WO2005042403A2 - Method for eliminating n2o during nitric acid production - Google Patents

Method for eliminating n2o during nitric acid production Download PDF

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Publication number
WO2005042403A2
WO2005042403A2 PCT/EP2004/011992 EP2004011992W WO2005042403A2 WO 2005042403 A2 WO2005042403 A2 WO 2005042403A2 EP 2004011992 W EP2004011992 W EP 2004011992W WO 2005042403 A2 WO2005042403 A2 WO 2005042403A2
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WIPO (PCT)
Prior art keywords
catalytically active
active materials
coated
filled
removal
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PCT/EP2004/011992
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German (de)
French (fr)
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WO2005042403A3 (en
Inventor
Heinz-Josef Kneuper
Karel Hellemans
Helmut Schachner
Andreas Spiegel
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Basf Aktiengesellschaft
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Publication of WO2005042403A2 publication Critical patent/WO2005042403A2/en
Publication of WO2005042403A3 publication Critical patent/WO2005042403A3/en

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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
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/24—Stationary reactors without moving elements inside
    • B01J19/248—Reactors comprising multiple separated flow channels
    • B01J19/2495—Net-type reactors
    • 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
    • B01D53/8631—Processes characterised by a specific device
    • 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
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/56—Foraminous structures having flow-through passages or channels, e.g. grids or three-dimensional monoliths
    • 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
    • B01J35/50—Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • B01J35/58—Fabrics or filaments
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
    • C01B21/24—Nitric oxide (NO)
    • C01B21/26—Preparation by catalytic or non-catalytic oxidation of ammonia
    • C01B21/265—Preparation by catalytic or non-catalytic oxidation of ammonia characterised by the catalyst
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/20—Nitrogen oxides; Oxyacids of nitrogen; Salts thereof
    • C01B21/24—Nitric oxide (NO)
    • C01B21/26—Preparation by catalytic or non-catalytic oxidation of ammonia
    • C01B21/28—Apparatus
    • 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)
    • 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
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

Definitions

  • the invention relates to methods for removing N 2 O in the production of nitric acid by means of coated spatial bodies.
  • N 2 O nitrogen oxide
  • the exhaust gas In the large-scale production of nitric acid, for example by the Ostwald process (Ullmann's Encyclopedia of Industrial Chemistry, 5th edition, volume A 17, pages 293 to 339 (1991)), ammonia is also burned with oxygen on a catalyst containing noble metals Nitric oxide and nitrogen dioxide (or nitrous oxide) as a rule also N 2 O (nitrous oxide) as a by-product. In contrast to the other nitrogen oxides formed, N 2 O is not absorbed by the water in the course of the absorption process. If no further stage for removing the "greenhouse gas" N 2 O is provided, it is found in the exhaust gas.
  • the previously known catalysts have the disadvantage that they are in the form of compact beds of individual shaped catalyst bodies whose gas permeability cannot be set in a targeted manner (pressure drop and high mechanical and static loads).
  • the high mechanical load can lead to catalyst abrasion when heating up to operating temperature and cooling down. This abrasion can be carried along with the process gas into downstream equipment.
  • the bed of shaped catalyst bodies can shift during operation. This can sometimes lead to being lost in some places "the mechanical support for the precious metal catalyst gauzes and tear the nets at these sites. This is particularly disadvantageous if precious metal nets are to be reused. Uneven bed height can also cause an uneven gas load of the N2O catalyst, followed by reduced efficiency (less degradation of N2O).
  • the object of the present invention was therefore to remedy the disadvantages mentioned above.
  • Molded bodies, nets, fabrics, knitted fabrics, wire packs, honeycomb bodies, ceramic monoliths, preferably honeycomb bodies, fabrics, knitted fabrics, nets, wire packs, particularly preferably woven fabrics, knitted fabrics, nets, are suitable as spatial bodies.
  • the spatial bodies are usually rigid, do not usually shift, reduce mechanical abrasion and offer more permanent mechanical support for the precious metal nets, as a result of which they are better protected against damage and cracks.
  • bodies with cavities can also be used, the cavities with shaped catalyst bodies e.g. according to DE-A-19805 202 and DE-A-198 19 882, can be filled.
  • Suitable materials for the wire mesh are all high-temperature stable materials such as stainless steel, Hasteloy C, V2A or Kanthai (Fe-Cr-Al alloy, e.g. material number 1.4767), preferably Kanthai.
  • One embodiment of the catalysts described are moldings with cavities such as. B. channels. These can be filled with a solid catalyst.
  • the wire mesh can be used in any form, for example as a fabric, as fabric layers or as fabric packs.
  • Tissue packs can be produced as follows:
  • Woven or knitted fabric packs can be produced, for example, in a simple manner, by winding or stacking two or more differently structured webs of the woven and knitted webs as three-dimensional bodies, which are largely adaptable to the reactor cross section. In the present case, largely means that no exact adaptation to the column cross section is required, but rather that manufacturing tolerances are permitted.
  • the pack is predominantly designed as a roll, which was obtained by winding two or more differently structured webs of the woven and knitted webs.
  • Other geometric shapes are also possible, in particular a cuboid shape obtained by stacking webs.
  • the wire of the tissue or tissue pack generally has a diameter of 5 to 5,000 ⁇ m, preferably 50 to 500 ⁇ m, particularly preferably 60 to 400 ⁇ m, in particular 70 to 250 ⁇ m and generally a mesh size of 5 to 5,000 ⁇ m, preferably 50 to 750 ⁇ m, particularly preferably 60 to 600 ⁇ m, in particular 70 to 450 ⁇ m.
  • Oxides such as MgO, CoO, MoO 3 , NiO, ZnO, Cr 2 O 3 , WO 3 , SrO, CuO / Cu 2 O, MnO 2 or V 2 O 5 , mixed oxides such as CuO-ZnO- are suitable as catalytically active materials.
  • AI 2 O 3 CoO-MgO, CoO-La 2 O 3 , La 2 CuO 4 .Nd 2 CuO 4 , Co-ZnO, or NiO-MoO 3 , perovskites such as LaMnO 3 , CoTiO 3 , LaTiO 3 , CoNiO 3 and Spinels such as CuAI 2 0 4 , ZnAI 2 O 4 , MgAI 2 O, (Cu, Zn) AI 2 O 4 , (Cu, Zn, Mg) AI 2 O 2 , (Cu, Zn, Ba) AI 2 O 4 , (Cu, Zn, Ca) AI 2 O 4 , La 2 NiO 4, preferably spinels such as CuAI 2 O, ZnAI 2 O 4 , MgAI 2 O 4 , (CuZn) AI 2 O 4 , (CuZnMg) AI 2 O, ( CuZnBa) - Al 2 O 4 , (CuZnCa) Al 2 O 4 , particularly preferably spinels such as
  • the catalytically active material preferably has 0.1 to 30% by weight of CuO, 0.1 to 40% by weight of the further metal oxide, in particular ZnO and 50 to 80% by weight of Al 2 O 3 .
  • a catalytically active material which is composed of approximately 8% by weight of CuO, 30% by weight of ZnO and 62% by weight of Al 2 O 3 is particularly preferred.
  • the smallest possible amounts of CuO and other metal oxide are present.
  • a maximum of 3.5% by weight of CuO and a maximum of 10% by weight of ZnO are preferably present.
  • the preparation of the catalytically active materials is generally known or can be produced by generally known methods for producing these materials.
  • the wire of the tissue or tissue packs can be coated as follows:
  • the wire of the tissue or tissue packs can e.g. at temperatures of 100 to 1500 ° C, preferably at 200 to 1400 ° C, particularly preferably at 300 to 1300 ° C.
  • the coating can take place before or after, preferably after the shaping to form tissue packs.
  • Coating with catalytically active materials can be carried out by vapor deposition, sputtering, impregnation, dipping, spraying or coating with powders, preferably with an aqueous and / or alcoholic solution or suspension, preferably with an aqueous suspension.
  • the solids content of the suspension is generally between 2 and 95%, preferably between 3 and 75%, particularly preferably between 5 and 65%.
  • the catalyst packs are generally heat-treated at temperatures from 100 to 1500 ° C., preferably 200 to 1300 ° C., particularly preferably at 300 to 1100 ° C.
  • the weight ratio of coating to wire can be varied within wide limits and is generally from 0.01: 1 to 10: 1, preferably 0.1: 1 to 2: 1, particularly preferably 0.3: 1 to 1: 1 ,
  • the catalysts of the invention can be placed anywhere in the reactor for the production of nitric acid after the production of the nitrogen oxides, preferably in a range in which the temperature is between 500 and 980 ° C., preferably 600 and 970 ° C., particularly preferably 700 and 960 ° C, in particular at the temperature level of the preceding ammonia oxidation at a pressure of 1 to 15 bar, particularly preferably between the noble metal network catalyst, optionally provided with a noble metal recovery network, and the heat exchanger.
  • the catalysts of the invention are generally used as a fixed bed packing.
  • the height of the catalyst bed is generally 1 to 150 cm, preferably 2 to 50 cm, particularly preferably 5 to 10 cm.
  • the residence time on the catalyst bed is generally less than 1 sec, preferably less than 0.5 sec, particularly preferably less than 0.3 s.
  • the catalysts according to the invention can be arranged in reactors for the catalytic oxidation of ammonia to nitrogen oxides, which in the flow direction contain a noble metal catalyst, optionally a noble metal recovery network and heat exchanger in the flow direction between noble metal catalyst / possibly noble metal recovery network and heat exchanger.
  • the device for producing nitric acid from ammonia comprises in this order
  • a reactor according to the preceding paragraph b) an absorption unit for the absorption of nitrogen oxides in an aqueous medium and optionally c) a reduction unit for the selective catalytic reduction of nitrogen oxides.
  • a Kanthal metal fabric strip (length 100 cm, width 3.7 cm), material number 1.4767 (from Montz GmbH, D-40705 Hilden) was air-annealed for 4 h at 900 ° C and then with a gear roller (module 1 , 0mm) corrugated and rolled up with a 97cm long, smooth metal fabric tape, so that a package with vertical channels with a diameter of 4.1 cm was created.
  • the package obtained in this way was mixed with a suspension of 100 g Disperal® AI25 (Sasol), 100 g water and 25 g catalytically active powder with the composition 20% by weight ZnO, 16% by weight CuO, 64% by weight.
  • -% AI 2 O 3 impregnated, dried at 120 ° C for 2 h and tempered in air at 950 ° C for 12 h. The weight gain of the package due to the impregnation was 11.6% after the annealing.
  • a Kanthal metal fabric tape was treated analogously to preparation example 1. 16.7 cm long and 2 cm wide pieces of this metal fabric band were corrugated with a gear roller (module 1.0 mm) and placed on top of one another, so that a 7 cm long, cuboid monolith with vertical channels and a height and Width of 2 cm was created and tied together with 3 V2A wires.
  • the package thus obtained was treated with a suspension of 100 g Disperal® AI25 (Sasol), 100 g water and 25 g catalytically active powder with the composition 20% by weight ZnO, 16% by weight CuO, 64% by weight Al 2 O 3 soaked, dried at 120 ° C for 2 h and air tempered to 900 ° C for 12 h.
  • the weight gain of the package due to the impregnation was 13.4% after the glow.
  • ammonia was in an ammonia-air mixture with a concentration of 12 vol .-% ammonia and 88 vol .-% air on a Pt / Rh network with a load of 36 g / h ammonia per cm 3 network area at a temperature converted from 900 ° C to nitrogen monoxide.
  • a 10 cm high layer of the catalyst from preparation example 1 which flowed through the reaction gas at a temperature of 800 ° C. with a residence time of approx. 0.03 s.
  • the breakdown of N 2 O was 92% (vol .-%).
  • the pressure drop across the catalyst bed was 250 mbar.
  • Example 2 The reaction was carried out analogously to Example 1. However, immediately behind the platinum network, a 10 cm high layer of a catalyst composed of 18% by weight CuO, 20% by weight ZnO and 62% by weight Al 2 O 3 in the form of 3- mm strands used. The breakdown of N 2 O was 85% (vol%). The pressure drop across the catalyst bed was 1450 mbar.

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Abstract

The invention concerns a method for eliminating N2O during nitric acid production, which consists in using as catalysts three-dimensional bodies coated or filled with materials with catalytic effect.

Description

Verfahren zur Entfernung von N2O bei der Salpetersäureherstellung-.Process for removing N 2 O in nitric acid production.
Beschreibungdescription
Die Erfindung betrifft Verfahren zur Entfernung von N2O bei der Salpetersäureherstellung durch beschichtete Raumkörper.The invention relates to methods for removing N 2 O in the production of nitric acid by means of coated spatial bodies.
Bei der großtechnischen Herstellung von Salpetersäure z.B. nach dem Ostwald- Verfahren (Ullmann's Encyclopedia of Industrial Chemistry, 5. Auflage, Band A 17, Sei- ten 293 bis 339 (1991)) entsteht bei der Verbrennung von Ammoniak mit Sauerstoff an einem edelmetallhaltigen Katalysator neben Stickstoffmonoxid und Stickstoffdioxid (beziehungsweise Distickstofftetroxid) in der Regel auch N2O (Distickstoffmonoxid) als Nebenprodukt. Im Gegensatz zu den anderen gebildeten Stickoxiden wird N2O im Laufe des Absorptionsverfahrens nicht vom Wasser absorbiert. Wird keine weitere Stufe zur Entfernung des "Treibhausgases" N2O vorgesehen, so findet es sich im Abgas wieder.In the large-scale production of nitric acid, for example by the Ostwald process (Ullmann's Encyclopedia of Industrial Chemistry, 5th edition, volume A 17, pages 293 to 339 (1991)), ammonia is also burned with oxygen on a catalyst containing noble metals Nitric oxide and nitrogen dioxide (or nitrous oxide) as a rule also N 2 O (nitrous oxide) as a by-product. In contrast to the other nitrogen oxides formed, N 2 O is not absorbed by the water in the course of the absorption process. If no further stage for removing the "greenhouse gas" N 2 O is provided, it is found in the exhaust gas.
Aus der US-A-5,478,549 ist ein Verfahren zur Herstellung von Salpetersäure nach Ostwald bekannt, bei dem der Gehalt an N2O dadurch vermindert wird, dass nach der Oxidation der Gasstrom bei einer Temperatur von mindestens 600CC über ein Katalysatorbett aus Zirkoniumoxid in Form zylindrischer Pellets, angeordnet unterhalb des Edelmetall-Rückgewinnungsnetzes, geführt wird.From US-A-5,478,549 a process for the production of nitric acid according to Ostwald is known, in which the content of N 2 O is reduced by the fact that after the oxidation the gas stream at a temperature of at least 600 C C over a catalyst bed made of zirconium oxide in Form cylindrical pellets, arranged below the precious metal recovery network.
Aus der DE-A-198 05202 und der DE-A-198 19882 sind Katalysatoren, in geometri- sehen Formen wie z.B. Pellets, Zylinder oder Stränge, zur katalytischen Zersetzung von N2O bei der großtechnischen Herstellung von Salpetersäure bekannt.DE-A-198 05202 and DE-A-198 19882 disclose catalysts, in geometric forms such as pellets, cylinders or strands, for the catalytic decomposition of N 2 O in the large-scale production of nitric acid.
Die bislang bekannten Katalysatoren haben den Nachteil, dass sie in Form kompakter Schüttungen einzelner Katalysatorformkörper vorliegen, deren Gasdurchlässigkeit nicht gezielt eingestellt werden kann (Druckabfall und hohe mechanische und statische Belastung). Durch die hohe mechanische Belastung kann es - beim Aufheizen auf Betriebstemperatur und beim Abkühlen -zu Katalysatorabrieb kommen. Dieser Abrieb kann mit dem Prozessgas in nachgeschaltete Apparate mitgeschleppt werden. Die Schüttung aus Katalysatorformkörpern kann sich während des Betriebes verschieben. Das kann teilweise dazu führen, dass an einigen Stellen" die mechanische Unterstützung für die Edelmetall-Katalysatornetze verloren geht und die Netze an diesen Stellen reißen. Dies ist insbesondere dann nachteilig, wenn Edelmetallnetze wiederverwendet werden sollen. Eine ungleichmäßige Schütthöhe kann auch zu einer ungleichmäßigen Gasbelastung des N2O-KataIysators führen, gefolgt von verminderter Effizienz (weni- ger Abbau von N2O). Der vorliegenden Erfindung lag daher die Aufgabe zugrunde, den zuvor genannten Nachteilen abzuhelfen.The previously known catalysts have the disadvantage that they are in the form of compact beds of individual shaped catalyst bodies whose gas permeability cannot be set in a targeted manner (pressure drop and high mechanical and static loads). The high mechanical load can lead to catalyst abrasion when heating up to operating temperature and cooling down. This abrasion can be carried along with the process gas into downstream equipment. The bed of shaped catalyst bodies can shift during operation. This can sometimes lead to being lost in some places "the mechanical support for the precious metal catalyst gauzes and tear the nets at these sites. This is particularly disadvantageous if precious metal nets are to be reused. Uneven bed height can also cause an uneven gas load of the N2O catalyst, followed by reduced efficiency (less degradation of N2O). The object of the present invention was therefore to remedy the disadvantages mentioned above.
Demgemäß wurde ein neues und verbessertes Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung gefunden, welches dadurch gekennzeichnet ist, daß man als Katalysatoren mit katalytisch aktiven Materialien beschichtetet oder gefüllt Raumkörper einsetzt.Accordingly, a new and improved process for the removal of N 2 O in the production of nitric acid has been found, which is characterized in that space bodies are used as catalysts coated or filled with catalytically active materials.
Als Raumkörper eignen sich Formkörper, Netze, Gewebe, Gestricke, Drahtpackungen, Wabenkörper, keramische Monolithe, bevorzugt Wabenkörper, Gewebe, Gestricke, Netze, Drahtpackungen, besonders bevorzugt Gewebe, Gestricke, Netze.Molded bodies, nets, fabrics, knitted fabrics, wire packs, honeycomb bodies, ceramic monoliths, preferably honeycomb bodies, fabrics, knitted fabrics, nets, wire packs, particularly preferably woven fabrics, knitted fabrics, nets, are suitable as spatial bodies.
Die Raumkörper sind in der Regel starr, verschieben sich in der Regel nicht, verringern den mechanischen Abrieb und bieten eine dauerhaftere mechanische Unterstützung für die Edelmetallnetze, wodurch diese vor Beschädigungen und Rissen besser geschützt sind. Alternativ können auch Raumkörper mit Hohlräumen eingesetzt werden, wobei die Hohlräume mit Katalysatorformkörpern z.B. gemäß DE-A-19805 202 und DE-A-198 19 882, aufgefüllt werden können.The spatial bodies are usually rigid, do not usually shift, reduce mechanical abrasion and offer more permanent mechanical support for the precious metal nets, as a result of which they are better protected against damage and cracks. Alternatively, bodies with cavities can also be used, the cavities with shaped catalyst bodies e.g. according to DE-A-19805 202 and DE-A-198 19 882, can be filled.
Als Material für die Drahtgewebe eignen sich alle hochtemperaturstabilen Werkstoffe wie Edelstahl, Hasteloy C, V2A oder Kanthai (Fe-Cr-Al-Legierung, z.B. Werkstoffnummer 1.4767), bevorzugt Kanthai.Suitable materials for the wire mesh are all high-temperature stable materials such as stainless steel, Hasteloy C, V2A or Kanthai (Fe-Cr-Al alloy, e.g. material number 1.4767), preferably Kanthai.
Eine Ausführungsform der beschriebenen Katalysatoren sind Formkörper mit Hohlräu- men wie z. B. Kanäle. Diese können mit einem festen Katalysator gefüllt werden.One embodiment of the catalysts described are moldings with cavities such as. B. channels. These can be filled with a solid catalyst.
Die Drahtgewebe können in beliebiger Form, beispielsweise als Gewebe, als Gewebeschichten oder als Gewebepackungen eingesetzt werden. Gewebepackungen lassen sich wie folgt herstellen:The wire mesh can be used in any form, for example as a fabric, as fabric layers or as fabric packs. Tissue packs can be produced as follows:
Gewebe- bzw. Gestrickepackung lassen sich zum Beispiel auf einfache Weise, durch Aufwickeln oder Aufeinanderlegen von zwei oder mehreren unterschiedlich strukturierten Bahnen der Gewebe- und Gestrickebahnen als Raumkörper herstellbar, die weitgehend dem Reaktorquerschnitt anpassbar sind. Unter weitgehend wird vorliegend verstanden, dass keine exakte Anpassung an den Kolonnenquerschnitt erforderlich ist, sondern dass fertigungstechnische Toleranzen erlaubt sind.Woven or knitted fabric packs can be produced, for example, in a simple manner, by winding or stacking two or more differently structured webs of the woven and knitted webs as three-dimensional bodies, which are largely adaptable to the reactor cross section. In the present case, largely means that no exact adaptation to the column cross section is required, but rather that manufacturing tolerances are permitted.
Die Packung ist vorwiegend als Rolle ausgebildet, die durch Aufwickeln von zwei oder mehreren unterschiedlich strukturierten Bahnen der Gewebe- und Gestrickebahnen erhalten wurde. Möglich sind jedoch auch andere geometrische Formen, insbesondere eine durch Aufeinanderlegen von Bahnen erhaltene Quaderform. Der Draht der Gewebe bzw. Gewebepackungen hat in der Regel einen Durchmesser von 5 bis 5.000 μm, bevorzugt 50 bis 500 μm, besonders bevorzugt 60 bis 400 μm, insbesondere 70 bis 250 μm und in der Regel eine Maschenweite von 5 bis 5.000 μm, bevorzugt 50 bis 750 μm, besonders bevorzugt 60 bis 600 μm, insbesondere 70 bis 450 μm.The pack is predominantly designed as a roll, which was obtained by winding two or more differently structured webs of the woven and knitted webs. However, other geometric shapes are also possible, in particular a cuboid shape obtained by stacking webs. The wire of the tissue or tissue pack generally has a diameter of 5 to 5,000 μm, preferably 50 to 500 μm, particularly preferably 60 to 400 μm, in particular 70 to 250 μm and generally a mesh size of 5 to 5,000 μm, preferably 50 to 750 μm, particularly preferably 60 to 600 μm, in particular 70 to 450 μm.
Als katalytisch aktive Materialien eignen sich Oxide wie z.B. MgO, CoO, MoO3, NiO, ZnO, Cr2O3, WO3, SrO, CuO/Cu2O, MnO2 oder V2O5, Mischoxide wie CuO-ZnO-AI2O3, CoO-MgO, CoO-La2O3, La2CuO4.Nd2CuO4, Co-ZnO, oder NiO-MoO3, Perovskite wie LaMnO3, CoTiO3, LaTiO3, CoNiO3 und Spinelle wie CuAI204, ZnAI2O4, MgAI2O , (Cu, Zn) AI2O4, (Cu, Zn, Mg) AI2O2, (Cu, Zn, Ba) AI2O4, (Cu, Zn, Ca) AI2O4, La2NiO4, bevorzugt Spinelle wie CuAI2O , ZnAI2O4, MgAI2O4, (CuZn) AI2O4, (CuZnMg) AI2O , (CuZnBa)- AI2O4, (CuZnCa) AI2O4, besonders bevorzugt Spinelle wie CuAI2O , (CuZn) AI2O4, (CuZnMg) AI2O4.Oxides such as MgO, CoO, MoO 3 , NiO, ZnO, Cr 2 O 3 , WO 3 , SrO, CuO / Cu 2 O, MnO 2 or V 2 O 5 , mixed oxides such as CuO-ZnO- are suitable as catalytically active materials. AI 2 O 3 , CoO-MgO, CoO-La 2 O 3 , La 2 CuO 4 .Nd 2 CuO 4 , Co-ZnO, or NiO-MoO 3 , perovskites such as LaMnO 3 , CoTiO 3 , LaTiO 3 , CoNiO 3 and Spinels such as CuAI 2 0 4 , ZnAI 2 O 4 , MgAI 2 O, (Cu, Zn) AI 2 O 4 , (Cu, Zn, Mg) AI 2 O 2 , (Cu, Zn, Ba) AI 2 O 4 , (Cu, Zn, Ca) AI 2 O 4 , La 2 NiO 4, preferably spinels such as CuAI 2 O, ZnAI 2 O 4 , MgAI 2 O 4 , (CuZn) AI 2 O 4 , (CuZnMg) AI 2 O, ( CuZnBa) - Al 2 O 4 , (CuZnCa) Al 2 O 4 , particularly preferably spinels such as CuAI 2 O, (CuZn) Al 2 O 4 , (CuZnMg) Al 2 O 4 .
Vorzugsweise weist das katalytisch aktive Material 0,1 bis 30 Gew.-% CuO, 0,1 bis 40 Gew.-% des weiteren Metalloxids, insbesondere ZnO und 50 bis 80 Gew.-% AI2O3 auf.The catalytically active material preferably has 0.1 to 30% by weight of CuO, 0.1 to 40% by weight of the further metal oxide, in particular ZnO and 50 to 80% by weight of Al 2 O 3 .
Besonders bevorzugt ist ein katalytisch aktives Material, das aus etwa 8 Gew.-% CuO, 30 Gew.-% ZnO und 62 Gew.-% AI2O3 aufgebaut ist. Neben dem Spinell liegen dabei möglichst geringe Mengen an CuO und weiterem Metalloxid vor. Vorzugsweise liegen maximal 3,5 Gew.-% CuO und maximal 10 Gew.-% ZnO vor.A catalytically active material which is composed of approximately 8% by weight of CuO, 30% by weight of ZnO and 62% by weight of Al 2 O 3 is particularly preferred. In addition to the spinel, the smallest possible amounts of CuO and other metal oxide are present. A maximum of 3.5% by weight of CuO and a maximum of 10% by weight of ZnO are preferably present.
Die Herstellung der katalytisch aktiven Materialien ist allgemein bekannt oder kann durch allgemein bekannte Verfahren zur Herstellung dieser Materialien hergestellt werden.The preparation of the catalytically active materials is generally known or can be produced by generally known methods for producing these materials.
Die Beschichtung des Drahtes der Gewebe bzw. Gewebepackungen kann wie folgt durchgeführt werden:The wire of the tissue or tissue packs can be coated as follows:
Vor der Beschichtung kann der Draht der Gewebe bzw. Gewebepackungen z.B. bei Temperaturen von 100 bis 1500°C, bevorzugt bei 200 bis 1400°C, besonders bevorzugt bei 300 bis 1300°C getempert werden.Before coating, the wire of the tissue or tissue packs can e.g. at temperatures of 100 to 1500 ° C, preferably at 200 to 1400 ° C, particularly preferably at 300 to 1300 ° C.
Die Beschichtung kann vor oder nach, bevorzugt nach der Formgebung zu Gewebepackungen erfolgen.The coating can take place before or after, preferably after the shaping to form tissue packs.
Die Beschichtung mit katalytisch aktiven Materialien kann durch Aufdampfen, Sputtern, Tränken, Tauchen, Besprühen oder Beschichten mit Pulvern, bevorzugt mit einer wässrigen und/oder alkoholischen Lösungen oder Suspension, bevorzugt mit einer wässrigen Suspension erfolgen. Der Feststoffgehalt der Suspension liegt in der Regel zwischen 2 und 95 %, bevorzugt zwischen 3 und 75 %, besonders bevorzugt zwischen 5 und 65 %.Coating with catalytically active materials can be carried out by vapor deposition, sputtering, impregnation, dipping, spraying or coating with powders, preferably with an aqueous and / or alcoholic solution or suspension, preferably with an aqueous suspension. The solids content of the suspension is generally between 2 and 95%, preferably between 3 and 75%, particularly preferably between 5 and 65%.
Nach der Beschichtung werden die Katalysatorpackungen in der Regel bei Temperaturen von 100 bis 1500°C, bevorzugt 200 bis 1300°C, besonders bevorzugt bei 300 bis 1100°C getempert.After coating, the catalyst packs are generally heat-treated at temperatures from 100 to 1500 ° C., preferably 200 to 1300 ° C., particularly preferably at 300 to 1100 ° C.
Das Gewichtsverhältnis von Beschichtung zum Draht kann in weiten Grenzen variiert werden und liegt in der Regel bei 0,01:1 bis 10:1, bevorzugt 0,1:1 bis 2:1, besonders bevorzugt 0,3:1 bis 1:1.The weight ratio of coating to wire can be varied within wide limits and is generally from 0.01: 1 to 10: 1, preferably 0.1: 1 to 2: 1, particularly preferably 0.3: 1 to 1: 1 ,
Die erfindungsgemäßen Katalysatoren können an beliebiger Stelle des Reaktors zur Saipetersäureherstellung nach der Herstellung der Stickoxide platziert werden, bevor- zugt in einem Bereich, in dem die Temperatur zwischen 500 und 980°C, bevorzugt 600 und 970°C, besonders bevorzugt 700 und 960°C, insbesondere auf dem Temperaturniveau der vorangegangenen Ammoniakoxidation bei einem Druck von 1 bis 15 bar liegt, besonders bevorzugt zwischen dem, ggf. mit einem Edelmetall-Rückgewinnungsnetz versehenen, Edelmetallnetzkatalysator und dem Wärmetauscher.The catalysts of the invention can be placed anywhere in the reactor for the production of nitric acid after the production of the nitrogen oxides, preferably in a range in which the temperature is between 500 and 980 ° C., preferably 600 and 970 ° C., particularly preferably 700 and 960 ° C, in particular at the temperature level of the preceding ammonia oxidation at a pressure of 1 to 15 bar, particularly preferably between the noble metal network catalyst, optionally provided with a noble metal recovery network, and the heat exchanger.
Die erfindungsgemäßen Katalysatoren werden in der Regel als Festbettpackung eingesetzt. Die Höhe des Katalysatorbetts beträgt in der Regel 1 bis 150 cm, bevorzugt 2 bis 50 cm, besonders bevorzugt 5 bis 10 cm. Die Verweilzeit am Katalysatorbett ist im Normalbetrieb in der Regel kleiner als 1 sec, bevorzugt kleiner als 0,5 sec, besonders bevorzugt kleiner als 0,3 s.The catalysts of the invention are generally used as a fixed bed packing. The height of the catalyst bed is generally 1 to 150 cm, preferably 2 to 50 cm, particularly preferably 5 to 10 cm. In normal operation, the residence time on the catalyst bed is generally less than 1 sec, preferably less than 0.5 sec, particularly preferably less than 0.3 s.
Die erfindungsgemäßen Katalysatoren können in Reaktoren zur katalytischen Oxi- dation von Ammoniak zu Stickoxiden, die in Flussrichtung in dieser Reihenfolge einen Edelmetallkatalysator, gegebenenfalls ein Edelmetall-Rückgewinnungsnetz und Wärmetauscher enthalten zwischen Edelmetallkatalysator/gegebenenfalis Edelmetall- Rückgewinnungsnetz und Wärmetauscher angeordnet werden.The catalysts according to the invention can be arranged in reactors for the catalytic oxidation of ammonia to nitrogen oxides, which in the flow direction contain a noble metal catalyst, optionally a noble metal recovery network and heat exchanger in the flow direction between noble metal catalyst / possibly noble metal recovery network and heat exchanger.
Die Vorrichtung zur Herstellung von Salpetersäure aus Ammoniak, umfasst in dieser ReihenfolgeThe device for producing nitric acid from ammonia comprises in this order
a) einen Reaktor gemäß vorangestelltem Absatz, b) eine Absorptionseinheit zur Absorption von Stickoxiden in einem wässrigen Medium und gegebenenfalls c) eine Reduktionseinheit zur selektiven katalytischen Reduktion von Stickoxiden. Beispielea) a reactor according to the preceding paragraph, b) an absorption unit for the absorption of nitrogen oxides in an aqueous medium and optionally c) a reduction unit for the selective catalytic reduction of nitrogen oxides. Examples
Herstellungsbeispiel 1Production Example 1
Ein Kanthal-Metallgewebe-Band (Länge 100 cm, Breite 3,7 cm), Werkstoffnummer 1.4767 (Fa. Montz GmbH, D-40705 Hilden) wurde 4 h bei 900°C an der Luft geglüht und anschließend mit einer Zahnradwalze (Modul 1 ,0mm) gewellt und mit einem 97cm langen, glatten Metallgewebeband aufgerollt, so dass ein Packung mit senkrechten Kanälen mit einem Durchmesser von 4,1 cm entstand. Die so erhaltene Packung wur- de mit einer Suspension aus 100 g Disperal® AI25 (Fa. Sasol), 100 g Wasser und 25 g katalytisch aktives Pulver der Zusammensetzung 20 Gew.-% ZnO, 16 Gew.-% CuO, 64 Gew.-% AI2O3 getränkt, bei 120°C für 2 h getrocknet und 12 h an der Luft bei 950°C getempert. Die Gewichtszunahme der Packung durch die Tränkung betrug nach dem Glühen 11 ,6 %.A Kanthal metal fabric strip (length 100 cm, width 3.7 cm), material number 1.4767 (from Montz GmbH, D-40705 Hilden) was air-annealed for 4 h at 900 ° C and then with a gear roller (module 1 , 0mm) corrugated and rolled up with a 97cm long, smooth metal fabric tape, so that a package with vertical channels with a diameter of 4.1 cm was created. The package obtained in this way was mixed with a suspension of 100 g Disperal® AI25 (Sasol), 100 g water and 25 g catalytically active powder with the composition 20% by weight ZnO, 16% by weight CuO, 64% by weight. -% AI 2 O 3 impregnated, dried at 120 ° C for 2 h and tempered in air at 950 ° C for 12 h. The weight gain of the package due to the impregnation was 11.6% after the annealing.
Herstellungsbeispiel 2Production Example 2
Analog Herstellbeispiel 1 wurde ein Kanthal-Metallgewebe-Band behandelt. Von diesem Metallgewebe-Band wurden 16,7 cm lange und 2 cm breite Stücke mit einer Zahn- radwalze (Modul 1 ,0 mm) gewellt und auf einander gelegt, so dass ein 7 cm langer, quaderförmiger Monolith mit senkrechten Kanälen und einer Höhe und Breite von 2 cm entstand und mit 3 V2A-Drähten zusammengebunden. Die so erhaltene Packung wurde mit einer Suspension aus 100 g Disperal® AI25 (Fa. Sasol), 100 g Wasser und 25 g katalytisch aktives Pulver der Zusammensetzung 20 Gew.-% ZnO, 16 Gew.-% CuO, 64 Gew.-% AI2O3 getränkt, bei 120°C für 2 h getrocknet und 12 h an der Luft auf 900°C getempert. Die Gewichtszunahme der Packung durch die Tränkung betrug nach dem Glühen 13,4 %.A Kanthal metal fabric tape was treated analogously to preparation example 1. 16.7 cm long and 2 cm wide pieces of this metal fabric band were corrugated with a gear roller (module 1.0 mm) and placed on top of one another, so that a 7 cm long, cuboid monolith with vertical channels and a height and Width of 2 cm was created and tied together with 3 V2A wires. The package thus obtained was treated with a suspension of 100 g Disperal® AI25 (Sasol), 100 g water and 25 g catalytically active powder with the composition 20% by weight ZnO, 16% by weight CuO, 64% by weight Al 2 O 3 soaked, dried at 120 ° C for 2 h and air tempered to 900 ° C for 12 h. The weight gain of the package due to the impregnation was 13.4% after the glow.
Beispiel 1example 1
In einer Laborapparatur wurde Ammoniak in einem Ammoniak-Luftgemisch mit einer Konzentration von 12 Vol.-% Ammoniak und 88 Vol.-% Luft an einem Pt/Rh-Netz mit einer Belastung von 36 g/h Ammoniak pro cm3 Netzfläche bei einer Temperatur von 900°C zu Stickstoffmonoxid umgesetzt. Unmittelbar hinter dem Platinnetz war eine 10 cm hohe Schicht des Katalysators aus Hersteilungsbeispiel 1 angeordnet, die das Reaktionsgas bei einer Temperatur von 800°C mit einer Verweilzeit von ca. 0,03 s durchströmte. Der Abbau an N2O betrug 92 % (Vol.-%). Der Druckabfall über der Kata- lysatorschüttung betrug 250 mbar. Beispiel 2In a laboratory apparatus ammonia was in an ammonia-air mixture with a concentration of 12 vol .-% ammonia and 88 vol .-% air on a Pt / Rh network with a load of 36 g / h ammonia per cm 3 network area at a temperature converted from 900 ° C to nitrogen monoxide. Immediately behind the platinum network was a 10 cm high layer of the catalyst from preparation example 1, which flowed through the reaction gas at a temperature of 800 ° C. with a residence time of approx. 0.03 s. The breakdown of N 2 O was 92% (vol .-%). The pressure drop across the catalyst bed was 250 mbar. Example 2
Analog Beispiel 1 wurde der Katalysators aus Herstellungsbeispiel 2 eingesetzt. Der Abbau an N2O betrug 90 % (Vol.-%). Der Druckabfall über der Katalysatorschüttung betrug 192 m bar.Analogously to example 1, the catalyst from preparation example 2 was used. The breakdown of N 2 O was 90% (% by volume). The pressure drop across the catalyst bed was 192 m bar.
Vergleichsbeispiel 1 (analog Beispiel 1 aus DE-A-198 19 882)Comparative Example 1 (analogous to Example 1 from DE-A-198 19 882)
Die Reaktionsdurchführung erfolgte analog Beispiel 1. Es wurde jedoch unmittelbar hinter dem Platinnetz eine 10 cm hohe Schicht eines Katalysators aus 18 Gew.-% CuO, 20 Gew.-% ZnO und 62 Gew.-% AI2O3 in Form von 3-mm-Strängen eingesetzt. Der Abbau an N2O betrug 85 % (Vol-%). Der Druckabfall über der Katalysator- schüttung betrug 1450 mbar.The reaction was carried out analogously to Example 1. However, immediately behind the platinum network, a 10 cm high layer of a catalyst composed of 18% by weight CuO, 20% by weight ZnO and 62% by weight Al 2 O 3 in the form of 3- mm strands used. The breakdown of N 2 O was 85% (vol%). The pressure drop across the catalyst bed was 1450 mbar.
Vergleichsbeispiel 2 (analog Beispiel 1 aus DE-A-198 19882)Comparative Example 2 (analogous to Example 1 from DE-A-198 19882)
Aufbau und Reaktion erfolgte analog Vergleichsbeispiel 1 jedoch wurden 6-mm- Stränge eingesetzt. Der Abbau an N2O betrug 80 % (Vol.-%). Der Druckabfall über der Katalysatorschüttung betrug 1345 mbar. The structure and reaction were analogous to Comparative Example 1, but 6 mm strands were used. The breakdown of N 2 O was 80% (vol .-%). The pressure drop across the catalyst bed was 1345 mbar.

Claims

Patentansprüche claims
1. Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung, dadurch gekennzeichnet, dass man als Katalysatoren mit katalytisch aktiven Materialien beschichtete oder gefüllte Raumkörper einsetzt.1. A process for the removal of N 2 O in the production of nitric acid, characterized in that space bodies coated or filled with catalytically active materials are used as catalysts.
2. Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung, dadurch gekennzeichnet, daß man als Katalysatoren Raumkörper oder Drahtgewebe und/oder -gestricke, die mit katalytisch aktiven Materialien beschichtet oder ge- füllt sind, einsetzt.2. A process for the removal of N 2 O in the production of sipic acid, characterized in that the catalysts used are three-dimensional bodies or wire mesh and / or knitted fabrics which are coated or filled with catalytically active materials.
3. Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung nach Anspruch 1 oder 2, dadurch gekennzeichnet, daß das mit katalytisch aktiven Materialien gefüllte oder beschichteten Raumkörper oder Drahtgewebe und/oder -gestricke ein Katalysatorbett mit einer Höhe von 1 bis 150 cm ausbildet.3. A process for the removal of N 2 O in the manufacture of sipic acid according to claim 1 or 2, characterized in that the space body or wire mesh and / or knitted fabric filled or coated with catalytically active materials forms a catalyst bed with a height of 1 to 150 cm.
4. Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung einem der Ansprüche 1 , 2 oder 3, dadurch gekennzeichnet, daß die Temperatur an dem mit katalytisch aktiven Materialien gefüllten oder beschichteten Raumkörpern oder Drahtgewebe und/oder -gestricke zwischen 500 und 980°C liegt.4. A process for the removal of N 2 O in the production of sipic acid according to one of claims 1, 2 or 3, characterized in that the temperature on the filled or coated with catalytically active materials or bodies or wire mesh and / or knitted fabrics between 500 and 980 ° C. lies.
5. Verfahren zur Entfernung von N2O bei der Saipetersäureherstellung einem der Ansprüche 1 , 2, 3 oder 4, dadurch gekennzeichnet, daß die Verweilzeit an dem mit katalytisch aktiven Materialien kleiner als 1 sec. beträgt.5. A process for the removal of N 2 O in the manufacture of sipic acid according to one of claims 1, 2, 3 or 4, characterized in that the residence time on the with catalytically active materials is less than 1 sec.
6. Katalysatoren zur Entfernung von N2O bei der Saipetersäureherstellung, dadurch gekennzeichnet, daß diese aus einem mit katalytisch aktiven Materialien gefüllten oder beschichteten Raumkörpern oder Drahtgeweben und/oder -gestricken aufgebaut sind.6. Catalysts for the removal of N 2 O in the manufacture of nitric acid, characterized in that they are constructed from a body or wire mesh and / or knitted fabric filled or coated with catalytically active materials.
7. Reaktor zur katalytischen Oxidation von Ammoniak zu Stickoxiden, der in Flussrichtung in dieser Reihenfolge einen Edelmetallkatalysator, gegebenenfalls ein Edelmetall-Rückgewinnungsnetz und Wärmetauscher enthält, dadurch gekennzeichnet, daß zwischen Edelmetallkatalysator/gegebenenfalls Edelmetall- Rückgewinnungsnetz und Wärmetauscher ein mit katalytisch aktiven Materialien gefüllte Raumkörper oder beschichtetes Drahtgewebe und/oder -gestricke angeordnet ist. 7. Reactor for the catalytic oxidation of ammonia to nitrogen oxides, which contains a noble metal catalyst, optionally a noble metal recovery network and heat exchanger in the flow direction, characterized in that between the noble metal catalyst / optionally noble metal recovery network and heat exchanger, a space filled with catalytically active materials or coated wire mesh and / or knitted fabric is arranged.
8. Vorrichtung zur Herstellung von Salpetersäure aus Ammoniak,, umfassend in dieser Reihenfolge a) einen Reaktor gemäß Anspruch 7, i b) eine Absorptionseinheit zur Absorption von Stickoxiden in einem wässrigen Medium und gegebenenfalls c) eine Reduktionseinheit zur selektiven katalytischen Reduktion von Stickoxiden. 8. Device for the production of nitric acid from ammonia, comprising in this order a) a reactor according to claim 7, i b) an absorption unit for the absorption of nitrogen oxides in an aqueous medium and optionally c) a reduction unit for the selective catalytic reduction of nitrogen oxides.
PCT/EP2004/011992 2003-10-29 2004-10-23 Method for eliminating n2o during nitric acid production WO2005042403A2 (en)

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