WO2024257923A1 - Catalyseur à base de carbone, pour la synthèse d'ammoniac, qui présente une activité élevée dans des conditions basse pression et basse température, et procédé de synthèse d'ammoniac l'utilisant - Google Patents

Catalyseur à base de carbone, pour la synthèse d'ammoniac, qui présente une activité élevée dans des conditions basse pression et basse température, et procédé de synthèse d'ammoniac l'utilisant Download PDF

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Publication number
WO2024257923A1
WO2024257923A1 PCT/KR2023/008347 KR2023008347W WO2024257923A1 WO 2024257923 A1 WO2024257923 A1 WO 2024257923A1 KR 2023008347 W KR2023008347 W KR 2023008347W WO 2024257923 A1 WO2024257923 A1 WO 2024257923A1
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catalyst
carbon
ammonia synthesis
metal
based support
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English (en)
Korean (ko)
Inventor
조강희
윤형철
김선형
주형국
범희태
전상구
이기봉
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Korea Institute of Energy Research KIER
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Korea Institute of Energy Research KIER
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Priority to PCT/KR2023/008347 priority Critical patent/WO2024257923A1/fr
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Anticipated expiration legal-status Critical
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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
    • 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
    • B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
    • B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
    • B01J23/46—Ruthenium, rhodium, osmium or iridium
    • 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
    • B01J23/74—Iron group metals
    • 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
    • B01J35/00—Catalysts, in general, 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
    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
    • B01J37/02—Impregnation, coating or precipitation
    • 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
    • C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
    • 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
    • C01B32/15—Nano-sized carbon materials
    • C01B32/158—Carbon nanotubes
    • C01B32/16—Preparation
    • C01B32/162—Preparation characterised by catalysts
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts

Definitions

  • the present invention relates to a carbon-based catalyst for ammonia synthesis exhibiting high activity under low pressure and low temperature conditions and a method for synthesizing ammonia using the same.
  • Ammonia is a compound composed of nitrogen and oxygen, with a molecular formula of NH3 , and exists as a gas with an irritating odor at room temperature. It is contained in small amounts in the atmosphere, and trace amounts are also contained in natural waters, and can exist in the soil as it is produced in the process of bacteria decomposing nitrogenous organic matter. Ammonia is used as a raw material for various chemical industries, in the production of ammonia water, and as a solvent for ionic substances.
  • the most common method for producing ammonia is the Haber-Bosch process, which synthesizes ammonia from hydrogen and nitrogen, and is performed at high pressure (over 200 atm) and high temperature (400–500°C) in the presence of an iron or ruthenium catalyst.
  • This reaction consumes a huge amount of energy, about 30 GJ/ton NH 3 , and has the problem of emitting a large amount of greenhouse gases equivalent to 1.8 ton CO 2 /ton NH 3 due to the fossil fuels used to supply this energy.
  • the catalytic activity may be inhibited due to the characteristic of nitrogen and hydrogen molecules to be competitively adsorbed on the catalyst surface, and since nitrogen among the reactants has a very stable structure of a triple bond, the ammonia synthesis rate through the catalytic reaction is generally only 20%.
  • the energy consumption has been reduced to 28 GJ/ton NH 3 , which is close to the theoretical value.
  • the energy required for ammonia synthesis must be further reduced, and since existing commercial catalysts are designed to operate under high temperature and high pressure conditions, their ammonia synthesis performance is very low under the low pressure and low temperature conditions that we want, so it is necessary to develop and use a technological catalyst that can sufficiently synthesize ammonia at much lower pressure (100 atm or less) and temperature (400°C or less) than the existing process conditions (400–500°C and 200 atm or more).
  • the purpose of the present invention is to provide a novel catalyst material and a method for producing the same which exhibits a much higher ammonia synthesis rate than existing commercial ammonia synthesis catalysts at a lower pressure (less than 100 atm) and lower temperature (400°C) than the existing Haber-Bosch process for producing ammonia.
  • the present invention provides a catalyst for ammonia synthesis, comprising: a carbon-based support supporting a first metal catalyst; and a second metal cocatalyst additionally supported on the carbon-based support supporting the first metal catalyst.
  • the carbon-based support may be selected from the group consisting of low-grade coal, carbon black, nanocellulose, biochar, activated carbon, activated carbon fiber, carbon nanotube, and ketchen black, and the carbon-based support may contain 1 to 10 mass% of nitrogen or oxygen relative to the mass of the carbon-based support.
  • the first metal may be selected from the group consisting of iron (Fe), ruthenium (Ru), cobalt (Co), nickel (Ni), and osmium (Os), and the first metal catalyst may be included in an amount of 1 to 20 mass% relative to the mass of the carbon-based support.
  • the second metal may be selected from the group consisting of lithium (Li), sodium (Na), potassium (K), rubidium (Rb), cesium (Cs), beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), and barium (Ba), and the second metal promoter may be included in an amount of 0.1 to 3 mmol/g relative to the mass of the carbon-based support.
  • the present invention provides a method for synthesizing ammonia at a temperature of 300 to 500°C and a pressure of 10 to 100 atm using the above-mentioned ammonia synthesis catalyst.
  • the present invention provides a method for producing a catalyst for ammonia synthesis, comprising the steps of: (a) supporting a first metal catalyst and a second metal promoter on a carbon-based support; and (b) treating the carbon-based support with acid.
  • the carbon-based support may be selected from the group consisting of low-grade coal, carbon black, nanocellulose, biochar, activated carbon, activated carbon fiber, carbon nanotubes, and ketchen black.
  • the first metal may be selected from the group consisting of iron (Fe), ruthenium (Ru), cobalt (Co), nickel (Ni), and osmium (Os), and the first metal catalyst may be included in an amount of 1 to 20 mass% relative to the mass of the carbon-based support.
  • the second metal may be selected from the group consisting of lithium (Li), sodium (Na), potassium (K), rubidium (Rb), cesium (Cs), beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), and barium (Ba), and the second metal promoter may be included in an amount of 0.1 to 3 mmol/g relative to the mass of the carbon-based support.
  • the acid treatment may be performed at 20 to 100°C using an acid selected from the group consisting of sulfuric acid, hydrochloric acid, and nitric acid.
  • ammonia can be synthesized with high efficiency at a lower temperature and pressure than the existing commercial Haber-Bosch process, thereby significantly reducing process energy consumption and carbon dioxide emissions.
  • Figure 1 is a TEM image of a catalyst for ammonia synthesis according to Example 1 of the present invention.
  • Figure 2 is an XRD graph of a catalyst for ammonia synthesis according to Example 5 of the present invention.
  • ammonia synthesis catalyst of the present invention will be described in detail with reference to the attached drawings below.
  • the ammonia synthesis catalyst of the present invention is characterized by comprising: a carbon-based support on which a first metal catalyst is supported; and a second metal cocatalyst additionally supported on the support on which the first metal catalyst is supported.
  • the carbon-based support may include a one-dimensional carbon-based material or other carbon-based material, and preferably may be selected from the group consisting of low-grade coal, carbon black, nanocellulose, biochar derived from natural plants, activated carbon, activated carbon fibers, carbon nanotubes and ketchen black, and more preferably may include nitrogen-containing carbon black, carbon black or carbon nanotubes.
  • the one-dimensional carbon-based material may be one or a combination of two or more selected from the group consisting of carbon nanotubes (CNTs), graphene nanoribbons (GNRs), carbon nanofibers, and carbon nanowires, and the carbon nanotubes may be single-walled carbon nanotubes (SWNTs) or multi-walled carbon nanotubes (MWNTs).
  • CNTs carbon nanotubes
  • GNRs graphene nanoribbons
  • MWNTs multi-walled carbon nanotubes
  • multi-walled carbon nanotubes may be used as the one-dimensional carbon-based material.
  • Multi-walled carbon nanotubes have superior mechanical strength, superior structural retention upon repeated tensile stretching, and a wide tensile range compared to carbon nanotubes such as single-walled carbon nanotubes, and thus are advantageous in being used as a support.
  • the one-dimensional carbon-based material may have a diameter of 10 to 200 nm, preferably 20 to 150 nm, and a length of 10 to 100 ⁇ m, preferably 20 to 80 ⁇ m, but is not limited thereto.
  • the above carbon-based support may contain 1 to 10 mass% of nitrogen or oxygen relative to the mass of the carbon-based support, preferably 2 to 9 mass%, and more preferably 3 to 8 mass%.
  • the specific surface area of the carbon-based support increases, so that the metal catalyst can be dispersed small and uniformly, thereby reducing the unit cost of the catalyst, and preventing sintering of the metal catalyst and cocatalyst when used for a long time.
  • the high electrical conductivity of the carbon-based support can be used to rapidly supply electrons to nitrogen molecules, thereby promoting the nitrogen dissociation step, and the step in which the hydrogenation reaction proceeds and ammonia is generated can be promoted because it binds well to the dissociated nitrogen atoms.
  • non-limiting examples of the first metal include a metal selected from the group consisting of iron (Fe), ruthenium (Ru), cobalt (Co), nickel (Ni), molybdenum (Mo), and osmium (Os), and preferably ruthenium.
  • the nitrogen bonding force is weakened by supplying electrons to nitrogen, a reactant of the ammonia synthesis reaction (Lewis base), and the reaction rate of the nitrogen dissociation step (the rate-determining step of the overall reaction) is accelerated, thereby allowing the reaction to proceed in the forward direction.
  • the method for synthesizing ammonia using the ammonia synthesis catalyst of the present invention can be carried out at a temperature of 300 to 500°C, and preferably, ammonia can be synthesized at a temperature of 350 to 450°C.
  • the method can be carried out at a pressure of 10 to 100 atm, and is characterized in that ammonia is synthesized at a pressure of preferably 30 to 80 atm.
  • the second metal in the method for supporting the second metal promoter, may be selected from the group consisting of lithium (Li), sodium (Na), potassium (K), rubidium (Rb), cesium (Cs), beryllium (Be), magnesium (Mg), calcium (Ca), strontium (Sr), and barium (Ba), and preferably barium, and at this time, as the barium promoter precursor, barium nitrate (Ba(NO 3 ) 2 ; barium nitrate), barium hydroxide (Ba(OH) 2 ; barium hydroxide), barium perchlorate (Ba(ClO 4 ) 2 ; barium perchlorate), barium isopropoxide (Ba(OCH(CH 3 ) 2 ) 2 ; barium isopropoxide), barium fluoride (BaF 2 ; barium fluoride), barium oxide (BaO; barium oxide), barium bromide (BaBr 2 ; barium bromide
  • the second metal promoter may be included in an amount of 0.1 to 3.0 mmol/g relative to the mass of the support, preferably 0.5 to 2.0 mmol/g, and most preferably 0.7 to 1.5 mmol/g.
  • the second metal promoter may be additionally pretreated before the step of supporting the second metal promoter.
  • the pretreatment step is a step of heating and calcining while flowing an inert gas such as nitrogen, argon, or helium; a reducing gas such as ammonia reaction synthesis gas (H 2 +N 2 ), hydrogen, diluted hydrogen (balance gas: an inert gas such as nitrogen, argon, or hydrogen); carbon monoxide, or diluted carbon monoxide (balance gas: an inert gas such as nitrogen, argon, or hydrogen); and the heating temperature varies depending on the component of the first metal, but is preferably heated at 250 to 700°C.
  • the acid treatment in step (b) may be performed using a strong acid at 20 to 100°C, preferably using an acid selected from the group consisting of sulfuric acid, hydrochloric acid, and nitric acid.
  • the concentration of the strong acid may be 0.05 to 1.0 M, preferably 0.1 to 0.9 M, and more preferably 0.3 to 0.8 M.
  • the catalyst for ammonia synthesis prepared in Example 1 was prepared in the same manner as that for the catalyst for ammonia synthesis prepared in Example 1, except that 0.16 g of ruthenium chloride precursor (RuCl 3 ⁇ xH 2 O, 37% Ru) was used instead of 0.27 g of ruthenium chloride precursor (RuCl 3 ⁇ xH 2 O, 37% Ru), and 0.27 g of barium nitrate (Ba(NO 3 ) 2 ) was mixed instead of 0.54 g of barium nitrate (Ba(NO 3 ) 2 ).
  • a catalyst for ammonia synthesis was prepared using the same manufacturing method as that of Example 1, except that a ruthenium chloride precursor (RuCl 3 ⁇ xH 2 O, 37% Ru) was not used.
  • a catalyst for ammonia synthesis was prepared using the same manufacturing method as that of Example 1, except that potassium nitrate (KNO 3 ) was used instead of barium nitrate (Ba(NO 3 ) 2 ).
  • a catalyst for ammonia synthesis was manufactured using the same manufacturing method as that of Example 1, except that a CeO 2 series support (ceria) was used instead of carbon black.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un catalyseur contenant un promoteur pour la synthèse d'ammoniac, et un procédé de synthèse d'ammoniac l'utilisant. Selon le matériau catalyseur de la présente invention, et son procédé de préparation, de l'ammoniac peut être synthétisé de manière hautement efficace à une température et une pression inférieures à celles rencontrées dans le processus d'Haber-Bosch commercial classique, et ainsi la présente invention présente les avantages de réduire significativement la consommation d'énergie de traitement et les émissions de dioxyde de carbone.
PCT/KR2023/008347 2023-06-16 2023-06-16 Catalyseur à base de carbone, pour la synthèse d'ammoniac, qui présente une activité élevée dans des conditions basse pression et basse température, et procédé de synthèse d'ammoniac l'utilisant Ceased WO2024257923A1 (fr)

Priority Applications (1)

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PCT/KR2023/008347 WO2024257923A1 (fr) 2023-06-16 2023-06-16 Catalyseur à base de carbone, pour la synthèse d'ammoniac, qui présente une activité élevée dans des conditions basse pression et basse température, et procédé de synthèse d'ammoniac l'utilisant

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PCT/KR2023/008347 WO2024257923A1 (fr) 2023-06-16 2023-06-16 Catalyseur à base de carbone, pour la synthèse d'ammoniac, qui présente une activité élevée dans des conditions basse pression et basse température, et procédé de synthèse d'ammoniac l'utilisant

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1389295A (zh) * 2002-06-10 2003-01-08 中国科学院大连化学物理研究所 碳纳米纤维负载的钌基氨合成催化剂及其制备
US20050053541A1 (en) * 2001-12-05 2005-03-10 Lucio Forni Catalysts for ammonia synthesis
WO2018215202A1 (fr) * 2017-05-22 2018-11-29 Siemens Aktiengesellschaft Catalyseur pour synthèse de l'ammoniac
CN110038615A (zh) * 2019-05-21 2019-07-23 福州大学 一种含氮元素的活性炭负载钌金属催化剂的制备方法
KR20230102614A (ko) * 2021-12-30 2023-07-07 한국에너지기술연구원 저압, 저온 조건에서 높은 활성을 보이는 암모니아 합성용 탄소계 촉매 및 이를 이용한 암모니아의 합성 방법

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20050053541A1 (en) * 2001-12-05 2005-03-10 Lucio Forni Catalysts for ammonia synthesis
CN1389295A (zh) * 2002-06-10 2003-01-08 中国科学院大连化学物理研究所 碳纳米纤维负载的钌基氨合成催化剂及其制备
WO2018215202A1 (fr) * 2017-05-22 2018-11-29 Siemens Aktiengesellschaft Catalyseur pour synthèse de l'ammoniac
CN110038615A (zh) * 2019-05-21 2019-07-23 福州大学 一种含氮元素的活性炭负载钌金属催化剂的制备方法
KR20230102614A (ko) * 2021-12-30 2023-07-07 한국에너지기술연구원 저압, 저온 조건에서 높은 활성을 보이는 암모니아 합성용 탄소계 촉매 및 이를 이용한 암모니아의 합성 방법

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JAFARI, A. ET AL.: "Influence of chemical treatments of activated carbon support on the performance and deactivation behavior of promoted Ru catalyst in ammonia synthesis", INTERNATIONAL JOURNAL OF HYDROGEN ENERGY, vol. 40, 2015, pages 3659 - 3671, XP029141783, DOI: 10.1016/j.ijhydene.2015.01.071 *

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