TWI685468B - Method and apparatus for producing product nitrogen gas and product argon - Google Patents

Method and apparatus for producing product nitrogen gas and product argon Download PDF

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Publication number
TWI685468B
TWI685468B TW108105261A TW108105261A TWI685468B TW I685468 B TWI685468 B TW I685468B TW 108105261 A TW108105261 A TW 108105261A TW 108105261 A TW108105261 A TW 108105261A TW I685468 B TWI685468 B TW I685468B
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Taiwan
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gas
rectification tower
oxygen
condenser
product
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TW108105261A
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Chinese (zh)
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TW201940415A (en
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廣瀬献児
馬克辛姆 蘭修
富田伸二
洛克 傑利
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法商液態空氣喬治斯克勞帝方法研究開發股份有限公司
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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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    • 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
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    • 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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    • 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
    • F25J3/0228—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 characterised by the separated product stream
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    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
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    • 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/92—Details relating to the feed point
    • 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
    • F25J2200/90—Details relating to column internals, e.g. structured packing, gas or liquid distribution
    • F25J2200/94—Details relating to the withdrawal point
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/40—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
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/50—Oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J2210/00—Processes characterised by the type or other details of the feed stream
    • F25J2210/58—Argon
    • 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
    • F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
    • 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
    • F25J2215/58—Argon
    • 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/52—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being oxygen enriched compared to air ("crude 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
    • F25J2235/00—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams
    • F25J2235/58—Processes or apparatus involving steps for increasing the pressure or for conveying of liquid process streams the fluid being argon or crude argon
    • 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
    • F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen

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  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
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Abstract

The problem addressed by the present invention lies in providing a method for producing high-purity nitrogen and argon with high energy efficiency by utilizing the cold of an oxygen-containing gas, and also an apparatus employed in said method. An apparatus 100 for producing product nitrogen gas and product argon, comprising: a first rectification column 2 into which raw air is introduced; a second rectification column 5 from which product nitrogen gas is drawn; a third rectification column 6 from which product argon gas is drawn; and a first condenser 3 configured to perform heat exchange between a gas accumulated in a column top portion of the first rectification column 2, and a liquid accumulated in a column bottom portion of the second rectification column 5, wherein an intermediate portion gas containing nitrogen is drawn from an intermediate portion of the second rectification column 5 and merged with a condenser gas drawn from the first condenser 3. The merged gases are expanded and cooled by means of an expansion turbine 8 whereby the cold thereof is utilized.

Description

製品氮氣及製品氬之製造方法及其製造裝置Manufacturing method and manufacturing device of product nitrogen and product argon

本發明係關於一種用以製造氮氣並且製造氬之氮及氬之製造方法及裝置。 The invention relates to a method and a device for producing nitrogen and argon for producing nitrogen and argon.

於藉由使用深冷分離法之氮製造裝置製造氮氣之方法中，提出藉由將自精餾塔之冷凝器部分導出之含有氧之氣體用作寒冷源而提高能量效率之方法(例如專利文獻1)。專利文獻1中，藉由將自精餾塔之中間部導出之流體導入至主熱交換器，使其與原料空氣進行熱交換，而用作寒冷源。揭示有利用膨脹渦輪使該用作寒冷源後之流體膨脹冷卻並再次導入至主熱交換器，進而利用其寒冷之方法。 In the method of producing nitrogen by a nitrogen production device using a cryogenic separation method, a method of improving energy efficiency by using an oxygen-containing gas discharged from a condenser portion of a rectification column as a cold source (for example, Patent Literature 1). In Patent Document 1, the fluid led from the middle part of the rectification column is introduced into the main heat exchanger to exchange heat with the raw material air, and is used as a cold source. It is disclosed that an expansion turbine is used to expand and cool the fluid used as a source of cold and then reintroduce it to the main heat exchanger to utilize its coldness.

已知有藉由使用深冷分離法之空氣分離裝置而製造氮、氬及氧之方法。氧與氬由於其沸點近似，故於欲製造氬之情形時，需要進行用以使氧與氬分離之精餾，該步驟中，一般亦製造高純度之氧(例如專利文獻2)。 A method of producing nitrogen, argon, and oxygen by using an air separation device using a cryogenic separation method is known. Oxygen and argon have similar boiling points, so in the case of argon production, it is necessary to perform rectification to separate oxygen and argon. In this step, generally high-purity oxygen is also produced (for example, Patent Document 2).

[先前技術文獻] [Prior Technical Literature]

[專利文獻] [Patent Literature]

[專利文獻1]美國專利第4,222,756號說明書 [Patent Document 1] Specification of US Patent No. 4,222,756

[專利文獻2]日本特開平8-61844號公報 [Patent Document 2] Japanese Patent Laid-Open No. 8-61844

難以使專利文獻1中揭示之將自精餾塔之冷凝器部分導出之含有氧之氣體用作寒冷源之方法應用於不僅製造氮亦製造氬之方法以提昇能量效率。又，專利文獻1中揭示之方法中，雖能夠製造氮，但未提及關於氬之製造。 It is difficult to apply the method disclosed in Patent Document 1 that uses the oxygen-containing gas discharged from the condenser portion of the rectification column as a cold source for a method of manufacturing not only nitrogen but also argon to improve energy efficiency. In addition, although the method disclosed in Patent Document 1 can produce nitrogen, it does not mention the production of argon.

然而，近年來，不僅想取出氮亦想取出氬之要求高漲。 However, in recent years, the demand for not only nitrogen but also argon has increased.

鑒於上述實際情況，本發明之目的在於提供一種藉由利用含氧氣體之寒冷而以高能量效率製造高純度之氮及氬之方法及用於該方法之裝置。 In view of the above actual circumstances, an object of the present invention is to provide a method for producing high-purity nitrogen and argon with high energy efficiency by utilizing the coldness of an oxygen-containing gas and an apparatus for the method.

(發明1) (Invention 1)

本發明之製品氮氣及製品氬氣之製造方法，包含：冷卻步驟，其使已去除既定之雜質之原料空氣冷卻；原料空氣導入步驟，其將上述預冷步驟中冷卻之上述原料空氣導入至第一精餾塔；第一富氧液體導入步驟，其將自上述第一精餾塔之塔底部導出之富氧液體導入至第二精餾塔；第二富氧液體導入步驟，其將自上述第一精餾塔之塔底部導出之富氧液體之至少一部分導入至配置於第三精餾塔之第二冷凝器；含氮液體導入步驟，其將上述第一精餾塔中冷凝之含氮液體作為環流液導入至上述第二精餾塔上部；膨脹步驟，其使自上述第二精餾塔之中間部導出之中間部氣體與自第一冷凝器導出之冷凝器氣體的混合氣體之至少一部分膨脹而產生寒冷，其中上述第一冷凝器係構成為使貯存於上述第一精餾塔之塔頂部之氣體與貯存於上述第二 精餾塔之塔底部之液體進行熱交換；含氬氣體導入步驟，其將自上述第二精餾塔之下部導出之含氬氣體導入至上述第三精餾塔；製品氮氣導出步驟，其自上述第二精餾塔之塔頂部導出製品氮氣；及製品氬導出步驟，其自上述第二精餾塔之中間部導出製品氬。 The manufacturing method of product nitrogen and product argon of the present invention includes: a cooling step, which cools the raw material air from which predetermined impurities have been removed; a raw material air introduction step, which introduces the raw material air cooled in the pre-cooling step to the first A rectification tower; the first oxygen-rich liquid introduction step, which introduces the oxygen-rich liquid led from the bottom of the first rectification tower to the second rectification tower; the second oxygen-rich liquid introduction step, which will be from the above At least a part of the oxygen-enriched liquid withdrawn from the bottom of the first rectification tower is introduced into the second condenser arranged in the third rectification tower; The liquid is introduced into the upper portion of the second rectification tower as a circulating liquid; the expansion step is such that at least the mixed gas of the middle portion gas drawn from the middle portion of the second rectification tower and the condenser gas drawn from the first condenser is at least A part of it expands to produce cold, wherein the first condenser is configured to store the gas stored in the top of the first rectification tower and the second The liquid at the bottom of the rectification tower is subjected to heat exchange; the argon-containing gas introduction step introduces the argon-containing gas derived from the lower part of the second rectification tower to the third rectification tower; the product nitrogen export step The product nitrogen is led out from the top of the second rectification tower; and the product argon extraction step is to export the product argon from the middle of the second rectification tower.

第一精餾塔運轉壓力高於第二精餾塔，能夠將原料空氣分離為富氧液體與氮氣。第二精餾塔中，製造含有氬與氧之氣體，供給至第三精餾塔。第三精餾塔中，製造製品氬。 The operating pressure of the first rectification tower is higher than that of the second rectification tower, which can separate the feed air into oxygen-rich liquid and nitrogen. In the second rectification tower, a gas containing argon and oxygen is produced and supplied to the third rectification tower. In the third distillation tower, the product argon is manufactured.

首先，經壓縮已去除既定之雜質之原料空氣藉由主熱交換器中之冷卻步驟冷卻，成為低溫之原料空氣。該原料空氣於原料空氣導入步驟中，導入至第一精餾塔。導入至第一精餾塔之原料空氣與第一精餾塔之塔頂部中冷凝之液體氮接觸進行精餾，並分離為富氧液體與氮氣。 First, the compressed raw material air from which certain impurities have been removed is cooled by the cooling step in the main heat exchanger to become a low-temperature raw material air. The raw material air is introduced into the first rectification tower in the raw material air introduction step. The raw material air introduced into the first rectification tower contacts the liquid nitrogen condensed in the top of the first rectification tower to perform rectification, and is separated into oxygen-enriched liquid and nitrogen.

貯存於第一精餾塔之下部之富氧液體於第一富氧液體導入步驟中，供給至第二精餾塔之既定之位置。供給至第二精餾塔之富氧液體為製品氮及製品氬之原料，亦用作第二精餾塔中之冷媒。 The oxygen-enriched liquid stored in the lower part of the first rectification tower is supplied to the predetermined position of the second rectification tower in the first oxygen-enriched liquid introduction step. The oxygen-rich liquid supplied to the second rectification tower is the raw material for product nitrogen and product argon, and is also used as the refrigerant in the second rectification tower.

貯存於第一精餾塔之下部之富氧液體之至少一部分於供給至第二精餾塔前，於第二富氧液體導入步驟中，供給至配置於第三精餾塔之第二冷凝器。導入之富氧液體於第二冷凝器中用作用以使氬冷凝之冷媒。 At least a part of the oxygen-rich liquid stored in the lower part of the first rectification tower is supplied to the second condenser arranged in the third rectification tower before the second rectification tower is introduced, and in the second oxygen-rich liquid introduction step . The introduced oxygen-rich liquid is used as a refrigerant for condensing argon in the second condenser.

第二冷凝器中氣化之富氧液體自第三精餾塔導出之後，作為冷媒供給至第二精餾塔之既定之位置。 After the oxygen-enriched liquid vaporized in the second condenser is discharged from the third rectification tower, it is supplied as a refrigerant to a predetermined position of the second rectification tower.

貯存於第一精餾塔之下部之富氧液體能夠經分流而將一部分供給至第二精餾塔，將未供給至第二精餾塔之部分供給至第二冷凝器，但亦可將富氧液體之全部供給至第二冷凝器之後，再供給至第二精餾塔。即便在富氧液體經分流，一部分不經由第二冷凝器而供給至第二精餾塔之情形時，由於經由第二冷凝器 之後之富氧液體亦會供給至第二精餾塔，故最終將富氧液體之總量供給至第二精餾塔。 The oxygen-rich liquid stored in the lower part of the first rectification tower can be partially supplied to the second rectification tower, and the part not supplied to the second rectification tower can be supplied to the second condenser, but the rich After all the oxygen liquid is supplied to the second condenser, it is supplied to the second rectification tower. Even when the oxygen-enriched liquid is split and a part is supplied to the second rectification tower without passing through the second condenser, the After that, the oxygen-enriched liquid is also supplied to the second rectification tower, so the total amount of oxygen-enriched liquid is finally supplied to the second rectification tower.

第一精餾塔中冷凝之含氮液體於含氮液體導入步驟中，作為環流液導入至第二精餾塔上部。 The nitrogen-containing liquid condensed in the first rectification column is introduced into the upper part of the second rectification column as a circulating liquid in the nitrogen-containing liquid introduction step.

第一精餾塔之冷凝器係構成為使貯存於第一精餾塔之塔頂部之氣體與貯存於第二精餾塔之塔底部之液體進行熱交換。冷凝器氣體自該冷凝器導出。冷凝器中冷凝之氣體作為環流液供給至第一精餾塔，冷凝器中氣化之液體作為冷凝器氣體供給至第二精餾塔。由於含氬氣體自第二精餾塔之下部被導出，故冷凝器氣體之主成分成為氧。其原因在於：為了藉由深冷分離而製造氬，需要將幾乎全部之氧高純度地濃縮進行回收。否則，由於氬與氧之沸點非常近，故氬容易混入至氧流而流出，無法實現氬之回收。因此，自第二精餾塔之底部導出之冷凝器氣體成為幾乎100%之純氧氣體。 The condenser of the first rectification tower is configured to exchange heat between the gas stored at the top of the tower of the first rectification tower and the liquid stored at the bottom of the tower of the second rectification tower. The condenser gas is discharged from the condenser. The gas condensed in the condenser is supplied as a circulating liquid to the first rectification tower, and the gasified liquid in the condenser is supplied as the condenser gas to the second rectification tower. Since the argon-containing gas is led out from the lower part of the second distillation column, the main component of the condenser gas becomes oxygen. The reason is that in order to produce argon by cryogenic separation, it is necessary to concentrate and recover almost all oxygen in high purity. Otherwise, because the boiling points of argon and oxygen are very close, argon is easily mixed into the oxygen stream and flows out, and argon cannot be recovered. Therefore, the condenser gas drawn from the bottom of the second rectification tower becomes almost 100% pure oxygen gas.

因此，於欲於主熱交換器中利用冷凝器氣體之寒冷之情形時，需要使用可耐氧氣使用之特殊素材之配管。進而，使於主熱交換器中利用寒冷後之冷凝器氣體膨脹冷卻，進而於主熱交換器中使用其寒冷之情形時，必須使用可耐氧氣使用之特殊素材之膨脹渦輪。將冷凝器氣體不經由主熱交換器而直接導入至膨脹渦輪，藉由膨脹渦輪使其膨脹冷卻之情形亦同樣地，必須使用能夠應對高濃度氧之特殊之膨脹渦輪。作為特殊素材，例如可列舉杜拉鋁等素材，但其難以獲取，價格昂貴。 Therefore, when you want to use the cold of the condenser gas in the main heat exchanger, you need to use piping of special materials that can withstand oxygen. Furthermore, in the case where the condenser gas after the cold is expanded and cooled in the main heat exchanger, and the cold is used in the main heat exchanger, an expansion turbine of a special material that can withstand the use of oxygen must be used. The condenser gas is directly introduced into the expansion turbine without passing through the main heat exchanger, and the case of expansion cooling by the expansion turbine is the same. A special expansion turbine capable of coping with high-concentration oxygen must be used. Examples of the special materials include materials such as Duralumin, but they are difficult to obtain and expensive.

因此本發明中，使自第二精餾塔之中間部導出之中間部氣體與上述冷凝器氣體合流之後，使其釋放寒冷並膨脹冷卻，進而使其產生寒冷。中間部氣體含有較多氮氣，故若與冷凝器氣體混合，則能夠使氣體中含有之氧濃度降低。藉此，能夠利用不使用可耐氧氣使用之特殊素材的通常之配管或膨脹渦輪。不使用特殊素材之膨脹渦輪或配管具有容易獲取，費用亦低廉之優點。 雖然藉由將製品氮氣代替中間部氣體混合於上述冷凝器氣體亦能夠使導入至膨脹渦輪之氣體中氧濃度降低，但由於會使製品氮氣量降低，故不理想。 Therefore, in the present invention, after the middle portion gas discharged from the middle portion of the second rectification column is merged with the condenser gas, it is allowed to release cold and expand and cool, thereby making it cold. The middle gas contains a lot of nitrogen, so if it is mixed with the condenser gas, the concentration of oxygen contained in the gas can be reduced. This makes it possible to use ordinary piping or expansion turbines that do not use special materials that can withstand oxygen. Expansion turbines or pipes that do not use special materials have the advantages of easy availability and low cost. Although the concentration of oxygen in the gas introduced into the expansion turbine can be reduced by mixing product nitrogen instead of the intermediate gas in the condenser gas, it is not preferable because it reduces the amount of product nitrogen.

將富氧液體自第一精餾塔之塔底部導入至第二精餾塔時，亦可經由過冷卻器，使導入至第二精餾塔前之富氧液體冷卻。其原因在於：能夠抑制因使富氧液體於第二精餾塔內部大量氣化而導致精餾效率降低之現象，精餾效率進一步提昇。過冷卻器中，通過富氧液體導出管及含氮液體導入管之流體藉由進行與通過製品氮氣導出管之製品氮氣之熱交換而被冷卻。 When the oxygen-rich liquid is introduced from the bottom of the first rectification tower to the second rectification tower, the oxygen-rich liquid before being introduced into the second rectification tower may also be cooled through the supercooler. The reason for this is that it is possible to suppress the phenomenon that the rectification efficiency is reduced due to a large amount of gasification of the oxygen-rich liquid inside the second rectification tower, and the rectification efficiency is further improved. In the subcooler, the fluid passing through the oxygen-enriched liquid outlet pipe and the nitrogen-containing liquid inlet pipe is cooled by performing heat exchange with the product nitrogen passing through the product nitrogen outlet pipe.

本發明中，能夠將氧氣之寒冷用於原料空氣之冷卻。藉由將以氧為主成分之冷凝器氣體與中間部氣體一起導入至主熱交換器，能夠利用冷凝器氣體及中間部氣體之寒冷之後，使其膨脹冷卻，並進而利用其寒冷。因此，尤其對於需要氮及氬但不需要氧氣之用途，能夠利用作為氣體製品而言不需要之氧之寒冷，故能夠提供一種能量效率較高之製品氮氣及製品氬之製造方法。 In the present invention, the coldness of oxygen can be used to cool the raw material air. By introducing the condenser gas mainly composed of oxygen into the main heat exchanger together with the middle gas, it is possible to use the coldness of the condenser gas and the middle gas, then expand and cool it, and then use its coldness. Therefore, especially for applications requiring nitrogen and argon but not requiring oxygen, it is possible to use the coldness of oxygen which is unnecessary as a gas product, so it is possible to provide a method for manufacturing nitrogen and argon with higher energy efficiency.

且說，第二精餾塔中，含有氮之氣體一面於第二精餾塔內部上升，一面與供給至第二精餾塔之上部之液體氮接觸而被精餾。該步驟中，伴隨含有氮之氣體之氬及氧之一部分亦於第二精餾塔內部上升。由於伴隨之氬及氧混入至製品氮氣中，故成為使製品氮氣之純度降低之因素。為使氧氮氬成分完全分離，製造高純度之製品氮氣，亦考慮設置多個蒸餾段，但存在成本變高之問題，同時，氧氮氬成分之完全之精餾分離需要極精密之運轉控制之調整，原料空氣之供給量等負載變動時，難以進行穩定之裝置之運轉。 In addition, in the second rectification tower, while the gas containing nitrogen rises inside the second rectification tower, it comes into contact with the liquid nitrogen supplied to the upper part of the second rectification tower to be rectified. In this step, a part of argon and oxygen accompanying the nitrogen-containing gas also rise inside the second rectification tower. Since the accompanying argon and oxygen are mixed into the product nitrogen, it becomes a factor that reduces the purity of the product nitrogen. In order to completely separate the oxygen, nitrogen and argon components and manufacture high-purity product nitrogen, multiple distillation stages are also considered, but there is a problem of high cost. At the same time, complete rectification and separation of the oxygen, nitrogen and argon components requires extremely precise operation control It is difficult to carry out stable operation of the device when the load of the raw air supply fluctuates due to the adjustment.

本發明中，藉由使含有氮之中間部氣體自第二精餾塔之中間部導出，能夠使於第二精餾塔內部上升之氬及氧之量降低。其結果為，製品氮氣中所含有之氬及氧之量降低，能夠不設置多個蒸餾段而提高製品氮氣之純度。 In the present invention, the amount of argon and oxygen rising inside the second rectifying tower can be reduced by leading the middle gas containing nitrogen from the middle of the second rectifying tower. As a result, the amount of argon and oxygen contained in the product nitrogen is reduced, and the purity of the product nitrogen can be improved without providing multiple distillation stages.

(發明2) (Invention 2)

本發明之製品氮氣及製品氬氣之製造裝置(100、101、102、103)，具 備：主熱交換器(1)，其使已去除既定之雜質之原料空氣冷卻；第一精餾塔(2)，其被導入冷卻之上述原料空氣；第二精餾塔(5)，其導出製品氮氣；第三精餾塔(6)，其導出製品氬；第一冷凝器(3)，其構成為使貯存於上述第一精餾塔之塔頂部之氣體與貯存於上述第二精餾塔之塔底部之液體進行熱交換；含氮液體導入管(11)，其將上述第一冷凝器(3)中冷凝之含氮液體之至少一部分作為環流液導入至上述第二精餾塔；含氬氣體導入管(17)，其使含氬氣體自上述第二精餾塔之下部導入至上述第三精餾塔；含氬液體導出管(19)，其將含氬液體自上述第三精餾塔之塔底部導入至上述第二精餾塔；冷凝器氣體導出管(14)，其使冷凝器氣體自上述第一冷凝器(3)之氣相部導出；中間部氣體導出管(15)，其使中間部氣體自上述第二精餾塔之中間部導出；膨脹渦輪(8)，其使上述冷凝器氣體與上述中間部氣體之混合氣體膨脹冷卻；製品氮氣導出管(16)，其使上述製品氮氣自上述第二精餾塔導出；及製品氬導出管(18)，其使上述製品氬自上述第三精餾塔之中間部導出。 The manufacturing device (100, 101, 102, 103) of the product nitrogen and product argon of the present invention has Preparation: Main heat exchanger (1), which cools the raw material air from which predetermined impurities have been removed; the first rectification tower (2), which is led to the cooled raw material air; the second rectification tower (5), which The product nitrogen is discharged; the third rectification tower (6), which leads the product argon; the first condenser (3), which is configured to store the gas stored at the top of the first rectification tower and the second rectification The liquid at the bottom of the distillation tower is subjected to heat exchange; a nitrogen-containing liquid introduction pipe (11) which introduces at least a part of the nitrogen-containing liquid condensed in the first condenser (3) as a circulating liquid to the second rectification tower Argon-containing gas introduction tube (17), which causes the argon-containing gas to be introduced from the lower part of the second rectification column to the third rectification column; an argon-containing liquid outlet tube (19), which takes the argon-containing liquid from the first The bottom of the third rectification tower is introduced into the second rectification tower; the condenser gas outlet pipe (14), which leads the condenser gas from the gas phase portion of the first condenser (3); the middle gas outlet pipe (15), which causes the middle gas to be led out from the middle part of the second rectification tower; an expansion turbine (8), which expands and cools the mixed gas of the condenser gas and the middle part gas; the product nitrogen outlet pipe (16 ), which leads the product nitrogen from the second rectification column; and product argon outlet tube (18), which causes the product argon to exit from the middle of the third rectification column.

再者，本說明書中用括號記載之符號表示一實施形態，並不限定於此。 In addition, the symbols described in parentheses in this specification indicate an embodiment, and are not limited thereto.

於不設置本發明中之中間部氣體導出管(15)之情形時，自冷凝器氣體導出管(14)導出之冷凝器氣體中之氧濃度變得極高(例如為99%以 上)。其原因在於：為了製造氬氣，藉由含氬氣體導入管(17)使含有氬之氣體自第二精餾塔(5)導出。 When the middle gas outlet pipe (15) in the present invention is not provided, the oxygen concentration in the condenser gas discharged from the condenser gas outlet pipe (14) becomes extremely high (for example, 99% on). The reason is that in order to produce argon gas, the argon-containing gas introduction pipe (17) is used to guide the argon-containing gas from the second rectification column (5).

本發明中，藉由設置中間部氣體導出管(15)，使含有氮之中間部氣體與含有高濃度之氧之冷凝器氣體合流，而使氧濃度降低(例如為70%以上97%以下)。因此，膨脹渦輪(8)不必使用能夠用於氧氣之特殊素材(例如杜拉鋁)。因此，具有容易獲取配管或膨脹渦輪，價格亦低廉之優點。 In the present invention, by providing an intermediate gas outlet pipe (15), the intermediate gas containing nitrogen and the condenser gas containing high concentration oxygen are merged to reduce the oxygen concentration (for example, 70% or more and 97% or less) . Therefore, the expansion turbine (8) does not need to use special materials (such as Duralumin) that can be used for oxygen. Therefore, it has the advantages of easy access to piping and expansion turbines, and low price.

冷凝器氣體與中間部氣體之混合氣體被導入至膨脹渦輪(8)而膨脹冷卻。藉此產生之寒冷被導入至主熱交換器(1)而用於與原料空氣之熱交換。 The mixed gas of the condenser gas and the intermediate gas is introduced into the expansion turbine (8) and expanded and cooled. The cold generated by this is introduced into the main heat exchanger (1) for heat exchange with the raw material air.

於導入至膨脹渦輪(8)前，冷凝器氣體與中間部氣體之混合氣體亦可被導入至主熱交換器(1)。於該情形時，冷凝器氣體與中間部氣體之混合氣體藉由於主熱交換器(1)中進行與原料空氣之熱交換而釋放其寒冷。進而於釋放寒冷之後導入至膨脹渦輪(8)而膨脹冷卻。膨脹冷卻之氣體再次導入至主熱交換器(1)而將其寒冷用於與原料空氣之熱交換。 Before being introduced into the expansion turbine (8), the mixed gas of the condenser gas and the intermediate gas can also be introduced into the main heat exchanger (1). In this case, the mixed gas of the condenser gas and the middle gas releases its cold by heat exchange with the raw material air in the main heat exchanger (1). Furthermore, after releasing the cold, it is introduced into an expansion turbine (8) to expand and cool. The expanded and cooled gas is introduced into the main heat exchanger (1) again and its coldness is used for heat exchange with the raw material air.

由於如上所述利用含有氧之氣體之寒冷，故而尤其於不需要作為製品氣體之氧之用途中，能夠以高能量效率製造製品氮氣及製品氬氣。 Since the cold of the oxygen-containing gas is utilized as described above, it is possible to produce product nitrogen and product argon with high energy efficiency, especially in applications that do not require oxygen as product gas.

進而於本發明中，藉由設置中間部氣體導出管(15)，能夠使伴隨第二精餾塔(5)內上升之氮氣而於第二精餾塔(5)內上升之氬及氧之量降低。因此，有自第二精餾塔(5)之塔頂部獲得之製品氮氣之純度變高之效果。 Furthermore, in the present invention, by providing an intermediate gas outlet pipe (15), it is possible to cause the argon and oxygen that rise in the second rectification tower (5) with the nitrogen gas that rises in the second rectification tower (5) The amount is reduced. Therefore, there is an effect that the purity of the product nitrogen obtained from the top of the second distillation column (5) becomes higher.

(發明3) (Invention 3)

上述發明之製品氮氣及製品氬氣之製造裝置中，可進而具備：富氧液體導出管(21)，其自上述第一精餾塔之塔底部導出貯存於上述第一精餾塔之塔底部之富氧液體；第二富氧液體導入管(13)，其將自上述富氧液體導出管(21)導出之富 氧液體導入至配置於上述第三精餾塔之第二冷凝器(7)；及第三富氧液體導入管(22)，其將自上述第二冷凝器導出之富氧液體導入至上述第二精餾塔。 The manufacturing apparatus for product nitrogen and product argon of the above invention may further include: an oxygen-rich liquid outlet pipe (21), which is led out from the bottom of the first rectification tower and stored at the bottom of the first rectification tower Oxygen-enriched liquid; the second oxygen-enriched liquid introduction pipe (13), which will be enriched from the oxygen-enriched liquid outlet pipe (21) Oxygen liquid is introduced into the second condenser (7) disposed in the third rectification tower; and a third oxygen-rich liquid introduction pipe (22), which introduces the oxygen-rich liquid led from the second condenser to the first Second distillation tower.

(發明4) (Invention 4)

發明3中，上述第三富氧液體導入管(22)可將氣體狀態之富氧液體自上述第二冷凝器(7)之氣相部導入至上述第二精餾塔(5)。 In invention 3, the third oxygen-rich liquid introduction pipe (22) can introduce the gas-rich oxygen-rich liquid from the gas phase portion of the second condenser (7) to the second rectification tower (5).

富氧液體係作為冷媒且作為製品氮及製品氬之原料導入至第二精餾塔(5)。然而，富氧液體之一部分或全部亦可導入至第二冷凝器(7)且於利用富氧液體之寒冷之後，送回至第二精餾塔(5)。於該情形時，第二冷凝器(7)中氣化之富氧液體以氣體狀態存在於第二冷凝器(7)之上部，藉由自第二冷凝器(7)之上部延伸之第三富氧液體導入管(22)送回至第二精餾塔(5)。 The oxygen-enriched liquid system is introduced into the second distillation column (5) as a refrigerant and as raw materials for product nitrogen and product argon. However, part or all of the oxygen-enriched liquid can also be introduced into the second condenser (7) and after the cold using the oxygen-enriched liquid is returned to the second rectification column (5). In this case, the oxygen-enriched liquid vaporized in the second condenser (7) exists in a gas state above the second condenser (7), by the third extending from the upper part of the second condenser (7) The oxygen-rich liquid introduction pipe (22) is sent back to the second rectification tower (5).

(發明5) (Invention 5)

上述發明之製品氮氣及製品氬氣之製造裝置可進而具有：第四精餾塔(9)，其配置於上述第二冷凝器之上部；及第四精餾塔塔頂部氣體導入管(23)，其將自上述第四精餾塔之塔頂部取出之第四精餾塔塔頂部氣體導入至上述第二精餾塔。 The manufacturing device of the product nitrogen and the product argon of the above invention may further include: a fourth rectification tower (9) disposed above the second condenser; and a gas introduction pipe (23) at the top of the fourth rectification tower It introduces the gas from the top of the fourth rectification tower taken from the top of the tower of the fourth rectification tower to the second rectification tower.

上述第三富氧液體導入管將液體狀態之富氧液體自上述第二冷凝器之液相部導入至上述第二精餾塔。 The third oxygen-enriched liquid introduction pipe introduces the liquid oxygen-enriched liquid from the liquid phase portion of the second condenser to the second rectification tower.

貯存於上述第一精餾塔之塔底部之富氧液體經由上述第四精餾塔之氣相部而導入至上述第二冷凝器。 The oxygen-rich liquid stored in the bottom of the first rectification column is introduced into the second condenser through the gas phase of the fourth rectification column.

藉由設置第四精餾塔(9)，能夠使富氧液體中含有之氬於第四精餾塔(9)內部進一步濃縮，供給至第二精餾塔(5)。因此，能夠降低第二精餾塔(5)中之分離之負載，提昇精餾效率，進而，亦能夠提昇氬之回收 率。 By providing the fourth rectification tower (9), the argon contained in the oxygen-rich liquid can be further concentrated inside the fourth rectification tower (9) and supplied to the second rectification tower (5). Therefore, it is possible to reduce the separation load in the second rectification tower (5), improve the rectification efficiency, and in turn, can also improve the recovery of argon rate.

(發明6) (Invention 6)

上述發明之製品氮氣及製品氬氣之製造裝置中，亦能夠進而具備： 第四精餾塔(9)，其配置於上述第二冷凝器之上部；及第一富氧液體導入管(12)，其將貯存於上述第一精餾塔之塔底部之富氧液體之至少一部分導入至上述第二精餾塔。 The production device for the product nitrogen and the product argon of the above invention can further include: A fourth rectification tower (9), which is arranged above the second condenser; and a first oxygen-rich liquid introduction pipe (12), which stores the oxygen-rich liquid stored in the bottom of the first rectification tower At least a part is introduced into the above-mentioned second distillation column.

(發明7) (Invention 7)

上述發明之製品氮氣及製品氬氣之製造裝置中，冷凝器氣體與中間部氣體之混合氣體被導入至膨脹渦輪(8)。該混合氣體可為自上述第一冷凝器(3)之氣相部直接取出之上述冷凝器氣體與自上述第二精餾塔(5)之中間部直接取出之上述中間部氣體的混合氣體。 In the manufacturing device for the product nitrogen and the product argon of the above invention, the mixed gas of the condenser gas and the intermediate gas is introduced into the expansion turbine (8). The mixed gas may be a mixed gas of the condenser gas directly taken out from the gas phase part of the first condenser (3) and the middle part gas taken out directly from the middle part of the second rectification column (5).

藉由膨脹渦輪(8)使冷凝器氣體與中間部氣體之混合氣體進而冷卻之後，能夠於主熱交換器(1)中利用其寒冷。藉由有效地利用混合氣體之寒冷，能夠提昇能量效率。 After the mixed gas of the condenser gas and the intermediate gas is further cooled by the expansion turbine (8), its coldness can be used in the main heat exchanger (1). By effectively using the coldness of the mixed gas, energy efficiency can be improved.

(發明8) (Invention 8)

又，該混合氣體亦可為將自上述第一冷凝器之氣相部直接取出之上述冷凝器氣體與自上述第二精餾塔之中間部直接取出之上述中間部氣體混合之後，經由上述主熱交換器的混合氣體。 In addition, the mixed gas may be obtained by mixing the condenser gas directly taken out from the gas phase part of the first condenser and the middle part gas taken directly from the middle part of the second rectification column, and then passing through the main The gas mixture of the heat exchanger.

亦能夠於將冷凝器氣體與中間部氣體之混合氣體導入至膨脹渦輪(8)之前，導入至主熱交換器(1)，利用其寒冷，進而藉由膨脹渦輪(8)使其膨脹冷卻之後，於主熱交換器(1)中利用其寒冷。藉由有效地利用混合氣體之寒冷，能夠提昇能量效率。 It can also be introduced into the main heat exchanger (1) before the mixed gas of the condenser gas and the intermediate gas is introduced into the expansion turbine (8), use its coldness, and then expand and cool it by the expansion turbine (8) , Use its coldness in the main heat exchanger (1). By effectively using the coldness of the mixed gas, energy efficiency can be improved.

(發明9) (Invention 9)

上述發明之製品氮氣及製品氬氣之製造裝置中，可構成為使上述含氮液體 配管(11)及上述富氧液體導出管(21)之至少任一者與上述製品氮氣導出管經由過冷卻器(4)。 In the manufacturing apparatus for the product nitrogen and the product argon of the above invention, the above nitrogen-containing liquid may be configured At least one of the piping (11) and the oxygen-enriched liquid outlet pipe (21) and the product nitrogen outlet pipe pass through a subcooler (4).

藉由經由過冷卻器(4)進行與溫度較低之製品氮氣之熱交換，而將含氮液體及/或富氧液體冷卻。藉此，能夠抑制導入至第二精餾塔(5)之含氮液體及/或富氧液體於第二精餾塔(5)內部大量氣化而降低精餾效率之現象。 The nitrogen-containing liquid and/or oxygen-enriched liquid is cooled by performing heat exchange with the product nitrogen at a lower temperature through the supercooler (4). Thereby, the phenomenon that the nitrogen-containing liquid and/or the oxygen-enriched liquid introduced into the second rectification tower (5) is gasified in a large amount inside the second rectification tower (5) can be suppressed, thereby reducing the rectification efficiency.

(發明10) (Invention 10)

上述發明之製品氮氣及製品氬氣之製造裝置中，中間部氣體導出管可於導入至上述過冷卻器後，與上述冷凝器氣體導出管於第一合流點(25)連接。第一合流點(25)為上述過冷卻器之後段且上述膨脹渦輪之前段。 In the manufacturing apparatus for the product nitrogen and the product argon of the above invention, the intermediate gas outlet pipe may be connected to the condenser gas outlet pipe at the first confluence point (25) after being introduced into the supercooler. The first confluence point (25) is the back stage of the supercooler and the front stage of the expansion turbine.

藉由將中間部氣體導入至過冷卻器(4)，而將中間部氣體之寒冷用於富氧液體及/或含氮液體之冷卻，故能夠實現能量效率之進一步提昇。 By introducing the intermediate gas to the supercooler (4), the cold of the intermediate gas is used for cooling the oxygen-rich liquid and/or the nitrogen-containing liquid, so that the energy efficiency can be further improved.

(發明11) (Invention 11)

上述發明之製品氮氣及製品氬氣之製造裝置中，上述第二精餾塔之中間部可為較上述含氮液體導入管(11)之上述第二精餾塔(5)側之安裝位置下方，且為較上述第一富氧液體導入管(12)之上述第二精餾塔(5)側之安裝位置上方。 In the apparatus for manufacturing product nitrogen and product argon of the above invention, the middle portion of the second rectification tower may be lower than the installation position on the side of the second rectification tower (5) of the nitrogen-containing liquid introduction pipe (11) And above the installation position on the second rectification tower (5) side of the first oxygen-enriched liquid introduction pipe (12).

藉由將中間部氣體導出管(15)安裝於較含氮液體導入管(11)下方，且較第一富氧液體導入管(12)上方，能夠將製品氮氣之純度維持得較高，並且將導入至膨脹渦輪(8)之氣體中之氧濃度控制為既定之濃度以下(例如97%以下)。 By installing the middle gas outlet pipe (15) below the nitrogen-containing liquid introduction pipe (11) and above the first oxygen-rich liquid introduction pipe (12), the purity of the product nitrogen can be maintained high, and The oxygen concentration in the gas introduced into the expansion turbine (8) is controlled to a predetermined concentration or less (for example, 97% or less).

(發明12) (Invention 12)

上述發明之製品氮氣及製品氬氣之製造裝置中，自中間部氣體導出管(15)導出之中間部氣體之導出流量相對於自冷凝器 氣體導出管(14)導出之冷凝器氣體之導出流量的比可為0.03以上且2以下。中間部氣體之導出流量相對於冷凝器氣體之導出流量的比較佳可為0.25以上且0.5以下。 In the manufacturing apparatus of the product nitrogen and the product argon of the above invention, the flow rate of the middle gas discharged from the middle gas outlet pipe (15) is relative to the self-condenser The ratio of the discharge flow rate of the condenser gas discharged from the gas discharge pipe (14) may be 0.03 or more and 2 or less. The comparison of the outlet flow rate of the gas in the middle portion with respect to the outlet flow rate of the condenser gas is preferably 0.25 or more and 0.5 or less.

藉由設為上述流量比，能夠將導入至主熱交換器(1)之冷凝器氣體及中間部氣體之混合氣體所含有之氧濃度維持於70%以上且97%以下，並且將溫度控制於-185℃以上且-165℃以下。 By setting the above flow rate ratio, the oxygen concentration contained in the mixed gas of the condenser gas and the intermediate gas introduced into the main heat exchanger (1) can be maintained at 70% or more and 97% or less, and the temperature can be controlled at -185°C or more and -165°C or less.

上述發明之製品氮氣及製品氬氣之製造裝置中，導入至膨脹渦輪(8)之氣體中之氧濃度可為70%以上且97以下。藉由使氧濃度為70%以上且97以下，能夠應用由廉價之材料(例如不鏽鋼)構成之膨脹渦輪(8)。 In the manufacturing device of the product nitrogen and the product argon of the above invention, the oxygen concentration in the gas introduced into the expansion turbine (8) may be 70% or more and 97 or less. By setting the oxygen concentration to 70% or more and 97 or less, it is possible to apply an expansion turbine (8) composed of an inexpensive material (for example, stainless steel).

根據以上所述之製品氮氣及製品氬之製造裝置，能夠不降低氬之回收率，藉由利用含有氧之冷凝器氣體及中間部氣體之寒冷，而以高能量效率製造製品氮氣及製品氬。又，於利用寒冷時，能夠不使用對氧氣具有耐久性之特殊構件，而使用利用一般之素材(例如不鏽鋼)之配管及膨脹渦輪。又，能夠製造氧及含氬量少之高純度之製品氮氣。 According to the manufacturing apparatus for product nitrogen and product argon described above, it is possible to manufacture product nitrogen and product argon with high energy efficiency by utilizing the cold of the condenser gas containing oxygen and the gas in the middle without reducing the recovery rate of argon. In addition, when using cold, it is possible to use piping and expansion turbines that use general materials (such as stainless steel) without using special members that are durable to oxygen. In addition, it can produce high-purity product nitrogen with a small amount of oxygen and argon.

1‧‧‧主熱交換器 1‧‧‧Main heat exchanger

2‧‧‧第一精餾塔 2‧‧‧First distillation tower

3‧‧‧第一冷凝器 3‧‧‧The first condenser

4‧‧‧過冷卻器 4‧‧‧Supercooler

5‧‧‧第二精餾塔 5‧‧‧Second distillation tower

6‧‧‧第三精餾塔 6‧‧‧The third distillation tower

7‧‧‧第二冷凝器 7‧‧‧Second condenser

8‧‧‧膨脹渦輪 8‧‧‧Expansion turbine

9‧‧‧第四精餾塔 9‧‧‧Fourth distillation tower

11‧‧‧含氮液體導入管 11‧‧‧Nitrogen-containing liquid introduction pipe

12‧‧‧第一富氧液體導入管 12‧‧‧The first oxygen-rich liquid introduction tube

13‧‧‧第二富氧液體導入管 13‧‧‧Second oxygen-rich liquid introduction tube

14‧‧‧冷凝器氣體導出管 14‧‧‧Condenser gas outlet pipe

15‧‧‧中間部氣體導出管 15‧‧‧ middle gas outlet tube

16‧‧‧製品氮氣導出管 16‧‧‧Product nitrogen outlet tube

17‧‧‧含氬氣體導入管 17‧‧‧Argon-containing gas introduction tube

18‧‧‧製品氬導出管 18‧‧‧Product argon outlet tube

19‧‧‧含氬液體導出管 19‧‧‧Argon-containing liquid outlet tube

21‧‧‧富氧液體導出管 21‧‧‧ Oxygen-rich liquid outlet pipe

22‧‧‧第三富氧液體導入管 22‧‧‧The third oxygen-rich liquid introduction tube

23‧‧‧第四精餾塔塔頂部氣體導入管 23‧‧‧The gas introduction pipe at the top of the fourth distillation tower

25‧‧‧第一合流點 25‧‧‧First meeting point

100‧‧‧製品氮氣及製品氬之製造裝置 100‧‧‧Production device for product nitrogen and product argon

圖1係表示實施形態1之製品氮氣及製品氬之製造裝置之構成例之圖。 FIG. 1 is a diagram showing a configuration example of a manufacturing apparatus for product nitrogen and product argon in Embodiment 1. FIG.

圖2係表示實施形態2之製品氮氣及製品氬之製造裝置之構成例之圖。 FIG. 2 is a diagram showing a configuration example of a manufacturing apparatus for product nitrogen and product argon in Embodiment 2. FIG.

圖3係表示實施形態3之製品氮氣及製品氬之製造裝置之構成例之圖。 FIG. 3 is a diagram showing a configuration example of a manufacturing apparatus for product nitrogen and product argon in Embodiment 3. FIG.

圖4係表示實施形態4之製品氮氣及製品氬之製造裝置之構成例之圖。 FIG. 4 is a diagram showing a configuration example of a manufacturing apparatus for product nitrogen and product argon in Embodiment 4. FIG.

以下針對本發明之一些實施形態進行說明。以下所說明之實施 形態係對本發明之一例進行說明者。本發明並不受以下之實施形態任何限定，亦包含於不變更本發明之主旨之範圍內所實施之各種變化形態。再者，以下所說明之所有構成未必為本發明之必須構成。 The following describes some embodiments of the present invention. Implementation described below The morphology describes an example of the present invention. The present invention is not limited by the following embodiments, and is also included in various modifications implemented within the scope of not changing the gist of the present invention. In addition, all the configurations described below are not necessarily required for the present invention.

針對本發明之氮製造方法之流程進行說明。 The flow of the nitrogen production method of the present invention will be described.

(冷卻步驟) (Cooling step)

冷卻步驟為使原料空氣於熱交換器中冷卻之步驟。導入至主熱交換器之原料空氣可為經過將自外部收集之原料空氣藉由1個或複數個壓縮機壓縮之壓縮步驟、及自壓縮之原料空氣去除既定之雜質之去除步驟的原料空氣。去除步驟中之雜質之去除方法並無特別限定，可藉由吸附、冷卻等已知之方法進行。去除之雜質並無特別限定，可為成為堵塞熱交換器等之原因之二氧化碳、水分等。 The cooling step is a step of cooling the raw material air in the heat exchanger. The raw material air introduced into the main heat exchanger may be a raw material air that has undergone a compression step of compressing the raw material air collected from the outside by one or more compressors, and a removal step of removing predetermined impurities from the compressed raw material air. The method for removing impurities in the removal step is not particularly limited, and can be performed by known methods such as adsorption and cooling. The impurities to be removed are not particularly limited, and may be carbon dioxide, moisture, etc. that cause blockage of the heat exchanger or the like.

壓縮步驟可包含使壓縮之原料空氣冷卻之冷卻步驟。於藉由複數個壓縮機壓縮原料空氣之情形時，可包含使利用各壓縮機壓縮之原料空氣冷卻之複數個冷卻步驟。 The compression step may include a cooling step of cooling the compressed raw material air. In the case where the raw material air is compressed by plural compressors, plural cooling steps for cooling the raw material air compressed by each compressor may be included.

冷卻步驟中，原料空氣藉由與下述之製品氮氣、冷凝器氣體、及中間部氣體中之至少任一者進行熱交換而冷卻。 In the cooling step, the raw material air is cooled by heat exchange with at least any one of the following product nitrogen, condenser gas, and intermediate gas.

圖1中所示之製品氮氣及製品氬氣之製造裝置100中，利用主熱交換器1實施冷卻步驟。 In the manufacturing apparatus 100 of product nitrogen and product argon shown in FIG. 1, the main heat exchanger 1 performs a cooling step.

(原料空氣導入步驟) (Step of introducing raw material air)

原料空氣導入步驟為將冷卻步驟中冷卻之原料空氣導入至第一精餾塔之步驟。可於導入至第一精餾塔前，使原料空氣膨脹冷卻。原料空氣之膨脹冷卻可藉由膨脹閥實施。導入至第一精餾塔之原料空氣之溫度例如為-170℃至-155℃之範圍，壓力例如為7.0barA至15barA之範圍。 The raw material air introduction step is a step of introducing the raw material air cooled in the cooling step to the first rectification tower. The raw material air can be expanded and cooled before being introduced into the first rectification tower. The expansion cooling of the raw material air can be implemented by an expansion valve. The temperature of the raw material air introduced into the first rectification tower is, for example, in the range of -170°C to -155°C, and the pressure is, for example, in the range of 7.0 barA to 15 barA.

原料空氣導入步驟中導入至第一精餾塔之原料空氣分離為富氧液體與氮 氣。富氧液體貯存於第一精餾塔之塔底部，氮氣利用配置於第一精餾塔之上部之冷凝器冷凝而成為液體氮。 The raw material air introduced into the first rectification tower in the raw material air introduction step is separated into oxygen-enriched liquid and nitrogen gas. The oxygen-enriched liquid is stored at the bottom of the first rectification tower, and nitrogen is condensed by the condenser disposed above the first rectification tower to become liquid nitrogen.

(第一富氧液體導入步驟) (The first oxygen-rich liquid introduction step)

第一富氧液體導入步驟為將貯存於第一精餾塔之塔底部之富氧液體導入至第二精餾塔之步驟。富氧液體導入至第二精餾塔之前，可將其一部分或全部導入至第三精餾塔之第二冷凝器。導入至第二精餾塔之富氧液體之溫度例如為-175℃以上且-160℃以下，一面於第二精餾塔之內部下降，一面與第二精餾塔中上升之氣體接觸，並貯存於配置於第一精餾塔與第二精餾塔之間之冷凝部。 The first oxygen-enriched liquid introduction step is a step of introducing the oxygen-enriched liquid stored at the bottom of the tower of the first rectification tower to the second rectification tower. Before the oxygen-rich liquid is introduced into the second rectification column, part or all of it can be introduced into the second condenser of the third rectification column. The temperature of the oxygen-enriched liquid introduced into the second rectification tower is, for example, above -175°C and below -160°C. While falling inside the second rectification tower, it is in contact with the gas rising in the second rectification tower, and It is stored in the condensation part arranged between the first rectification tower and the second rectification tower.

自第一精餾塔之塔底部導出之富氧液體可藉由於導入至第二精餾塔之前經由過冷卻器而被冷卻，亦可不經由過冷卻器。 The oxygen-rich liquid drawn from the bottom of the first rectification tower may be cooled by a supercooler before being introduced into the second rectification tower, or may not pass through the subcooler.

(第二富氧液體導入步驟) (Second oxygen-rich liquid introduction step)

第二富氧液體導入步驟為將貯存於第一精餾塔之塔底部之富氧液體之一部分或全部(例如貯存於塔底部之富氧液體之10%以上且100%以下)導入至第三精餾塔之步驟。導入至第三精餾塔之富氧液體於配置於第三精餾塔之上部之冷凝部中，與氬氣進行熱交換。自配置於第三精餾塔之上部之冷凝部之上部導出之氣化之富氧液體被送回至第二精餾塔。 The second oxygen-enriched liquid introduction step is to introduce part or all of the oxygen-enriched liquid stored at the bottom of the first distillation column (for example, 10% or more and 100% or less of the oxygen-enriched liquid stored at the bottom of the column) to the third Steps in the rectification tower. The oxygen-rich liquid introduced into the third rectification tower is heat-exchanged with argon gas in the condensing section arranged above the third rectification tower. The vaporized oxygen-enriched liquid discharged from the upper part of the condensation part arranged above the third rectification column is sent back to the second rectification column.

此處，氣化之富氧液體與自第二精餾塔上部下降之液體接觸而被精餾。 Here, the vaporized oxygen-enriched liquid comes into contact with the liquid descending from the upper part of the second rectification tower to be rectified.

(含氮液體導入步驟) (Step of introducing nitrogen-containing liquid)

含氮液體導入步驟為將藉由在第一冷凝器中冷凝而獲得之液體氮作為環流液導入至第二精餾塔上部之步驟。第一冷凝器構成為使貯存於第一精餾塔之塔頂部之氣體與貯存於上述第二精餾塔之塔底部之液體進行熱交換。導入至第二精餾塔之含氮液體之溫度例如為-192℃以上且-175℃以下。 The nitrogen-containing liquid introduction step is a step of introducing liquid nitrogen obtained by condensing in the first condenser as a circulating liquid to the upper part of the second rectification column. The first condenser is configured to exchange heat between the gas stored at the top of the first rectification column and the liquid stored at the bottom of the second rectification column. The temperature of the nitrogen-containing liquid introduced into the second rectification tower is, for example, -192°C or higher and -175°C or lower.

自第一冷凝器導出之含氮氧液可藉由於導入至第二精餾塔之前經由過冷卻器而被冷卻，亦可不經由過冷卻器。 The nitrogen-containing oxygen liquid discharged from the first condenser may be cooled by a subcooler before being introduced into the second rectification tower, or may not pass through the subcooler.

(含氬氣體導入步驟) (Step of introducing argon-containing gas)

含氬氣體導入步驟為將自第二精餾塔之下部導出之含氬氣體導入至第三精餾塔之步驟。導入至第三精餾塔之含氬氣體藉由精餾分離為含氬富氧液體與製品氬。 The argon-containing gas introduction step is a step of introducing the argon-containing gas drawn out from the lower part of the second rectification tower to the third rectification tower. The argon-containing gas introduced into the third rectification tower is separated into argon-containing oxygen-rich liquid and product argon by rectification.

(製品氬氣導出步驟) (Product argon export step)

製品氬氣導出步驟為將第三精餾塔中獲得之製品氬氣自第三精餾塔導出之步驟。製品氬氣之純度例如為99.9%以上。 The product argon export step is a step of exporting the product argon obtained in the third rectification tower from the third rectification tower. The purity of the product argon is, for example, 99.9% or more.

(製品氮氣導出步驟) (Product nitrogen export step)

製品氮氣導出步驟為自第二精餾塔之塔頂部導出製品氮氣之步驟。製品氮氣之純度例如為99.9999%以上。自第二精餾塔之塔頂部導出之製品氮氣之溫度例如可為-192℃以上且-175℃以下，製品氮氣雖可於過冷卻器中使富氧液體、及/或液體氮冷卻，但亦可不設置過冷卻器。製品氮氣進而自冷端側導入至主熱交換器，於進行與原料空氣之熱交換之後，自溫端側導出。自主熱交換器導出之製品氮氣之溫度例如可為0℃以上。 The product nitrogen extraction step is a step of extracting product nitrogen from the top of the second distillation column. The purity of the product nitrogen is, for example, 99.9999% or more. The temperature of the product nitrogen discharged from the top of the second rectification tower can be, for example, above -192°C and below -175°C. Although the product nitrogen can cool the oxygen-enriched liquid and/or liquid nitrogen in the supercooler, but It is also possible not to set a supercooler. The product nitrogen is further introduced into the main heat exchanger from the cold end side, and after heat exchange with the raw material air, it is led out from the warm end side. The temperature of the product nitrogen discharged from the autonomous heat exchanger may be, for example, above 0°C.

(膨脹步驟) (Expansion step)

膨脹步驟為使冷凝器氣體與中間部氣體之混合氣體於主熱交換器中釋放寒冷之後進行膨脹冷卻，使膨脹冷卻之氣體再次於主熱交換器中釋放寒冷的步驟。冷凝器氣體與中間部氣體之混合氣體例如以-185℃以上且-165℃以下之溫度導入至主熱交換器之冷端側。在此，藉由進行與原料空氣之熱交換而釋放寒冷，該混合氣體之溫度例如成為-120℃以上且-80℃以下。該混合氣體利用膨脹渦輪而膨脹冷卻，其溫度例如成為-140℃以上且-100℃以下，再次導入至主熱交換器之冷端側。此處，該混合氣體於進行與原料空氣之熱交換而釋放寒冷之後，自主熱交換器之溫端側釋放。 The expansion step is a step of causing the mixed gas of the condenser gas and the middle gas to release cold in the main heat exchanger and then performing expansion cooling, so that the expanded cooled gas releases cold again in the main heat exchanger. The mixed gas of the condenser gas and the middle gas is introduced to the cold end side of the main heat exchanger at a temperature of -185°C or higher and -165°C or lower, for example. Here, by performing heat exchange with the raw material air to release cold, the temperature of the mixed gas is, for example, -120°C or higher and -80°C or lower. This mixed gas is expanded and cooled by an expansion turbine, and the temperature thereof is, for example, -140°C or more and -100°C or less, and then introduced again to the cold end side of the main heat exchanger. Here, after the heat exchange with the raw material air is performed to release cold, the mixed gas is released at the temperature end side of the main heat exchanger.

冷凝器氣體之氧濃度例如為99%以上，但藉由與中間部氣體混合，氧濃度 例如降低至70%以上且97%以下。 The oxygen concentration of the condenser gas is, for example, 99% or more, but by mixing with the middle gas, the oxygen concentration For example, it is reduced to more than 70% and less than 97%.

(實施形態1) (Embodiment 1)

針對實施形態1之製品氮氣及製品氬之製造裝置，參照圖1進行說明。 The manufacturing apparatus of the product nitrogen and product argon of Embodiment 1 will be described with reference to FIG. 1.

實施形態1之製品氮氣及製品氬之製造裝置100具備：主熱交換器1、第一精餾塔2、第二精餾塔5、第三精餾塔6、含氮液體導入管11、第一富氧液體導入管12、第二富氧液體導入管13、冷凝器氣體導出管14、中間部氣體導出管15、膨脹渦輪8、製品氮氣導出管16、含氬氣體導入管17及製品氬導出管18。 The manufacturing apparatus 100 for product nitrogen and product argon in Embodiment 1 includes: a main heat exchanger 1, a first rectification tower 2, a second rectification tower 5, a third rectification tower 6, a nitrogen-containing liquid introduction pipe 11, and a first An oxygen-rich liquid inlet pipe 12, a second oxygen-rich liquid inlet pipe 13, a condenser gas outlet pipe 14, an intermediate gas outlet pipe 15, an expansion turbine 8, a product nitrogen outlet pipe 16, an argon-containing gas inlet pipe 17 and a product argon Export tube 18.

製品氮氣及製品氬氣之製造裝置100為藉由深冷分離製造氮氣及氬氣之裝置，為可不製造作為製品氣體使用之氧氣之裝置。 The manufacturing apparatus 100 for product nitrogen and product argon is an apparatus for manufacturing nitrogen and argon by cryogenic separation, and is an apparatus that does not manufacture oxygen used as a product gas.

主熱交換器1為使原料空氣冷卻之熱交換器。於導入至主熱交換器之前，原料空氣(例如原料空氣量為1000Nm3/h)藉由壓縮機(未圖示)而被壓縮，去除既定之雜質。所謂既定之雜質，並無特別限定，可為成為堵塞熱交換器等之原因之二氧化碳、水分等。 The main heat exchanger 1 is a heat exchanger that cools raw material air. Before being introduced into the main heat exchanger, the raw material air (for example, the raw material air amount is 1000 Nm 3 /h) is compressed by a compressor (not shown) to remove predetermined impurities. The so-called predetermined impurities are not particularly limited, and may be carbon dioxide, moisture, etc. that cause clogging of the heat exchanger or the like.

於主熱交換器1內部，原料空氣與下述之製品氮氣、冷凝器氣體、及中間部氣體中之至少一者進行熱交換。藉此，原料空氣冷卻至其液化點附近。原料空氣之溫度例如於導入至主熱交換器1時為20℃，例如利用主熱交換器1冷卻至-170℃~-155℃。 Inside the main heat exchanger 1, the raw material air exchanges heat with at least one of the following product nitrogen, condenser gas, and intermediate gas. By this, the raw material air is cooled to the vicinity of its liquefaction point. The temperature of the raw material air is, for example, 20°C when introduced into the main heat exchanger 1, and is cooled to -170°C to -155°C by the main heat exchanger 1, for example.

第一精餾塔2中，導入利用主熱交換器1冷卻之原料空氣進行精餾。第一精餾塔2之理論段數為30段至80段，例如可設為50段。第一精餾塔2之運轉壓力範圍為7barA~15barA，運轉壓力例如可設為9barA。 In the first rectification tower 2, raw material air cooled by the main heat exchanger 1 is introduced for rectification. The number of theoretical stages of the first rectification column 2 is from 30 stages to 80 stages, for example, it can be set to 50 stages. The operating pressure of the first rectification column 2 ranges from 7 barA to 15 barA, and the operating pressure can be set to 9 barA, for example.

第二精餾塔5中，自塔頂部取出製品氮氣。第二精餾塔5之理論段數為40段至120段，例如可設為80段。第二精餾塔5之運轉壓力範圍為1.5barA~6barA，運轉壓力例如可設為2.5barA。 In the second rectification tower 5, the product nitrogen is taken from the top of the tower. The number of theoretical stages of the second rectification column 5 is 40 stages to 120 stages, for example, 80 stages. The operating pressure of the second rectification column 5 ranges from 1.5 barA to 6 barA, and the operating pressure can be set to 2.5 barA, for example.

第三精餾塔6中，取出製品氬氣。第三精餾塔6之理論段數為100 段至300段，例如可設為180段。第三精餾塔6之運轉壓力範圍為1.5barA~6barA，運轉壓力例如可設為2.5barA。 In the third distillation column 6, the product argon gas is taken out. The number of theoretical stages of the third distillation column 6 is 100 It can be set from 180 to 300 steps, for example. The operating pressure of the third rectification column 6 ranges from 1.5 barA to 6 barA, and the operating pressure can be set to 2.5 barA, for example.

以使貯存於第一精餾塔之塔頂部之氣體與貯存於上述第二精餾塔之塔底部之液體進行熱交換之方式配置第一冷凝器3。第一精餾塔2中，原料空氣分離為富氧液體與氮氣，富氧液體貯存於第一精餾塔2之塔底部。第一冷凝器3中，分離之氮氣被冷凝而成為液體氮。藉由於配置於第一冷凝器3之上之第二精餾塔5之內部下降，而將下述之富氧液體用作第一冷凝器3之冷媒。 The first condenser 3 is arranged in such a manner that the gas stored at the top of the tower of the first rectification tower and the liquid stored at the bottom of the tower of the second rectification tower are exchanged. In the first rectification tower 2, the raw material air is separated into oxygen-enriched liquid and nitrogen, and the oxygen-enriched liquid is stored at the bottom of the tower of the first rectification tower 2. In the first condenser 3, the separated nitrogen gas is condensed to become liquid nitrogen. Since the inside of the second rectification tower 5 disposed above the first condenser 3 descends, the oxygen-enriched liquid described below is used as the refrigerant of the first condenser 3.

第一冷凝器3中冷凝獲得之液體氮之至少一部分(例如利用第一冷凝器3冷凝之液體氮之10%以上且97%以下)經由含氮液體導入管11，作為環流液向第二精餾塔5之上部導入。所謂第二精餾塔5之上部，為較第二精餾塔5之內部之精餾部之最上段上方，例如於第二精餾塔5之理論段數為80段之情形時，為較80段上方。 At least a part of the liquid nitrogen obtained by condensation in the first condenser 3 (for example, 10% or more and 97% or less of the liquid nitrogen condensed by the first condenser 3) passes through the nitrogen-containing liquid introduction pipe 11 as a circulating liquid to the second The upper part of the distillation column 5 is introduced. The upper part of the second rectification tower 5 is higher than the uppermost section of the rectification section inside the second rectification tower 5, for example, when the theoretical section number of the second rectification tower 5 is 80, it is Above paragraph 80.

再者，第二精餾塔2可配置於第一冷凝器3之上方，亦能夠橫向配置。 Furthermore, the second rectification column 2 can be arranged above the first condenser 3, and can also be arranged laterally.

貯存於第一精餾塔2之塔底部之富氧液體藉由富氧液體導出管21自第一精餾塔之塔底部導出。該富氧液體之一部分或全部(例如貯存於塔底部之富氧液體之10%以上且100%以下)經由第一富氧液體導入管12而導入至第二精餾塔5，貯存於第一精餾塔2之塔底部之富氧液體中之未導入至第二精餾塔5之部分經由第二富氧液體導入管13導入至第三精餾塔6。 The oxygen-rich liquid stored in the bottom of the first rectification tower 2 is led out from the bottom of the first rectification tower through an oxygen-rich liquid outlet pipe 21. Part or all of the oxygen-enriched liquid (for example, 10% or more and 100% or less of the oxygen-enriched liquid stored at the bottom of the tower) is introduced into the second rectification column 5 through the first oxygen-enriched liquid introduction pipe 12 and stored in the first The portion of the oxygen-rich liquid at the bottom of the rectification tower 2 that is not introduced into the second rectification tower 5 is introduced into the third rectification tower 6 via the second oxygen-rich liquid introduction pipe 13.

第一富氧液體導入管12之第二精餾塔5側之安裝位置為較含氮液體導入管11及下述中間部氣體導出管15下方。 The installation position of the first oxygen-enriched liquid introduction pipe 12 on the second rectification column 5 side is below the nitrogen-containing liquid introduction pipe 11 and the intermediate gas outlet pipe 15 described below.

含氮液體導入管11之第二精餾塔5側之安裝位置例如為較第二精餾塔內之填充有精餾填充劑之位置上方。第一富氧液體導入管12之第二精餾塔5側之安裝位置例如可為較第二精餾塔之高度之2/4上方，較3/4下方。 The installation position of the nitrogen-containing liquid introduction pipe 11 on the second rectification column 5 side is, for example, above the position filled with the rectification filler in the second rectification column. The installation position of the first oxygen-enriched liquid introduction pipe 12 on the second rectification tower 5 side may be, for example, 2/4 above the height of the second rectification tower, and 3/4 below the height.

於利用理論段數算出之情形時，第一富氧液體導入管12之第二精餾塔5側 之安裝位置例如為相當於前段數乘以0.5以上且0.7以下之段數之位置。具體而言，於第二精餾塔5理論段數為80段之情形時，為較40段(80×0.5=40)上方，且為較56段(80×0.7=56)下方。 In the case of calculation using the theoretical number of stages, the first oxygen-rich liquid introduction pipe 12 is on the second rectification tower 5 side The installation position is, for example, a position equivalent to the number of the front stage multiplied by the number of the stages above 0.5 and below 0.7. Specifically, when the number of theoretical stages of the second distillation column 5 is 80, it is higher than 40 stages (80×0.5=40) and lower than 56 stages (80×0.7=56).

第二富氧液體導入管13配置為使富氧液體導入至配置於第三精餾塔6之上方之第二冷凝器。經由第二富氧液體導入管13之富氧液體為了使於第三精餾塔6內部上升之氬氣冷凝而於第二冷凝器7中用作冷媒。第二冷凝器7中氣化之富氧液體可自第二冷凝器7排出之後，與第一富氧液體導入管12合流，導入至第二精餾塔5。 The second oxygen-enriched liquid introduction pipe 13 is configured to introduce the oxygen-enriched liquid to the second condenser arranged above the third rectification column 6. The oxygen-rich liquid passing through the second oxygen-rich liquid introduction pipe 13 is used as a refrigerant in the second condenser 7 in order to condense the argon gas rising inside the third rectification column 6. After the oxygen-enriched liquid vaporized in the second condenser 7 can be discharged from the second condenser 7, it merges with the first oxygen-enriched liquid introduction pipe 12 and is introduced into the second rectification tower 5.

冷凝器氣體導出管14為導出自第一冷凝器3排出之冷凝器氣體之配管，其中第一冷凝器3構成為使貯存於第一精餾塔2之塔頂部之氣體與貯存於第二精餾塔5之塔底部之液體進行熱交換。冷凝器氣體中之氧濃度例如為99.9%以上。 The condenser gas outlet pipe 14 is a pipe for leading the condenser gas discharged from the first condenser 3, wherein the first condenser 3 is configured such that the gas stored at the top of the first rectification tower 2 and the second The liquid at the bottom of the distillation column 5 undergoes heat exchange. The oxygen concentration in the condenser gas is, for example, 99.9% or more.

中間部氣體導出管15為自第二精餾塔5之中間部導出中間部氣體之配管。中間部氣體導出管15為較含氮液體導入管11之第二精餾塔側之安裝位置下方，且為較第一富氧液體導入管12之上述第二精餾塔側之安裝位置上方。於第二精餾塔5之理論段數為80段之情形時，中間部氣體導出管15之安裝位置例如為56段以上且79段以下之位置。中間部氣體中之氮濃度例如為80%以上且99%以下。 The middle portion gas outlet pipe 15 is a pipe for leading the middle portion gas from the middle portion of the second distillation column 5. The middle gas outlet pipe 15 is below the installation position on the second rectification column side of the nitrogen-containing liquid introduction pipe 11 and above the installation position on the second rectification tower side of the first oxygen-rich liquid introduction pipe 12. When the theoretical number of the second rectification column 5 is 80, the installation position of the middle gas outlet pipe 15 is, for example, 56 or more and 79 or less. The nitrogen concentration in the intermediate gas is, for example, 80% or more and 99% or less.

冷凝器氣體導出管14與中間部氣體導出管15於主熱交換器1之前段合流，中間部氣體與冷凝器氣體於該處混合。混合之氣體中之氧濃度例如為70%以上且97%以下。 The condenser gas outlet pipe 14 and the intermediate gas outlet pipe 15 merge at the front stage of the main heat exchanger 1 where the intermediate gas and the condenser gas are mixed. The oxygen concentration in the mixed gas is, for example, 70% or more and 97% or less.

中間部氣體之導出流量相對於冷凝器氣體之導出流量的比可為0.1以上且2以下，較佳可為0.2以上且0.5以下。 The ratio of the outlet flow rate of the intermediate gas to the outlet flow rate of the condenser gas may be 0.1 or more and 2 or less, preferably 0.2 or more and 0.5 or less.

膨脹渦輪8為使藉由經由主熱交換器1於主熱交換器1之內部進行 與原料空氣之熱交換而釋放寒冷後之中間部氣體及冷凝器氣體之混合氣體膨脹冷卻的膨脹渦輪。最初導入至主熱交換器時之中間部氣體及冷凝器氣體之混合氣體之溫度例如為-185℃以上且-165℃以下，自主熱交換器1導出而導入至膨脹渦輪8之前之溫度例如為-120℃以上且-80℃以下。該混合氣體藉由膨脹渦輪8而膨脹冷卻，例如成為-140℃以上且-100℃以下之溫度。經膨脹冷卻之混合氣體再次導入至主熱交換器1，藉由進行與原料空氣之熱交換而釋放寒冷之後，自主熱交換器1排出。 The expansion turbine 8 is performed by passing through the main heat exchanger 1 inside the main heat exchanger 1 An expansion turbine that expands and cools the mixed gas of the middle gas and the condenser gas after the heat exchange with the raw material air to release cold. The temperature of the mixed gas of the middle gas and the condenser gas when initially introduced into the main heat exchanger is, for example, -185°C or more and -165°C or less, and the temperature before the main heat exchanger 1 is led out and introduced to the expansion turbine 8 is, for example, -120°C or more and -80°C or less. The mixed gas is expanded and cooled by the expansion turbine 8 and becomes, for example, a temperature of -140°C or higher and -100°C or lower. The mixed gas after expansion and cooling is reintroduced into the main heat exchanger 1, and after releasing heat by exchanging heat with the raw material air, the main heat exchanger 1 is discharged.

製品氮氣導出管16為自第二精餾塔5之塔頂部導出製品氮氣之配管。導出之製品氮氣之溫度例如為-192℃以上且-175℃以下之範圍，可直接作為氮氣供給，亦可藉由導入至主熱交換器1進行與原料空氣之熱交換而釋放寒冷，作為例如0℃以上~20℃以下之溫度之氮氣供給。進而可於導入至主熱交換器1之前，於過冷卻器4中進行熱交換。 The product nitrogen outlet pipe 16 is a pipe for leading the product nitrogen gas from the top of the second distillation column 5. The temperature of the exported product nitrogen is, for example, in the range of -192°C or more and -175°C or less, and can be directly supplied as nitrogen, or can be released by introducing heat into the main heat exchanger 1 to exchange heat with the raw material air, as for example Nitrogen supply at temperatures above 0°C to below 20°C. Furthermore, heat can be exchanged in the subcooler 4 before being introduced into the main heat exchanger 1.

於過冷卻器4之內部，含氮液體及富氧液體與製品氮氣進行熱交換。即，於過冷卻器4之內部，利用製品氮氣之寒冷而將含氮液體及富氧液體冷卻。 Inside the subcooler 4, the nitrogen-containing liquid and the oxygen-rich liquid exchange heat with the product nitrogen. That is, inside the subcooler 4, the nitrogen-containing liquid and the oxygen-rich liquid are cooled by the coldness of the product nitrogen.

藉由使含氮液體及富氧液體冷卻，能夠抑制含氮液體及富氧液體於第二精餾塔5內部大量氣化而降低第二精餾塔5之精餾效率之現象，但亦可不設置過冷卻器。 By cooling the nitrogen-containing liquid and the oxygen-enriched liquid, it is possible to suppress a large amount of gasification of the nitrogen-containing liquid and the oxygen-enriched liquid inside the second rectification tower 5 to reduce the rectification efficiency of the second rectification tower 5, but Set the subcooler.

於未設置過冷卻器4之情形時，於第一冷凝器3中冷凝之含氮液體藉由含氮液體導入管11而直接導入至第二精餾塔5之上部。同樣地，自第一精餾塔2之塔底部經由富氧液體導出管21導出之富氧液體直接導入至第二精餾塔5之中間部。自第二精餾塔4之塔頂部經由製品氮氣導出管16導出之製品氮氣直接導入至主熱交換器1，於利用製品氮氣之寒冷之後，自主熱交換器1排出。 When the subcooler 4 is not provided, the nitrogen-containing liquid condensed in the first condenser 3 is directly introduced to the upper part of the second rectification tower 5 through the nitrogen-containing liquid introduction pipe 11. Similarly, the oxygen-enriched liquid led out from the bottom of the first rectification column 2 through the oxygen-enriched liquid outlet pipe 21 is directly introduced into the middle part of the second rectification column 5. The product nitrogen discharged from the top of the second rectification tower 4 through the product nitrogen outlet pipe 16 is directly introduced into the main heat exchanger 1, and after the coldness of the product nitrogen is utilized, the main heat exchanger 1 is discharged.

含氬氣體導入管17為將含氬氣體自第二精餾塔5之下部導入至第 三精餾塔6之配管。含氬氣體導入管17之第二精餾塔5側之安裝位置為較第一富氧液體導入管12下方，例如於第二精餾塔5之理論段數為80段之情形時，為20段以上且40段以下之位置。 The argon-containing gas introduction pipe 17 is for introducing argon-containing gas from the lower part of the second rectification tower 5 to the first The piping of the third rectification tower 6. The installation position of the second rectification tower 5 side of the argon-containing gas introduction pipe 17 is below the first oxygen-rich liquid introduction pipe 12, for example, when the theoretical section number of the second rectification tower 5 is 80, it is 20 The position above paragraph and below paragraph 40.

導入至第三精餾塔6之含氬氣體藉由精餾而分離為含氬富氧液體與製品氬氣。製品氬氣自製品氬氣導出管18導出。另一方面，貯存於第三精餾塔6之塔底部之含氬富氧液體經由含氬液體導出管19導入至第二精餾塔5。含氬液體導出管19之位置為較製品氬氣導出管18下方。 The argon-containing gas introduced into the third rectification tower 6 is separated into argon-containing oxygen-rich liquid and product argon by rectification. The product argon gas is led out from the product argon gas outlet pipe 18. On the other hand, the argon-containing oxygen-rich liquid stored in the bottom of the third rectification column 6 is introduced into the second rectification column 5 through the argon-containing liquid outlet pipe 19. The argon-containing liquid outlet pipe 19 is located below the product argon gas outlet pipe 18.

(實施形態2) (Embodiment 2)

針對實施形態2之製品氮氣及製品氬之製造裝置101，參照圖2進行說明。由於與實施形態1之製品氮氣及製品氬之製造裝置相同之符號之組件具有相同之功能，故省略其說明。 The manufacturing apparatus 101 of product nitrogen and product argon of Embodiment 2 will be described with reference to FIG. 2. Since the components with the same symbols as the manufacturing apparatus for the product nitrogen and product argon in Embodiment 1 have the same function, their descriptions are omitted.

實施形態2中，中間部氣體經由中間部氣體導出管152導入至過冷卻器4。於過冷卻器4中，中間部氣體溫度上升至-170℃左右之後，與冷凝器氣體混合。 In the second embodiment, the intermediate gas is introduced into the subcooler 4 through the intermediate gas outlet pipe 152. In the subcooler 4, after the temperature of the intermediate gas rises to about -170°C, it is mixed with the condenser gas.

藉此，能夠使富氧液體及/或含氮液體進一步冷卻，能夠提昇第二及第三精餾塔中之精餾效率。 By this, the oxygen-rich liquid and/or the nitrogen-containing liquid can be further cooled, and the rectification efficiency in the second and third rectification towers can be improved.

中間部氣體導出管152經由過冷卻器4，於第一合流點25與冷凝器氣體導出管14連接。第一合流點位於過冷卻器4之後段且膨脹渦輪8之前段。於將導入至膨脹渦輪之前之中間部氣體與冷凝器氣體之混合氣體導入至主熱交換器1之情形時，第一合流點位於過冷卻器4之後段且主熱交換器1之前段。 The intermediate gas outlet pipe 152 is connected to the condenser gas outlet pipe 14 at the first junction 25 via the subcooler 4. The first confluence point is located after the subcooler 4 and before the expansion turbine 8. In the case where the mixed gas of the intermediate gas and the condenser gas before being introduced into the expansion turbine is introduced into the main heat exchanger 1, the first confluence point is located after the subcooler 4 and before the main heat exchanger 1.

於第一合流點25，中間部氣體與冷凝器氣體混合而生成混合氣體。該混合氣體中之氧濃度例如為70%以上且97%以下，故不必使用可應對高濃度氧之特殊之膨脹渦輪。 At the first junction 25, the intermediate gas and the condenser gas are mixed to generate a mixed gas. The oxygen concentration in the mixed gas is, for example, 70% or more and 97% or less, so it is not necessary to use a special expansion turbine that can handle high-concentration oxygen.

(實施形態3) (Embodiment 3)

針對實施形態3之製品氮氣及製品氬之製造裝置102，參照圖3進行說明。 由於與實施形態1或實施形態2之製品氮氣及製品氬之製造裝置相同之符號之組件具有相同之功能，故省略其說明。 The manufacturing apparatus 102 for product nitrogen and product argon in the third embodiment will be described with reference to FIG. 3. Since the components with the same symbols as the manufacturing apparatuses for the product nitrogen and product argon in Embodiment 1 or Embodiment 2 have the same functions, their descriptions are omitted.

可於配置於第三精餾塔6之第二冷凝器之上部配置使於第二冷凝器中蒸發之富氧液體精餾之第四精餾塔9。於第二冷凝器中氣化之富氧液體於第四精餾塔9中進而分離為富集氧之液體與富集氮之氣體。此處富集氮之氣體係自第四精餾塔9之塔頂部即第三精餾塔6之塔上部取出，經由氣相側之第一富氧液體導入管121而向第二精餾塔導入。另一方面，於第四精餾塔9中進而富集氧之液體貯存於第二冷凝器7，經由液相側之第一富氧液體導入管122導入至第二精餾塔。藉由如此將在第四精餾塔9中分離為氣相與液相之富氧液體分別導入至第二精餾塔5，能夠提昇第二精餾塔之精餾效率。 A fourth rectification tower 9 for rectifying the oxygen-enriched liquid evaporated in the second condenser may be disposed above the second condenser disposed in the third rectification tower 6. The oxygen-enriched liquid vaporized in the second condenser is further separated into the oxygen-enriched liquid and the nitrogen-enriched gas in the fourth rectification tower 9. Here, the nitrogen-enriched gas system is taken out from the top of the fourth rectification tower 9, that is, the upper part of the third rectification tower 6, and passes through the first oxygen-rich liquid introduction pipe 121 on the gas phase side to the second rectification tower Import. On the other hand, the liquid enriched in oxygen in the fourth rectification tower 9 is stored in the second condenser 7 and introduced into the second rectification tower through the first oxygen-rich liquid introduction pipe 122 on the liquid phase side. By thus introducing the oxygen-enriched liquid separated into the gas phase and the liquid phase in the fourth rectification tower 9 into the second rectification tower 5 respectively, the rectification efficiency of the second rectification tower can be improved.

實施形態3中，貯存於第一精餾塔2之塔底部之富氧液體藉由富氧液體導出管21而自第一精餾塔2導出。繼而，富氧液體自第二富氧液體導入管133向第四精餾塔9之上部導入，經由第四精餾塔9向第二冷凝器7導入。 In Embodiment 3, the oxygen-rich liquid stored in the bottom of the first rectification column 2 is discharged from the first rectification column 2 through the oxygen-rich liquid outlet pipe 21. Then, the oxygen-enriched liquid is introduced from the second oxygen-enriched liquid introduction pipe 133 to the upper part of the fourth rectification tower 9 and introduced into the second condenser 7 via the fourth rectification tower 9.

經由富氧液體導出管之富氧液體可導入至過冷卻器4，亦可不導入至過冷卻器4。 The oxygen-enriched liquid passing through the oxygen-enriched liquid outlet pipe may or may not be introduced into the supercooler 4.

(另一實施形態) (Another embodiment)

作為另一實施形態，亦能夠設為實施形態3中之中間部氣體導出管15經由過冷卻器4之構成。 As another embodiment, the intermediate gas outlet pipe 15 in Embodiment 3 may be configured to pass through the supercooler 4.

(實施形態4) (Embodiment 4)

針對實施形態4之製品氮氣及製品氬之製造裝置103，參照圖4進行說明。由於與實施形態1~32之製品氮氣及製品氬之製造裝置相同之符號之組件具有相同之功能，故省略其說明。 The manufacturing apparatus 103 of product nitrogen and product argon of Embodiment 4 will be described with reference to FIG. 4. Since the components with the same symbols as the manufacturing apparatus for the product nitrogen and the product argon of Embodiments 1 to 32 have the same function, their description is omitted.

實施形態1至實施形態3中，第一冷凝器3配置於第一精餾塔2之上，進而，第二精餾塔5配置於第一冷凝器3之上。然而，存在若以此方式朝上方向堆積， 則精餾塔整體之高度變得非常高，建設、設置變困難之情況。因此，實施形態4中，將相當於第二精餾塔之上部之部分(以541進行圖示)配置於第一精餾塔2及第一冷凝器3之橫向。 In the first to third embodiments, the first condenser 3 is arranged on the first rectification column 2, and further, the second rectification column 5 is arranged on the first condenser 3. However, if there is accumulation in this way upward, Then, the overall height of the rectification tower becomes very high, and construction and installation become difficult. Therefore, in the fourth embodiment, a portion corresponding to the upper part of the second rectification column (shown as 541) is arranged laterally of the first rectification column 2 and the first condenser 3.

實施形態4中，第二精餾塔由圖4中以542所示之區域與以541所示之區域之2個區域構成。於第二精餾塔之第一區域541之塔底部，自第二區域542之塔頂部通過配管41供給氣體。另一方面，於第二區域542之塔頂部，自第一區域541之塔底部經由配管42與環流液泵30供給流體。 In the fourth embodiment, the second rectification tower is composed of two areas, the area indicated by 542 and the area indicated by 541 in FIG. 4. At the bottom of the first zone 541 of the second distillation column, gas is supplied from the top of the second zone 542 through the pipe 41. On the other hand, at the top of the tower in the second area 542, fluid is supplied from the bottom of the tower in the first area 541 via the piping 42 and the circulating fluid pump 30.

中間部氣體導出管154自第二精餾塔之上部541之中間部導出中間部氣體，與冷凝器氣體導出管14合流。 The middle portion gas outlet pipe 154 leads the middle portion gas from the middle portion of the upper portion 541 of the second rectification column and merges with the condenser gas outlet pipe 14.

同樣地，第四精餾塔9亦視需要分割為2個區域，第四精餾塔之上部能夠配置於第三精餾塔6及第二冷凝器7之橫向。 Similarly, the fourth rectification tower 9 is also divided into two regions as needed, and the upper part of the fourth rectification tower can be arranged laterally of the third rectification tower 6 and the second condenser 7.

(實施例1) (Example 1)

於使用實施形態1之氮製造裝置100(圖2中所示)，以1295kg/hr使用具有氮75.6重量%、具有溫度20℃、壓力9.0barA之空氣作為原料之情形時，藉由模擬證實了各部之壓力(barA)、溫度(℃)及流量(kg/h)等。 In the case of using the nitrogen production apparatus 100 of the first embodiment (shown in FIG. 2 ), using 1295 kg/hr of nitrogen with 75.6% by weight, temperature of 20° C., and pressure of 9.0 barA as the raw material, it was confirmed by simulation Pressure (barA), temperature (℃) and flow rate (kg/h) of each part.

(結果) (result)

使藉由原料空氣壓縮機(未圖示)而自外部收集之原料空氣壓力自1.013barA升壓至9.0barA。 The feed air pressure collected from the outside by the feed air compressor (not shown) was increased from 1.013 barA to 9.0 barA.

其後，將去除部中已去除二氧化碳、水分之原料空氣向主熱交換器1導入。導入至主熱交換器1時之原料空氣之溫度為20℃。 Thereafter, the raw material air from which the carbon dioxide and moisture have been removed in the removal section is introduced into the main heat exchanger 1. The temperature of the raw material air introduced into the main heat exchanger 1 was 20°C.

自主熱交換器1導出之原料空氣之溫度為-160℃。將原料空氣向第一精餾塔2導入而進行精餾。第一精餾塔2之運轉壓為8.8barA。第一精餾塔2之理論段數為50段。 The temperature of the raw material air discharged from the autonomous heat exchanger 1 is -160°C. The raw material air is introduced into the first rectification tower 2 to perform rectification. The operating pressure of the first rectification column 2 is 8.8 barA. The number of theoretical stages of the first rectification tower 2 is 50 stages.

貯存於第一精餾塔2之塔底部之富氧液體中之10重量%經由第一富氧液體導 入管12，以溫度-180℃導入至第二精餾塔5之理論段50之位置。貯存於第一精餾塔2之塔底部之富氧液體中之未導入至第二精餾塔5之部分經由第二富氧液體導入管13，以溫度-180℃向第三精餾塔6之第二冷凝器導入。 10% by weight of the oxygen-rich liquid stored at the bottom of the first distillation column 2 is conducted through the first oxygen-rich liquid The inlet pipe 12 is introduced into the theoretical section 50 of the second rectification tower 5 at a temperature of -180°C. The portion of the oxygen-rich liquid stored in the bottom of the first rectification tower 2 that has not been introduced into the second rectification tower 5 passes through the second oxygen-rich liquid introduction pipe 13 to the third rectification tower 6 at a temperature of -180°C. The second condenser is introduced.

分離至第一精餾塔之上部之氮氣於第一冷凝器3中冷凝而生成液體氮。獲得之氮中之40重量%經由含氮液體導入管11，以溫度-190℃向第二精餾塔5之上部導入。導入位置為較理論段數80之位置上方。自配置於第一精餾塔2與第二精餾塔5之中間之第一冷凝器之上部，含有99重量%氧氣之冷凝器氣體自冷凝器氣體導出管14排出。 The nitrogen gas separated to the upper part of the first rectification tower is condensed in the first condenser 3 to generate liquid nitrogen. 40% by weight of the obtained nitrogen is introduced into the upper part of the second rectification column 5 through the nitrogen-containing liquid introduction pipe 11 at a temperature of -190°C. The introduction position is above the position of the theoretical segment number 80. From the upper part of the first condenser arranged between the first rectification tower 2 and the second rectification tower 5, the condenser gas containing 99% by weight of oxygen is discharged from the condenser gas outlet pipe 14.

自第二精餾塔5之中間部經由中間部氣體導出管排出中間部氣體。中間部氣體之組成為氮85重量%、氧13重量%、氬2重量%。中間部氣體導出管15之安裝位置為理論段數55段之位置。 The middle gas is discharged from the middle part of the second rectification column 5 through the middle gas outlet pipe. The composition of the middle gas is 85% by weight of nitrogen, 13% by weight of oxygen, and 2% by weight of argon. The installation position of the gas outlet pipe 15 in the middle portion is the position of the theoretical number of 55 steps.

中間部氣體與冷凝器氣體混合，成為混合氣體，以溫度-170℃向主熱交換器1導入並釋放寒冷。混合氣體之氧濃度為84%。其後，自主熱交換器1導出之混合氣體以-110℃導入至膨脹渦輪8而膨脹冷卻，以溫度-130℃再次導入至主熱交換器1。其後，於主熱交換器1之內部進行與原料空氣之熱交換而釋放寒冷，並自主熱交換器1排出。 The intermediate gas is mixed with the condenser gas to become a mixed gas, which is introduced into the main heat exchanger 1 at a temperature of -170°C to release cold. The oxygen concentration of the mixed gas is 84%. After that, the mixed gas discharged from the main heat exchanger 1 is introduced into the expansion turbine 8 at -110°C to be expanded and cooled, and is introduced into the main heat exchanger 1 again at a temperature of -130°C. Thereafter, heat exchange with the raw material air is performed inside the main heat exchanger 1 to release cold, and is discharged from the main heat exchanger 1.

自第二精餾塔5之塔頂部經由製品氮氣導出管16導出溫度-185℃之製品氮氣(純度為99.99重量%)。製品氮氣藉由利用過冷卻器4進行熱交換而溫度上升至-170℃，其後，進而於主熱交換器1中釋放寒冷，成為15℃之製品氮氣。製品氮氣之純度為99.99重量%，含氬量為10ppm、含氧量為100ppb。 From the top of the second rectification column 5, the product nitrogen (purity 99.99% by weight) with a temperature of -185°C is led out through the product nitrogen outlet pipe 16. The temperature of the product nitrogen is increased to -170°C by heat exchange with the subcooler 4, and then, the cold is released in the main heat exchanger 1 to become the product nitrogen of 15°C. The purity of the product nitrogen is 99.99% by weight, the argon content is 10 ppm, and the oxygen content is 100 ppb.

自第二精餾塔5之下部，含氬氣體(氬濃度為10重量%)經由含氬氣體導入管導入至第三精餾塔6而被精餾。第三精餾塔6之運轉壓力為2.5barA，理論段數為200段。製品氬導出管18配置於第二冷凝器之下部，導出純度99.9重量%之製品氬。 From the lower part of the second rectification tower 5, an argon-containing gas (argon concentration of 10% by weight) is introduced into the third rectification tower 6 through an argon-containing gas introduction pipe and is rectified. The operating pressure of the third rectification column 6 is 2.5 barA, and the theoretical number of stages is 200 stages. The product argon outlet pipe 18 is arranged at the lower part of the second condenser and leads the product argon with a purity of 99.9% by weight.

貯存於第三精餾塔6之塔底部之富氧含氬液體經由含氬液體導出管19而送回至第二精餾塔5。含氬液體含有氧92重量%與氬8重量%。 The oxygen-rich argon-containing liquid stored at the bottom of the third rectification column 6 is returned to the second rectification column 5 through the argon-containing liquid outlet pipe 19. The argon-containing liquid contains 92% by weight of oxygen and 8% by weight of argon.

自配置於第三精餾塔6之上部之第二冷凝器7之上部排出氣化之富氧液體，與第一富氧液體導入管12合流而向第二精餾塔5導入。 The vaporized oxygen-enriched liquid is discharged from the upper portion of the second condenser 7 disposed above the third rectification tower 6, merges with the first oxygen-enriched liquid introduction pipe 12, and is introduced into the second rectification tower 5.

藉由以上之構成，能夠獲得溫度20℃、壓力2.2barA之製品氮氣(935kg/hr)及溫度-175℃、壓力2.3barA之製品氬(14kg/hr)。製品氮氣及製品氬之製造所必需之能量為110kW，能夠有效地利用中間部氣體及冷凝器氣體之寒冷，故可謂能夠以高能量效率製造製品氮氣及製品氬氣。又，製造時，能夠不使用可耐氧氣使用之特殊材料，而使用一般所使用之膨脹渦輪。進而，藉由設置中間部氣體導出管15，能夠降低製品氮氣中之氬及氧濃度，可獲得高純度之製品氮氣。 With the above configuration, the product nitrogen (935 kg/hr) at a temperature of 20°C and a pressure of 2.2 barA and the product argon (14 kg/hr) at a temperature of -175°C and a pressure of 2.3 barA can be obtained. The energy required for the production of product nitrogen and product argon is 110kW, which can effectively use the coldness of the middle gas and the condenser gas, so it can be said that the product nitrogen and product argon can be produced with high energy efficiency. In addition, during manufacturing, it is possible to use an expansion turbine that is generally used without using special materials that can withstand oxygen. Furthermore, by providing the middle gas outlet pipe 15, the concentration of argon and oxygen in the product nitrogen can be reduced, and product nitrogen with high purity can be obtained.

1‧‧‧主熱交換器 1‧‧‧Main heat exchanger

2‧‧‧第一精餾塔 2‧‧‧First distillation tower

3‧‧‧第一冷凝器 3‧‧‧The first condenser

4‧‧‧過冷卻器 4‧‧‧Supercooler

5‧‧‧第二精餾塔 5‧‧‧Second distillation tower

6‧‧‧第三精餾塔 6‧‧‧The third distillation tower

7‧‧‧第二冷凝器 7‧‧‧Second condenser

8‧‧‧膨脹渦輪 8‧‧‧Expansion turbine

11‧‧‧含氮液體導入管 11‧‧‧Nitrogen-containing liquid introduction pipe

12‧‧‧第一富氧液體導入管 12‧‧‧The first oxygen-rich liquid introduction tube

13‧‧‧第二富氧液體導入管 13‧‧‧Second oxygen-rich liquid introduction tube

14‧‧‧冷凝器氣體導出管 14‧‧‧Condenser gas outlet pipe

15‧‧‧中間部氣體導出管 15‧‧‧ middle gas outlet tube

16‧‧‧製品氮氣導出管 16‧‧‧Product nitrogen outlet tube

17‧‧‧含氬氣體導入管 17‧‧‧Argon-containing gas introduction tube

18‧‧‧製品氬導出管 18‧‧‧Product argon outlet tube

19‧‧‧含氬液體導出管 19‧‧‧Argon-containing liquid outlet tube

21‧‧‧富氧液體導出管 21‧‧‧ Oxygen-rich liquid outlet pipe

22‧‧‧第三富氧液體導入管 22‧‧‧The third oxygen-rich liquid introduction tube

100‧‧‧製品氮氣及製品氬之製造裝置 100‧‧‧Production device for product nitrogen and product argon

Claims (11)

一種製品氮氣及製品氬之製造方法，包含：冷卻步驟，其使已去除既定之雜質之原料空氣冷卻；原料空氣導入步驟，其將上述冷卻步驟中冷卻之上述原料空氣導入至第一精餾塔；第一富氧液體導入步驟，其將自上述第一精餾塔之塔底部導出之富氧液體導入至第二精餾塔；第二富氧液體導入步驟，其將自上述第一精餾塔之塔底部導出之富氧液體之至少一部分導入至配置於第三精餾塔之第二冷凝器；含氮液體導入步驟，其將第一冷凝器中冷凝之含氮液體作為環流液導入至上述第二精餾塔上部；膨脹步驟，其使自上述第二精餾塔之中間部導出之中間部氣體與自上述第一冷凝器導出之冷凝器氣體之混合氣體之至少一部分，藉由在主熱交換器中進行與上述原料空氣之熱交換而釋放寒冷後被膨脹而產生寒冷，藉由再度導入至上述主熱交換器而進一步釋放寒冷，其中上述第一冷凝器係構成為使貯存於上述第一精餾塔之塔頂部之氣體與貯存於上述第二精餾塔之塔底部之液體進行熱交換；含氬氣體導入步驟，其將自上述第二精餾塔之下部導出之含氬氣體導入至上述第三精餾塔；製品氮氣導出步驟，其自上述第二精餾塔之塔頂部導出製品氮氣；及製品氬導出步驟，其自上述第三精餾塔之中間部導出製品氬。 A method for manufacturing product nitrogen and product argon, comprising: a cooling step, which cools the raw material air from which predetermined impurities have been removed; a raw material air introduction step, which introduces the raw material air cooled in the cooling step to the first rectification tower ; The first oxygen-rich liquid introduction step, which introduces the oxygen-rich liquid led from the bottom of the first rectification tower to the second rectification tower; the second oxygen-rich liquid introduction step, which will be from the first rectification At least a part of the oxygen-enriched liquid withdrawn from the bottom of the tower is introduced into the second condenser disposed in the third rectification tower; the nitrogen-containing liquid introduction step is to introduce the nitrogen-containing liquid condensed in the first condenser as a circulating liquid to The upper part of the second rectification tower; the expansion step, which causes at least a part of the mixed gas of the middle gas from the middle of the second rectification tower and the condenser gas from the first condenser, by The main heat exchanger performs heat exchange with the raw material air to release cold and then expands to generate cold. The cold is further released by being introduced into the main heat exchanger again, wherein the first condenser is configured to store in The gas at the top of the tower of the first rectification tower and the liquid stored at the bottom of the tower of the second rectification tower are subjected to heat exchange; The gas is introduced into the third rectification tower; the product nitrogen export step, which exports product nitrogen from the top of the second rectification tower; and the product argon export step, which exports product argon from the middle of the third rectification tower . 一種製品氮氣及製品氬之製造裝置，具備：主熱交換器，其使已去除既定之雜質之原料空氣冷卻；第一精餾塔，其被導入冷卻之上述原料空氣； 第二精餾塔，其導出製品氮氣；第三精餾塔，其導出製品氬；第一冷凝器，其構成為使貯存於上述第一精餾塔之塔頂部之氣體與貯存於上述第二精餾塔之塔底部之液體進行熱交換；含氮液體導入管，其將上述第一冷凝器中冷凝之含氮液體之至少一部分作為環流液導入至上述第二精餾塔；含氬氣體導入管，其使含氬氣體自上述第二精餾塔之下部導入至上述第三精餾塔；含氬液體導出管，其使含氬液體自上述第三精餾塔之塔底部導入至上述第二精餾塔；冷凝器氣體導出管，其使冷凝器氣體自上述第一冷凝器之氣相部導出；中間部氣體導出管，其使中間部氣體自上述第二精餾塔之中間部導出；膨脹渦輪，其使上述冷凝器氣體與上述中間部氣體之混合氣體經由上述主熱交換器後膨脹冷卻；配管，其將上述膨脹渦輪中膨脹冷卻之氣體導入至上述主熱交換器；製品氮氣導出管，其使上述製品氮氣自上述第二精餾塔導出；及製品氬導出管，其使上述製品氬自上述第三精餾塔之中間部導出。 A manufacturing device for product nitrogen and product argon, comprising: a main heat exchanger, which cools the raw material air from which predetermined impurities have been removed; a first rectification tower, which is introduced into the cooled raw material air; The second rectification tower, which leads the product nitrogen; the third rectification tower, which leads the product argon; the first condenser, which is configured to store the gas stored at the top of the first rectification tower and the second The liquid at the bottom of the rectification tower is subjected to heat exchange; a nitrogen-containing liquid introduction pipe that introduces at least a part of the nitrogen-containing liquid condensed in the first condenser as a circulating liquid to the second rectification tower; an argon-containing gas is introduced A tube that introduces argon-containing gas from the lower part of the second rectification column to the third rectification column; an argon-containing liquid outlet tube that introduces the argon-containing liquid from the bottom of the third rectification column to the first Second rectification tower; condenser gas outlet pipe, which leads the condenser gas from the gas phase of the first condenser; middle gas outlet pipe, which leads the middle gas from the middle of the second rectification tower Expansion turbine, which expands and cools the mixed gas of the condenser gas and the intermediate gas after passing through the main heat exchanger; piping, which introduces the expansion and cooling gas in the expansion turbine to the main heat exchanger; product nitrogen A discharge pipe that discharges the product nitrogen from the second rectification tower; and a product argon discharge pipe that discharges the product argon from the middle portion of the third rectification tower. 如請求項2所述之製品氮氣及製品氬之製造裝置，其中，具備：富氧液體導出管，其使貯存於上述第一精餾塔之塔底部之富氧液體自上述第一精餾塔之塔底部導出；第二富氧液體導入管，其將自上述富氧液體導出管導出之富氧液體導入至配置於上述第三精餾塔之第二冷凝器；及第三富氧液體導入管，其將自上述第二冷凝器導出之富氧液體導入至上述第二精餾塔。 The manufacturing device for product nitrogen and product argon according to claim 2, further comprising: an oxygen-enriched liquid outlet pipe that allows the oxygen-enriched liquid stored at the bottom of the first rectification tower from the first rectification tower The bottom of the tower is led out; a second oxygen-enriched liquid introduction pipe that introduces the oxygen-enriched liquid led out of the oxygen-enriched liquid outlet pipe to the second condenser disposed in the third rectification tower; and the third oxygen-enriched liquid introduction A pipe that introduces the oxygen-rich liquid discharged from the second condenser to the second rectification tower. 如請求項3所述之製品氮氣及製品氬之製造裝置，其中，上述第三富氧液體導入管將氣體狀態之富氧液體自上述第二冷凝器之氣相部導入至上述第二精餾塔。 The production device for product nitrogen and product argon according to claim 3, wherein the third oxygen-rich liquid introduction pipe introduces the gas-rich oxygen-rich liquid from the gas phase portion of the second condenser to the second rectification tower. 如請求項3所述之製品氮氣及製品氬之製造裝置，其進而具有：第四精餾塔，其配置於上述第二冷凝器之上部；及第四精餾塔塔頂部氣體導入管，其將自上述第四精餾塔之塔頂部取出之第四精餾塔塔頂部氣體導入至上述第二精餾塔；上述第三富氧液體導入管將液體狀態之富氧液體自上述第二冷凝器之液相部導入至上述第二精餾塔；貯存於上述第一精餾塔之塔底部之富氧液體經由上述第四精餾塔之氣相部而導入至上述第二冷凝器。 The manufacturing device for product nitrogen and product argon according to claim 3, further comprising: a fourth rectification tower disposed above the second condenser; and a gas introduction pipe at the top of the fourth rectification tower, which The gas from the top of the fourth rectification tower taken from the top of the fourth rectification tower is introduced into the second rectification tower; the third oxygen-rich liquid introduction pipe condenses the oxygen-rich liquid in liquid state from the second The liquid phase of the reactor is introduced into the second rectification tower; the oxygen-rich liquid stored in the bottom of the first rectification tower is introduced into the second condenser through the gas phase of the fourth rectification tower. 如請求項2至4中任一項所述之製品氮氣及製品氬之製造裝置，其進而具備第一富氧液體導入管，將貯存於上述第一精餾塔之塔底部之富氧液體之至少一部分導入至上述第二精餾塔。 The production device for product nitrogen and product argon as described in any one of claims 2 to 4 further includes a first oxygen-rich liquid introduction pipe, which stores the oxygen-rich liquid stored at the bottom of the first distillation column At least a part is introduced into the above-mentioned second distillation column. 如請求項2至4中任一項所述之製品氮氣及製品氬之製造裝置，其中，上述混合氣體為自上述第一冷凝器之氣相部直接取出之上述冷凝器氣體與自上述第二精餾塔之中間部直接取出之上述中間部氣體的混合氣體。 The manufacturing apparatus for product nitrogen and product argon according to any one of claims 2 to 4, wherein the mixed gas is the condenser gas directly taken out from the gas phase part of the first condenser and the second gas from the second The mixed gas of the gas in the middle part directly taken out in the middle part of the rectification tower. 如請求項3或4所述之製品氮氣及製品氬之製造裝置，其中，上述含氮液體導入管及上述富氧液體導出管之至少任一者與上述製品氮氣導出管經由過冷卻器。 The apparatus for manufacturing product nitrogen and product argon according to claim 3 or 4, wherein at least one of the nitrogen-containing liquid introduction pipe and the oxygen-enriched liquid outlet pipe and the product nitrogen outlet pipe pass through a subcooler. 如請求項8所述之製品氮氣及製品氬之製造裝置，其中，上述中間部氣體導出管於導入至上述過冷卻器之後，與上述冷凝器氣體導出管於第一合流點連接，上述第一合流點為上述過冷卻器之後段且上述膨脹渦輪之前段。 The manufacturing apparatus for product nitrogen and product argon according to claim 8, wherein the intermediate gas outlet pipe is connected to the condenser gas outlet pipe at the first confluence point after being introduced into the subcooler, the first The confluence point is the rear stage of the aforementioned supercooler and the preceding stage of the aforementioned expansion turbine. 如請求項6所述之製品氮氣及製品氬之製造裝置，其中，上述 第二精餾塔之中間部為較上述含氮液體導入管之上述第二精餾塔側之安裝位置下方，且為較上述第一富氧液體導入管之上述第二精餾塔側之安裝位置上方。 The manufacturing device for product nitrogen and product argon as described in claim 6, wherein the above The middle part of the second rectification tower is below the installation position of the second rectification tower side of the nitrogen-containing liquid introduction pipe, and is installed from the second rectification tower side of the first oxygen-rich liquid introduction pipe Above the location. 如請求項2至4中任一項所述之製品氮氣及製品氬之製造裝置，其中，自上述中間部氣體導出管導出之上述中間部氣體之導出流量，相對於自上述冷凝器氣體導出管導出之上述冷凝器氣體之導出流量的比為0.03以上且2以下。 The apparatus for manufacturing product nitrogen and product argon according to any one of claims 2 to 4, wherein the flow rate of the middle gas discharged from the middle gas outlet pipe is different from that of the condenser gas outlet pipe The ratio of the outlet flow rate of the above-mentioned condenser gas to be discharged is 0.03 or more and 2 or less.
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