JP2019171231A - Refined gas production apparatus and refined gas production method - Google Patents

Refined gas production apparatus and refined gas production method Download PDF

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JP2019171231A
JP2019171231A JP2018059380A JP2018059380A JP2019171231A JP 2019171231 A JP2019171231 A JP 2019171231A JP 2018059380 A JP2018059380 A JP 2018059380A JP 2018059380 A JP2018059380 A JP 2018059380A JP 2019171231 A JP2019171231 A JP 2019171231A
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purification tower
oxygen
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JP6655645B2 (en
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真子 田中
Masako Tanaka
真子 田中
貴紀 貝川
Takanori KAIGAWA
貴紀 貝川
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Air Water Inc
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/26—Drying gases or vapours
    • C—CHEMISTRY; METALLURGY
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    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/04—Purification or separation of nitrogen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B23/00—Noble gases; Compounds thereof

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Abstract

To provide a refined gas production apparatus which combines suppression of a hydrogen amount in refined gas with reduction of the number of devices when raw material gas includes at least a moisture content and oxygen, and to provide a refined gas production method.SOLUTION: The refined gas production apparatus is provided that comprises: a refining tower for obtaining refined gas by removing at least a moisture content and oxygen in raw material gas, the refining tower includes a first region and a second region, the first region is a region for adsorbing off the moisture content in the raw material gas, and a second region is a region for obtaining refined gas by removing at least oxygen in the raw material gas having passed through the first region. The refined gas production method is also provided that comprises: introducing the raw material gas into the refining tower including the first region and the second region; adsorbing off at least moisture content in the raw material gas at the first region; removing, in the second region, at least oxygen in the raw material gas from which moisture content is adsorbed off at the first region; and deriving, as the refining gas, the raw material gas from which oxygen is removed at the second region.SELECTED DRAWING: Figure 1

Description

本発明は、精製ガスの製造装置および精製ガスの製造方法に関する。   The present invention relates to a purified gas production apparatus and a purified gas production method.

特開平５−４８０９号公報（特許文献１）は、ヘリウム等の不活性ガスに含まれる酸素や水分等の不純物を、ジルコニウム−バナジウム二元合金等のゲッター金属を用いて除去する精製方法を開示している。   Japanese Patent Laid-Open No. 5-4809 (Patent Document 1) discloses a purification method for removing impurities such as oxygen and moisture contained in an inert gas such as helium by using a getter metal such as a zirconium-vanadium binary alloy. is doing.

特開平７−３１８７７号公報（特許文献２）は、不純物として酸素および水分を含む不活性ガスを、ニッケル等を主成分とするゲッター剤と加熱条件下において接触させることにより不活性ガスから酸素を除去し、その後不活性ガスに残存する水分を常温において吸着除去し、精製ガスを製造することを開示している。   Japanese Patent Laid-Open No. 7-31877 (Patent Document 2) discloses that oxygen is removed from an inert gas by bringing an inert gas containing oxygen and moisture as impurities into contact with a getter agent mainly composed of nickel or the like under heating conditions. It is disclosed that the purified gas is produced by removing the moisture remaining in the inert gas after adsorption at room temperature.

特開平５−４８０９号公報Japanese Patent Laid-Open No. 5-4809 特開平７−３１８７７号公報JP 7-31877 A

本発明者らは、不活性ガス中の酸素をゲッター剤を用いて除去することにより精製ガスを製造することを試みた。その結果、メカニズムは不明であるが、不活性ガス中に不純物として水分も含まれている場合には、精製ガス中に微量の水素が含まれるという新たな知見を得た。すなわち、特許文献１や特許文献２に開示される精製方法を用いた場合、原料ガスに不純物として水分が含まれている場合には、精製ガス中に微量の水素が含まれると考えられる。そのため、精製ガス中の水素を除去する設備を新たに設ける必要があり得る。なお、本明細書において「精製ガス」とは、原料ガス中に含まれる不純物の濃度が低減されたガスを示す。   The present inventors tried to produce purified gas by removing oxygen in an inert gas using a getter agent. As a result, the mechanism is unknown, but when the inert gas contains moisture as an impurity, a new finding has been obtained that a small amount of hydrogen is contained in the purified gas. That is, when the purification methods disclosed in Patent Document 1 and Patent Document 2 are used, if the raw material gas contains moisture as an impurity, it is considered that a small amount of hydrogen is contained in the purified gas. Therefore, it may be necessary to newly provide equipment for removing hydrogen in the purified gas. In the present specification, the “purified gas” refers to a gas in which the concentration of impurities contained in the raw material gas is reduced.

加えて、特許文献１において開示される精製ガスの製造方法に用いられるジルコニウム−バナジウム二元合金等のゲッター金属は、高価であるという問題もあった。   In addition, getter metals such as zirconium-vanadium binary alloys used in the method for producing purified gas disclosed in Patent Document 1 have a problem of being expensive.

また、特許文献２において開示される精製ガスの製造方法は、原料ガス中の酸素を除去する工程と原料ガスから水分を除去する工程との間に、原料ガスを常温まで冷却する工程が必要となる。すなわち、原料ガス中の酸素を除去するための設備と原料ガス中の水分を除去するための設備との間に、冷却手段を設ける必要があった。また、連続運転を行う際には、水分を除去するためのゼオライト塔および酸素を除去するためのゲッター塔が、それぞれ２塔、合計４塔必要であった。すなわち、機器点数が多いため、初期投資額や当該機器のメンテナンスに要する費用等、コストの削減に改善の余地があった。   Further, the method for producing purified gas disclosed in Patent Document 2 requires a step of cooling the raw material gas to room temperature between the step of removing oxygen in the raw material gas and the step of removing moisture from the raw material gas. Become. That is, it is necessary to provide a cooling means between the equipment for removing oxygen in the raw material gas and the equipment for removing moisture in the raw material gas. Moreover, when performing a continuous operation, the zeolite tower for removing a water | moisture content and the getter tower for removing oxygen needed 2 towers, respectively, a total of 4 towers. In other words, since the number of devices is large, there is room for improvement in cost reduction such as initial investment amount and costs required for maintenance of the device.

本発明の目的は、原料ガスが不純物として少なくとも水分および酸素を含む際に、精製ガス中の水素量の抑制と、機器点数の削減とが両立された精製ガスの製造装置および精製ガスの製造方法を提供することにある。   An object of the present invention is to provide a refined gas production apparatus and a refined gas production method in which, when the raw material gas contains at least moisture and oxygen as impurities, the reduction of the amount of hydrogen in the refined gas and the reduction in the number of equipment are compatible. Is to provide.

本発明は、以下に示す精製ガスの製造装置および精製ガスの製造方法を提供する。   The present invention provides a purified gas production apparatus and a purified gas production method described below.

［１］ 原料ガス中の少なくとも水分および酸素を除去し、精製ガスを得るための精製塔を備え、前記精製塔は、第１領域および第２領域を含み、前記第１領域は、前記原料ガス中の少なくとも水分を吸着除去するための領域であり、前記第２領域は、前記第１領域を経た前記原料ガス中の少なくとも酸素を除去し、精製ガスを得るための領域である、精製ガスの製造装置。   [1] A purification tower for removing at least moisture and oxygen in the raw material gas and obtaining a purified gas is provided. The purification tower includes a first region and a second region, and the first region includes the raw material gas. Of the purified gas, which is a region for adsorbing and removing at least moisture therein, and wherein the second region is a region for removing at least oxygen in the source gas that has passed through the first region to obtain a purified gas. Manufacturing equipment.

［２］ 前記第１領域は、脱湿剤を含み、前記第２領域は、ゲッター剤を含む、［１］に記載の製造装置。   [2] The manufacturing apparatus according to [1], wherein the first region includes a dehumidifying agent, and the second region includes a getter agent.

［３］ 前記ゲッター剤は、銅を含む、［２］に記載の製造装置。   [3] The manufacturing apparatus according to [2], wherein the getter agent includes copper.

［４］ 前記原料ガスは、窒素および希ガスからなる群より選択される一種以上のガスを含む、［１］〜［３］のいずれかに記載の製造装置。   [4] The manufacturing apparatus according to any one of [1] to [3], wherein the source gas includes one or more gases selected from the group consisting of nitrogen and a rare gas.

［５］ 反応器と、前記反応器と前記精製塔とを接続するための接続路であって、前記反応器から前記精製塔へ前記原料ガスを導入するための第１接続路と、前記反応器と前記精製塔とを接続するための接続路であって、前記精製塔から導出される前記精製ガスを前記反応器へ戻すための第２接続路と、を更に備える、［１］〜［４］のいずれかに記載の製造装置。   [5] A reactor, a connection path for connecting the reactor and the purification tower, a first connection path for introducing the source gas from the reactor to the purification tower, and the reaction [1] to [1] to [2], a connection path for connecting a reactor to the purification tower, and a second connection path for returning the purified gas led out from the purification tower to the reactor. 4]. The manufacturing apparatus according to any one of 4).

［６］ 原料ガスを、第１領域および第２領域を含む精製塔に導入すること、前記第１領域において、前記原料ガス中の少なくとも水分を吸着除去すること、前記第２領域において、前記第１領域にて水分が吸着除去された前記原料ガス中の少なくとも酸素を除去すること、前記第２領域にて酸素が除去された前記原料ガスを、精製ガスとして導出すること、を含む、精製ガスの製造方法。   [6] Introducing the source gas into a purification tower including the first region and the second region, adsorbing and removing at least moisture in the source gas in the first region, and in the second region, the first region Removing at least oxygen in the source gas from which moisture has been adsorbed and removed in one region, and deriving the source gas from which oxygen has been removed in the second region as a purified gas. Manufacturing method.

［７］ 前記第１領域は、脱湿剤を含み、前記第２領域は、ゲッター剤を含む、［６］に記載の製造方法。   [7] The manufacturing method according to [6], wherein the first region includes a dehumidifying agent and the second region includes a getter agent.

［８］ 前記ゲッター剤は、銅を含む、［７］に記載の製造方法。   [8] The method according to [7], wherein the getter agent includes copper.

［９］ 前記原料ガスは、窒素および希ガスからなる群より選択される一種以上のガスを含む、［６］〜［８］のいずれかに記載の製造方法。   [9] The manufacturing method according to any one of [6] to [8], wherein the source gas includes one or more gases selected from the group consisting of nitrogen and a rare gas.

［１０］ 反応器から導出されたガスを、前記原料ガスとして前記精製塔に導入すること、および、前記精製塔から導出された前記精製ガスを、前記反応器に導入すること、を更に含む、［６］〜［９］のいずれかに記載の製造方法。   [10] The method further includes introducing the gas derived from the reactor into the purification tower as the raw material gas, and introducing the purified gas derived from the purification tower into the reactor. [6] The production method according to any one of [9].

本発明によれば、原料ガスが不純物として少なくとも水分および酸素を含む際に、精製ガス中の水素量の抑制と、機器点数の削減とが両立された精製ガスの製造装置および精製ガスの製造方法を提供することができる。   According to the present invention, when the raw material gas contains at least moisture and oxygen as impurities, the purified gas manufacturing apparatus and the purified gas manufacturing method satisfy both the suppression of the amount of hydrogen in the purified gas and the reduction in the number of equipment. Can be provided.

本発明に係る、精製ガスを製造するための装置構成の一例を示す概略図である。It is the schematic which shows an example of the apparatus structure for manufacturing refined gas based on this invention.

以下、実施の形態を示しながら、本発明について詳細に説明する。   Hereinafter, the present invention will be described in detail with reference to embodiments.

＜精製ガスの製造装置＞
図１は、本発明に係る精製ガスを製造するための装置構成の一例を示す概略図である。精製ガスの製造装置１００は、原料ガス中の少なくとも水分および酸素を除去し、精製ガスを得るための精製塔（第１精製塔１および第２精製塔２）を備える。精製塔は、第１領域（１Ａ,２Ａ）および第２領域（１Ｂ,２Ｂ）を含む。第１領域（１Ａ,２Ａ）は、原料ガス中の少なくとも水分を吸着除去するための領域である。第２領域（１Ｂ,２Ｂ）は、第１領域（１Ａ,２Ａ）を経た原料ガス中の少なくとも酸素を除去し、精製ガスを得るための領域である。 <Purified gas production equipment>
FIG. 1 is a schematic view showing an example of the configuration of an apparatus for producing purified gas according to the present invention. The purified gas production apparatus 100 includes purification towers (first purification tower 1 and second purification tower 2) for removing at least moisture and oxygen in the raw material gas and obtaining purified gas. The purification tower includes a first region (1A, 2A) and a second region (1B, 2B). The first region (1A, 2A) is a region for adsorbing and removing at least moisture in the source gas. The second region (1B, 2B) is a region for removing the at least oxygen in the raw material gas that has passed through the first region (1A, 2A) to obtain a purified gas.

図１においては精製塔が２塔の例が示されているが、精製塔は１塔であってもよいし、３塔以上であってもよい。精製塔を連続運転する観点からは、精製塔は２塔以上であることが望ましい。たとえば図１に示すように製造装置１００が第１精製塔１と第２精製塔２とを含む場合、第１精製塔１を精製ガスの製造に使用し、第２精製塔２を後述する再生ガスにて再生することができる。第２精製塔２が再生されれば、第２精製塔２を精製ガスの製造に使用し、第１精製塔１を後述する再生ガスにて再生することができる。すなわち、精製ガスの製造を連続して行うことができる。なお、以下の説明では、精製塔として第１精製塔１が説明される。   Although FIG. 1 shows an example of two purification towers, the purification tower may be one tower or three or more towers. From the viewpoint of continuously operating the purification tower, it is desirable that the purification tower is two or more. For example, as shown in FIG. 1, when the production apparatus 100 includes a first purification tower 1 and a second purification tower 2, the first purification tower 1 is used for producing purified gas, and the second purification tower 2 is regenerated as described later. It can be regenerated with gas. If the 2nd purification tower 2 is regenerated, the 2nd purification tower 2 can be used for manufacture of purified gas, and the 1st purification tower 1 can be regenerated with regeneration gas mentioned below. That is, it is possible to continuously produce purified gas. In the following description, the first purification tower 1 is described as a purification tower.

＜精製塔＞
第１精製塔１は、第１領域１Ａおよび第２領域１Ｂを含む。第１領域１Ａは、原料ガス中の少なくとも水分を吸着除去するための領域である。第２領域１Ｂは、第１領域１Ａを経た原料ガス中の少なくとも酸素を除去し、精製ガスを得るための領域である。 <Purification tower>
The first purification tower 1 includes a first region 1A and a second region 1B. The first region 1A is a region for adsorbing and removing at least moisture in the source gas. The second region 1B is a region for obtaining purified gas by removing at least oxygen in the raw material gas that has passed through the first region 1A.

《原料ガス》
原料ガスは、不純物として少なくとも水分および酸素を含む。原料ガスは、主成分として、たとえば窒素（Ｎ２）および希ガス等を含んでもよい。本明細書において「主成分」とは、原料ガスを構成する成分（ガス）のうち、最も体積含有量が多い成分（ガス）を意味し、「希ガス」とは、ヘリウム（Ｈｅ）、ネオン（Ｎｅ）、アルゴン（Ａｒ）、クリプトン（Ｋｒ）、およびキセノン（Ｘｅ）のいずれかを示す。原料ガスは、上記のガスを複数含んでもよい。 《Raw material gas》
The source gas contains at least moisture and oxygen as impurities. The source gas may contain, for example, nitrogen (N 2 ) and a rare gas as main components. In this specification, “main component” means a component (gas) having the largest volume content among components (gas) constituting the source gas, and “rare gas” means helium (He), neon. One of (Ne), argon (Ar), krypton (Kr), and xenon (Xe) is shown. The source gas may include a plurality of the above gases.

《第１領域》
第１領域１Ａは、原料ガス中の少なくとも水分を吸着するための領域である。第１領域１Ａは、脱湿剤を含むことが望ましい。第１領域１Ａが脱湿剤を含むことにより、原料ガス中の少なくとも水分がより効果的に吸着されるものと考えられる。 << First area >>
The first region 1A is a region for adsorbing at least moisture in the source gas. The first region 1A preferably includes a dehumidifying agent. It is considered that at least moisture in the raw material gas is more effectively adsorbed by the first region 1A containing the dehumidifying agent.

脱湿剤は、原料ガス中の少なくとも水分を吸着できる剤であればよい。脱湿剤は特に制限されるべきではない。脱湿剤は、たとえばアルミナゲルや合成ゼオライト（モレキュラシーブス）等であってもよい。たとえばアルミナゲルと合成ゼオライト（モレキュラシーブス）とを組み合わせて脱湿剤として用いてもよい。   The dehumidifying agent may be any agent that can adsorb at least water in the raw material gas. The dehumidifying agent should not be particularly limited. The dehumidifying agent may be, for example, alumina gel or synthetic zeolite (Molecular Sieves). For example, alumina gel and synthetic zeolite (Molecular Sieves) may be used in combination as a dehumidifying agent.

《第２領域》
第２領域１Ｂは、第１領域１Ａを経た原料ガス中の少なくとも酸素を除去し、精製ガスを得るための領域である。第２領域１Ｂは、ゲッター剤を含むことが望ましい。第２領域１Ｂがゲッター剤を含むことにより、第１領域１Ａを経た原料ガス中の酸素がより効果的に除去されるものと考えられる。また、第１領域１Ａにおいて原料ガス中の水分が吸着除去されているため、第２領域１Ｂがゲッター剤を含んでいても、精製ガス中に微量の水素が含まれることが抑制されると期待される。 << Second area >>
The second region 1B is a region for obtaining purified gas by removing at least oxygen in the raw material gas that has passed through the first region 1A. The second region 1B preferably contains a getter agent. By including the getter agent in the second region 1B, it is considered that oxygen in the source gas that has passed through the first region 1A is more effectively removed. In addition, since moisture in the raw material gas is adsorbed and removed in the first region 1A, it is expected that even if the second region 1B contains a getter agent, a trace amount of hydrogen is suppressed in the purified gas. Is done.

本明細書において「ゲッター剤」とは、原料ガスから少なくとも酸素を除去する作用を有する物質を示す。ゲッター剤は特に制限されるべきではない。原料ガスから少なくとも酸素を除去する作用を有し得る物質は、ゲッター剤として用い得る。ゲッター剤は、たとえばシリカ、アルミナ、ゼオライト、活性炭等の担体に銅等の金属が担持されたものであり得る。すなわち、ゲッター剤は銅を含んでもよい。銅は安価で入手しやすいため、精製ガスの製造装置１００のランニングコストが低減され得ると期待される。ゲッター剤が銅を含む場合、下記式（１）の反応により酸素が除去されると考えられる。   In this specification, the “getter agent” refers to a substance having an action of removing at least oxygen from a source gas. The getter agent should not be particularly limited. A substance capable of removing at least oxygen from the source gas can be used as a getter agent. The getter agent may be one in which a metal such as copper is supported on a carrier such as silica, alumina, zeolite, or activated carbon. That is, the getter agent may contain copper. Since copper is inexpensive and easily available, it is expected that the running cost of the purified gas production apparatus 100 can be reduced. When a getter agent contains copper, it is thought that oxygen is removed by reaction of following formula (1).

［式１］
２Ｃｕ＋Ｏ２ → ２ＣｕＯ ・・・（１） [Formula 1]
2Cu + O 2 → 2CuO (1)

ゲッター剤が銅を含む場合、たとえば１５０℃程度の加熱条件下で水素とゲッター剤とを反応させることにより、下記式（２）の反応により銅が還元されると考えられる。すなわち、ゲッター剤を再生することができる。再生されたゲッター剤は、再度原料ガスから少なくとも酸素を除去するために用い得る。   When the getter agent contains copper, for example, it is considered that copper is reduced by the reaction of the following formula (2) by reacting hydrogen with the getter agent under heating conditions of about 150 ° C. That is, the getter agent can be regenerated. The regenerated getter agent can be used again to remove at least oxygen from the source gas.

［式２］
ＣｕＯ＋Ｈ２ → Ｃｕ＋Ｈ２Ｏ ・・・（２） [Formula 2]
CuO + H 2 → Cu + H 2 O (2)

《その他の構成１》
原料ガスは、反応器（図示せず）より導入されるガスであってもよい。また、精製ガスは、反応器（図示せず）に導出されるガスであってもよい。すなわち本発明に係る精製ガスの製造装置１００は、反応器と第１精製塔１とを接続するための接続路であって、反応器から第１精製塔１へ原料ガスを導入するための第１接続路（図示せず）を有してもよい。また、反応器（図示せず）と第１精製塔１とを接続するための接続路であって、第１精製塔１から導出される精製ガスを反応器（図示せず）へ戻すための第２接続路（図示せず）を更に有してもよい。 <Other configuration 1>
The source gas may be a gas introduced from a reactor (not shown). The purified gas may be a gas led out to a reactor (not shown). That is, the purified gas production apparatus 100 according to the present invention is a connection path for connecting the reactor and the first purification tower 1, and is the first for introducing the raw material gas from the reactor to the first purification tower 1. One connection path (not shown) may be provided. Further, it is a connection path for connecting a reactor (not shown) and the first purification column 1 for returning the purified gas derived from the first purification column 1 to the reactor (not shown). You may further have a 2nd connection path (not shown).

《その他の構成２》
本発明に係る精製ガスの製造装置１００は、第１領域１Ａおよび第２領域１Ｂを再生するための再生ガスを供給するための、再生ガス供給路Ｌ１を含むことが望ましい。再生ガスは、加熱された窒素、および水素を含むことが望ましい。加熱された窒素により、第１領域１Ａが再生され得る。水素により、第２領域１Ｂが再生され得る。精製ガスの製造装置１００は、窒素を加熱するためのヒータ６０を備えることが望ましい。水素は、加熱された窒素と混合され、昇温され得る。 <Other configuration 2>
The purified gas production apparatus 100 according to the present invention preferably includes a regeneration gas supply path L1 for supplying regeneration gas for regenerating the first region 1A and the second region 1B. The regeneration gas preferably includes heated nitrogen and hydrogen. The first region 1A can be regenerated by the heated nitrogen. The second region 1B can be regenerated by hydrogen. The purified gas production apparatus 100 preferably includes a heater 60 for heating nitrogen. Hydrogen can be mixed with heated nitrogen and heated.

＜精製ガスの製造方法＞
本発明に係る精製ガスの製造方法は、原料ガスを第１領域および第２領域を含む精製塔に導入すること（原料ガス導入工程）を含む。第１領域において、原料ガス中の少なくとも水分が吸着除去される（水分吸着除去工程）。第２領域において、第１領域にて水分が吸着除去された原料ガス中の少なくとも酸素が除去される（酸素除去工程）。第２領域にて酸素が除去された原料ガスは、精製ガスとして導出される（精製ガス導出工程）。以下図１を参照して、第１精製塔１が使用されていると仮定し、精製ガスの製造方法の各工程について説明する。 <Production method of purified gas>
The method for producing purified gas according to the present invention includes introducing a source gas into a purification tower including a first region and a second region (source gas introduction step). In the first region, at least water in the source gas is adsorbed and removed (moisture adsorption removal step). In the second region, at least oxygen in the source gas from which moisture has been removed by adsorption in the first region is removed (oxygen removal step). The source gas from which oxygen has been removed in the second region is derived as a purified gas (purified gas deriving step). Hereinafter, with reference to FIG. 1, assuming that the first purification tower 1 is used, each step of the method for producing purified gas will be described.

《原料ガス導入工程》
本工程は、原料ガスを第１領域１Ａおよび第２領域１Ｂを含む第１精製塔１に導入する工程である。原料ガスは、少なくとも水分および酸素を含む限り、特に限定されない。原料ガスは、主成分として、たとえば窒素および希ガス等を含んでもよい。主成分および希ガスの定義は、上述の通りである。原料ガスは、反応器（図示せず）から導出されるガスであってもよい。原料ガスは、昇圧機（図示せず）により所定の圧力まで昇圧されてから第１精製塔１に導入されてもよい。原料ガスは、減圧弁（図示せず）により所定の圧力まで減圧されてから第１精製塔１に導入されてもよい。 <Raw material gas introduction process>
This step is a step of introducing the source gas into the first purification tower 1 including the first region 1A and the second region 1B. The source gas is not particularly limited as long as it contains at least moisture and oxygen. The source gas may contain, for example, nitrogen and a rare gas as main components. The definitions of the main component and the rare gas are as described above. The source gas may be a gas derived from a reactor (not shown). The source gas may be introduced into the first purification tower 1 after being boosted to a predetermined pressure by a booster (not shown). The source gas may be introduced into the first purification column 1 after being reduced in pressure to a predetermined pressure by a pressure reducing valve (not shown).

《水分吸着除去工程》
本工程は、第１領域１Ａにおいて原料ガス導入工程により導入された原料ガス中の少なくとも水分を吸着除去する工程である。原料ガス中の水分は、たとえば第１領域１Ａに含まれる脱湿剤により吸着除去され得る。用い得る脱湿剤は、上述の通りである。本工程は、たとえば０．１ＭａＧ以上０．９ＭＰａＧ以下の圧力で行われてもよく、たとえば１０℃以上４０℃以下の温度で行われてもよい。 《Moisture adsorption removal process》
This step is a step of adsorbing and removing at least moisture in the source gas introduced by the source gas introduction step in the first region 1A. The moisture in the source gas can be removed by adsorption with, for example, a dehumidifying agent contained in the first region 1A. Dehumidifying agents that can be used are as described above. This step may be performed, for example, at a pressure of 0.1 MaG or more and 0.9 MPaG or less, for example, a temperature of 10 ° C. or more and 40 ° C. or less.

《酸素除去工程》
本工程は、第１領域１Ａにて水分が吸着除去された原料ガス中の少なくとも酸素を第２領域１Ｂにおいて除去する工程である。原料ガス中の酸素は、たとえば第２領域１Ｂに含まれるゲッター剤により除去され得る。用い得るゲッター剤およびゲッター剤による酸素除去のメカニズムは、上述の通りである。水分が吸着除去された原料ガス中の少なくとも酸素が除去されることにより、精製ガスが製造される。また、水分吸着除去工程において原料ガス中の水分が吸着除去されているため、ゲッター剤を用いた精製ガスの製造の際に、精製ガス中に微量の水素が含まれることが抑制されると期待される。 <Oxygen removal process>
This step is a step of removing at least oxygen in the source gas from which moisture has been adsorbed and removed in the first region 1A in the second region 1B. Oxygen in the source gas can be removed, for example, by a getter agent contained in the second region 1B. The getter agent that can be used and the mechanism of oxygen removal by the getter agent are as described above. Purified gas is produced by removing at least oxygen in the raw material gas from which moisture has been adsorbed and removed. In addition, since moisture in the raw material gas is adsorbed and removed in the moisture adsorption and removal process, it is expected that a small amount of hydrogen will be contained in the purified gas when producing purified gas using a getter agent. Is done.

本工程は、たとえば０．１ＭａＧ以上０．９ＭＰａＧ以下の圧力で行われてもよく、たとえば１０℃以上４０℃以下の温度で行われてもよい。すなわち、水分吸着除去工程と酸素除去工程とは、同一の圧力および温度条件で行い得る。水分吸着除去工程から酸素除去工程に移行する際に圧力調整手段や温度調整手段を要しないため、機器点数の削減が期待される。   This step may be performed, for example, at a pressure of 0.1 MaG or more and 0.9 MPaG or less, for example, a temperature of 10 ° C. or more and 40 ° C. or less. That is, the moisture adsorption removal step and the oxygen removal step can be performed under the same pressure and temperature conditions. Since no pressure adjusting means or temperature adjusting means is required when shifting from the moisture adsorption removing process to the oxygen removing process, a reduction in the number of equipment is expected.

《精製ガス導出工程》
本工程は、酸素除去工程により製造された精製ガスを導出する工程である。精製ガスは、要求される使用圧力に応じて昇圧機（図示せず）により所定の圧力まで昇圧されてもよい。精製ガスは、要求される使用圧力に応じて減圧弁（図示せず）により所定の圧力まで減圧されてもよい。精製ガスは、たとえば反応器に導入されてもよい。 《Purified gas derivation process》
This step is a step of deriving the purified gas produced by the oxygen removal step. The purified gas may be pressurized to a predetermined pressure by a booster (not shown) according to the required working pressure. The purified gas may be depressurized to a predetermined pressure by a pressure reducing valve (not shown) according to the required working pressure. The purified gas may be introduced into the reactor, for example.

＜精製塔の再生方法＞
第１精製塔１および第２精製塔２は、再生ガスにより再生し得る。以下、第２精製塔２の再生方法について説明する。第２精製塔２の再生方法は、脱圧工程、加熱工程、加熱再生工程、冷却工程、パージ工程、復圧工程、および両塔運転工程を含むことが望ましい。以下、各工程について説明する。第２精製塔２の再生で操作するバルブはＶ２１〜Ｖ２５、Ｖ６０、およびＶ６１である。なお、第１精製塔１のバルブは、Ｖ１１およびＶ１５が開（ＯＰＥＮ）とされ、Ｖ１２〜Ｖ１４が閉（ＣＬＯＳＥ）とされている。 <Regeneration method of purification tower>
The first purification tower 1 and the second purification tower 2 can be regenerated with a regeneration gas. Hereinafter, a method for regenerating the second purification tower 2 will be described. The regeneration method of the second purification tower 2 desirably includes a depressurization step, a heating step, a heating regeneration step, a cooling step, a purge step, a pressure reduction step, and a both-column operation step. Hereinafter, each step will be described. The valves operated in the regeneration of the second purification tower 2 are V21 to V25, V60, and V61. In addition, as for the valve | bulb of the 1st refinement | purification tower 1, V11 and V15 are open (OPEN), and V12-V14 are closed (CLOSE).

《脱圧工程》
本工程は、Ｖ２４を開とし、その他のバルブを閉とすることにより、第２精製塔２内のガスをベントに放出し、第２精製塔２内の圧力を大気圧近くまで脱圧する工程である。第２精製塔２が大気圧近くまで脱圧されることにより、第１領域２Ａに吸着された水分の脱着が容易になることに加え、後述の工程において再生ガスを第２精製塔２に導入する際に、再生ガスの昇圧手段を省略し得る。たとえば、第２精製塔２内の圧力が略大気圧に達するまでを脱圧工程としてもよい。 《Decompression process》
This step is a step of releasing the gas in the second purification tower 2 to the vent and depressurizing the pressure in the second purification tower 2 to near atmospheric pressure by opening V24 and closing other valves. is there. By depressurizing the second purification column 2 to near atmospheric pressure, it becomes easy to desorb moisture adsorbed in the first region 2A, and in addition, a regeneration gas is introduced into the second purification column 2 in a process described later. In doing so, the boosting means for the regeneration gas can be omitted. For example, the depressurization step may be performed until the pressure in the second purification column 2 reaches substantially atmospheric pressure.

《加熱工程》
本工程は、脱圧工程の後に行われる工程である。本工程においては、Ｖ２３、Ｖ２４、およびＶ６０を開とし、その他のバルブを閉とし、ヒータ６０により加熱された窒素ガスを第２精製塔２に流通させ、第２精製塔２を加熱する工程である。ヒータ６０出口の窒素ガスの温度は、たとえば１２０℃以上２２０℃以下であってもよい。たとえば、第１領域２Ａおよび第２領域２Ｂの温度が約１２０℃〜２２０℃に達するまでを加熱工程としてもよい。 《Heating process》
This step is a step performed after the depressurization step. In this step, V23, V24, and V60 are opened, the other valves are closed, the nitrogen gas heated by the heater 60 is circulated through the second purification tower 2, and the second purification tower 2 is heated. is there. The temperature of the nitrogen gas at the outlet of the heater 60 may be, for example, 120 ° C. or higher and 220 ° C. or lower. For example, the heating process may be performed until the temperature of the first region 2A and the second region 2B reaches about 120 ° C to 220 ° C.

《加熱再生工程》
本工程は、加熱工程の後に行われる工程である。本工程においては、Ｖ２３、Ｖ２４、Ｖ６０、およびＶ６１を開とし、その他のバルブを閉とし、ヒータ６０により加熱された窒素ガス、および水素ガス（すなわち、再生ガス）を第２精製塔２に流通させ、第１領域２Ａおよび第２領域２Ｂを再生する工程である。本工程中の第１領域２Ａおよび第２領域２Ｂの温度は、約１２０℃〜２２０℃に保たれることが望ましい。ヒータ６０により加熱された窒素ガスにより、第１領域２Ａが再生されると考えられる。Ｖ６１を介して導入された水素ガスにより、第２領域２Ｂが再生されると考えられる。たとえば、再生ガスを第２精製塔２に導入してから０．５時間〜３時間が経過するまでを加熱再生工程としてもよい。加熱再生工程に要する時間は、原料ガス中の水分量、原料ガス中の酸素量、第２精製塔２の容量、および再生ガスの温度等に応じて適宜調整され得る。 《Heating regeneration process》
This step is a step performed after the heating step. In this step, V23, V24, V60, and V61 are opened, the other valves are closed, and nitrogen gas and hydrogen gas (that is, regeneration gas) heated by the heater 60 are circulated to the second purification tower 2. And regenerating the first region 2A and the second region 2B. It is desirable that the temperature of the first region 2A and the second region 2B during this step be maintained at about 120 ° C to 220 ° C. It is considered that the first region 2A is regenerated by the nitrogen gas heated by the heater 60. It is considered that the second region 2B is regenerated by the hydrogen gas introduced through V61. For example, the heating regeneration process may be performed until 0.5 hours to 3 hours have elapsed after the regeneration gas is introduced into the second purification tower 2. The time required for the heating regeneration step can be appropriately adjusted according to the amount of water in the source gas, the amount of oxygen in the source gas, the capacity of the second purification tower 2, the temperature of the regeneration gas, and the like.

《冷却工程》
本工程は、加熱再生工程の後に行われる工程である。本工程においては、Ｖ２３、Ｖ２４、およびＶ６０を開とし、その他のバルブを閉とし、常温の窒素ガスを第２精製塔２に流通させ、第２精製塔２を冷却する工程である。たとえば、第１領域２Ａおよび第２領域２Ｂの温度が常温に達するまでを冷却工程としてもよい。 《Cooling process》
This step is a step performed after the heating regeneration step. In this step, V23, V24, and V60 are opened, other valves are closed, nitrogen gas at room temperature is circulated through the second purification tower 2, and the second purification tower 2 is cooled. For example, the cooling process may be performed until the temperatures of the first region 2A and the second region 2B reach room temperature.

《パージ工程》
本工程は、冷却工程の後に行われる工程である。本工程においては、Ｖ２２およびＶ２４を開とし、その他のバルブを閉とし、精製ガスを第１精製塔１から第２精製塔２に導入し、第２精製塔２を精製ガスにてパージする工程である。たとえば、精製ガスによる第２精製塔２のパージを開始してから５分〜２０分が経過するまでをパージ工程としてもよい。パージ工程に要する時間は、第２精製塔２の容量により適宜調整され得る。 << Purge process >>
This step is a step performed after the cooling step. In this step, V22 and V24 are opened, other valves are closed, purified gas is introduced from the first purification column 1 to the second purification column 2, and the second purification column 2 is purged with the purified gas. It is. For example, the purge process may be performed until 5 to 20 minutes have elapsed after the purge of the second purification tower 2 with the purified gas is started. The time required for the purge step can be appropriately adjusted depending on the capacity of the second purification column 2.

《復圧工程》
本工程は、パージ工程の後に行われる工程である。本工程においては、Ｖ２２を開とし、その他のバルブを閉とし、精製ガスを第１精製塔１から第２精製塔２に導入し、第２精製塔２を昇圧する工程である。たとえば、第２精製塔２の圧力が第２精製塔２の運転圧力に達するまでを復圧工程としてもよい。第２精製塔２の運転圧力は、たとえば０．１ＭａＧ以上０．９ＭＰａＧ以下であってもよい。 《Recompression process》
This step is a step performed after the purge step. In this step, V22 is opened, the other valves are closed, purified gas is introduced from the first purification column 1 to the second purification column 2, and the pressure of the second purification column 2 is increased. For example, the return pressure process may be performed until the pressure of the second purification tower 2 reaches the operating pressure of the second purification tower 2. The operating pressure of the second purification tower 2 may be, for example, 0.1 MaG or more and 0.9 MPaG or less.

《両塔運転工程》
本工程は、復圧工程の後に行われる工程である。本工程においては、Ｖ２１およびＶ２５を開とし、その他のバルブを閉とし、第１精製塔１および第２精製塔２により精製ガスを製造する工程である。本工程は、たとえば５分〜２０分行われてもよい。両塔運転工程を経た後、第２精製塔２を用いた精製ガスの製造が行い得る。第１精製塔１は、前述の脱圧工程、加熱工程、加熱再生工程、冷却工程、パージ工程、復圧工程、および両塔運転工程により再生され得る。 << both tower operation process >>
This step is a step performed after the decompression step. In this step, V21 and V25 are opened, the other valves are closed, and purified gas is produced by the first purification column 1 and the second purification column 2. This step may be performed, for example, for 5 minutes to 20 minutes. After going through both tower operation steps, the purified gas can be produced using the second purification tower 2. The first purification tower 1 can be regenerated by the above-described depressurization process, heating process, heating regeneration process, cooling process, purge process, pressure recovery process, and both tower operation process.

以上のとおり、精製ガスの製造装置１００が２つの精製塔を備えることにより、１塔を原料ガス中の不純物の除去（すなわち、精製ガスの製造）に使用し、その間に他の精製塔を再生することができる。すなわち、精製ガスの製造を連続して行うことができる。以下の表１には、各工程における、Ｖ２１〜Ｖ２５、Ｖ６０、およびＶ６１のポジションが示されている。   As described above, the purified gas production apparatus 100 includes two purification towers, so that one tower is used for removing impurities in the raw material gas (that is, production of the purified gas), and the other purification tower is regenerated in the meantime. can do. That is, it is possible to continuously produce purified gas. Table 1 below shows the positions of V21 to V25, V60, and V61 in each step.

Figure 2019171231
Figure 2019171231

以下、実施例を示して本発明をさらに具体的に説明するが、本発明はこれらの例によって限定されるものではない。   EXAMPLES Hereinafter, although an Example is shown and this invention is demonstrated further more concretely, this invention is not limited by these examples.

＜精製ガスの製造＞
《実施例１》
図１に記載の構成を有する装置が用意された。下記の条件にて主成分としてヘリウムを含有する原料ガス中に含まれる水分および酸素を除去し、精製ガスが製造された。その後、精製ガス中の酸素、水分、および水素量が測定された。なお、［ＮＬ］は、標準状態に換算したガスの体積［Ｌ］を表している。 <Manufacture of purified gas>
Example 1
An apparatus having the configuration shown in FIG. 1 was prepared. Water and oxygen contained in the raw material gas containing helium as a main component was removed under the following conditions, and a purified gas was produced. Thereafter, the amounts of oxygen, moisture, and hydrogen in the purified gas were measured. [NL] represents the gas volume [L] converted to the standard state.

（精製ガスの製造条件）
原料ガス流量：３００ＮＬ／ｍｉｎ、
原料ガス中の酸素濃度：１０ｖｏｌ．ｐｐｍ、
原料ガスの露点：−２０℃、
精製塔吸着圧力：０．２ＭＰａＧ、
精製塔吸着温度：２０℃、
ゲッター剤：［酸化亜鉛：酸化アルミニウム：酸化銅＝約４５：約１２：約４３（質量比）］、
脱湿剤：商品名：「Ｆ−９」（東ソー（株）より入手）。 (Production conditions for purified gas)
Source gas flow rate: 300 NL / min,
Oxygen concentration in source gas: 10 vol. ppm,
Dew point of source gas: -20 ° C
Purification tower adsorption pressure: 0.2 MPaG,
Purification tower adsorption temperature: 20 ° C.
Getter agent: [Zinc oxide: Aluminum oxide: Copper oxide = about 45: about 12: about 43 (mass ratio)]
Dehumidifier: Trade name: “F-9” (obtained from Tosoh Corporation).

（精製ガスの製造）
反応器から導出されたガスが原料ガスとして第１精製塔１に導入された。第１精製塔１内の第１領域１Ａにおいて、原料ガス中の水分が脱湿剤により吸着除去された。第１領域１Ａを経た原料ガスに含まれる酸素が、第２領域１Ｂにおいてゲッター剤により除去された。これにより、精製ガスが製造された。精製ガスは、上記反応器に導入された。 (Production of purified gas)
The gas led out from the reactor was introduced into the first purification tower 1 as a raw material gas. In the first region 1A in the first purification tower 1, moisture in the raw material gas was removed by adsorption with a dehumidifying agent. Oxygen contained in the source gas passed through the first region 1A was removed by the getter agent in the second region 1B. Thereby, purified gas was produced. Purified gas was introduced into the reactor.

《実施例２〜実施例９》
下記表１に示されるように、原料ガスの主成分、原料ガス中の酸素濃度、および原料ガスの露点等が変更されたことを除いては、実施例１と同様に精製ガスが製造された。なお、実施例３〜実施例６においては、シミュレーション値である。当該シミュレーション値と実機において採取されるデータとは、ほぼ一致するものと考えられる。 << Examples 2 to 9 >>
As shown in Table 1 below, a purified gas was produced in the same manner as in Example 1 except that the main component of the source gas, the oxygen concentration in the source gas, the dew point of the source gas, and the like were changed. . In Example 3 to Example 6, it is a simulation value. It is considered that the simulation value and the data collected in the actual machine almost coincide.

《比較例１》
図１に示される第１精製塔１において、第１領域１Ａと第２領域１Ｂとが入れ替えられた。反応器から導出されたガスが原料ガスとして第１精製塔１に導入された。第１精製塔１内の第２領域１Ｂにおいて、原料ガス中の酸素がゲッター剤により除去された。第２領域１Ｂを経た原料ガスに含まれる水分が、第１領域１Ａにおいて脱湿剤により吸着除去された。これにより、精製ガスが製造された。 << Comparative Example 1 >>
In the 1st refinement | purification tower 1 shown by FIG. 1, 1st area | region 1A and 2nd area | region 1B were replaced. The gas derived from the reactor was introduced into the first purification tower 1 as a raw material gas. In the second region 1B in the first purification tower 1, oxygen in the source gas was removed by the getter agent. Moisture contained in the source gas that has passed through the second region 1B was adsorbed and removed by the dehumidifying agent in the first region 1A. Thereby, purified gas was produced.

＜評価＞
各実施例および各比較例において製造された精製ガスに含まれる酸素、水分、および水素量が、ガスクロマトグラフィー（商品名：「ＧＣ２０１４ＡＴＦ」（（株）島津製作所より入手）により測定された。結果は以下の表２に示されている。 <Evaluation>
The amounts of oxygen, moisture, and hydrogen contained in the purified gas produced in each example and each comparative example were measured by gas chromatography (trade name: “GC2014ATF” (obtained from Shimadzu Corporation). Is shown in Table 2 below.

Figure 2019171231
Figure 2019171231

＜結果＞
上記表２に示されるように、実施例は精製ガス中の水素量が０．１ｖｏｌ．ｐｐｍ以下に抑制されていた。対して、比較例１においては精製ガス中の水素量が０．５ｖｏｌ．ｐｐｍという高い値であった。すなわち、原料ガス中の少なくとも水分を吸着除去するための領域である第１領域と、第１領域を経た原料ガス中の少なくとも酸素を除去し精製ガスを得るための第２領域とを含む精製塔を備えた製造装置により製造された精製ガスは、水素含有量が抑制されていることが示された。 <Result>
As shown in Table 2 above, in the examples, the amount of hydrogen in the purified gas was 0.1 vol. It was suppressed to ppm or less. On the other hand, in Comparative Example 1, the amount of hydrogen in the purified gas was 0.5 vol. The value was as high as ppm. That is, a purification tower including a first region that is a region for removing at least moisture in the source gas by adsorption, and a second region for removing at least oxygen in the source gas that has passed through the first region to obtain a purified gas. It was shown that the purified gas produced by the production apparatus equipped with the hydrogen content is suppressed.

本発明においては、１つの精製塔内に第１領域と第２領域とが含まれている。そのため、少なくとも２塔の精製塔があれば、連続運転を行い得る。また、第１領域と第２領域との間に冷却手段を設けることを要しなかった。加えて、精製ガス中の水素量が抑制されているため、精製ガス中の水素を除去するための設備も要さないと考えられる。すなわち、原料ガスが不純物として少なくとも水分および酸素を含む際に、精製ガス中の水素量の抑制と、機器点数の削減とが両立された精製ガスの製造装置および精製ガスの製造方法が提供されることが示された。   In the present invention, the first region and the second region are included in one purification tower. Therefore, if there are at least two purification towers, continuous operation can be performed. Moreover, it was not necessary to provide a cooling means between the first region and the second region. In addition, since the amount of hydrogen in the purified gas is suppressed, it is considered that no equipment for removing hydrogen in the purified gas is required. That is, when the raw material gas contains at least moisture and oxygen as impurities, a purified gas manufacturing apparatus and a purified gas manufacturing method are provided, in which both the amount of hydrogen in the purified gas is reduced and the number of equipment is reduced. It was shown that.

実施例の結果から、第１領域は脱湿剤を含み、第２領域はゲッター剤を含んでもよく、ゲッター剤は銅を含んでもよいことが示された。   The results of the examples show that the first region contains a dehumidifying agent, the second region may contain a getter agent, and the getter agent may contain copper.

実施例の結果から、原料ガスは、窒素および希ガスからなる群より選択される一種以上のガスを含んでもよいことが示された。   From the results of Examples, it was shown that the source gas may contain one or more gases selected from the group consisting of nitrogen and rare gases.

実施例の結果から、精製ガスの製造装置は、反応器と、反応器と精製塔とを接続するための接続路であって、反応器から精製塔へ原料ガスを導入するための第１接続路と、反応器と精製塔とを接続するための接続路であって、精製塔から導出される精製ガスを反応器へ戻すための第２接続路とを更に備えてもよいことが示された。   From the results of the examples, the refined gas production apparatus is a connection path for connecting the reactor and the reactor to the purification tower, and the first connection for introducing the raw material gas from the reactor to the purification tower. It is shown that the apparatus may further comprise a connection path for connecting the reactor and the reactor to the purification tower, and a second connection path for returning the purified gas led out from the purification tower to the reactor. It was.

比較例１は、精製ガス中の水素量が実施例と比して多かった。水分および酸素を含む原料ガスをゲッター剤を含む第２領域に導入したため、精製ガス中に微量の水素が含まれたものと考えられる。   In Comparative Example 1, the amount of hydrogen in the purified gas was larger than that in Examples. Since the source gas containing moisture and oxygen was introduced into the second region containing the getter agent, it is considered that a small amount of hydrogen was contained in the purified gas.

今回開示された実施例および実施形態はすべての点で例示であって制限的なものではない。特許請求の範囲の記載によって確定される技術的範囲は、特許請求の範囲と均等の意味および範囲内でのすべての変更を含む。   The examples and embodiments disclosed herein are illustrative and non-restrictive in every respect. The technical scope defined by the description of the scope of claims includes all modifications within the meaning and scope equivalent to the scope of claims.

１ 第１精製塔、２ 第２精製塔、６０ ヒータ、１Ａ，２Ａ 第１領域、１Ｂ，２Ｂ 第２領域、Ｖ１１，Ｖ１２，Ｖ１３，Ｖ１４，Ｖ１５，Ｖ２１，Ｖ２２，Ｖ２３，Ｖ２４，Ｖ２５，Ｖ６０，Ｖ６１ バルブ。   1 1st refining tower, 2nd refining tower, 60 heater, 1A, 2A 1st area, 1B, 2B 2nd area, V11, V12, V13, V14, V15, V21, V22, V23, V24, V25, V60 , V61 valve.

Claims (10)

原料ガス中の少なくとも水分および酸素を除去し、精製ガスを得るための精製塔を備え、
前記精製塔は、第１領域および第２領域を含み、
前記第１領域は、前記原料ガス中の少なくとも水分を吸着除去するための領域であり、
前記第２領域は、前記第１領域を経た前記原料ガス中の少なくとも酸素を除去し、精製ガスを得るための領域である、
精製ガスの製造装置。 A purification tower for removing at least moisture and oxygen in the raw material gas and obtaining a purified gas is provided,
The purification tower includes a first region and a second region,
The first region is a region for adsorbing and removing at least moisture in the source gas,
The second region is a region for obtaining purified gas by removing at least oxygen in the source gas that has passed through the first region.
Purified gas production equipment. 前記第１領域は、脱湿剤を含み、
前記第２領域は、ゲッター剤を含む、
請求項１に記載の製造装置。 The first region includes a dehumidifying agent;
The second region includes a getter agent.
The manufacturing apparatus according to claim 1. 前記ゲッター剤は、銅を含む、請求項２に記載の製造装置。   The manufacturing apparatus according to claim 2, wherein the getter agent contains copper. 前記原料ガスは、窒素および希ガスからなる群より選択される一種以上のガスを含む、請求項１〜請求項３のいずれか１項に記載の製造装置。   The said raw material gas is a manufacturing apparatus of any one of Claims 1-3 containing 1 or more types of gas selected from the group which consists of nitrogen and a noble gas. 反応器と、
前記反応器と前記精製塔とを接続するための接続路であって、前記反応器から前記精製塔へ前記原料ガスを導入するための第１接続路と、
前記反応器と前記精製塔とを接続するための接続路であって、前記精製塔から導出される前記精製ガスを前記反応器へ戻すための第２接続路と、を更に備える、
請求項１〜請求項４のいずれか１項に記載の製造装置。 A reactor,
A connection path for connecting the reactor and the purification tower, the first connection path for introducing the raw material gas from the reactor to the purification tower;
A connection path for connecting the reactor and the purification tower, and a second connection path for returning the purified gas led out from the purification tower to the reactor;
The manufacturing apparatus of any one of Claims 1-4. 原料ガスを、第１領域および第２領域を含む精製塔に導入すること、
前記第１領域において、前記原料ガス中の少なくとも水分を吸着除去すること、
前記第２領域において、前記第１領域にて水分が吸着除去された前記原料ガス中の少なくとも酸素を除去すること、
前記第２領域にて酸素が除去された前記原料ガスを、精製ガスとして導出すること、を含む、
精製ガスの製造方法。 Introducing a source gas into a purification tower including a first region and a second region;
Adsorbing and removing at least moisture in the source gas in the first region;
Removing at least oxygen in the source gas from which moisture has been adsorbed and removed in the first region in the second region;
Deriving the source gas from which oxygen has been removed in the second region as a purified gas,
A method for producing purified gas. 前記第１領域は、脱湿剤を含み、
前記第２領域は、ゲッター剤を含む、
請求項６に記載の製造方法。 The first region includes a dehumidifying agent;
The second region includes a getter agent.
The manufacturing method according to claim 6. 前記ゲッター剤は、銅を含む、請求項７に記載の製造方法。   The manufacturing method according to claim 7, wherein the getter agent contains copper. 前記原料ガスは、窒素および希ガスからなる群より選択される一種以上のガスを含む、請求項６〜請求項８のいずれか１項に記載の製造方法。   The manufacturing method according to any one of claims 6 to 8, wherein the source gas includes one or more gases selected from the group consisting of nitrogen and a rare gas. 反応器から導出されたガスを、前記原料ガスとして前記精製塔に導入すること、
および、
前記精製塔から導出された前記精製ガスを、前記反応器に導入すること、
を更に含む、請求項６〜請求項９のいずれか１項に記載の製造方法。 Introducing the gas derived from the reactor into the purification tower as the source gas,
and,
Introducing the purified gas derived from the purification tower into the reactor;
The manufacturing method according to any one of claims 6 to 9, further comprising:
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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59107910A (en) * 1982-12-10 1984-06-22 Toshiba Corp Method for purifying gaseous argon
JPH054809A (en) * 1990-09-14 1993-01-14 Japan Pionics Co Ltd Purification of pare gas
JPH0731877A (en) * 1993-05-11 1995-02-03 Japan Pionics Co Ltd Refining of inert gas and device therefor
JPH08252431A (en) * 1995-01-20 1996-10-01 Sinco Eng Spa Method for purifying inert gas containing impurity generated from organic compound
JP2000233909A (en) * 1999-02-10 2000-08-29 Kyodo Oxygen Co Ltd Method for refining waste argon gas from single crystal producing furnace
JP2004149393A (en) * 2002-11-01 2004-05-27 Japan Pionics Co Ltd Method for refining inert gas
JP2008137847A (en) * 2006-12-01 2008-06-19 Air Liquide Japan Ltd Xenon retrieval system and retrieval device
JP2012051753A (en) * 2010-08-31 2012-03-15 Taiyo Nippon Sanso Corp Method and apparatus for purifying gas
JP2012229151A (en) * 2011-04-12 2012-11-22 Sumitomo Seika Chem Co Ltd Method and device for purifying argon gas

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1023471C (en) * 1991-04-29 1994-01-12 四川化工总厂 Process for producing industrial nitrogen
US6099619A (en) * 1997-10-09 2000-08-08 Uop Llc Purification of carbon dioxide
CN201694842U (en) * 2010-06-30 2011-01-05 哈尔滨黎明气体有限公司 High-purity argon depth purification device
CN104694705B (en) * 2015-02-06 2016-08-31 中南大学 A kind of degree of depth device for deoxidizing and application thereof

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59107910A (en) * 1982-12-10 1984-06-22 Toshiba Corp Method for purifying gaseous argon
JPH054809A (en) * 1990-09-14 1993-01-14 Japan Pionics Co Ltd Purification of pare gas
JPH0731877A (en) * 1993-05-11 1995-02-03 Japan Pionics Co Ltd Refining of inert gas and device therefor
JPH08252431A (en) * 1995-01-20 1996-10-01 Sinco Eng Spa Method for purifying inert gas containing impurity generated from organic compound
JP2000233909A (en) * 1999-02-10 2000-08-29 Kyodo Oxygen Co Ltd Method for refining waste argon gas from single crystal producing furnace
JP2004149393A (en) * 2002-11-01 2004-05-27 Japan Pionics Co Ltd Method for refining inert gas
JP2008137847A (en) * 2006-12-01 2008-06-19 Air Liquide Japan Ltd Xenon retrieval system and retrieval device
JP2012051753A (en) * 2010-08-31 2012-03-15 Taiyo Nippon Sanso Corp Method and apparatus for purifying gas
JP2012229151A (en) * 2011-04-12 2012-11-22 Sumitomo Seika Chem Co Ltd Method and device for purifying argon gas

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