WO2019171882A1 - 粗一酸化炭素ガスから酸素を除去する方法、および一酸化炭素ガスの精製方法 - Google Patents

粗一酸化炭素ガスから酸素を除去する方法、および一酸化炭素ガスの精製方法 Download PDF

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Publication number
WO2019171882A1
WO2019171882A1 PCT/JP2019/004705 JP2019004705W WO2019171882A1 WO 2019171882 A1 WO2019171882 A1 WO 2019171882A1 JP 2019004705 W JP2019004705 W JP 2019004705W WO 2019171882 A1 WO2019171882 A1 WO 2019171882A1
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Prior art keywords
carbon monoxide
monoxide gas
oxygen
crude
gas
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PCT/JP2019/004705
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English (en)
French (fr)
Japanese (ja)
Inventor
孝爾 横野
晃裕 桑名
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住友精化株式会社
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Priority to CN201980014954.9A priority Critical patent/CN111770892B/zh
Priority to JP2020504879A priority patent/JP7119064B2/ja
Priority to KR1020207028118A priority patent/KR102596869B1/ko
Publication of WO2019171882A1 publication Critical patent/WO2019171882A1/ja

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
    • B01J21/18—Carbon
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/40—Carbon monoxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0001—Separation or purification processing
    • C01B2210/0009—Physical processing
    • C01B2210/0014—Physical processing by adsorption in solids
    • C01B2210/0015—Physical processing by adsorption in solids characterised by the adsorbent
    • C01B2210/0017—Carbon-based materials
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0045—Oxygen
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B2210/00—Purification or separation of specific gases
    • C01B2210/0043—Impurity removed
    • C01B2210/0051—Carbon dioxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the present invention relates to a method for removing oxygen from crude carbon monoxide gas.
  • the present invention further relates to a method for purifying carbon monoxide gas using such an oxygen removal method.
  • Carbon monoxide is used in a wide range of industries such as chemical synthesis and metal refining. Recently, high-purity carbon monoxide of about 99.995 mol% is used as a cleaning and etching gas in the silicon semiconductor manufacturing process.
  • a general method for producing carbon monoxide a method for obtaining carbon monoxide by proceeding a formic acid dehydration reaction (HCOOH ⁇ H 2 O + CO) using a zeolite-based catalyst modified with a mineral acid is known ( For example, see Patent Documents 1 and 2).
  • the crude carbon monoxide gas obtained by the above reaction contains water, hydrogen, oxygen, nitrogen, methane, carbon dioxide, unreacted formic acid mist, and the like as impurities. By removing these impurities, high-purity carbon monoxide (hereinafter sometimes referred to as “purified carbon monoxide gas”) is obtained.
  • the metal catalyst in the method of converting oxygen into carbon dioxide by reacting oxygen with carbon monoxide using the metal catalyst, a part of the metal catalyst can be mixed into the product carbon monoxide gas. It is known that the mixed metal has a metal carbonyl structure in the product carbon monoxide gas, and the metal carbonyl exists only in a trace amount, and has a great adverse effect in the semiconductor manufacturing process. Therefore, in the production of product carbon monoxide gas, avoidance of mixing of metal components is strongly desired.
  • JP-A-10-007413 Japanese Patent Laid-Open No. 7-33421 Japanese Patent Laid-Open No. 60-161317
  • the present invention has been made under such circumstances. From the crude carbon monoxide gas containing oxygen, the oxygen from the crude carbon monoxide gas is avoided as much as possible while avoiding contamination of the problematic metal. It is a main problem to provide a method for removing. *
  • activated carbon acts as a catalyst for the reaction between oxygen and carbon monoxide by contacting crude carbon monoxide gas containing oxygen with activated carbon, and carbon dioxide is generated.
  • the present invention has been completed.
  • a method for removing oxygen from a crude carbon monoxide gas characterized by contacting the crude carbon monoxide gas containing oxygen with activated carbon not supporting a metal. Is done.
  • the crude carbon monoxide gas and the activated carbon are contacted by introducing the crude carbon monoxide gas into a catalyst tank filled with the activated carbon.
  • the oxygen concentration in the crude carbon monoxide gas is 0.1 to 1000 mol ppm.
  • the contact temperature between the crude carbon monoxide gas and the activated carbon is in the range of 20 to 80 ° C.
  • the contact temperature between the crude carbon monoxide gas and the activated carbon is in the range of 30 to 50 ° C.
  • the oxygen removal step and the carbon dioxide removal step are repeated until the carbon monoxide has a target purity.
  • the carbon monoxide purification apparatus mainly includes a catalyst tank 1 filled with activated carbon 1a and a gas cleaning container 2 containing an alkaline aqueous solution 2a.
  • Crude carbon monoxide gas as a raw material gas is supplied to the catalyst tank 1 through a line 3, and the line 3 is provided with a compressor 4 for pressurizing the crude carbon monoxide gas to a predetermined pressure.
  • a part of oxygen contained as impurities in the crude carbon monoxide gas is converted into carbon dioxide by reaction with carbon monoxide and removed.
  • the product gas discharged from the catalyst tank 1 is sent to the gas cleaning container 2 through the line 5 and further introduced into the alkaline aqueous solution 2 a through the introduction pipe 6.
  • carbon dioxide which is an acidic gas
  • purified carbon monoxide gas is taken out via the line 7.
  • the line 7 is connected to a discharge line 7a and a circulation line 7b, and on-off valves 8 and 9 are provided on these lines 7a and 7b, respectively.
  • Carbon oxide gas is removed.
  • the on-off valve 9 is opened (the on-off valve 8 is closed), and is passed through the circulation line 7b. Insufficient purified carbon monoxide gas is sent back to the catalyst tank 1 for additional oxygen removal. If no pressurization is required, the compressor 4 may be replaced with a blower.
  • Crude carbon monoxide gas as a raw material gas contains carbon monoxide as a main component, oxygen as an impurity, and the like.
  • Crude carbon monoxide gas is, for example, a carbon monoxide gas produced by a formic acid dehydration reaction (HCOOH ⁇ H 2 O + CO) using a zeolite-based catalyst modified with a mineral acid, and then the produced H 2 O and unreacted HCOOH in a condenser. Is obtained by separating from The purity of carbon monoxide as a main component in the crude carbon monoxide gas is, for example, 99.9 mol% or more and less than 100 mol%.
  • the purity of the carbon monoxide in the crude carbon monoxide gas is preferably 99.99 mol% or more and less than 100 mol%.
  • the concentration of oxygen in the crude carbon monoxide gas is preferably 0.1 to 1000 mol ppm. If the oxygen concentration exceeds 1000 mol ppm, oxygen may not be removed and may remain in the purified carbon monoxide gas. From the viewpoint of oxygen removal efficiency, the oxygen concentration in the crude carbon monoxide gas is more preferably 0.1 to 100 mol ppm.
  • the crude carbon monoxide gas may contain, for example, hydrogen, nitrogen, carbon dioxide, and methane as impurities other than oxygen. The concentration of each of these impurities is, for example, about 0.1 to 10 mol ppm.
  • the activated carbon 1a filled in the catalyst tank 1 may be any of plant systems such as coconut shells and wood, and mineral systems such as coal and petroleum.
  • plant systems such as coconut shells and wood
  • mineral systems such as coal and petroleum.
  • shape of the activated carbon any of powder, crushed, columnar, spherical, and honeycomb may be used.
  • the activated carbon 1a filled in the catalyst layer 1 does not carry a metal and exhibits a catalytic function as the activated carbon 1a alone.
  • oxygen contained in the crude carbon monoxide gas reacts with carbon monoxide and is converted to carbon dioxide.
  • the processing amount of the crude carbon monoxide gas in the catalyst tank 1 is, for example, 0.01 to 70 / min in terms of space velocity, and preferably 5 to 50 / min from the viewpoint of oxidation reaction efficiency.
  • the temperature of the catalyst tank 1 filled with the activated carbon 1a (that is, the contact temperature between the crude carbon monoxide gas and the activated carbon) is preferably in the range of 20 to 80 ° C., more preferably 30 to 50 ° C.
  • the pressure of the crude carbon monoxide gas introduced into the catalyst tank 1 filled with activated carbon 1a is, for example, 0.1 to 10 MPa. From the viewpoint of reaction efficiency, it is preferably 9 to 10 MPa.
  • the catalyst tank 1 filled with the activated carbon 1a only needs to maintain the airtightness of the tank when a high-pressure gas is passed, and the shape thereof may be any of a cylindrical shape, a square shape, and a spherical shape.
  • oxygen contained in the crude carbon monoxide gas reacts with carbon monoxide and is converted to carbon dioxide.
  • Carbon dioxide generated by the conversion is removed by distillation or a separation method using a PSA apparatus, or passing through a molecular sieve or an alkaline aqueous solution. From an economical viewpoint, as shown in FIG. 1, washing (absorption) with an alkaline aqueous solution is preferable, and a caustic soda aqueous solution is preferable as the alkaline aqueous solution 2a.
  • High-purity carbon monoxide (product carbon monoxide gas) can be obtained by washing the processing gas obtained after alkali washing with water and then drying the moisture with a molecular sieve.
  • the method according to the present embodiment can remove oxygen contained as impurities while avoiding metal contamination by using a single activated carbon 1a as a catalyst, it can be used in industrial applications such as semiconductor manufacturing processes. Suitable for producing pure carbon monoxide.
  • Example 1 An SUS tube having an inner diameter of 11 cm and a length of 120 cm was filled with 5.2 kg of activated carbon (granular white birch G2X, manufactured by Osaka Gas Chemical Co., Ltd.) to prepare a catalyst tank. Crude carbon monoxide gas (raw gas) compressed to 9.8 MPa was continuously introduced into the catalyst tank at a space velocity of 36.6 / min while maintaining the temperature of the catalyst tank at 20 to 25 ° C. The oxygen concentration in the introduced crude carbon monoxide gas was 1.40 mol ppm, and carbon dioxide was not detected. The oxygen and carbon dioxide concentrations were analyzed by gas chromatography (pulse discharge photoionization detector: PDD).
  • PDD pulse discharge photoionization detector
  • the carbon monoxide gas discharged from the catalyst tank outlet was analyzed to confirm the concentrations of oxygen and carbon dioxide.
  • the oxygen concentration was 1.35 mol ppm and the carbon dioxide concentration was 0.10 mol ppm.
  • Example 2 The experiment was performed in the same manner as in Example 1 except that the temperature of the catalyst tank was changed to 35 to 40 ° C. When the carbon monoxide gas discharged from the catalyst tank was analyzed, the oxygen concentration was 1.00 mol ppm and the carbon dioxide concentration was 0.80 mol ppm.
  • Example 3 An SUS tube having an inner diameter of 1 cm and a length of 30 cm was charged with 10.6 g of activated carbon (granular white birch G2X, manufactured by Osaka Gas Chemical Co., Ltd.) to prepare a catalyst tank. Carbon monoxide gas (raw material gas) compressed to 0.1 MPa was continuously introduced into the catalyst tank at a space velocity of 8.7 / min while maintaining the temperature of the catalyst tank at 40 to 45 ° C. The oxygen concentration in the introduced crude carbon monoxide gas was 25.0 mol ppm, and no carbon dioxide was detected. When carbon monoxide gas discharged from the catalyst tank outlet was analyzed, the oxygen concentration was 23.2 mol ppm and the carbon dioxide concentration was 4.2 mol ppm after 1 hour. After 2 hours, the oxygen concentration was 23.6 mol ppm and the carbon dioxide concentration was 4.7 mol ppm. After two months, the oxygen concentration was 23.4 mol ppm and the carbon dioxide concentration was 4.5 mol ppm.
  • activated carbon granular white bir
  • Example 1 The same experiment as in Example 3 was performed using Al 2 O 3 (manufactured by Sumitomo Chemical Co., Ltd.) instead of the activated carbon in Example 3.
  • the oxygen concentration was 24.5 mol ppm and the carbon dioxide concentration was 0 mol ppm after 1 hour. After 2 hours, the oxygen concentration was 25 mol ppm and the carbon dioxide concentration was 0 mol ppm.
  • Example 1 the oxygen concentration in the crude carbon monoxide gas before treatment in the catalyst tank was 1.40 mol ppm, but the oxygen concentration in the product gas discharged from the catalyst tank was 1.35 mol. Reduced to ppm, 0.10 mol ppm of carbon dioxide was produced. From this, it is understood that the activated carbon in the catalyst tank acts as a catalyst and reacts oxygen and carbon monoxide to generate carbon dioxide. The reason why the oxygen reaction rate is small is that the oxygen concentration is originally very low. The lower the oxygen concentration in the crude carbon monoxide gas, the stronger the tendency of the reaction rate to decrease. Further, even when the reaction rate is low, as described with reference to FIG. 1, the target purity of carbon monoxide gas can be reached by repeating the same oxygen removal step.
  • Example 3 it can be understood that oxygen can be removed by slightly raising the reaction temperature to 40 to 45 ° C. even if the reaction pressure in the catalyst tank is reduced to atmospheric pressure. It is also understood that the catalytic activity of activated carbon does not decrease even if the reaction is continued for 2 months, and it is understood that there is no problem even if it is repeated until the purity of carbon monoxide for the purpose of removing oxygen is achieved. The Further, when Reference Example 1 is compared with Example 3, even if Al 2 O 3 is used under the same reaction conditions as activated carbon, no catalytic action is exhibited, and the catalytic action of activated carbon alone can be confirmed.
  • Catalyst tank 1a Activated carbon
  • Gas cleaning container 2a Alkaline aqueous solution
  • Compressor 7b Circulation line

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Catalysts (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
PCT/JP2019/004705 2018-03-06 2019-02-08 粗一酸化炭素ガスから酸素を除去する方法、および一酸化炭素ガスの精製方法 WO2019171882A1 (ja)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201980014954.9A CN111770892B (zh) 2018-03-06 2019-02-08 从粗一氧化碳气体除去氧的方法和一氧化碳气体的精制方法
JP2020504879A JP7119064B2 (ja) 2018-03-06 2019-02-08 粗一酸化炭素ガスから酸素を除去する方法、および一酸化炭素ガスの精製方法
KR1020207028118A KR102596869B1 (ko) 2018-03-06 2019-02-08 미정제 일산화탄소 가스로부터 산소를 제거하는 방법 및 일산화탄소 가스의 정제 방법

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JP2018-039259 2018-03-06
JP2018039259 2018-03-06

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20230057464A (ko) 2020-10-08 2023-04-28 가부시끼가이샤 레조낙 산소 분자의 제거 방법 및 일산화탄소의 정제 방법

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JPH02189389A (ja) * 1989-01-18 1990-07-25 Kawasaki Steel Corp 一酸化炭素を主成分とするガスの精製方法
JP2000034115A (ja) * 1998-07-21 2000-02-02 Sumitomo Seika Chem Co Ltd 高純度一酸化炭素の製造方法

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JPS63251496A (ja) * 1987-04-08 1988-10-18 Kawasaki Steel Corp 一酸化炭素を主成分とするガスの精製方法
JPH02189389A (ja) * 1989-01-18 1990-07-25 Kawasaki Steel Corp 一酸化炭素を主成分とするガスの精製方法
JP2000034115A (ja) * 1998-07-21 2000-02-02 Sumitomo Seika Chem Co Ltd 高純度一酸化炭素の製造方法

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20230057464A (ko) 2020-10-08 2023-04-28 가부시끼가이샤 레조낙 산소 분자의 제거 방법 및 일산화탄소의 정제 방법

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JPWO2019171882A1 (ja) 2021-02-18
KR20200127225A (ko) 2020-11-10
CN111770892A (zh) 2020-10-13
CN111770892B (zh) 2023-06-30
KR102596869B1 (ko) 2023-11-02
TW201938487A (zh) 2019-10-01
JP7119064B2 (ja) 2022-08-16

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