower 22 of the expansion turbine 17 and further boosted to a high pressure, and then introduced into the main heat exchanger 16 via the pipe 86. It is cooled to the second set temperature, which is a high temperature, and extracted to the piping 56 before reaching the cold end of the main heat exchanger 16, becomes expansion air, and is introduced into the expansion turbine 17.
- the expansion air is adiabatically expanded to a second set pressure that is lower than the first set pressure in the expansion turbine 17 and becomes low-temperature air in the pipe 57.
- a part of this low-temperature air is diverted to the pipe 59 and introduced into the lower part of the intermediate pressure tower through the valve 32 and the pipe 60, and the rest of the low-temperature air is diverted to the pipe 58 and the cold end of the main heat exchanger 16. Then, the temperature is recovered to return air to the pipe 61, which is sucked into the first compression stage 15a of the circulating compressor 15 and circulated.
- the expansion rate in the expansion turbine 17 can be increased, and the amount of cold generation can be increased.
- the air liquefaction separation apparatus shown in the third embodiment of FIG. 3 is a cold expansion that adiabatically expands the expansion air (cold expansion air) having the relatively low temperature as the expansion turbine that performs the expansion process.
- a turbine 17a and a thermal expansion turbine 17b that adiabatically expands expansion air (temperature expansion air) having a third set temperature that is relatively higher than the second set temperature are provided, and braking of both the expansion turbines 17a and 17b is provided.
- a cold expansion turbine braking blower 22a and a warm expansion turbine braking blower 22b are provided.
- the circulated air that has been pressurized by the second compression stage 15b of the circulating compressor 15 and has become high pressure after the pressurized purified air and the pressurized return air have joined together is combined with the first shunt air in the pipe 52.
- the second diverted air divided into the second diverted air in the pipe 53 and further divided into the pipe 53 is further pressurized by the cold expansion turbine brake blower 22a, and introduced into the main heat exchanger 16 from the pipe 86 to be set in the second setting. In the state cooled to the temperature, it is extracted into the pipe 56 and becomes cold expansion air.
- the cold expansion air is converted into the first low-temperature air near the first set temperature by performing the first expansion step in the cold expansion turbine 17a and adiabatically expanding to the second set pressure.
- a part of the first low-temperature air is diverted from the pipe 57 to the pipe 59, introduced into the lower portion of the intermediate pressure tower 11 via the valve 32 and the pipe 60, and the remaining first low-temperature air diverted to the pipe 58 is main heat.
- the temperature is recovered by being introduced into the cold end of the exchanger 16, it becomes the return air of the pipe 61 and is sucked into the first compression stage 15 a of the circulating compressor 15 and circulated in the same manner as described above.
- the first divided air divided into the pipe 52 is further pressurized by the hot expansion turbine braking blower 22b and introduced into the main heat exchanger 16 from the pipe 87, and reaches a third set temperature higher than the second set temperature. After being cooled, a part of the air is diverted as third diverted air, and is extracted to the pipe 88 to become hot expansion air.
- the warm expansion air undergoes a second expansion step in the thermal expansion turbine 17b and adiabatically expands to the second set pressure, whereby a second temperature higher than the first set temperature and lower than the third set temperature.
- the air liquefaction separation apparatus shown in the fourth embodiment of FIG. 4 is a multistage compressor having the first compression stage 15a, the second compression stage 15b, and the third compression stage 15c. It is a thing.
- the circulating air whose pressure has been increased in the second compression stage 15b of the circulating compressor 15 is divided into the first divided air in the pipe 52 and the second divided air in the pipe 53, as described above, and the first divided air is subjected to thermal expansion.
- the pressure is further increased by the turbine braking blower 22b and introduced into the main heat exchanger 16 from the pipe 87, and a part of the pressure is diverted to the pipe 88 as the third diverted air at the third set temperature to form the temperature expansion air. It is introduced into the turbine 17b.
- the second low-temperature air is obtained as described above. After being introduced into the main heat exchanger 16 from the pipe 89 and recovered in temperature, it is circulated to the circulation compressor 15 through the pipe 61. To do.
- the second shunt air in the pipe 53 is further pressurized to a high pressure by the third compression stage 15c and the cold expansion turbine braking blower 22a, and then introduced into the main heat exchanger 16 through the pipe 86, and at the second set temperature.
- the air is drawn into the pipe 56 to be cold expansion air, and is adiabatically expanded to the second set pressure by the cold expansion turbine 17a, thereby becoming the first low-temperature air near the first set temperature.
- a part of the first low-temperature air in the pipe 57 is introduced from the pipe 59 through the valve 32 and the pipe 60 to the lower portion of the intermediate pressure tower 11, and the remaining first low-temperature air is introduced into the main heat exchanger 16 from the pipe 58. Then, it merges with the second low-temperature air, recovers the temperature, becomes the return air of the pipe 61, is sucked into the circulation compressor 15 and circulates.
- a generator 23 is installed instead of the cold expansion turbine braking blower 22a in the fourth embodiment, and the generator 23 brakes the cold expansion turbine 17a.
- the second shunt air that has been shunted to the pipe 53 and increased in pressure by the third compression stage 15c of the circulating compressor 15 is introduced into the main heat exchanger 16 from the pipe 90 at the same pressure.
- motor braking and oil braking other than blower braking can be employed for braking the expansion turbine.
- the air liquefaction separation apparatus shown in the sixth embodiment of FIG. 6 is boosted to a first set pressure higher than the operating pressure of the intermediate pressure tower 11 by the raw air compressor 13 and purified by the adsorption device 14. And the boosted feedback air that has been boosted by the circulating compressor 15 and further boosted by the cold expansion turbine braking blower 22a and the warm expansion turbine braking blower 22b.
- the pressurized purified air led out from the adsorption device 14 to the pipe 91 is branched into the pipe 92 and the pipe 93 that constitute the circulating air confluence pipe.
- the boosted feedback air obtained by boosting the feedback air of the pipe 61 by the circulating compressor 15 is divided into a pipe 94 directed to the cold expansion turbine brake blower 22a and a pipe 95 directed to the warm expansion turbine brake blower 22b.
- liquid oxygen LO 2 , liquid crude argon LAr, and liquid nitrogen LN 2 are collected as liquid products.
- the liquid liquefaction separation apparatus collects only liquid oxygen LO 2 as the liquid product.
- a combination of liquid oxygen LO 2 and liquid crude argon LAr, or liquid oxygen LO 2 and liquid nitrogen LN 2 is possible.
- the circulation compressor a compressor having four or more compression stages according to the suction pressure, the discharge pressure, and the processing amount can be used.
- cryogenic air separation unit shown in the third embodiment, a specific example of a case where liquid oxygen 1500 Nm 3 / h, liquid nitrogen 1000 Nm 3 / h and liquid argon 50 Nm 3 / h taken .
- [Nm 3 / h] represents the flow rate per hour converted to 0 ° C. and 1 atmosphere.
- the raw material air (8800 Nm 3 / h) is pressurized to about 850 kPaG by the raw material air compressor 13 and then introduced into the adsorption device 14 using activated alumina gel and zeolite and contained in the raw material air. Impurities such as water vapor and carbon dioxide are adsorbed and removed for purification.
- Purified raw material air (pressure-purified air) is introduced between the first compression stage 15a and the second compression stage 15b of the circulating compressor 15, and is supplied with pressure-returned return air (12800 Nm 3) discharged from the first compression stage 15a. / H), the pressure is increased to 2700 kPaG in the second compression stage 15b, and becomes circulating air.
- Part of the circulating air (first shunt air 7700 Nm 3 / h) is boosted to 4000 kPaG by the hot expansion turbine braking blower 22 b and then introduced into the main heat exchanger 16.
- Part of the first shunt air (third shunt air 4000 Nm 3 / h) is extracted from the main heat exchanger 16 when it is cooled to the third set temperature by the main heat exchanger 16, and is supplied to the thermal expansion turbine 17b.
- second low-temperature air is obtained.
- the remaining part of the first diverted air (3700 Nm 3 / h) is cooled to the first set temperature by the main heat exchanger 16, reduced to the pressure corresponding to the intermediate pressure tower by the valve 31, and then passed through the pipe 55 to the intermediate pressure tower. 11 is introduced.
- the remainder of the circulating air (second shunt air 13900 Nm 3 / h) is boosted to 4000 kPaG by the cold expansion turbine braking blower 22 a and introduced into the main heat exchanger 16, and is cooled to the second set temperature by the main heat exchanger 16. Then, it is introduced into the cold expansion turbine 17a and adiabatically expands to become the first low-temperature air.
- a part of the first low-temperature air (8800 Nm 3 / h) is introduced into the main heat exchanger 16 and merges with the second low-temperature air to recover the temperature by serving as a cooling source for the raw air (circulation air). Return air.
- the remainder (5100 Nm 3 / h) of the first low-temperature air is introduced into the lower part of the intermediate pressure tower 11 through the valve 32 and the pipe 60.
- the flow rate, temperature, pressure, and oxygen composition of the gas and liquid flowing through the main piping are shown in Table 1, and the main specifications of the adsorption device comparing the adsorption device in the present example with the conventional adsorption device are shown in Table 2. .
- Table 2 the amount of activated alumina or less is a relative value when the conventional apparatus is 100.
- SYMBOLS 11 Medium pressure tower, 12 ... Low pressure tower, 13 ... Raw material air compressor, 14 ... Adsorption apparatus, 15 ... Circulating compressor, 15a ... 1st compression stage, 15b ... 2nd compression stage, 15c ... 3rd compression stage, DESCRIPTION OF SYMBOLS 16 ... Main heat exchanger, 17 ... Expansion turbine, 17a ... Cold expansion turbine, 17b ... Warm expansion turbine, 18 ... Main condenser, 19 ... Coarse argon tower, 20 ... Argon condenser, 21 ... Subcooler, 22 ... Brake blower, 22a ... Cold expansion turbine brake blower, 22b ... Warm expansion turbine brake blower, 23 ... Generator, 51 ... Circulating air confluence line
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Abstract
Description
Claims (8)
- 圧縮、精製、冷却した原料空気を中圧塔及び低圧塔にて低温蒸留することにより少なくとも液体酸素を製品として採取する空気液化分離方法であって、原料空気の全量を前記中圧塔の運転圧力より高い第1設定圧力に昇圧して昇圧原料空気とする原料空気圧縮工程と、該昇圧原料空気から不純物を吸着除去して昇圧精製空気とする吸着精製工程と、該昇圧精製空気と後述する昇圧帰還空気とを合流させて循環空気とする循環空気合流工程と、該循環空気を2分流した第1分流空気を第1設定温度に冷却して中圧塔導入空気とし、第2分流空気を前記第1設定温度より高い第2設定温度に冷却して膨張用空気とする冷却工程と、該膨張用空気を前記第1設定圧力より低い第2設定圧力に断熱膨張させることにより低温空気とする膨張工程と、該低温空気の一部を前記中圧塔に導入する工程と、該低温空気の残部を温度回復させて帰還空気とする昇温工程と、該帰還空気を昇圧して前記昇圧帰還空気とする循環圧縮工程と、前記中圧塔導入空気を前記中圧塔に導入する工程とを備えている空気液化分離方法。
- 圧縮、精製、冷却した原料空気を中圧塔及び低圧塔にて低温蒸留することにより少なくとも液体酸素を製品として採取する空気液化分離方法であって、原料空気の全量を前記中圧塔の運転圧力より高い第1設定圧力に昇圧して昇圧原料空気とする原料空気圧縮工程と、該昇圧原料空気から不純物を吸着除去して昇圧精製空気とする吸着精製工程と、該昇圧精製空気と後述する昇圧帰還空気とを合流させて循環空気とする循環空気合流工程と、該循環空気を3分流した第1分流空気を第1設定温度に冷却して中圧塔導入空気とし、第2分流空気を前記第1設定温度より高い第2設定温度に冷却して冷膨張用空気とし、さらに、第3分流空気を前記第2設定温度より高い第3設定温度に冷却して温膨張用空気とする冷却工程と、前記冷膨張用空気を前記第1設定圧力より低い第2設定圧力に断熱膨張させることにより第1低温空気とする第1膨張工程と、前記温膨張用空気を前記第2設定圧力に断熱膨張させることにより前記第1設定温度より高い温度の第2低温空気とする第2膨張工程と、該第1低温空気の一部を前記中圧塔に導入する工程と、該第1低温空気の残部と前記第2低温空気とを温度回復させて帰還空気とする昇温工程と、該帰還空気を昇圧して前記昇圧帰還空気とする循環圧縮工程と、前記中圧塔導入空気を前記中圧塔に導入する工程とを備えている空気液化分離方法。
- 前記循環空気を、前記第1設定圧力より高い圧力に昇圧する循環空気昇圧工程を備えている請求項1又は2記載の空気液化分離方法。
- 圧縮、精製、冷却した原料空気を中圧塔及び低圧塔にて低温蒸留することにより少なくとも液体酸素を製品として採取する空気液化分離装置であって、原料空気の全量を前記中圧塔の運転圧力より高い第1設定圧力に昇圧して昇圧原料空気とする原料空気圧縮機と、該昇圧原料空気から不純物を吸着除去して昇圧精製空気とする吸着装置と、該昇圧精製空気と後述する昇圧帰還空気とを合流させて循環空気とする循環空気合流管路と、該循環空気を2分流した第1分流空気を第1設定温度に冷却して中圧塔導入空気とし、第2分流空気を前記第1設定温度より高い第2設定温度に冷却して膨張用空気とする主熱交換器と、該膨張用空気を前記第1設定圧力より低い第2設定圧力に断熱膨張させて低温空気とする膨張タービンと、該低温空気の一部を前記中圧塔に導入する配管と、該低温空気の残部を前記主熱交換器で温度回復させた帰還空気を昇圧して前記昇圧帰還空気とする循環圧縮機と、前記中圧塔導入空気を前記中圧塔に導入する配管とを備えている空気液化分離装置。
- 圧縮、精製、冷却した原料空気を中圧塔及び低圧塔にて低温蒸留することにより少なくとも液体酸素を製品として採取する空気液化分離装置であって、原料空気の全量を前記中圧塔の運転圧力より高い第1設定圧力に昇圧して昇圧原料空気とする原料空気圧縮機と、該昇圧原料空気から不純物を吸着除去して昇圧精製空気とする吸着装置と、該昇圧精製空気と後述する昇圧帰還空気とを合流させて循環空気とする循環空気合流管路と、該循環空気を3分流した第1分流空気を第1設定温度に冷却して中圧塔導入空気とし、第2分流空気を前記第1設定温度より高い第2設定温度に冷却して冷膨張用空気とし、さらに、第3分流空気を前記第2設定温度より高い第3設定温度に冷却して温膨張用空気とする主熱交換器と、前記冷膨張用空気を前記第1設定圧力より低い第2設定圧力に断熱膨張させて第1低温空気とする冷膨張タービンと、前記温膨張用空気を前記第2設定圧力に断熱膨張させて第2低温空気とする温膨張タービンと、前記第1低温空気の一部を前記中圧塔に導入する配管と、該第1低温空気の残部と前記第2低温空気とを前記主熱交換器で温度回復させた帰還空気を昇圧して前記昇圧帰還空気とする循環圧縮機と、前記中圧塔導入空気を前記中圧塔に導入する配管とを備えている空気液化分離装置。
- 前記循環空気を、前記第1設定圧力より高い圧力に昇圧する循環空気圧縮機を備えている請求項4又は5記載の空気液化分離装置。
- 前記循環空気昇圧機は、前記膨張タービンに設けられた膨張タービン制動ブロワである請求項6記載の空気液化分離装置。
- 前記膨張タービンの制動を、ブロワ、発電機、油圧ポンプのいずれかで行う請求項4乃至6いずれか1項記載の空気液化分離装置。
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2010
- 2010-07-20 CN CN201080032477.8A patent/CN102472575B/zh active Active
- 2010-07-20 WO PCT/JP2010/062158 patent/WO2011010630A1/ja active Application Filing
- 2010-07-20 US US13/386,466 patent/US20120131951A1/en not_active Abandoned
- 2010-07-20 KR KR1020117028238A patent/KR20120040685A/ko not_active Application Discontinuation
- 2010-07-22 TW TW099124121A patent/TWI525298B/zh active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS53117690A (en) * | 1977-03-19 | 1978-10-14 | Air Prod & Chem | Method of producing liquid oxygen and*or liquid nitrogen and apparatus therefor |
JPS5495552U (ja) * | 1977-12-16 | 1979-07-06 | ||
JPS57182069A (en) * | 1981-04-20 | 1982-11-09 | Air Prod & Chem | Method and device for separating air |
US4705548A (en) * | 1986-04-25 | 1987-11-10 | Air Products And Chemicals, Inc. | Liquid products using an air and a nitrogen recycle liquefier |
JPH06159930A (ja) * | 1992-07-20 | 1994-06-07 | Air Prod And Chem Inc | 空気の低温蒸留方法 |
Also Published As
Publication number | Publication date |
---|---|
CN102472575A (zh) | 2012-05-23 |
JP5643491B2 (ja) | 2014-12-17 |
TWI525298B (zh) | 2016-03-11 |
KR20120040685A (ko) | 2012-04-27 |
CN102472575B (zh) | 2014-11-05 |
TW201109602A (en) | 2011-03-16 |
US20120131951A1 (en) | 2012-05-31 |
JP2011027318A (ja) | 2011-02-10 |
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