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CN118836642A - Method for producing ultra-high purity oxygen and ultra-high purity oxygen apparatus - Google Patents

Method for producing ultra-high purity oxygen and ultra-high purity oxygen apparatus Download PDF

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Publication number
CN118836642A
CN118836642A CN202410447901.9A CN202410447901A CN118836642A CN 118836642 A CN118836642 A CN 118836642A CN 202410447901 A CN202410447901 A CN 202410447901A CN 118836642 A CN118836642 A CN 118836642A
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CN
China
Prior art keywords
oxygen
nitrogen
heat exchanger
rectifying column
raw material
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202410447901.9A
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Chinese (zh)
Inventor
广濑献儿
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Publication of CN118836642A publication Critical patent/CN118836642A/en
Pending legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/0403—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of nitrogen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04012—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling
    • F25J3/04036—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of warm gaseous streams; details of intake or interstage cooling of oxygen
    • 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
    • F25J3/04006—Providing pressurised feed air or process streams within or from the air fractionation unit
    • F25J3/04048—Providing pressurised feed air or process streams within or from the air fractionation unit by compression of cold gaseous streams, e.g. intermediate or oxygen enriched (waste) streams
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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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
    • F25J3/0426—The cryogenic component does not participate in the fractionation
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
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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
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04321—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of oxygen
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
    • F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
    • F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
    • F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
    • F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
    • F25J3/04363—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of oxygen
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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
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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
    • F25J3/04—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
    • F25J3/044—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 single pressure main column system only
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    • F25J3/04412—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system in a classical double column flowsheet, i.e. with thermal coupling by a main reboiler-condenser in the bottom of low pressure respectively top of high pressure column
    • 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
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    • F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
    • F25J3/04406—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a dual pressure main column system
    • F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
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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
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    • 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
    • F25J3/04521—Coupling of the air fractionation unit to an air gas-consuming unit, so-called integrated processes
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Abstract

本发明的课题是提供可以从由水电解得到的副产氧除去低沸点成分而以低成本获得超高纯度氧的超高纯度氧制造方法。解决手段是超高纯度氧制造方法包含下述工序：将包含低沸点成分作为杂质的原料氧从主热交换器1的温端导入、冷却后导入到氧精馏塔5，从氧精馏塔5的下部以气体或液体的形式导出除去了上述低沸点成分的制品超高纯度氧的工序。

The object of the present invention is to provide a method for producing ultra-high purity oxygen which can remove low-boiling-point components from by-product oxygen obtained by water electrolysis and obtain ultra-high purity oxygen at low cost. The solution is that the method for producing ultra-high purity oxygen includes the following steps: introducing raw material oxygen containing low-boiling-point components as impurities from the warm end of the main heat exchanger 1, cooling and then introducing it into the oxygen fractionation tower 5, and extracting the product ultra-high purity oxygen from which the low-boiling-point components are removed from the lower part of the oxygen fractionation tower 5 in the form of gas or liquid.

Description

超高纯度氧制造方法及超高纯度氧装置Ultra-high purity oxygen production method and ultra-high purity oxygen device

技术领域Technical Field

本发明涉及超高纯度氧制造方法和超高纯度氧装置。特别是涉及杂质浓度被控制在ppb水平以下的超高纯度氧的制造。The present invention relates to a method and apparatus for producing ultra-high purity oxygen, and more particularly to the production of ultra-high purity oxygen with impurity concentration controlled below the ppb level.

背景技术Background Art

作为氧中的杂质，甲烷等高沸点成分和氩等低沸点成分被控制为ppb水平以下的高纯度氧的需求特别是面向半导体产业。There is a demand for high-purity oxygen in which impurities such as methane and low-boiling-point components such as argon are controlled to below the ppb level, particularly in the semiconductor industry.

作为将杂质除去的方法，已知将催化剂与吸附材料并用的方法、将氧液化而通过精馏操作进行分离的深冷分离法，但特别是关于氩杂质，由于化学上为非活性、分子尺寸与氧分子极其接近，因此难以通过吸附法、分子筛而除去，深冷分离法是适当的。As methods for removing impurities, there are known methods of using a catalyst and an adsorbent material in combination, and a cryogenic separation method of liquefying oxygen and separating it by distillation operation. However, in particular, with regard to argon impurities, since they are chemically inactive and their molecular size is extremely close to that of oxygen molecules, they are difficult to remove by adsorption or molecular sieves, and cryogenic separation methods are appropriate.

作为获得超高纯度氧的方法，已知将由空气分离装置供给的液态氧(参照例如专利文献1)或液态氧(参照例如专利文献2)精馏的方法；或从将空气精馏的精馏塔导出除去了高沸点成分的含氧液，通过氧精馏塔将氩除去的方法。As a method for obtaining ultra-high purity oxygen, there are known methods of distilling liquid oxygen (see, for example, Patent Document 1) or liquid oxygen (see, for example, Patent Document 2) supplied from an air separation device; or a method of removing argon by extracting an oxygen-containing liquid from a distillation tower that distills air and removing high-boiling point components through an oxygen distillation tower.

专利文献3是在复式精馏系统中制造超高纯度氧的方法，专利文献4是在单式氮精馏系统中制造超高纯度氧的方法。Patent Document 3 is a method for producing ultra-high purity oxygen in a double distillation system, and Patent Document 4 is a method for producing ultra-high purity oxygen in a single nitrogen distillation system.

然而，作为制造超高纯度氧的原料，有时以将水电解而产生氢时的副产氧作为原料。该来源于水电解的氧与由以大气成分作为原料的空气分离装置获得的氧不同，不包含来源于大气的甲烷等高沸点成分，另一方面，包含若干溶解于水的低沸点成分。水中的低沸点杂质能够通过利用了氮气、氧气的鼓泡法等减少，但从高水平的杂质除去及其稳定度的观点考虑，期望通过深冷分离法来控制。However, as a raw material for producing ultra-high purity oxygen, by-product oxygen when water is electrolyzed to produce hydrogen is sometimes used as a raw material. The oxygen derived from water electrolysis is different from the oxygen obtained by the air separation device using atmospheric components as raw materials. It does not contain high-boiling components such as methane derived from the atmosphere, but contains a number of low-boiling components dissolved in water. Low-boiling impurities in water can be reduced by bubbling methods using nitrogen and oxygen, but from the perspective of high-level impurity removal and stability, it is expected to be controlled by cryogenic separation methods.

在现有技术中，对于氧气的深冷分离，专利文献2所记载的技术的应用是妥当的，但利用多个热交换器、压缩机的氮热介质循环的成本高，需要更低成本的技术开发。In the prior art, the application of the technology described in Patent Document 2 is appropriate for cryogenic separation of oxygen, but the cost of circulating nitrogen heat medium using a plurality of heat exchangers and compressors is high, and the development of a more cost-effective technology is needed.

现有技术文献Prior art literature

专利文献Patent Literature

专利文献1：日本专利第3929799号Patent Document 1: Japanese Patent No. 3929799

专利文献2：日本特开2021-55890号公报Patent Document 2: Japanese Patent Application Publication No. 2021-55890

专利文献3：美国专利第5,049,173号Patent Document 3: U.S. Patent No. 5,049,173

专利文献4：国际申请公开WO2014/173496A2Patent document 4: International application publication WO2014/173496A2

发明内容Summary of the invention

发明所要解决的课题Problems to be solved by the invention

本公开提供能够从由水电解得到的副产氧除去低沸点成分而以低成本获得超高纯度氧的超高纯度氧制造方法和超高纯度氧装置。The present disclosure provides a method for producing ultra-high purity oxygen and an ultra-high purity oxygen apparatus capable of removing low-boiling-point components from by-product oxygen obtained by water electrolysis to obtain ultra-high purity oxygen at low cost.

用于解决课题的方法Methods for solving problems

本公开的超高纯度氧制造方法可以在具备主热交换器(1)、氮精馏塔(第一(中压)精馏塔(2))、氮冷凝器(3)、氧精馏塔(5)、氧蒸发器(6)的空气分离装置中应用。The ultra-high purity oxygen production method disclosed in the present invention can be applied to an air separation device including a main heat exchanger (1), a nitrogen fractionator (a first (medium pressure) fractionator (2)), a nitrogen condenser (3), an oxygen fractionator (5), and an oxygen evaporator (6).

上述超高纯度氧制造方法包含下述工序：The above-mentioned method for producing ultra-high purity oxygen comprises the following steps:

将包含低沸点成分(例如，氮、氩)作为杂质的原料氧从主热交换器(1)的温端导入、冷却后导入到氧精馏塔(5)，从氧精馏塔(5)的下部或氧蒸发器(6)以气体或液体的形式导出除去了上述低沸点成分的制品超高纯度氧的工序。A process in which raw material oxygen containing low-boiling point components (e.g., nitrogen, argon) as impurities is introduced from the warm end of a main heat exchanger (1), cooled, and then introduced into an oxygen distillation tower (5), and a product ultra-high purity oxygen from which the low-boiling point components have been removed is discharged in the form of gas or liquid from the lower part of the oxygen distillation tower (5) or an oxygen evaporator (6).

上述超高纯度氧制造方法可以包含下述工序：将通过上述主热交换器(1)而至少一部分液化了的原料氧导入到上述氧精馏塔(5)的工序。The ultra-high purity oxygen production method may include the step of introducing the raw material oxygen at least partially liquefied by passing through the main heat exchanger (1) into the oxygen fractionator (5).

上述超高纯度氧制造方法可以包含下述工序：在上述氧蒸发器(6)中，利用通过上述主热交换器(1)而冷却了的原料空气的一部分、通过上述主热交换器(1)而冷却了的原料氧的一部分、以及从中压精馏塔(2)导出的液体或气体中的一种以上作为热介质，将从氧精馏塔(5)的底部(51)供给的液态氧蒸发，将其蒸气流供给到氧精馏塔(5)的底部(51)的工序。The above-mentioned ultra-high purity oxygen production method may include the following steps: in the above-mentioned oxygen evaporator (6), using a part of the raw air cooled by passing through the above-mentioned main heat exchanger (1), a part of the raw oxygen cooled by passing through the above-mentioned main heat exchanger (1), and one or more of the liquid or gas discharged from the medium-pressure distillation tower (2) as heat medium, the liquid oxygen supplied from the bottom (51) of the oxygen distillation tower (5) is evaporated, and its vapor flow is supplied to the bottom (51) of the oxygen distillation tower (5).

上述氧精馏塔(5)可以在其顶部或上方具备上述氧冷凝器(7)。The oxygen fractionation tower (5) may include the oxygen condenser (7) at or above the top thereof.

从中压精馏塔(2)导出的液体或气体可举出例如，含氧液、含氧气体、液态氮、或氮气等。Examples of the liquid or gas discharged from the medium-pressure distillation column (2) include oxygen-containing liquid, oxygen-containing gas, liquid nitrogen, and nitrogen gas.

上述超高纯度氧制造方法可以包含下述工序：在上述氧冷凝器(7)中，将从中压精馏塔(2)供给的液态氮或含氧液、从空气分离装置的外部供给的液态氮或液态空气作为冷却介质，将从上述氧精馏塔(5)供给的含有低沸点成分的氧流液化，作为其回流液而供给到氧精馏塔(5)的顶部(53)的工序。The above-mentioned ultra-high purity oxygen production method may include the following steps: in the above-mentioned oxygen condenser (7), liquid nitrogen or oxygen-containing liquid supplied from the medium-pressure distillation tower (2) and liquid nitrogen or liquid air supplied from the outside of the air separation device are used as cooling media, and the oxygen flow containing low-boiling point components supplied from the above-mentioned oxygen distillation tower (5) is liquefied and supplied to the top (53) of the oxygen distillation tower (5) as its reflux liquid.

为了保持上述主热交换器(1)的热平衡，可以包含下述工序：将从上述主热交换器(1)的中途导出的原料氧的一部分用膨胀涡轮(92)进行膨胀并冷却后，再次供给到主热交换器(1)的工序。In order to maintain the thermal balance of the main heat exchanger (1), the following step may be included: a step of expanding and cooling a portion of the raw oxygen discharged from the middle of the main heat exchanger (1) by an expansion turbine (92) and then supplying it to the main heat exchanger (1) again.

“超高纯度氧”的氧的浓度为99.99999％以上。The oxygen concentration of “ultra-high purity oxygen” is 99.99999% or more.

“原料氧”可以为通过水电解分解而生成的副产氧(高纯度氧氧浓度为99.99％左右)。The “raw material oxygen” may be by-product oxygen (high-purity oxygen having an oxygen concentration of approximately 99.99%) generated by decomposition of water by electrolysis.

本公开的超高纯度氧制造装置(A1、A2、A3)可以具备：The ultra-high purity oxygen production device (A1, A2, A3) disclosed in the present invention may include:

将原料空气和原料氧导入的主热交换器(1)；A main heat exchanger (1) for introducing feed air and feed oxygen;

具有将通过上述主热交换器(1)而进行了热交换的原料空气导入的底部(21)的第一(中压)精馏塔(2)；A first (medium-pressure) distillation tower (2) having a bottom (21) into which the raw air subjected to heat exchange in the main heat exchanger (1) is introduced;

将从上述第一精馏塔(2)的塔顶(23)导出的富氮气体冷凝的至少一个氮冷凝器(3)；at least one nitrogen condenser (3) for condensing the nitrogen-rich gas discharged from the top (23) of the first distillation column (2);

具有将通过上述氮冷凝器(3)而冷凝了的富氮气体和/或从上述第一精馏塔(2)的塔顶(23)导出的富氮气体通过过冷器(8)冷却后，导入的塔顶(43)的第二(低压)精馏塔(4)；A second (low-pressure) distillation tower (4) having a nitrogen-rich gas condensed by the nitrogen condenser (3) and/or the nitrogen-rich gas discharged from the tower top (23) of the first distillation tower (2) is introduced into the tower top (43) after being cooled by a subcooler (8);

使从上述氮冷凝器(3)的气相导出的气体部分地通过上述主热交换器(1)后导入的膨胀涡轮(92)；The gas discharged from the gas phase of the nitrogen condenser (3) is partially passed through the main heat exchanger (1) and then introduced into the expansion turbine (92);

具有将通过上述主热交换器(1)而进行了热交换的上述原料氧导入的塔顶(53)或精制部(52)的氧精馏塔(5)；an oxygen fractionation tower (5) having a tower top (53) or a refining section (52) for introducing the raw material oxygen subjected to heat exchange in the main heat exchanger (1);

配置在上述氧精馏塔(5)的底部(51)的下方，将通过上述主热交换器而冷却了的原料空气的一部分、通过上述主热交换器而冷却了的原料氧的一部分、以及从构成氮精馏塔的中压精馏塔导出的液体或气体中的一种以上作为热介质(例如，将从上述第一精馏塔(2)的底部(21)导出的富氧液作为热介质)，使液态氧蒸发的氧蒸发器(6)；以及an oxygen evaporator (6) disposed below the bottom (51) of the oxygen fractionator (5) and evaporating liquid oxygen using one or more of a portion of the raw material air cooled by passing through the main heat exchanger, a portion of the raw material oxygen cooled by passing through the main heat exchanger, and a liquid or gas discharged from a medium-pressure fractionator constituting the nitrogen fractionator as a heat medium (for example, the oxygen-rich liquid discharged from the bottom (21) of the first fractionator (2) is used as a heat medium); and

将从上述第一精馏塔(2)的底部(21)导出的富氧液、与通过上述氮冷凝器(3)而冷凝了的精制气体和/或从上述第一精馏塔(2)的塔顶(23)导出的精制气体、与从上述第二精馏塔(4)的塔顶(43)导出的富氮气体进行热交换的过冷器(8)。A subcooler (8) for performing heat exchange between the oxygen-rich liquid discharged from the bottom (21) of the first fractionator (2) and the purified gas condensed by the nitrogen condenser (3) and/or the purified gas discharged from the top (23) of the first fractionator (2) and the nitrogen-rich gas discharged from the top (43) of the second fractionator (4).

上述超高纯度氧制造装置(A1、A2、A3)可以具备：The ultra-high purity oxygen production device (A1, A2, A3) may include:

将从上述氧精馏塔(5)的塔顶(53)导出的含有低沸点成分的氧气冷凝的氧冷凝器(7)。An oxygen condenser (7) is provided for condensing the oxygen gas containing low-boiling-point components discharged from the top (53) of the oxygen fractionation tower (5).

上述超高纯度氧制造装置(A1、A2、A3)可以具备：The ultra-high purity oxygen production device (A1, A2, A3) may include:

将上述原料空气经由主热交换器(1)向上述第一精馏塔(2)的底部(21)的气相或精制部(22)的下部导入的原料空气管道线(L1)；A raw air pipeline (L1) for introducing the raw air into the gas phase at the bottom (21) of the first distillation tower (2) or the lower part of the refining section (22) via the main heat exchanger (1);

将从上述第一精馏塔(2)的底部(21)导出的富氧液经由上述过冷器(8)向上述第二精馏塔(4)的精馏部(42)的中间段导入的第一富氧液管道线(L21a)；a first oxygen-rich liquid pipeline (L21a) for introducing the oxygen-rich liquid discharged from the bottom (21) of the first distillation tower (2) into the middle section of the distillation section (42) of the second distillation tower (4) via the subcooler (8);

将从上述第一精馏塔(2)的塔顶(23)导出的富氮气体向上述氮冷凝器(3)输送，向从上述塔顶(23)导出的管道线(L231)合流的冷凝管道线(L23)；The nitrogen-rich gas discharged from the tower top (23) of the first distillation tower (2) is transported to the nitrogen condenser (3) and connected to the condensation pipeline (L23) which merges with the pipeline (L231) discharged from the tower top (23);

将从上述第一精馏塔(2)的塔顶(23)导出的富氮气体经由上述过冷器(8)向第二精馏塔(4)的塔顶(43)导入的第一循环气体管道线(L231)；a first circulating gas pipeline (L231) for introducing the nitrogen-rich gas discharged from the tower top (23) of the first distillation tower (2) to the tower top (43) of the second distillation tower (4) via the subcooler (8);

使从上述氮冷凝器(3)的气相导出的气体部分地通过上述主热交换器(1)，接着在膨胀涡轮(92)中使用，再次使其通过上述主热交换器(1)的第一废气管道线(L31)；The gas discharged from the gas phase of the nitrogen condenser (3) is partially passed through the main heat exchanger (1), then used in the expansion turbine (92), and then passed through the first exhaust gas line (L31) of the main heat exchanger (1);

将从上述第二精馏塔(4)的塔顶(43)导出的富氮气体经由上述过冷器(8)，使其通过上述主热交换器(1)的制品氮气管道线(L43)；The nitrogen-rich gas discharged from the top (43) of the second distillation tower (4) is passed through the subcooler (8) and then through the product nitrogen pipeline (L43) of the main heat exchanger (1);

将上述原料氧经由上述主热交换器(1)向上述氧精馏塔(5)的塔顶(53)或精馏部(52)导入的原料氧管道线(L10)；a raw oxygen pipeline (L10) for introducing the raw oxygen into the top (53) or the distillation section (52) of the oxygen distillation tower (5) via the main heat exchanger (1);

将上述原料氧从上述原料氧管道线(L10)的主热交换器(1)的中途分支，向对上述膨胀涡轮(92)连接前的上述第一废气管道线(L31)合流的分支原料氧管道线(L11)；The raw oxygen is branched from the main heat exchanger (1) of the raw oxygen line (L10) and connected to a branched raw oxygen line (L11) that merges with the first exhaust gas line (L31) before being connected to the expansion turbine (92);

使从上述氧精馏塔(5)的塔顶(53)导出的含有低沸点成分的氧气向废气管道线(L31)合流，或使其通过上述主热交换器(1)的第二废气管道线(L53)；The oxygen gas containing low-boiling-point components discharged from the top (53) of the oxygen fractionator (5) is merged with the exhaust gas line (L31), or is passed through the second exhaust gas line (L53) of the main heat exchanger (1);

用于将从上述第一精馏塔(2)的底部(21)导出的富氧液向上述氧蒸发器(6)导入，向上述第二精馏塔(4)的精馏部(42)的中间段导入，或向将从上述氧精馏塔(5)的塔顶(53)导出的含有低沸点成分的氧气冷凝的氧冷凝器(7)的冷热液部(71)导入的第二富氧液管道线(L21b)；a second oxygen-rich liquid pipeline (L21b) for introducing the oxygen-rich liquid discharged from the bottom (21) of the first distillation tower (2) into the oxygen evaporator (6), into the middle section of the distillation section (42) of the second distillation tower (4), or into the cold and hot liquid section (71) of the oxygen condenser (7) for condensing the oxygen containing low-boiling point components discharged from the top (53) of the oxygen distillation tower (5);

将从上述氧冷凝器(7)的冷热液部(71)导出的富氧液向上述第二精馏塔(4)的精馏部(42)的中间段导入的第二循环气体管道线(L71)；a second circulating gas pipeline (L71) for introducing the oxygen-rich liquid discharged from the cold and hot liquid section (71) of the oxygen condenser (7) into the middle section of the distillation section (42) of the second distillation tower (4);

将从上述氧冷凝器(7)的塔顶(73)导出的气体向上述第二精馏塔(4)的精馏部(42)的中间段导入的第三循环气体管道线(L73)；a third circulating gas line (L73) for introducing the gas discharged from the top (73) of the oxygen condenser (7) into the middle section of the distillation section (42) of the second distillation tower (4);

从上述氧蒸发器(6)的蒸发液部(61)取出超高纯度氧(液)的超高纯度氧取出管道线(L61)。An ultra-high purity oxygen take-out pipeline (L61) for taking out ultra-high purity oxygen (liquid) from the evaporating liquid section (61) of the oxygen evaporator (6).

其它公开的超高纯度氧制造装置(B1、B2)可以具备：Other disclosed ultra-high purity oxygen production devices (B1, B2) may include:

将原料空气和原料氧导入的主热交换器(1)；A main heat exchanger (1) for introducing feed air and feed oxygen;

具有将通过上述主热交换器(1)而进行了热交换的原料空气导入的底部(21)的氮精馏塔(2)；a nitrogen distillation tower (2) having a bottom (21) into which the raw air subjected to heat exchange in the main heat exchanger (1) is introduced;

将从上述氮精馏塔(2)的塔顶(23)导出的富氮气体冷凝的第一氮冷凝器(3)；a first nitrogen condenser (3) for condensing the nitrogen-rich gas discharged from the top (23) of the nitrogen rectification column (2);

将从上述氮精馏塔(2)的塔顶(23)导出的富氮气体冷凝的第二氮冷凝器(30)；a second nitrogen condenser (30) for condensing the nitrogen-rich gas discharged from the top (23) of the nitrogen rectification column (2);

使从上述第一氮冷凝器(3)的气相导出的气体部分地通过上述主热交换器(1)后导入的膨胀涡轮(92)；The gas discharged from the gas phase of the first nitrogen condenser (3) is partially passed through the main heat exchanger (1) and then introduced into the expansion turbine (92);

与上述膨胀涡轮(92)连接，将从上述第二氮冷凝器(30)的气相导出的气体压缩的压缩机(91)；a compressor (91) connected to the expansion turbine (92) for compressing the gas discharged from the gas phase of the second nitrogen condenser (30);

具有将通过上述主热交换器(1)而进行了热交换的上述原料氧导入的塔顶(53)或精制部(52)的氧精馏塔(5)；以及an oxygen fractionation tower (5) having a tower top (53) or a refining section (52) into which the raw material oxygen subjected to heat exchange in the main heat exchanger (1) is introduced; and

配置在上述氧精馏塔(5)的底部(51)的下方，将从上述氮精馏塔(2)的底部(21)导出的富氧液作为热介质，使液态氧蒸发的氧蒸发器(6)。An oxygen evaporator (6) is arranged below the bottom (51) of the oxygen fractionation tower (5) and evaporates liquid oxygen using the oxygen-rich liquid discharged from the bottom (21) of the nitrogen fractionation tower (2) as a heat medium.

上述超高纯度氧制造装置(B1、B2)可以具备：The ultra-high purity oxygen production device (B1, B2) may include:

将上述原料空气经由主热交换器(1)向上述氮精馏塔(2)的底部(21)的气相或精馏部(22)的下部导入的原料空气管道线(L1)；a raw air pipeline (L1) for introducing the raw air into the gas phase at the bottom (21) of the nitrogen fractionation tower (2) or the lower part of the fractionation section (22) via the main heat exchanger (1);

将从上述氮精馏塔(2)的底部(21)导出的富氧液向上述第二氮冷凝器(30)的冷热液部(未图示)导入的第一富氧液管道线(L21a)；a first oxygen-rich liquid pipeline (L21a) for introducing the oxygen-rich liquid discharged from the bottom (21) of the nitrogen rectification tower (2) into the cold and hot liquid parts (not shown) of the second nitrogen condenser (30);

将从上述氮精馏塔(2)的塔顶(23)导出的富氮气体向上述第一氮冷凝器(3)输送，向上述塔顶(23)返回的第一冷凝管道线(L231)；A first condensation pipeline (L231) for conveying the nitrogen-rich gas discharged from the tower top (23) of the nitrogen rectification tower (2) to the first nitrogen condenser (3) and returning to the tower top (23);

将从上述氮精馏塔(2)的塔顶(23)导出的富氮气体向上述第二氮冷凝器(30)输送，向上述塔顶(23)返回的第二冷凝管道线(L232)；A second condensation pipeline (L232) for conveying the nitrogen-rich gas discharged from the tower top (23) of the nitrogen rectification tower (2) to the second nitrogen condenser (30) and returning to the tower top (23);

使从上述氮精馏塔(2)的塔顶(23)导出的富氮气体通过上述主热交换器(1)的制品氮气管道线(L23)；Passing the nitrogen-rich gas discharged from the top (23) of the nitrogen rectification tower (2) through the product nitrogen pipeline (L23) of the main heat exchanger (1);

将从上述氮精馏塔(2)的精馏部(22)导出的含氧液向上述氧精馏塔(5)的塔顶(53)或精馏部(52)导入的含氧液管道线(L22)；an oxygen-containing liquid pipeline (L22) for introducing the oxygen-containing liquid discharged from the distillation section (22) of the nitrogen distillation tower (2) to the tower top (53) or the distillation section (52) of the oxygen distillation tower (5);

使从上述第一氮冷凝器(3)的塔顶的气相(31)导出的气体部分地通过上述主热交换器(1)，接着在膨胀涡轮(92)中使用，再次使其通过上述主热交换器(1)的第一废气管道线(L31)；The gas discharged from the gas phase (31) at the top of the first nitrogen condenser (3) is partially passed through the main heat exchanger (1), then used in the expansion turbine (92), and then passed through the first exhaust gas line (L31) of the main heat exchanger (1) again;

使从上述第二氮冷凝器(30)的塔顶的气相(301)导出的气体用上述压缩机(91)压缩，接着使其部分地通过上述主热交换器(1)，向上述氮精馏塔(2)的精馏部(22)的下部导入的再循环气体管道线(L301)；The gas discharged from the gas phase (301) at the top of the second nitrogen condenser (30) is compressed by the compressor (91), and then partially passes through the main heat exchanger (1) and is introduced into a recycle gas line (L301) at the lower part of the distillation section (22) of the nitrogen distillation column (2);

将上述原料氧经由主热交换器(1)向上述氧精馏塔(5)的塔顶(53)或精馏部(52)导入的原料氧管道线(L10)；A raw oxygen pipeline (L10) for introducing the raw oxygen into the top (53) or the distillation section (52) of the oxygen distillation tower (5) via the main heat exchanger (1);

将上述原料氧从上述原料氧管道线(L10)的主热交换器(1)的中途分支，向对上述膨胀涡轮(92)连接前的上述第一废气管道线(L31)合流的分支原料氧管道线(L11)；The raw oxygen is branched from the main heat exchanger (1) of the raw oxygen line (L10) and connected to a branched raw oxygen line (L11) that merges with the first exhaust gas line (L31) before being connected to the expansion turbine (92);

使从上述氧精馏塔(5)的塔顶(53)导出的含有低沸点成分的氧气向废气管道线(L31)合流，或使其通过上述主热交换器(1)的第二废气管道线(L53)；The oxygen gas containing low-boiling-point components discharged from the top (53) of the oxygen fractionator (5) is merged with the exhaust gas line (L31), or is passed through the second exhaust gas line (L53) of the main heat exchanger (1);

用于将从上述氮精馏塔(2)的底部(21)导出的富氧液向上述氧蒸发器(6)导入，向上述第二氮冷凝器(30)的冷热液部(未图示)导入的第二富氧液管道线(L21b)；以及a second oxygen-rich liquid pipeline (L21b) for introducing the oxygen-rich liquid drawn from the bottom (21) of the nitrogen fractionation tower (2) into the oxygen evaporator (6) and into the cold and hot liquid parts (not shown) of the second nitrogen condenser (30); and

从上述氧蒸发器(6)的蒸发液部(61)取出超高纯度氧(液)的超高纯度氧取出管道线(L61)。An ultra-high purity oxygen take-out pipeline (L61) for taking out ultra-high purity oxygen (liquid) from the evaporating liquid section (61) of the oxygen evaporator (6).

上述超高纯度氧制造装置(A1、A2、A3、B1、B2)的上述氧蒸发器(6)可以利用通过上述主热交换器(1)而冷却了的原料空气的一部分、通过上述主热交换器(1)而冷却了的原料氧的一部分、以及从上述中压精馏塔(4)导出的含氧液或液态氮之中的1种以上作为热介质。The oxygen evaporator (6) of the ultra-high purity oxygen production device (A1, A2, A3, B1, B2) can utilize a portion of the raw air cooled by passing through the main heat exchanger (1), a portion of the raw oxygen cooled by passing through the main heat exchanger (1), and one or more of the oxygen-containing liquid or liquid nitrogen discharged from the medium-pressure distillation tower (4) as heat medium.

上述超高纯度氧制造装置(A1、A2、A3、B1)可以具有：The ultra-high purity oxygen production device (A1, A2, A3, B1) may include:

流量测量器、压力测定仪、温度测定仪、液体水平测定仪等各种测量器；Various measuring instruments such as flow meter, pressure meter, temperature meter, liquid level meter, etc.

控制阀、分隔阀等各种阀；以及Various valves such as control valves, isolation valves, etc.; and

将各要素间连接的管道。The pipes that connect the elements.

(作用效果)(Effect)

(1)可以在制造氮气的空气分离装置、氮产生装置中组合氧精馏塔，与以往技术相比，以少的设备构成有效率地将由水电解得到的副产氧生成为超高纯度氧。(1) An oxygen fractionator can be combined with an air separation device or a nitrogen generation device for producing nitrogen gas, and by-product oxygen obtained by water electrolysis can be efficiently converted into ultra-high purity oxygen with a smaller equipment configuration than in the conventional technology.

(2)特别是，通过主热交换器将原料氧液化的工艺与在专利文献2中看到那样的氧气的精制方法不同，由于在空气分离装置的主热交换器冷端部可以充分地确保足以将氧液化的低温，因此才能够实现。(2) In particular, the process of liquefying the raw oxygen by the main heat exchanger is different from the oxygen purification method as seen in Patent Document 2, and is only possible because a sufficiently low temperature sufficient to liquefy the oxygen can be ensured at the cold end of the main heat exchanger of the air separation device.

(3)如果与需要循环氮压缩机、专用的主热交换器的现有方法相比，则可以在相对于每1装置的设备投资成本方面实现大的成本降低，同时，也可以减少循环氮压缩机所需要的电力。(3) Compared with the conventional method which requires a circulating nitrogen compressor and a dedicated main heat exchanger, it is possible to achieve a significant cost reduction in terms of equipment investment cost per device, and at the same time, it is possible to reduce the power required for the circulating nitrogen compressor.

(4)在使用水电解装置的半导体制造工艺中是有用的。(4) It is useful in a semiconductor manufacturing process using a water electrolysis device.

附图说明BRIEF DESCRIPTION OF THE DRAWINGS

图1为显示实施方式1的超高纯度氧制造装置的图。FIG. 1 is a diagram showing an ultra-high purity oxygen production apparatus according to Embodiment 1. FIG.

图2为显示实施方式2的超高纯度氧制造装置的图。FIG. 2 is a diagram showing an ultra-high purity oxygen production apparatus according to a second embodiment.

图3为显示实施方式3的超高纯度氧制造装置的图。FIG3 is a diagram showing an ultra-high purity oxygen production apparatus according to a third embodiment.

图4为显示实施方式4的超高纯度氧制造装置的图。FIG. 4 is a diagram showing an ultra-high purity oxygen production apparatus according to a fourth embodiment.

图5为显示实施方式5的超高纯度氧制造装置的图。FIG5 is a diagram showing an ultra-high purity oxygen production apparatus according to a fifth embodiment.

具体实施方式DETAILED DESCRIPTION

以下对本公开的若干实施方式进行说明。以下说明的实施方式说明本公开的一例。本公开不受以下实施方式任何限定，也包含在不变更本公开的主旨的范围中实施的各种变形方式。另外，并非以下说明的构成全部都是本公开的必需构成。上游、下游以气流的流动方向作为基准。Several embodiments of the present disclosure are described below. The embodiments described below illustrate an example of the present disclosure. The present disclosure is not limited by the following embodiments, and also includes various deformation modes implemented within the scope of the main purpose of the present disclosure. In addition, not all the structures described below are necessary structures of the present disclosure. The upstream and downstream are based on the flow direction of the airflow.

(实施方式1)(Implementation Method 1)

使用图1说明实施方式1的超高纯度氧装置A1。An ultra-high purity oxygen plant A1 according to the first embodiment will be described with reference to FIG. 1 .

超高纯度氧装置A1构成具备主热交换器1、中压精馏塔2、氮冷凝器3、低压精馏塔4、膨胀涡轮92、氧精馏塔5、氧蒸发器6、和过冷器8的空气分离装置。The ultra-high purity oxygen plant A1 is an air separation plant including a main heat exchanger 1 , a medium-pressure fractionator 2 , a nitrogen condenser 3 , a low-pressure fractionator 4 , an expansion turbine 92 , an oxygen fractionator 5 , an oxygen evaporator 6 , and a subcooler 8 .

关于主热交换器1，原料空气和原料氧从温端被导入并从冷端被导出，制品氮气、废气从冷端被导入而从温端被导出。原料空气进行规定的杂质、水分除去。原料氧为水电解的副生成物的氧，包含低沸点成分(例如，氮、氩)作为杂质。原料氧的氧浓度为99.99％左右。Regarding the main heat exchanger 1, raw air and raw oxygen are introduced from the warm end and discharged from the cold end, and product nitrogen and exhaust gas are introduced from the cold end and discharged from the warm end. The raw air is subjected to predetermined impurities and water removal. Raw oxygen is oxygen produced as a by-product of water electrolysis and contains low-boiling-point components (e.g., nitrogen, argon) as impurities. The oxygen concentration of raw oxygen is about 99.99%.

为了通过深冷分离法将氧中的低沸点成分除去，期望首先将氧液化后在精馏塔内与含有氧的蒸气流进行热和物质交换，在液相中将氧浓缩同时将低沸点成分除去，因此在本实施方式中，用主热交换器1将原料氧的至少一部分液化后向氧精馏塔5供给原料氧。In order to remove low-boiling-point components in oxygen by cryogenic separation, it is desired to first liquefy the oxygen and then exchange heat and matter with a vapor flow containing oxygen in a distillation tower, thereby concentrating the oxygen in the liquid phase and removing the low-boiling-point components. Therefore, in the present embodiment, at least a portion of the raw oxygen is liquefied by the main heat exchanger 1 and then the raw oxygen is supplied to the oxygen distillation tower 5.

中压精馏塔2具有将通过主热交换器1而冷却了的原料空气导入的底部21、和精馏部22、塔顶23。原料空气管道线L1为将原料空气经由主热交换器1向中压精馏塔2的底部21的气相或精制部22的下部导入的管道线。第一富氧液管道线L21a为将从中压精馏塔2的底部21导出的富氧液经由过冷器8向低压精馏塔4的精馏部42的中间段导入的管道线。第一富氧液管道线L21a与第二富氧液管道线L21b可以从富氧液的主管道线L21分支。冷凝管道线L23为将从中压精馏塔2的塔顶23导出的富氮气体向氮冷凝器3输送，向从塔顶23导出的第一循环气体管道线L231合流的管道线。第一循环气体管道线L231为将从中压精馏塔2的塔顶23导出的富氮气体经由过冷器8向低压精馏塔4的塔顶43导入的管道线。The medium-pressure fractionation tower 2 has a bottom 21 into which the raw air cooled by the main heat exchanger 1 is introduced, a fractionation section 22, and a tower top 23. The raw air pipeline L1 is a pipeline for introducing the raw air to the gas phase of the bottom 21 of the medium-pressure fractionation tower 2 or the lower part of the fractionation section 22 via the main heat exchanger 1. The first oxygen-rich liquid pipeline L21a is a pipeline for introducing the oxygen-rich liquid led out from the bottom 21 of the medium-pressure fractionation tower 2 to the middle section of the fractionation section 42 of the low-pressure fractionation tower 4 via the subcooler 8. The first oxygen-rich liquid pipeline L21a and the second oxygen-rich liquid pipeline L21b can be branched from the main pipeline L21 of the oxygen-rich liquid. The condensation pipeline L23 is a pipeline for conveying the nitrogen-rich gas led out from the tower top 23 of the medium-pressure fractionation tower 2 to the nitrogen condenser 3 and merging with the first circulating gas pipeline L231 led out from the tower top 23. The first circulating gas line L231 is a line that introduces the nitrogen-rich gas discharged from the top 23 of the medium-pressure fractionation tower 2 to the top 43 of the low-pressure fractionation tower 4 via the subcooler 8 .

氮冷凝器3将从中压精馏塔2的塔顶23导出的富氮气体冷凝。第一废气管道线L31使从氮冷凝器3的气相导出的气体部分地通过主热交换器1，接着在膨胀涡轮92中使用，使其再次通过主热交换器1的管道线。The nitrogen condenser 3 condenses the nitrogen-rich gas discharged from the top 23 of the medium-pressure rectification column 2. The first exhaust gas line L31 allows the gas discharged from the gas phase of the nitrogen condenser 3 to partially pass through the main heat exchanger 1, and then be used in the expansion turbine 92, and then pass through the pipeline of the main heat exchanger 1 again.

低压精馏塔4具有将通过氮冷凝器3而冷凝了的富氮气体和/或从中压精馏塔2的塔顶23导出的富氮气体通过过冷器8冷却后，进行导入的塔顶43、精馏部42。制品氮气管道线L43为使从低压第二精馏塔4的塔顶43导出的富氮气体经由过冷器8而通过主热交换器1的管道线。The low-pressure fractionator 4 includes a top 43 and a fractionator 42, into which the nitrogen-rich gas condensed by the nitrogen condenser 3 and/or the nitrogen-rich gas discharged from the top 23 of the medium-pressure fractionator 2 is introduced after being cooled by the subcooler 8. The product nitrogen gas pipeline L43 is a pipeline that allows the nitrogen-rich gas discharged from the top 43 of the low-pressure second fractionator 4 to pass through the main heat exchanger 1 via the subcooler 8.

膨胀涡轮92使从氮冷凝器3的气相导出的气体部分地通过主热交换器1后导入。在膨胀涡轮92中使用后的气体再次向主热交换器1输送，作为废气而被导出。The expansion turbine 92 introduces a part of the gas discharged from the gas phase of the nitrogen condenser 3 through the main heat exchanger 1. The gas used in the expansion turbine 92 is sent to the main heat exchanger 1 again and discharged as exhaust gas.

氧精馏塔5具有将通过主热交换器1而进行了热交换的原料氧导入的塔顶53或精制部52。原料氧管道线L10为将原料氧经由主热交换器1向氧精馏塔5的塔顶53或精馏部52导入的管道线。第二废气管道线L53为使从氧精馏塔5的塔顶53导出的含有低沸点成分的氧气向与膨胀涡轮92相比靠下游且与主热交换器1相比靠上游的废气管道线L31合流的管道线。The oxygen distillation tower 5 has a tower top 53 or a refining section 52 for introducing the raw oxygen that has undergone heat exchange through the main heat exchanger 1. The raw oxygen pipeline L10 is a pipeline for introducing the raw oxygen to the tower top 53 or the distillation section 52 of the oxygen distillation tower 5 via the main heat exchanger 1. The second exhaust gas pipeline L53 is a pipeline for merging the oxygen gas containing low-boiling point components derived from the tower top 53 of the oxygen distillation tower 5 with the exhaust gas pipeline L31 downstream of the expansion turbine 92 and upstream of the main heat exchanger 1.

氧蒸发器6被配置在氧精馏塔5的底部51的下方，将从中压精馏塔2的底部21导出的富氧液作为热介质，使液态氧蒸发。第二富氧液管道线L21b为用于将从中压精馏塔2的底部21导出的富氧液向氧蒸发器6导入，向低压精馏塔4的精馏部42的中间段导入的管道线。超高纯度氧取出管道线L61为从氧蒸发器6的蒸发液部61取出超高纯度氧(液)的管道线。The oxygen evaporator 6 is arranged below the bottom 51 of the oxygen fractionation tower 5, and uses the oxygen-rich liquid extracted from the bottom 21 of the medium-pressure fractionation tower 2 as a heat medium to evaporate liquid oxygen. The second oxygen-rich liquid pipeline L21b is a pipeline for introducing the oxygen-rich liquid extracted from the bottom 21 of the medium-pressure fractionation tower 2 to the oxygen evaporator 6 and to the middle section of the fractionation section 42 of the low-pressure fractionation tower 4. The ultra-high purity oxygen extraction pipeline L61 is a pipeline for extracting ultra-high purity oxygen (liquid) from the evaporation liquid section 61 of the oxygen evaporator 6.

为了向氧精馏塔5供给蒸气流，氧蒸发器6被配置在氧精馏塔5的下方。氧蒸发器6将从氧精馏塔5的底部51供给的液态氧蒸发而将其蒸气流供给到氧精馏塔5的底部51。利用原料氧的一部分作为热介质。作为其它实施方式，也可以利用从主热交换器1供给的原料空气的一部分、从中压精馏塔2供给的含氧液或液态氮的一部分。In order to supply a vapor stream to the oxygen fractionator 5, an oxygen evaporator 6 is arranged below the oxygen fractionator 5. The oxygen evaporator 6 evaporates the liquid oxygen supplied from the bottom 51 of the oxygen fractionator 5 and supplies its vapor stream to the bottom 51 of the oxygen fractionator 5. A part of the raw material oxygen is used as a heat medium. As another embodiment, a part of the raw material air supplied from the main heat exchanger 1, or a part of the oxygen-containing liquid or liquid nitrogen supplied from the medium-pressure fractionator 2 may be used.

作为热介质使用了的气体可以被液化而作为低压精馏塔4的回流液、主热交换器1、过冷器8的冷却介质而使用。作为热介质使用了的液体由于被过冷，因此减压时的蒸发损失减少。The gas used as the heat medium can be liquefied and used as the reflux liquid of the low-pressure fractionator 4, the main heat exchanger 1, and the cooling medium of the subcooler 8. Since the liquid used as the heat medium is subcooled, the evaporation loss during decompression is reduced.

过冷器8将从中压精馏塔2的底部21导出的富氧液、与通过氮冷凝器3而冷凝了的精制气体和/或从中压精馏塔2的塔顶23导出的精制气体、与从低压精馏塔4的塔顶43导出的富氮气体进行热交换。The subcooler 8 performs heat exchange between the oxygen-rich liquid discharged from the bottom 21 of the medium-pressure fractionation tower 2, the purified gas condensed by the nitrogen condenser 3 and/or the purified gas discharged from the top 23 of the medium-pressure fractionation tower 2, and the nitrogen-rich gas discharged from the top 43 of the low-pressure fractionation tower 4.

(实施方式2)(Implementation Method 2)

使用图2说明实施方式2的超高纯度氧装置A2。The ultra-high purity oxygen apparatus A2 according to the second embodiment will be described with reference to FIG. 2 .

超高纯度氧装置A2以与实施方式1的超高纯度氧装置A1不同的构成作为中心进行说明，相同的构成省略说明或简单说明。相同符号具有相同功能。超高纯度氧装置A2具备将从氧精馏塔5的塔顶53导出的含有低沸点成分的氧气冷凝的氧冷凝器7。The ultra-high purity oxygen device A2 is described mainly with respect to the configuration different from the ultra-high purity oxygen device A1 of the first embodiment, and the same configuration is omitted or simply described. The same symbols have the same functions. The ultra-high purity oxygen device A2 is provided with an oxygen condenser 7 for condensing the oxygen gas containing low boiling point components extracted from the top 53 of the oxygen fractionation tower 5.

第二富氧液管道线L21b为将从中压精馏塔2的底部21导出的富氧液向氧蒸发器6导入，在放出热后，向氧冷凝器7的冷热液部71导入的管道线。第二循环气体管道线L71为将从氧冷凝器7的冷热液部71导出的富氧液向低压精馏塔4的精馏部42的中间段导入的管道线。第三循环气体管道线L73为将从氧冷凝器7的塔顶73导出的气体向低压精馏塔4的精馏部42的中间段导入的管道线。The second oxygen-rich liquid pipeline L21b is a pipeline that introduces the oxygen-rich liquid derived from the bottom 21 of the medium-pressure distillation tower 2 to the oxygen evaporator 6, and after releasing heat, to the cold and hot liquid section 71 of the oxygen condenser 7. The second circulating gas pipeline L71 is a pipeline that introduces the oxygen-rich liquid derived from the cold and hot liquid section 71 of the oxygen condenser 7 to the middle section of the distillation section 42 of the low-pressure distillation tower 4. The third circulating gas pipeline L73 is a pipeline that introduces the gas derived from the tower top 73 of the oxygen condenser 7 to the middle section of the distillation section 42 of the low-pressure distillation tower 4.

为了提高超高纯度氧的回收率，将氧冷凝器7配置在氧精馏塔5的上方。由此，可以在维持超高纯度氧的纯度的同时，提高能够对被供给的原料氧进行回收的超高纯度氧量。作为氧冷凝器7的冷却介质，可以利用从中压精馏塔2或低压精馏塔4供给的含氧液、液态氮、通过氧蒸发器6而冷凝了的液态原料空气。此外也可以从外部供给液态氮或液态空气。In order to improve the recovery rate of ultra-high purity oxygen, the oxygen condenser 7 is arranged above the oxygen fractionation tower 5. As a result, the amount of ultra-high purity oxygen that can be recovered from the supplied raw oxygen can be increased while maintaining the purity of the ultra-high purity oxygen. As the cooling medium of the oxygen condenser 7, the oxygen-containing liquid supplied from the medium-pressure fractionation tower 2 or the low-pressure fractionation tower 4, liquid nitrogen, and liquid raw air condensed by the oxygen evaporator 6 can be used. In addition, liquid nitrogen or liquid air can also be supplied from the outside.

(实施方式3)(Implementation 3)

使用图3说明实施方式3的超高纯度氧装置A3。An ultra-high purity oxygen apparatus A3 according to the third embodiment will be described with reference to FIG. 3 .

超高纯度氧装置A3以与实施方式2的超高纯度氧装置A2不同的构成作为中心进行说明，相同构成省略说明或简单说明。相同符号具有相同功能。超高纯度氧装置A3具备分支原料氧管道线L11。分支原料氧管道线L11为将原料氧从原料氧管道线L10的主热交换器1的中途分支，向对膨胀涡轮92连接前的第一废气管道线L31合流的管道线。The ultra-high purity oxygen device A3 is described mainly with respect to the configuration different from the ultra-high purity oxygen device A2 of the second embodiment, and the same configuration is omitted or simply described. The same symbols have the same functions. The ultra-high purity oxygen device A3 is provided with a branch raw material oxygen pipeline L11. The branch raw material oxygen pipeline L11 is a pipeline that branches the raw material oxygen from the main heat exchanger 1 of the raw material oxygen pipeline L10 and merges with the first exhaust gas pipeline L31 before connecting to the expansion turbine 92.

为了保持主热交换器1的热平衡，原料高压氧的一部分从主热交换器1的中途被导出，通过膨胀涡轮92被膨胀而冷却后，再次被供给到主热交换器1。由此，能够将原料氧的液化所需要的冷热供给到主热交换器1。在具有剩余的原料氧的情况下，为了有助于空气分离装置、氮产生装置的冷热平衡保持，可以利用该冷热。In order to maintain the heat balance of the main heat exchanger 1, a part of the raw high-pressure oxygen is led out from the middle of the main heat exchanger 1, expanded and cooled by the expansion turbine 92, and then supplied to the main heat exchanger 1 again. In this way, the cold and heat required for liquefaction of the raw oxygen can be supplied to the main heat exchanger 1. In the case of excess raw oxygen, the cold and heat can be used to contribute to the maintenance of the cold and heat balance of the air separation device and the nitrogen generation device.

(实施方式4)(Implementation 4)

使用图4说明实施方式4的超高纯度氧装置B1。The ultra-high purity oxygen plant B1 according to the fourth embodiment will be described with reference to FIG. 4 .

超高纯度氧装置B1具备主热交换器1、氮精馏塔2、第一氮冷凝器3、第二氮冷凝器30、膨胀涡轮92、压缩机91、氧精馏塔5、和氧蒸发器6。与实施方式1～3的不同是，为单式的氮精馏塔，具备2个氮冷凝器、和再循环气体用的压缩机。主要说明不同的构成。The ultra-high purity oxygen device B1 includes a main heat exchanger 1, a nitrogen fractionator 2, a first nitrogen condenser 3, a second nitrogen condenser 30, an expansion turbine 92, a compressor 91, an oxygen fractionator 5, and an oxygen evaporator 6. The difference from Embodiments 1 to 3 is that it is a single nitrogen fractionator, and is equipped with two nitrogen condensers and a compressor for recirculating gas. The different configurations will be mainly described.

氮精馏塔2具有通过主热交换器1而冷却了的原料空气被导入的底部21、精馏部22、塔顶23。The nitrogen fractionator 2 includes a bottom portion 21 into which the raw material air cooled by the main heat exchanger 1 is introduced, a fractionating section 22 , and a top portion 23 .

第一氮冷凝器3将从氮精馏塔2的塔顶23导出的富氮气体冷凝。第二氮冷凝器30将从氮精馏塔2的塔顶23导出的富氮气体冷凝。膨胀涡轮92使从第一氮冷凝器3的气相被导出的气体部分地通过主热交换器1后导入。压缩机91与膨胀涡轮92连接，将从第二氮冷凝器30的气相导出的气体压缩。氧蒸发器6被配置在氧精馏塔5的底部51的下方，将从氮精馏塔2的底部21导出的富氧液作为热介质，使液态氧蒸发。The first nitrogen condenser 3 condenses the nitrogen-rich gas discharged from the top 23 of the nitrogen fractionation column 2. The second nitrogen condenser 30 condenses the nitrogen-rich gas discharged from the top 23 of the nitrogen fractionation column 2. The expansion turbine 92 partially introduces the gas discharged from the gas phase of the first nitrogen condenser 3 through the main heat exchanger 1. The compressor 91 is connected to the expansion turbine 92 and compresses the gas discharged from the gas phase of the second nitrogen condenser 30. The oxygen evaporator 6 is arranged below the bottom 51 of the oxygen fractionation column 5 and evaporates liquid oxygen using the oxygen-rich liquid discharged from the bottom 21 of the nitrogen fractionation column 2 as a heat medium.

原料空气管道线L1为将原料空气经由主热交换器1向氮精馏塔2的底部21的气相或精制部22的下部导入的管道线。第一富氧液管道线L21a为将从氮精馏塔2的底部21导出的富氧液向第二氮冷凝器30的冷热液部(未图示)导入的管道线。第一冷凝管道线L231为将从氮精馏塔2的塔顶23导出的富氮气体向第一氮冷凝器3输送，向塔顶23返回的管道线。第二冷凝管道线L232为将从氮精馏塔2的塔顶23导出的富氮气体向第二氮冷凝器30输送，向塔顶23返回的管道线。制品氮气管道线L23为使从氮精馏塔2的塔顶23导出的富氮气体通过主热交换器1，作为制品氮气而导出的管道线。The raw air line L1 is a line for introducing the raw air to the gas phase of the bottom 21 of the nitrogen fractionator 2 or the lower part of the refining section 22 via the main heat exchanger 1. The first oxygen-rich liquid line L21a is a line for introducing the oxygen-rich liquid discharged from the bottom 21 of the nitrogen fractionator 2 to the cold and hot liquid parts (not shown) of the second nitrogen condenser 30. The first condensation line L231 is a line for conveying the nitrogen-rich gas discharged from the top 23 of the nitrogen fractionator 2 to the first nitrogen condenser 3 and returning to the top 23. The second condensation line L232 is a line for conveying the nitrogen-rich gas discharged from the top 23 of the nitrogen fractionator 2 to the second nitrogen condenser 30 and returning to the top 23. The product nitrogen gas line L23 is a line for passing the nitrogen-rich gas discharged from the top 23 of the nitrogen fractionator 2 through the main heat exchanger 1 and discharging it as product nitrogen gas.

第一废气管道线L31为使从第一氮冷凝器3的塔顶的气相31导出的气体部分地通过主热交换器1，接着在膨胀涡轮92中被使用，再次使其通过主热交换器1的管道线。再循环气体管道线L301为将从第二氮冷凝器30的塔顶的气相301导出的气体用压缩机91压缩，接着使其部分地通过主热交换器1，向氮精馏塔2的精馏部22的下部导入的管道线。原料氧管道线L10为将原料氧经由主热交换器1向氧精馏塔5的塔顶53导入的管道线。第二废气管道线L53为使从氧精馏塔5的塔顶53导出的含有低沸点成分的氧气向废气管道线L31合流的管道线。第二富氧液管道线L21b为用于将从氮精馏塔2的底部21导出的富氧液向氧蒸发器6导入，向第二氮冷凝器30的冷热液部(未图示)导入的管道线。超高纯度氧取出管道线L61为从氧蒸发器6的蒸发液部61取出超高纯度氧(液)的管道线。The first exhaust gas line L31 is a line that partially passes the gas discharged from the gas phase 31 at the top of the first nitrogen condenser 3 through the main heat exchanger 1, is then used in the expansion turbine 92, and is again passed through the main heat exchanger 1. The recirculation gas line L301 is a line that compresses the gas discharged from the gas phase 301 at the top of the second nitrogen condenser 30 by the compressor 91, partially passes through the main heat exchanger 1, and is introduced to the lower part of the distillation section 22 of the nitrogen distillation tower 2. The raw material oxygen line L10 is a line that introduces the raw material oxygen to the top 53 of the oxygen distillation tower 5 via the main heat exchanger 1. The second exhaust gas line L53 is a line that allows the oxygen gas containing low-boiling-point components discharged from the top 53 of the oxygen distillation tower 5 to merge with the exhaust gas line L31. The second oxygen-rich liquid line L21b is a line for introducing the oxygen-rich liquid drawn out from the bottom 21 of the nitrogen fractionation tower 2 to the oxygen evaporator 6 and to the cold and hot liquid parts (not shown) of the second nitrogen condenser 30. The ultra-high purity oxygen extraction line L61 is a line for extracting ultra-high purity oxygen (liquid) from the evaporation liquid part 61 of the oxygen evaporator 6.

(实施方式5)(Implementation method 5)

使用图5说明实施方式5的超高纯度氧装置B2。实施方式5与实施方式4的基本构成相同。不同点是原料氧管道线L10、和含氧液管道线L22。An ultra-high purity oxygen plant B2 according to Embodiment 5 will be described with reference to Fig. 5. Embodiment 5 has the same basic configuration as Embodiment 4. The difference lies in the raw oxygen line L10 and the oxygen-containing liquid line L22.

原料氧管道线L10为将原料氧经由主热交换器1向氧精馏塔5的精馏部52的中间段导入的管道线。含氧液管道线L22为将从氮精馏塔2的精馏部22的中间段(与原料空气导入管道线L1相比靠上方位置)导出的含氧液向氧精馏塔5的塔顶53导入的管道线。The raw oxygen line L10 is a line for introducing raw oxygen into the middle section of the distillation section 52 of the oxygen distillation tower 5 via the main heat exchanger 1. The oxygen-containing liquid line L22 is a line for introducing the oxygen-containing liquid drawn out from the middle section of the distillation section 22 of the nitrogen distillation tower 2 (above the raw air introduction line L1) into the tower top 53 of the oxygen distillation tower 5.

即，向氧精馏塔5的中间段导入原料氧，向氧精馏塔5的塔顶53供给来自氮精馏塔2的中间段的含氧液。含氧液为了不包含来源于大气的高沸点杂质，从与氮精馏塔的原料空气供给段相比靠上段被导出。通过该构成，从而可以将用于将原料氧冷凝的液体供给到氧精馏塔，同时，能够将来源于氮精馏塔的氧精制为高纯度氧，针对高纯度氧的需求，可以一边将水电解装置与氮产生装置的运转率最佳化，一边制造高纯度氧。例如，在氢需求少，另一方面，具有大量高纯度氧需求的情况下，通过一边将来源于水电解装置的氧精制为高纯度氧，一边将来自氮精馏塔的含氧液用氧精馏塔精制来获得高纯度氧的不足部分。通过这样，从而不需要根据高纯度氧需求而运转耗电大的水电解装置，可以将电力消耗量最佳化。That is, raw material oxygen is introduced into the middle section of the oxygen fractionator 5, and the oxygen-containing liquid from the middle section of the nitrogen fractionator 2 is supplied to the tower top 53 of the oxygen fractionator 5. The oxygen-containing liquid is discharged from the upper section than the raw material air supply section of the nitrogen fractionator in order not to contain high-boiling impurities derived from the atmosphere. With this configuration, the liquid for condensing the raw material oxygen can be supplied to the oxygen fractionator, and at the same time, the oxygen derived from the nitrogen fractionator can be refined into high-purity oxygen. In response to the demand for high-purity oxygen, high-purity oxygen can be produced while optimizing the operating rates of the water electrolysis device and the nitrogen generation device. For example, when the demand for hydrogen is small and there is a large demand for high-purity oxygen, the insufficient part of the high-purity oxygen can be obtained by refining the oxygen derived from the water electrolysis device into high-purity oxygen while refining the oxygen-containing liquid from the nitrogen fractionator with the oxygen fractionator. In this way, it is not necessary to operate the water electrolysis device with high power consumption according to the demand for high-purity oxygen, and the power consumption can be optimized.

(实施例)(Example)

实施方式1的超高纯度氧制造装置A1(空气分离装置(氮产生装置))中，将流量1000Nm3/h、温度20℃、压力7.7bar的原料空气导入到主热交换器1，冷却后向中压精馏塔2的底部21导入原料空气。原料空气在以7.5bar运转的中压精馏塔2的塔内被精馏，从塔顶23导出液态氮408Nm3/h，从塔底部21导出含氧液(富氧液)592Nm3/h。In the ultra-high purity oxygen production apparatus A1 (air separation apparatus (nitrogen production apparatus)) of the first embodiment, raw air at a flow rate of 1000 Nm 3 /h, a temperature of 20°C, and a pressure of 7.7 bar is introduced into the main heat exchanger 1, and after cooling, the raw air is introduced into the bottom 21 of the medium-pressure fractionation tower 2. The raw air is fractionated in the medium-pressure fractionation tower 2 operated at 7.5 bar, and 408 Nm 3 /h of liquid nitrogen is discharged from the tower top 23, and 592 Nm 3 /h of oxygen-containing liquid (oxygen-rich liquid) is discharged from the tower bottom 21.

通过管道L231导出的液态氮(通过冷凝器3而冷凝了的氮气)、与通过管道L21a导出的含氧液(富氧液)分别通过过冷器8而被冷却了后，液态氮(通过冷凝器3而冷凝了的氮气)被供给到以2.5barA运转的低压精馏塔4的顶部43。含氧液(富氧液)被供给到低压精馏塔4的中间部。液态氮与含氧液一边与从氮冷凝器3被供给的蒸气流进行热和物质交换，一边被精馏，从低压精馏塔4的顶部43导出氮气730Nm3/h，从底部31导出废气270Nm3/h。The liquid nitrogen (nitrogen gas condensed by the condenser 3) discharged through the pipe L231 and the oxygen-containing liquid (oxygen-enriched liquid) discharged through the pipe L21a are cooled by the subcooler 8, respectively, and then the liquid nitrogen (nitrogen gas condensed by the condenser 3) is supplied to the top 43 of the low-pressure distillation column 4 operated at 2.5 barA. The oxygen-containing liquid (oxygen-enriched liquid) is supplied to the middle part of the low-pressure distillation column 4. The liquid nitrogen and the oxygen-containing liquid are distilled while exchanging heat and substances with the vapor flow supplied from the nitrogen condenser 3, and 730 Nm 3 /h of nitrogen gas is discharged from the top 43 of the low-pressure distillation column 4, and 270 Nm 3 /h of exhaust gas is discharged from the bottom 31.

通过管道L43而被导出的氮气在被过冷器8加温后进一步被主热交换器1加温，以温度17.5℃、压力2.3barA从主热交换器1的温端被导出。The nitrogen gas discharged through the pipe L43 is heated by the subcooler 8 and then further heated by the main heat exchanger 1 , and discharged from the warm end of the main heat exchanger 1 at a temperature of 17.5° C. and a pressure of 2.3 barA.

通过管道L31而被导出的废气在利用主热交换器1加温到-120℃后通过膨胀涡轮92而膨胀、冷却后再次被供给到主热交换器1，以温度17.5℃、压力1.15barA从主热交换器1的温端被导出。The exhaust gas discharged through the pipe L31 is heated to -120°C by the main heat exchanger 1, expanded by the expansion turbine 92, cooled, and then supplied to the main heat exchanger 1 again, and discharged from the warm end of the main heat exchanger 1 at a temperature of 17.5°C and a pressure of 1.15 barA.

包含氩1ppm作为杂质的原料氧以流量30Nm3/h、温度20℃、压力10barA被导入到主热交换器1，被冷却到-153.5℃，被液化。被冷却了的液态氧在减压后供给到以1.5barA运转的氧精馏塔5(NTP＝60)的顶部53，一边与从氧蒸发器6被供给的蒸气流进行热和物质交换，一边被精馏。作为氧蒸发器6的热介质，含氧液(富氧液)从中压精馏塔2的底部21被供给310Nm3/h，被冷却后，被供给到低压精馏塔4的精馏部42的中间部。从氧蒸发器6的蒸发液部61或氧精馏部5的塔底部获得低沸点成分(氩杂质)含量被减少到10ppb的超高纯度氧液7.3Nm3/h。Raw material oxygen containing 1 ppm of argon as an impurity is introduced into the main heat exchanger 1 at a flow rate of 30 Nm 3 /h, a temperature of 20°C, and a pressure of 10 barA, and is cooled to -153.5°C and liquefied. The cooled liquid oxygen is depressurized and supplied to the top 53 of the oxygen fractionator 5 (NTP=60) operated at 1.5 barA, and is rectified while exchanging heat and substances with the vapor flow supplied from the oxygen evaporator 6. As the heat medium of the oxygen evaporator 6, an oxygen-containing liquid (oxygen-rich liquid) is supplied from the bottom 21 of the medium-pressure fractionator 2 at 310 Nm 3 /h, and after being cooled, is supplied to the middle part of the fractionation section 42 of the low-pressure fractionator 4. From the evaporating liquid section 61 of the oxygen evaporator 6 or the bottom of the oxygen fractionator 5, 7.3 Nm 3 /h of ultra-high purity oxygen liquid with the low boiling point component (argon impurity) content reduced to 10 ppb is obtained.

(其它实施方式)(Other embodiments)

(1)虽然没有特别写明，但可以在各管道线设置压力调整装置、流量控制装置等，进行压力调整或流量调整。(1) Although not specifically stated, pressure regulating devices, flow control devices, etc. may be installed in each pipeline to adjust the pressure or flow.

(2)虽然没有特别写明，但可以在各线设置控制阀、分隔阀等。(2) Although not specifically stated, control valves, separation valves, etc. may be installed in each line.

(3)虽然没有特别写明，但可以在各塔设置压力调整装置、温度测定装置等，进行压力调整或温度调整。(3) Although not specifically stated, each tower may be provided with a pressure regulating device, a temperature measuring device, etc. to perform pressure regulation or temperature regulation.

符号的说明Explanation of symbols

1 热交换器1 Heat exchanger

2 中压精馏塔2 Medium pressure distillation tower

3 氮冷凝器3 Nitrogen condenser

4低压精馏塔4Low pressure distillation tower

5氧精馏塔5 Oxygen distillation tower

6氧蒸发器6 Oxygen Evaporator

7氧冷凝器7. Oxygen Condenser

8过冷器8. Subcooler

91压缩机91 compressor

92膨胀涡轮。92Expansion turbine.

Claims (8)

1. An ultra-high purity oxygen production method using an air separation device provided with a main heat exchanger, a nitrogen rectifying column, a nitrogen condenser, an oxygen rectifying column, and an oxygen evaporator, the ultra-high purity oxygen production method comprising the steps of:
Introducing raw material oxygen containing a low boiling point component as an impurity from a temperature end of a main heat exchanger, cooling the raw material oxygen to liquefy at least a part of the raw material oxygen, introducing the liquefied raw material oxygen into an oxygen rectifying column, and introducing ultra-high purity oxygen from which the low boiling point component is removed from a lower part of the oxygen rectifying column or an oxygen evaporator in a gas or liquid form; and
And a step of evaporating liquid oxygen supplied from the bottom of the oxygen rectifying column and supplying a vapor stream thereof to the bottom of the oxygen rectifying column using, as a heat medium, one or more of a part of raw material air cooled by the main heat exchanger, a part of raw material oxygen cooled by the main heat exchanger, and a liquid or gas discharged from a medium-pressure rectifying column constituting the nitrogen rectifying column.
2. The method for producing ultra-high purity oxygen according to claim 1, further comprising the steps of: and liquefying an oxygen stream containing a low boiling point component supplied from the oxygen rectifying column as a reflux liquid thereof by using liquid nitrogen or an oxygen-containing liquid supplied from the medium pressure rectifying column and liquid nitrogen or liquid air supplied from the outside of the air separation device as a cooling medium in an oxygen condenser provided above or at the top of the oxygen rectifying column.
3. The method for producing ultra-high purity oxygen according to claim 1, further comprising the steps of: and a step of cooling a part of the raw material oxygen discharged from the middle of the main heat exchanger by expansion with an expansion turbine and then supplying the cooled part to the main heat exchanger again.
4. An ultra-high purity oxygen production apparatus comprising:
a main heat exchanger for introducing raw material air and raw material oxygen;
a first rectifying column having a bottom for introducing the raw material air subjected to heat exchange by the main heat exchanger;
at least one nitrogen condenser condensing nitrogen-rich gas conducted from the top of the first rectifying column;
a second rectifying column having a top through which the nitrogen-rich gas condensed by the nitrogen condenser and/or the nitrogen-rich gas discharged from the top of the first rectifying column is cooled by a subcooler and then introduced;
an oxygen rectifying column having a column top or a refining section into which the raw material oxygen subjected to heat exchange by the main heat exchanger is introduced;
An oxygen evaporator disposed below the bottom of the oxygen rectifying column, for evaporating liquid oxygen using, as a heat medium, one or more of a part of raw material air cooled by the main heat exchanger, a part of raw material oxygen cooled by the main heat exchanger, and liquid or gas discharged from a medium-pressure rectifying column constituting the nitrogen rectifying column; and
And a subcooler that exchanges heat between the oxygen-enriched liquid discharged from the bottom of the first rectifying column, the purified gas condensed by the nitrogen condenser and/or the purified gas discharged from the top of the first rectifying column, and the nitrogen-enriched gas discharged from the top of the second rectifying column.
5. The ultra-high purity oxygen production apparatus according to claim 4, comprising an expansion turbine for introducing gas discharged from the gas phase of the nitrogen condenser partially through the main heat exchanger.
6. The ultra-high purity oxygen production apparatus according to claim 4, comprising an oxygen condenser for condensing oxygen containing low boiling components, which is introduced from a top of the oxygen rectifying column.
7. The ultra-high purity oxygen production apparatus according to claim 4, comprising:
A raw material oxygen pipeline for introducing the raw material oxygen to the top of the oxygen rectifying column or the rectifying portion via the main heat exchanger;
A branched raw material oxygen pipeline which branches the raw material oxygen from the middle of the main heat exchanger of the raw material oxygen pipeline and merges into a pipeline before the expansion turbine is connected; and
An ultra-high purity oxygen extraction line for extracting ultra-high purity oxygen from the evaporation liquid portion of the oxygen evaporator.
8. An ultra-high purity oxygen production apparatus comprising:
a main heat exchanger for introducing raw material air and raw material oxygen;
A nitrogen rectifying column having a bottom for introducing raw material air subjected to heat exchange by the main heat exchanger;
a first nitrogen condenser for condensing the nitrogen-rich gas discharged from the top of the nitrogen rectifying column;
a second nitrogen condenser for condensing the nitrogen-rich gas discharged from the top of the nitrogen rectifying column;
An expansion turbine that is introduced after the gas that is led out from the gas phase of the first nitrogen condenser is partially passed through the main heat exchanger;
a compressor for compressing the gas from the gas phase of the second nitrogen condenser;
an oxygen rectifying column having a column top or a refining unit for introducing the raw material oxygen subjected to heat exchange by the main heat exchanger; and
An oxygen evaporator disposed below the bottom of the oxygen rectifying column, and configured to evaporate liquid oxygen using one or more of a part of raw material air cooled by the main heat exchanger, a part of raw material oxygen cooled by the main heat exchanger, and liquid or gas discharged from the nitrogen rectifying column as a heat medium.
CN202410447901.9A 2023-04-24 2024-04-15 Method for producing ultra-high purity oxygen and ultra-high purity oxygen apparatus Pending CN118836642A (en)

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