EP2678104A1 - Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé - Google Patents

Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé

Info

Publication number
EP2678104A1
EP2678104A1 EP12719449.6A EP12719449A EP2678104A1 EP 2678104 A1 EP2678104 A1 EP 2678104A1 EP 12719449 A EP12719449 A EP 12719449A EP 2678104 A1 EP2678104 A1 EP 2678104A1
Authority
EP
European Patent Office
Prior art keywords
weight
catalyst
zinc
zinc oxide
oxide
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.)
Withdrawn
Application number
EP12719449.6A
Other languages
German (de)
English (en)
Inventor
Marcin Wilk
Marek Inger
Magdalena SARAMOK
Pawel Kowalik
Zbigniew Sojka
Andrzej Kotarba
Pawel Stelmachowski
Witold Piskorz
Filip Zasada
Andrzej Adamski
Gabriela MANIAK
Ewelina Franczyk
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.)
Instytut Nawozow Sztucznych
Uniwersytet Jagiellonski
Original Assignee
Instytut Nawozow Sztucznych
Uniwersytet Jagiellonski
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 PL393991A external-priority patent/PL220431B1/pl
Priority claimed from PL393992A external-priority patent/PL220569B1/pl
Application filed by Instytut Nawozow Sztucznych, Uniwersytet Jagiellonski filed Critical Instytut Nawozow Sztucznych
Publication of EP2678104A1 publication Critical patent/EP2678104A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • 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
    • 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
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/19—Catalysts containing parts with different compositions
    • 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
    • B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
    • B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
    • 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
    • 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
    • B01J37/04—Mixing
    • 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
    • B01D2255/202—Alkali metals
    • B01D2255/2027—Sodium
    • 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
    • B01D2255/20792—Zinc
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/40—Mixed oxides
    • 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
    • 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
    • B01J2523/00—Constitutive chemical elements of heterogeneous 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
    • 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 subject of the present Invention Is a composite catalyst for the low-temperature decomposition of nitrous oxide in tail gases from nitric acid installations as well as a method of producing It.
  • nitrous oxide has been defined as one of the six greenhouse gases, whose potential for causing this effect is some 296 times that of carbon dioxide.
  • One o1 the largest sources of of nitrous oxide emission is the chemical Industry, and In particular, nitric acid Installations, whose participation In the global emission of this gas Is 20 %.
  • Nitrous oxide is formed as a by-product of the catalytic oxidation of ammonia, During the technological process of nitric acid manufacturing, the nitrous oxide does not undergo any reactions and Is emitted Into the atmosphere In Its entirety along with the other tail gases.
  • nitrous oxide in nitric acid installations can occur by way of decomposition or reduction In the presence of an appropriate catalyst, wherein this process can be performed at both high and low temperatures.
  • high temperatures 800 - 940 e C
  • the decomposition of nitrous oxide occurs in the stream of nitroeo gases rich in nitric oxide NO, formed due to ammonia oxidation
  • the removal of nitrous oxide may be performed by way of the catalytic reduction or catalytic decomposition in the tall, gas stream, which Is directed Into the atmosphere upon NO x reduction.
  • the low-temperature process may be realised through catalytic reduction or decomposition, In the case of reduction, the most frequently used reductant Is ammonia or hydrocarbons. For economic reasons, direct decomposition Is preferable.
  • the main limitation of the direct use of decomposition is that the low temperature of the tail gasses that prevents effective catalyst functioning.
  • Patent description WO2001/051181 discloses a two-stage removal process for NO* and nitrous oxide from the tail gases of nitric acid installations at low temperature area. According to said description, the removal of nitrous oxide may occur through the catalytic decomposition on a zeolite catalyst at a temperature of 425 - 520"C or through catalytic reduction with a hydrocarbon at a temperature of 300 - 520 a C, Patent description No. PCT/NO02/00439 discloses a method of obtaining and activating a zeolite catalyst, its composition and use in nitrous oxide removal.
  • Polish patent description No. 386 890, 2008 discloses a catalyst for the low-temperature decomposition of nitrous oxide, based on cobalt oxide which contains, in addition to the main component, nickel oxide, zinc oxide as well as alkali earth metal oxides, such as Ca and/or Mg and alkali metal oxides, such as Na and/or K.
  • the goal of the present invention is to deliver a composite catalyst for removing nitrous oxide from the tail gasses of nitric acid installation at a temperature below 450 °C in a form that facilitates ts use in an industrial reactor, as well as to present a method of producing it.
  • the active components are ions of cobalt, zinc and potassium, possibly sodium, and the catalyst composition additionally comprises zinc oxide and graphite not incorporated in the spinel structure, which enhance the durability of the catalyst tablets.
  • the composite catalyst according to the present invention contains cobalt oxide at 25 - 88.6 % by weight, zinc oxide at 10.99 - 60 % by weight as the substantive components, wherein the zinc oxide is introduced in two stages, during precipitation as well as prior to the forming of the catalyst.
  • the ratio of zinc oxide introduced during the precipitation to the zinc oxide added prior to the formation is 1 :0.26-13.3 and it also contains components which improve activity in the form of alkali metals at 0.01 -5 % by weight calculated in terms of the oxides of these metals, and graphite at 0.4-10 %.
  • the alkali metals present in catalyst composition are sodium and/or potassium.
  • the essence of the present invention relating to a method of producing a composite catalyst is based on the fact that a solution with a total concentration of cobalt and zinc cations in the range of 0.8-2.5 mol/dm 3 and the ratio of cobalt to zinc in the range of 1 :0.12-0.17 is mixed, preferably in a circulatory system, and potassium carbonate or potassium hydroxide at a concentration of 1 .0-1 .5 mol/dm 3 is added in an amount at least 1 :0.4 to a solution of cobalt nitrate and zinc nitrate to reach a pH of 9-10.
  • the precipitate is rinsed to reach a potassium concentration of 0.4 - 1 % by weight, and then it is dried and calcined at a temperature of 450 °C and possibly impregnated with a solution of potassium carbonate at a concentration of 0.03 - 0.1 mol/dm 3 .
  • zinc oxide calcined at a temperature of 250 - 600 °C is added at 1 - 50% by weight and graphite at 0.4 - 10 % by weight.
  • the mixture is thoroughly mixed and formed in molds, which results in the formation of a product, active in the decomposition reaction of nitrous oxide at a temperature below 450 °C.
  • An additional advantage of such use of zinc oxide is a better dispersion of the active phase nanoparticles which facilitates access of reagents and removal of reaction products of the decomposition of nitrous oxide. Furthermore, using the selection of the calcination temperature of zinc oxide as well as the amount of added graphite, one can control the size of zinc oxide grains as well as the porosity of the entire system of diphase catalyst.
  • Composite catalysts of various compositions according to the present invention were tested in a quartz reactor, through which passed a mixture of nitrous oxide and helium or tail gases from a pilot nitric acid installation.
  • the composition of the tail gases was identical to that occurring in industrial nitric acid installation.
  • the research on the 5 % of nitrous oxide in helium mixture was performed in a flow-through quartz reactor with sinter, in the range of temperatures from ambient to 450 °C, at a GHSV load of 7000 h " .
  • the composition of the post-reaction mixture was determined using a mass spectrometer, measuring the partial pressures of nitrous oxide as well as its decomposition products: oxygen and nitrogen.
  • the precipitate was maintained in the parent solution for 15 h at ambient temperature, after which the precipitate was drained off and rinsed, until reaching a pH of filtrate equal 7.0-7.5.
  • the resulting precipitate was dried at a temperature of 120 °C for 15 hours, and then the filtrate was impregnated with a 0.06 molar solution of potassium carbonate, dried at a temperature of 120 °C and calcined at a temperature of 400-450 °C for4 hours, gradually increasing the temperature from 120 to 400 °C.
  • the mixer was loaded with 450 gof the initially produced catalyst, 150 g of zinc oxide calcined at a temperature of 450 °C, which constitutes 24.88 % by weight, as well as 3 g of graphite which constitutes 0.5 % by weight and mixed until homogeneity was obtained.
  • a phase analysis using powder diffraction demonstrated the presence of only spinel and zinc oxide phases.
  • the specific surface area determined via N 2 -BET method was 39 m 2 /g.
  • GHSV a catalyst
  • Example 2 In a vessel of 10000 cm 3 volume we dissolved 1554.0 g of cobalt(ll) nitrate hexahydrate and 244.5 g of zinc (II) nitrate hexahydrate in 3100 cm 3 of distilled water such a way that the total cation concentration in the solution was 2M, and the ratio of cobalt ions to zinc ions was 1 :0.153.
  • the resulting solution mixture was mixed using a mechanical mixer, at the same time adding the precipitant in the form of a solution of potassium hydroxide at a concentration of 1 .5 mol/dm 3 . This was performed until a pH of solution was reached at the range of 9.0-9.5, which resulted in precipitation.
  • the precipitate was maintained in the parent solution for 15 h at ambient temperature, after which the precipitate was drained off and rinsed with volumes of water, controlling the potassium content in the precipitate.
  • the rinse was terminated, and the resulting precipitate was dried at a temperature of 120 °C for 15 hours and calcined at a temperatue of 400-450 °C for 4 hours, gradually increasing the temperature from 120 to 400 °C.
  • the mixer was loaded with 300 g of the produced catalyst precursor, 300 g of zinc oxide calcined at a temperature of 450°C, which constitutes 49.75 % by weight, as well as 3 g of graphite which constitutes 0.5 % by weight and mixed until homogeneity was obtained.
  • Example 3 In a vessel of 10000 cm 3 volume we dissolved 1554.0 g of cobalt(ll) nitrate hexahydrate and 244.5 g of zinc (II) nitrate hexahydrate in 3100 cm 3 of distilled water. The resulting solution mixture was mixed using a mechanical mixer, at the same time adding the precipitant in the form of a solution of potassium carbonate at a concentration of 1 .2 mol/dm 3 . This was performed until a solution pH was reached at the range of 9.0-9.5. The precipitate was maintained in the parent solution for 15 h at ambient temperature, after which the precipitate was drained off and rinsed.
  • the resulting precipitate was dried and then the precipitate was impregnated with a 0.1 molar solution of potassium carbonate, dried and calcined.
  • 450 g of the obtained mass was mixed until homogeneity was obtained with 150 g of zinc oxide calcined at the temperature of 450 °C, which constitutes 49.75 % by weight, as well as 3 g of graphite .
  • Example 4 Catalyst was prepared using the method of Example 3, with the difference that the impregnation was made with the use of a 0.8 mol/dm 3 solution of sodium carbonate in place of the potassium carbonate solution, and then the resulting 450 g of dry mass was supplemented with 150 g of zinc oxide as well as 5 g of graphite and thoroughly mixed.

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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

L'invention concerne un catalyseur composite qui contient 25 - 88,6% en poids en oxyde de cobalt, 10,99 - 60% en poids en oxyde de zinc comme composants importants ; l'oxyde de zinc est introduit en deux étapes, lors de la précipitation et avant la formation du catalyseur. Le rapport de l'oxyde de zinc introduit lors de la précipitation et de l'oxyde de zinc ajouté avant la formation du catalyseur est de 1 :00,26-13,3 , il contient également des composants qui améliorent l'activité, sous la forme de métaux alcalins à 0,01 - 5% en poids en termes d'oxydes de ces métaux, et du graphite à 0,4 - 10%. De préférence, les métaux alcalins présents dans la composition du catalyseur sont le sodium et/ou le potassium.
EP12719449.6A 2011-02-22 2012-02-22 Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé Withdrawn EP2678104A1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
PL393991A PL220431B1 (pl) 2011-02-22 2011-02-22 Sposób wytwarzania kompozytowego katalizatora do niskotemperaturowego rozkładu podtlenku azotu
PL393992A PL220569B1 (pl) 2011-02-22 2011-02-22 Kompozytowy katalizator do niskotemperaturowego rozkładu podtlenku azotu
PCT/IB2012/050810 WO2012114288A1 (fr) 2011-02-22 2012-02-22 Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé

Publications (1)

Publication Number Publication Date
EP2678104A1 true EP2678104A1 (fr) 2014-01-01

Family

ID=46045035

Family Applications (1)

Application Number Title Priority Date Filing Date
EP12719449.6A Withdrawn EP2678104A1 (fr) 2011-02-22 2012-02-22 Catalyseur composite conçu pour la décomposition à basse température d'oxyde nitreux, et procédé de fabrication associé

Country Status (2)

Country Link
EP (1) EP2678104A1 (fr)
WO (1) WO2012114288A1 (fr)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CZ2018398A3 (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

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1263711B (de) * 1964-08-06 1968-03-21 Huels Chemische Werke Ag Verfahren zur Herstellung von eines Hydrierkatalysators
US4430315A (en) * 1981-12-28 1984-02-07 The Dow Chemical Company Catalytic decomposition of hypochlorite using substituted cobalt oxide spinels
DE10001539B4 (de) 2000-01-14 2006-01-19 Uhde Gmbh Verfahren zur Beseitigung von NOx und N2O
WO2009142520A1 (fr) * 2008-05-21 2009-11-26 Uniwersytet Jagiellonski Catalyseur pour la décomposition à basse température d’oxyde de diazote et son procédé de préparation
PL386890A1 (pl) 2008-12-22 2010-07-05 Instytut Nawozów Sztucznychinstytut Nawozów Sztucznych Sposób wytwarzania katalizatora do niskotemperaturowego rozkładu podtlenku azotu

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
See references of WO2012114288A1 *

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Publication number Publication date
WO2012114288A1 (fr) 2012-08-30

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