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WO2021085422A1 - Appareil de production de monoxyde de carbone, installation chimique et installation - Google Patents

Appareil de production de monoxyde de carbone, installation chimique et installation Download PDF

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Publication number
WO2021085422A1
WO2021085422A1 PCT/JP2020/040279 JP2020040279W WO2021085422A1 WO 2021085422 A1 WO2021085422 A1 WO 2021085422A1 JP 2020040279 W JP2020040279 W JP 2020040279W WO 2021085422 A1 WO2021085422 A1 WO 2021085422A1
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WIPO (PCT)
Prior art keywords
carbon monoxide
production apparatus
monoxide production
containing gas
gas
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.)
Ceased
Application number
PCT/JP2020/040279
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English (en)
Japanese (ja)
Inventor
晃平 吉川
杉政　昌俊
篤 宇根本
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.)
Hitachi Ltd
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Hitachi Ltd
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Filing date
Publication date
Application filed by Hitachi Ltd filed Critical Hitachi Ltd
Publication of WO2021085422A1 publication Critical patent/WO2021085422A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16—Alumino-silicates
    • B01J20/18—Synthetic zeolitic molecular sieves
    • 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
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • 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
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • 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

Definitions

  • the present invention relates to a carbon monoxide production apparatus, a chemical plant and a plant.
  • Patent Document 1 describes a catalyst and a CO production method for obtaining CO from a gas containing CH 4 and other hydrocarbons at 700 ° C. to 800 ° C. using a catalyst containing ruthenium as an active ingredient.
  • Patent Document 2 uses a catalyst containing a carbonate of Ca, Sr, Ba and a composite oxide of Ti, Al, Zr, Fe, W, and Mo as active components, and CO is subjected to a reverse shift reaction at a temperature of 700 ° C. or higher.
  • a catalyst for obtaining CO and a method for producing CO are described.
  • the present invention has been made in view of the above problems, and an object of the present invention is to provide a carbon monoxide production apparatus, a chemical plant, and a plant having a high CO production rate at a low temperature.
  • the carbon monoxide production apparatus includes a convertible reverse shift catalyst to a gas comprising CO and H 2 O gas containing CO 2 and H 2, of H 2 O adsorbed It is characterized by comprising a reaction vessel having an adsorbent.
  • Carbon monoxide production equipment according to a comparative example Carbon monoxide production apparatus according to Example 1. Carbon monoxide production apparatus according to Example 2. Carbon monoxide production apparatus according to Example 3.
  • the present invention relates to an apparatus for producing a CO from a gas containing CO 2 and H 2, a chemical plant and a plant, reverse shift which can be converted into a gas containing CO and H 2 O gas containing CO 2 and H 2
  • a reaction vessel having a catalyst and an H 2 O adsorbent capable of adsorbing H 2 O is provided.
  • the reverse shift catalyst refers to a catalyst that promotes a reverse shift reaction that produces CO and H 2 O from CO 2 and H 2.
  • the reverse shift catalyst preferably contains at least one element selected from Cu, Co, and Mn as the active component (group A). By having these elements, the reverse shift reaction can be efficiently promoted.
  • the precursor of the active ingredient (group A) include nitrates, acetates, chlorides, hydroxides, and the like of each element.
  • an impregnation method, a coprecipitation method, a kneading method, a mechanical alloying method, a vapor deposition method and the like can be considered.
  • the active ingredient (Group A) is preferably in the form of an oxide or a metal.
  • Examples of the method for obtaining the oxide of the active ingredient include firing in a gas atmosphere containing oxygen such as in the atmosphere.
  • Examples of the method for obtaining the active component (group A) in a metallic state include a method in which firing is performed in the atmosphere to form an oxide, and then a reduction treatment is performed in a gas atmosphere containing H 2. Further, in view of storage stability, the active ingredient (A group) was charged into the catalytic reaction vessel while the state of the oxide was reduced by flowing H 2 gas prior to performing the reverse shift reaction, metallic state It may be changed to.
  • the reverse shift catalyst preferably has an oxide containing at least one element selected from Si, Al, Zr, and Ce as the carrier component (group B).
  • oxides containing Ce are particularly high in the ability to promote redox, and should be added from the viewpoint of having the effect of promoting the oxidation / reduction of the active component (group A) and improving the catalytic performance. Is preferable.
  • the carrier component (group B) is Ce and an oxide containing rare earth elements such as Zr, Y, La, Pr, Nd, Pm, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Tb, and Lu. It is more preferable to have. By combining these, the oxidation / reduction reaction can be further promoted.
  • the composition ratio of the active component (group A) and the carrier component (group B) is preferably 0.1% by weight or more and 30% by weight or less in group A with respect to group B. More preferably, it is 1% by weight or more and 10% by weight or less.
  • Catalyst preparation> Catalyst A and catalysts 1 to 7 were prepared by the methods shown below.
  • Catalyst 1 The specific surface area of 100 m 2 / g or more powdered CeO 2 10 g, was impregnated and dried nitrate Cu aqueous solution so as to be 10 wt% with respect to CeO 2 by weight of metal Cu terms. Then, after firing at 500 ° C. for 1 hour in an air atmosphere, a reduction treatment was carried out at 500 ° C. for 1 hour in a hydrogen atmosphere.
  • Catalyst 2 The specific surface area of 100 m 2 / g or more powdered CeO 2 10 g, was impregnated and dried nitrate Co solution so as to be 10 wt% with respect to CeO 2 by weight of metal Co terms. Then, after firing at 500 ° C. for 1 hour in an air atmosphere, a reduction treatment was carried out at 500 ° C. for 1 hour in a hydrogen atmosphere.
  • Catalyst 4 The specific surface area of 200 meters 2 / g or more powdered SiO 2 10 g, was impregnated and dried nitrate Cu aqueous solution so as to be 10 wt% with respect to SiO 2 by weight of metal Cu terms. Then, after firing at 500 ° C. for 1 hour in an air atmosphere, a reduction treatment was carried out at 500 ° C. for 1 hour in a hydrogen atmosphere.
  • Catalyst 7 10 g of powdered Al 2 O 3 having a specific surface area of 100 m 2 / g or more was impregnated with an aqueous solution of Cu nitrate so as to be 24 wt% based on the weight of Al 2 O 3 in terms of metallic Cu, and dried. Then, after firing at 500 ° C. for 1 hour in an air atmosphere, a reduction treatment was carried out at 500 ° C. for 1 hour in a hydrogen atmosphere.
  • ⁇ Catalyst evaluation test> The catalyst powder prepared as described above was press-molded and then crushed into pellets. Then, 3 mL of each pellet was weighed with a measuring cylinder and filled in a catalytic reaction vessel. The reaction gas at the time of measurement was CO 2 (2%) -H 2 (8%) -N 2 (balance). The residence time of the reaction gas was 0.2 seconds.
  • Table 1 shows the test results of each catalyst.
  • CH 4 was selectively produced at a low temperature (500 ° C.).
  • CO was selectively produced at a low temperature (500 ° C.). It is considered that this is because the catalysts 1 to 7 are reverse shift catalysts containing Cu, Co, and Mn. Further, it can be seen that the reverse shift catalyst containing Cu among Cu, Co and Mn has a higher CO production rate at a lower temperature of 200 ° C to 300 ° C. Furthermore, it was found that the CO production rate was particularly high when CeO 2 was selected as the carrier component. From this result, it was found that the reverse shift catalyst containing any one of Cu, Co and Mn as an active ingredient selectively promotes the reverse shift reaction at a lower temperature than the conventional one.
  • the adsorbent used in combination with the reverse shift catalyst preferably has an oxide containing at least one element selected from Si and Al, and more preferably a zeolite containing Si and Al.
  • Zeolites may contain at least one element selected from Si, Al, Li, K, Na, Ca and Mg.
  • the pore size of the zeolite is preferably 10 angstroms or less. More preferably, it is 3 angstroms or more and 4 angstroms or less, in which H 2 O easily enters the pores and CO does not easily enter the pores.
  • Crystalline form of the zeolite may variously idea, in enhancing the adsorption selectivity of H 2 O, A-type, X-type, LSX type is preferred. Particularly preferably, it is type A. More preferably, it is a zeolite of type A and containing at least one element selected from K, Na and Ca.
  • the Si / Al ratio of zeolite varies, but is preferably 100 or less, more preferably 10 or less in terms of element ratio.
  • the 1 angstrom is 0.1 nm.
  • composition ratio of the reverse shift catalyst and the H 2 O adsorbent can be set variously depending on the catalytic activity and the adsorption capacity, but the weight ratio of the reverse shift catalyst / H 2 O adsorbent is preferably 10 or less, more preferably 1 or less. is there.
  • FIG. 1 shows the configuration of the carbon monoxide production apparatus 100 according to Comparative Example 1 using the reverse shift catalyst.
  • the carbon monoxide production apparatus 100 of Comparative Example 1 includes a flow rate control device 1 that controls the flow rates of a CO 2- containing gas source, an H 2- containing gas source, and a CO 2- containing gas, and a flow rate that controls the flow rate of the H 2- containing gas source.
  • Control equipment 2 catalyst tower 10 (reaction vessel) filled with 10 kg of adjusted catalyst (reverse shift catalyst containing Cu and CeO 2 ), and piping equipment for discharging CO-containing gas from catalyst tower 1 (not shown). ) Consists of.
  • the catalyst tower 10 is heated to 500 ° C. by an electric furnace.
  • CO 2 containing gas is 100% CO 2
  • H 2 containing gas was used 100% H 2.
  • the total pressure of the gas containing CO 2 and H 2 flowing through the catalyst tower 10 is set to 1 atm.
  • One atmospheric pressure is 1013.25 hp.
  • FIG. 2 shows the configuration of the carbon monoxide production apparatus 200 according to the first embodiment.
  • the reaction vessel (composite tower 20) has the same configuration as the carbon monoxide production apparatus 100 except that the reaction vessel (composite tower 20) is filled with 10 kg of the catalyst and 10 kg of the A-type zeolite containing K.
  • the composite tower 20 is heated to 300 ° C. by an electric furnace. CO 2 containing gas is 100% CO 2, H 2 containing gas was used 100% H 2. The total pressure of the gas containing CO 2 and H 2 flowing through the composite tower 20 is set to 1 atm.
  • the zeolite adsorbs and removes H 2 O produced as a by-product in the reverse shift catalytic reaction, so that the distributed CO is distributed. It was converted to CO by the reverse shift reaction to 100% 2. Then, after the H 2 O adsorption in the H 2 O adsorbent was saturated, 25% of the distributed CO 2 was converted to CO. That is, the carbon monoxide production apparatus 200 was able to temporarily obtain a gas containing high-purity CO.
  • the flow rate ratio of CO 2 and H 2 in the above embodiment can be adjusted by the flow rate control device.
  • the flow control device uses a CO2-containing gas and an H2-containing gas so that the ratio of CO 2 to H 2 is 1.0 or more and 4.0 or less in terms of molar ratio. It is preferable to control the flow rate of.
  • the flow rate control device include a flow rate control valve controlled by a pressure difference, a blower that actively circulates gas by electric power, a compressor, and the like.
  • FIG. 3 shows the configuration of the carbon monoxide production apparatus 300 according to the second embodiment.
  • the carbon monoxide production apparatus 300 of Example 2 is a heat exchanger 31 as an apparatus for heating the pre-reaction gas and heating the composite tower 20 (reaction vessel) in addition to the carbon monoxide production apparatus 200 of Example 1.
  • Boiler 32 piping for circulating boiler exhaust gas , CO 2 recovery device 33 for recovering and concentrating CO 2 from boiler exhaust gas, H 2 O electrolytic device 34 as a device for obtaining H 2-containing gas
  • composite tower comprising a pipe for use decompressor 35 for decompressing the inside 20, of H 2 O-containing gas discharged from the vacuum device 35 as a heating source of the CO 2 recovering apparatus 33.
  • the CO-containing gas generated in the composite tower 20 can be used in, for example, a chemical plant.
  • the heating gas for example, boiler exhaust gas (combustion exhaust gas) is used.
  • the heat exchanger 31 is exemplified as the device for heating the composite tower 20 in FIG. 3, any temperature control device capable of heating and cooling the composite tower may be used.
  • the pipe for circulating the gas in which the CO 2- containing gas and the H 2- containing gas are mixed to the upper part of the composite tower 20.
  • the upper part means the upper side from the vertical center of the composite tower 20.
  • Carbon monoxide production instrumentation 300 to elimination of H 2 O adsorbed, and the decompressor 35 for decompressing the inside of the composite column 20, be provided with a pipe connecting the pressure reducing device 35 and the composite tower 20 Good.
  • the pipe connected to the decompression device 35 is preferably connected to the upper part of the composite tower 20. Examples of the decompression device 35 include a compressor and a compressor.
  • a temperature measuring device for measuring the internal temperature of the composite tower 20 in the composite tower 20.
  • a thermocouple can be used.
  • Other reaction conditions setting catalyst it is possible to detect the temperature rise due to heat generation of the temperature drop, and H 2 O adsorbed by the endothermic reverse shift reaction.
  • the detection of H 2 O adsorption heat is particularly effective in detecting the adsorption saturation of the H 2 O adsorbent, and a plurality of H 2 O adsorption materials may be installed inside the composite tower 20.
  • the CO 2 recovery device 33 for recovering and concentrating CO 2 from the boiler exhaust gas a temperature swing type adsorption separation device, a pressure swing type adsorption separation device, or a chemical absorption device using amine can be used.
  • the CO-containing gas obtained in the carbon monoxide production package 300 may be used in a chemical plant.
  • a CO-containing gas produced by a CO production apparatus can be used for the Fischer-Tropsch reaction in a chemical plant or the synthesis of methanol.
  • the flow for continuously producing high-concentration CO using this device is shown below.
  • the carbon monoxide production apparatus of the present application can continuously produce high-purity CO.
  • FIG. 4 shows the configuration of the carbon monoxide production apparatus 400 according to the third embodiment.
  • the pressurizing device 41 for pressurizing the CO 2- containing gas and the pressurizing device 42 for pressurizing the H 2-containing gas are installed in the carbon monoxide manufacturing apparatus 300 of the second embodiment.
  • the CO 2- containing gas and the H 2- containing gas can be pressurized and distributed to the composite tower 20.
  • the flow for continuously producing a high concentration of CO using the carbon monoxide production apparatus 400 is shown below.
  • the carbon monoxide production apparatus of the present application can continuously produce high-purity CO at a relatively low temperature.
  • a metal member such as stainless steel may be used because the required temperature is low unlike the conventional reverse shift reaction.
  • Carbon monoxide production equipment 100,200,300,400 Carbon monoxide production equipment 20 Composite tower (reaction vessel) 31 Heat exchanger 32 Boiler 33 CO 2 recovery device 34 H 2 O electrolyzer 35 Decompression device 41,42 Pressurization device

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Catalysts (AREA)

Abstract

Afin de résoudre le problème mentionné ci-dessus, un appareil de production de monoxyde de carbone selon la présente invention est caractérisé en ce qu'il est équipé d'un récipient de réaction (20) contenant un catalyseur de conversion inverse apte à convertir un gaz comprenant du CO2 et de l'H2 en un gaz comprenant du CO et de l'H2O et un matériau adsorbant apte à absorber l'H2O. L'invention concerne également une installation chimique et une installation chacune équipée de l'appareil de production de monooxyde de carbone.
PCT/JP2020/040279 2019-11-01 2020-10-27 Appareil de production de monoxyde de carbone, installation chimique et installation Ceased WO2021085422A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2019-199675 2019-11-01
JP2019199675A JP2021070616A (ja) 2019-11-01 2019-11-01 一酸化炭素製造装置、化学プラントおよびプラント

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WO2021085422A1 true WO2021085422A1 (fr) 2021-05-06

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JP7739116B2 (ja) * 2021-09-30 2025-09-16 大阪瓦斯株式会社 逆水性ガスシフト触媒、逆水性ガスシフト触媒前駆体、電解反応システム、炭化水素類製造システム、及び二酸化炭素の変換方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6315973B1 (en) * 1995-04-10 2001-11-13 Air Products And Chemicals, Inc. Process for operating equilibrium controlled reactions
WO2017121817A1 (fr) * 2016-01-12 2017-07-20 Stichting Energieonderzoek Centrum Nederland Procédé et système de production d'éther diméthylique
WO2018221698A1 (fr) * 2017-05-31 2018-12-06 古河電気工業株式会社 Structure de catalyseur de conversion directe ou inverse et procédé de production de celle-ci, dispositif de réaction directe ou inverse, procédé de production de dioxyde de carbone et d'hydrogène, et procédé de production de monoxyde de carbone et d'eau

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6315973B1 (en) * 1995-04-10 2001-11-13 Air Products And Chemicals, Inc. Process for operating equilibrium controlled reactions
WO2017121817A1 (fr) * 2016-01-12 2017-07-20 Stichting Energieonderzoek Centrum Nederland Procédé et système de production d'éther diméthylique
WO2018221698A1 (fr) * 2017-05-31 2018-12-06 古河電気工業株式会社 Structure de catalyseur de conversion directe ou inverse et procédé de production de celle-ci, dispositif de réaction directe ou inverse, procédé de production de dioxyde de carbone et d'hydrogène, et procédé de production de monoxyde de carbone et d'eau

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