WO2009142520A1 - Catalyseur pour la décomposition à basse température d’oxyde de diazote et son procédé de préparation - Google Patents

Catalyseur pour la décomposition à basse température d’oxyde de diazote et son procédé de préparation Download PDF

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Publication number
WO2009142520A1
WO2009142520A1 PCT/PL2009/000050 PL2009000050W WO2009142520A1 WO 2009142520 A1 WO2009142520 A1 WO 2009142520A1 PL 2009000050 W PL2009000050 W PL 2009000050W WO 2009142520 A1 WO2009142520 A1 WO 2009142520A1
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WO
WIPO (PCT)
Prior art keywords
catalyst
solution
oxide
nitrate
cobalt
Prior art date
Application number
PCT/PL2009/000050
Other languages
English (en)
Inventor
Marcin Wilk
Marek Inger
Urszula Prokop
Ewelina Franczyk
Zbigniew Sojka
Andrzej Kotarba
Andrzej Adamski
Pawel Stelmachowski
Witold Piskorz
Filip Zasada
Original Assignee
Uniwersytet Jagiellonski
Instytut Nawozów Sztucznych
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from PL385251A external-priority patent/PL213796B1/pl
Application filed by Uniwersytet Jagiellonski, Instytut Nawozów Sztucznych filed Critical Uniwersytet Jagiellonski
Publication of WO2009142520A1 publication Critical patent/WO2009142520A1/fr

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Classifications

    • 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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8621—Removing nitrogen compounds
    • B01D53/8625—Nitrogen oxides
    • B01D53/8628—Processes characterised by a specific catalyst
    • 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
    • B01J23/005—Spinels
    • 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
    • B01J23/80—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 zinc, cadmium or mercury
    • 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
    • B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J35/61—Surface area
    • B01J35/613—10-100 m2/g
    • 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
    • B01J37/03—Precipitation; Co-precipitation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/202—Alkali metals
    • B01D2255/2022—Potassium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/204—Alkaline earth metals
    • B01D2255/2045—Calcium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20746—Cobalt
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20753—Nickel
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/40—Nitrogen compounds
    • B01D2257/402—Dinitrogen oxide
    • 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
    • Y02C20/10—Capture or disposal of greenhouse gases of nitrous oxide (N2O)

Definitions

  • the invention provides a catalyst for low-temperature decomposition of dinitrogen oxide in tail gases from a nitric acid plant and a process for the preparation thereof
  • Dinitrogen oxide (N 2 O) is formed as a by-product during catalytic oxidation of ammonia in nitric acid manufacture plants, is not absorbed in water and is discharged with tail gases into the atmosphere.
  • the emission of dinitrogen oxide from a nitric acid plant has significant impact on the greenhouse effect, due to global warming potential for dinitrogen oxide being 310 times higher of that for carbon dioxide.
  • dinitrogen oxide can add up to destroying the ozone layer in the stratosphere. The effective removal thereof from tail gases of both stationary and mobile sources is therefore necessary.
  • Catalytic decomposition of dinitrogen oxide in nitric acid production plants can be carried out at both high and low temperatures.
  • a catalyst is placed in ammonia oxidizer directly below catalytic gauzes for ammonia oxidation.
  • a catalyst is placed in a special reactor, in the tail gas stream which is heated in heat exchangers of the nitric acid plant.
  • dinitrogen oxide removal can be carried out by both selective catalytic reduction and by direct decomposition of N 2 O into oxygen and nitrogen.
  • Low-temperature catalytic decomposition of dinitrogen oxide is definitely more beneficial as compared with reduction, due to the lack of the necessity of using additional reducing agents and a relatively low operating temperature.
  • use of a catalyst in the tail gas stream allows to minimize losses connected to possible depletion of the gas blend in NO x , being a starting material for the nitric acid production.
  • use of a catalyst in a low temperature zone is connected with the requirement of high activity, resistance to other components present in the tail gas stream, i.e.
  • the invention was aimed at providing a catalyst for removal of dinitrogen oxide from tail gases from a nitric acid plant at the temperature below 45O 0 C, having a high activity and resistance to tail gas components.
  • the catalyst of the invention is characterized in that it comprises (calculated as simple oxides): cobalt oxide at the level of 45.00-99.97 weight %, nickel oxide at the level of 0.01-30.00 weight %, zinc oxide at the level of 0.01-20.00 weight % as principal structural components and activity promoters in the form of alkali metals, such as Na and/or K, at the level of 0.01-5.00 weight % and formation-enhancing alkaline earth metal oxides, such as Ca and/or Mg at the level of 0.01-5.00 weight %.
  • cobalt, nickel and zinc ions introduced at the synthesis step form a solid oxide solution of a spinel (Co 3 O 4 ) structure.
  • nickel and zinc ions are incorporated into the spinel Co 3 O 4 structure, while alkaline promoters remain at the surface of the catalyst.
  • a process for the preparation of a catalyst of the invention is characterized in that a solution of cobalt(II) nitrate at a concentration of from 50 to 120 g/dm 3 , nickel(II) nitrate at a concentration from 0.01 to 35.00 g/dm 3 , zinc nitrate at a concentration from 0.01 to 30.00 g/dm 3 is stirred vigorously, most preferably in a circulation system, and a precipitating agent is added simultaneously, at the temperature from ambient to 100°C.
  • a ratio of the precipitating agent to the solution of cobalt, nickel and zinc nitrates should be at least 1.0:0.4 for pH of the solution to range of 9.0-9.5, resulting in the forming of a precipitate.
  • the precipitate is then left in the mother solution at the ambient temperature for at least 15 hrs, and filtered off and washed with water until obtaining the filtrate at pH 7.0-7.5.
  • the prepared precursor is dried at 120°C for at least 15 hrs and calcined at 400-450°C for at least 4 hrs, with gradual heating of the precipitate from 120 to 400°C, to obtain a final product, which is optionally comminuted, and then formed into desired shapes and calcined at 450°C for at least 4 hrs.
  • the cobalt(II) nitrate solution is prepared by dissolving cobalt(II) nitrate hexahydrate in water, at the room temperature
  • the nickel(II) nitrate solution is prepared by dissolving nickel(II) nitrate hexahydrate in water, at the room temperature
  • the zinc nitrate solution is prepared by dissolving zinc nitrate in water, at the room temperature.
  • an aqueous solution of potassium carbonate and/or sodium carbonate or ammonia at a concentration of 150 g of the reagent/1 is used, which is added to the solution of nitrates at the rate of 5 cmVmin.
  • promoters in the form of alkali metals, Na and/or K, and alkaline earth metals, Mg and/or Ca are added at the precipitation step and/or during the precursor impregnation after the calcination.
  • promoters in the form of alkali metals such as sodium and potassium
  • alkaline earth metals such as magnesium and calcium
  • promoters in the form of alkali metals such as sodium and potassium
  • alkaline earth metals such as magnesium and calcium
  • the catalysts according to the invention with different compositions were tested in a quartz reactor, through which a mixture of dinitrogen oxide and helium or tail gases from a nitric acid pilot plant were passed.
  • Composition of the tail gas was identical with the one of a commercial nitric acid plant.
  • Studies on a mixture of 5 % of dinitrogen oxide in helium were carried out in a flow quartz reactor with a frit, at the temperature range from the room temperature to 450°C.
  • Composition of a post-reaction mixture was measured on a mass spectrometer by measuring partial pressures of dinitrogen oxide and decomposition products thereof: oxygen and nitrogen.
  • a decomposition degree of dinitrogen oxide at 300°C was measured to be 95 %, while the sole products of decomposition were dioxygen and dinitrogen.
  • tail gases comprising: 917 ppm of NO x , 874 ppm of N 2 O, 0.40 vol. % of H 2 O, 0.68 vol. % O 2 , with N 2 as a remainder
  • studies were carried out at 400 0 C and at catalyst loading (GHSV) of about 29000 h "1 .
  • Composition of gases before and after a catalyst bed was measured on a FT-IR analyzer. When the above-mentioned parameters were used, the decomposition degree of N 2 O was found to be 99 %.
  • Example 1 The invention is illustrated by the following examples.
  • Example 1 The invention is illustrated by the following examples.
  • the precipitate was left in the mother solution for 15 h at the ambient temperature, followed by filtering and washing the precipitate until pH of the filtrate was 7.0-7.5.
  • the precursor prepared in the process was dried at 120 0 C for 15 hrs, and calcined at 400-450 0 C for 4 hrs, with gradual heating of the precipitate from 120 to 400 0 C.
  • the ready catalyst was shaped into pellets and comminuted to obtain granulate of the size of 0.6 -1.0 mm which was calcined at 45O 0 C for 4 hrs.
  • the obtained catalyst contained 70.0 wt. % Of Co 3 O 4 , 21.0 wt. % OfNi 2 O 3 , 7.0 wt. % of ZnO, 1.9 wt.
  • the precipitate was left in the mother solution for 15 h at the ambient temperature, followed by filtering and washing the precipitate until pH of the filtrate was 7.0-7.5.
  • the precursor prepared in the process was dried at 120 0 C for 15 hrs, and calcined at 400- 45O 0 C for 4 hrs, with gradual heating of the precipitate from 120 to 400 0 C.
  • the ready catalyst was shaped into pellets and comminuted to obtain granulate of the size of 0,6- 1 ,0 mm which was calcined at 45O 0 C for 4 hrs.
  • the obtained catalyst contained 71.0 wt. % Of Co 3 O 4 , 14.0 wt. % Of Ni 2 O 3 , 13.0 wt. % of ZnO, 1.9 wt. % of CaO and 0.1 wt. % of K 2 O.
  • Phase analysis of a sample by an X-ray powder diffractometry revealed the presence of a spinel phase only.
  • the surface area was measured to be 69 m 2 /g by the N 2 -BET method.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Catalysts (AREA)

Abstract

La présente invention concerne un catalyseur pour la décomposition à basse température d’oxyde de diazote dans des gaz résiduaires provenant d’une installation de production d’acide nitrique à base d’oxyde de cobalt comportant, en termes d’oxydes simples : 45,00 à 99,97% en poids d’oxyde de cobalt, 0,01 à 30% en poids d’oxyde de nickel, 0,01 à 20% en poids d’oxyde de zinc comme principaux constituants structurels et des promoteurs d’activité sous forme de métaux alcalins, tels que Na et/ou K compris entre 0,01 et 5% en poids et des oxydes métalliques alcalino-terreux comme agents facilitant la conformation, tels Ca et/ou Mg compris entre 0,01 et 5% en poids. L’invention concerne également un procédé pour la préparation d’un catalyseur.
PCT/PL2009/000050 2008-05-21 2009-05-19 Catalyseur pour la décomposition à basse température d’oxyde de diazote et son procédé de préparation WO2009142520A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
PL385251A PL213796B1 (pl) 2008-05-21 2008-05-21 Katalizator do niskotemperaturowego rozkładu podtlenku azotu
PLP385251 2008-05-21
PL28689008 2008-12-22
PLP286890 2008-12-22

Publications (1)

Publication Number Publication Date
WO2009142520A1 true WO2009142520A1 (fr) 2009-11-26

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Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012114288A1 (fr) * 2011-02-22 2012-08-30 Instytut Nawozów Sztucznych Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé
WO2014025274A1 (fr) * 2012-08-07 2014-02-13 Uniwersytet Jagielloński Catalyseur oxyde à plusieurs constituants pour l'oxydation de méthane à basse température et son procédé de préparation
CN105536799A (zh) * 2016-03-01 2016-05-04 重庆工商大学 纳米Co3O4催化剂的制备方法及其应用
CN105736943A (zh) * 2016-03-16 2016-07-06 山东康宝生化科技有限公司 一种真空泵尾气防静电、防火、防爆输送装置及方法
WO2016126576A1 (fr) * 2015-02-03 2016-08-11 Gencell Ltd. Catalyseur à base de nickel pour la décomposition de l'ammoniac
JP2016529099A (ja) * 2013-07-31 2016-09-23 シエル・インターナシヨナル・リサーチ・マートスハツペイ・ベー・ヴエー 亜酸化窒素分解触媒
CN106215938A (zh) * 2016-07-12 2016-12-14 上海纳米技术及应用国家工程研究中心有限公司 一种二氧化钛促进的四氧化三钴催化剂及其制备和应用
CZ307989B6 (cs) * 2018-08-07 2019-10-02 Vysoká Škola Báňská - Technická Univerzita Ostrava Způsob přípravy katalyzátoru pro odstranění oxidu dusného z odpadních průmyslových plynů a katalyzátor připravený tímto způsobem
CN112007648A (zh) * 2020-07-29 2020-12-01 合肥皖科凌霄环境科技合伙企业(有限合伙) 一种用于直链烷烃低温催化降解催化剂及其制备方法
CN114558580A (zh) * 2022-01-25 2022-05-31 晋中学院 水滑石基CoNiV复合氧化物催化剂的制备方法及逃逸氨脱除应用
CN114984967A (zh) * 2022-06-27 2022-09-02 中国科学技术大学 钴氧化物催化剂及其制备方法以及用于氨分解的方法
CN115245739A (zh) * 2021-12-17 2022-10-28 中国石油天然气股份有限公司 一种催化分解一氧化二氮的反应工艺方法

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FILIP ZASADA ET AL: "Potassium Promotion of Cobalt Spinel Catalyst for N2O Decompositionâ Accounted by Work Function Measurements and DFT Modelling", CATALYSIS LETTERS, KLUWER ACADEMIC PUBLISHERS-PLENUM PUBLISHERS, NE, vol. 127, no. 1-2, 30 September 2008 (2008-09-30), pages 126 - 131, XP019640354, ISSN: 1572-879X *
LIANG YAN, TONG REN, XIAOLAI WANG, DONG JI, JISHUAN SUO: "Catalytic decomposition of N2O over MxCo1-xCo2O4 (M=Ni, Mg) spinel oxides", APPLIED CATALYSIS B: ENVIRONMENTAL, vol. 45, 2003, pages 85 - 90, XP002546039 *
LIANG YAN, TONG REN, XIAOLAI WANG, QIANG GAO, DONG JI, JISHUAN SUO: "Excellent catalytic performance of ZnxCo1-xCo2O4 spinel catalysts for the decomposition of nitrous oxide", CATALYSIS COMMUNICATIONS, vol. 4, 2003, pages 505 - 509, XP002546038 *
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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2012114288A1 (fr) * 2011-02-22 2012-08-30 Instytut Nawozów Sztucznych Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé
WO2014025274A1 (fr) * 2012-08-07 2014-02-13 Uniwersytet Jagielloński Catalyseur oxyde à plusieurs constituants pour l'oxydation de méthane à basse température et son procédé de préparation
JP2016529099A (ja) * 2013-07-31 2016-09-23 シエル・インターナシヨナル・リサーチ・マートスハツペイ・ベー・ヴエー 亜酸化窒素分解触媒
US9782722B2 (en) 2013-07-31 2017-10-10 Shell Oil Company Nitrous oxide decomposition catalyst
JP2020182945A (ja) * 2013-07-31 2020-11-12 シエル・インターナシヨナル・リサーチ・マートスハツペイ・ベー・ヴエー 亜酸化窒素分解触媒
IL253738B (en) * 2015-02-03 2022-11-01 Gencell Ltd A nickel-based catalyst for the decomposition of ammonia
WO2016126576A1 (fr) * 2015-02-03 2016-08-11 Gencell Ltd. Catalyseur à base de nickel pour la décomposition de l'ammoniac
EP3253487A4 (fr) * 2015-02-03 2018-08-01 Gencell Ltd. Catalyseur à base de nickel pour la décomposition de l'ammoniac
IL253738B2 (en) * 2015-02-03 2023-03-01 Gencell Ltd A nickel-based catalyst for the decomposition of ammonia
CN105536799A (zh) * 2016-03-01 2016-05-04 重庆工商大学 纳米Co3O4催化剂的制备方法及其应用
CN105736943A (zh) * 2016-03-16 2016-07-06 山东康宝生化科技有限公司 一种真空泵尾气防静电、防火、防爆输送装置及方法
CN106215938A (zh) * 2016-07-12 2016-12-14 上海纳米技术及应用国家工程研究中心有限公司 一种二氧化钛促进的四氧化三钴催化剂及其制备和应用
WO2020030204A1 (fr) 2018-08-07 2020-02-13 Vysoká Škola Báňská - Technická Univerzita Ostrava Procédé de préparation d'un catalyseur pour l'élimination d'oxyde nitreux de gaz industriels usés et catalyseur préparé par ce procédé
CZ307989B6 (cs) * 2018-08-07 2019-10-02 Vysoká Škola Báňská - Technická Univerzita Ostrava Způsob přípravy katalyzátoru pro odstranění oxidu dusného z odpadních průmyslových plynů a katalyzátor připravený tímto způsobem
CN112007648A (zh) * 2020-07-29 2020-12-01 合肥皖科凌霄环境科技合伙企业(有限合伙) 一种用于直链烷烃低温催化降解催化剂及其制备方法
CN115245739A (zh) * 2021-12-17 2022-10-28 中国石油天然气股份有限公司 一种催化分解一氧化二氮的反应工艺方法
CN115245739B (zh) * 2021-12-17 2023-09-05 中国石油天然气股份有限公司 一种催化分解一氧化二氮的反应工艺方法
CN114558580A (zh) * 2022-01-25 2022-05-31 晋中学院 水滑石基CoNiV复合氧化物催化剂的制备方法及逃逸氨脱除应用
CN114558580B (zh) * 2022-01-25 2023-10-27 晋中学院 水滑石基CoNiV复合氧化物催化剂的制备方法及逃逸氨脱除应用
CN114984967A (zh) * 2022-06-27 2022-09-02 中国科学技术大学 钴氧化物催化剂及其制备方法以及用于氨分解的方法

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