DE2743031C2 - Catalytic converters for the elimination of nitrogen oxides in exhaust gases - Google Patents
Catalytic converters for the elimination of nitrogen oxides in exhaust gasesInfo
- Publication number
- DE2743031C2 DE2743031C2 DE19772743031 DE2743031A DE2743031C2 DE 2743031 C2 DE2743031 C2 DE 2743031C2 DE 19772743031 DE19772743031 DE 19772743031 DE 2743031 A DE2743031 A DE 2743031A DE 2743031 C2 DE2743031 C2 DE 2743031C2
- Authority
- DE
- Germany
- Prior art keywords
- catalysts
- exhaust gases
- nitrogen oxides
- metal phthalocyanines
- mpc
- 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.)
- Expired
Links
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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1825—Ligands comprising condensed ring systems, e.g. acridine, carbazole
- B01J31/183—Ligands comprising condensed ring systems, e.g. acridine, carbazole with more than one complexing nitrogen atom, e.g. phenanthroline
-
- 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
- B01J2231/00—Catalytic reactions performed with catalysts classified in B01J31/00
- B01J2231/60—Reduction reactions, e.g. hydrogenation
- B01J2231/64—Reductions in general of organic substrates, e.g. hydride reductions or hydrogenations
- B01J2231/641—Hydrogenation of organic substrates, i.e. H2 or H-transfer hydrogenations, e.g. Fischer-Tropsch processes
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/02—Compositional aspects of complexes used, e.g. polynuclearity
- B01J2531/0238—Complexes comprising multidentate ligands, i.e. more than 2 ionic or coordinative bonds from the central metal to the ligand, the latter having at least two donor atoms, e.g. N, O, S, P
- B01J2531/0241—Rigid ligands, e.g. extended sp2-carbon frameworks or geminal di- or trisubstitution
- B01J2531/025—Ligands with a porphyrin ring system or analogues thereof, e.g. phthalocyanines, corroles
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/845—Cobalt
-
- 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
- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
- B01J2531/847—Nickel
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biomedical Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Description
Substanzsubstance
Metall-% 10 63 10 71 10 79 11 80Metal% 10 63 10 71 10 79 11 80
Je nach dem verwendeten MPc können verschiedene Reaktionen wahlweise, z. B. Zerfall oder Reduktion, katalysiert werden.Depending on the MPc used, various reactions can be selected, e.g. B. decay or reduction, be catalyzed.
Herstellung und Wirkung der neuen Katalysatoren werden in den nachstehenden Beispielen gezeigt. Eingesetzt wurde reines NO, das in Pulsen oder kontinuierlich strömend einem Trägergas beigemischt über die Katalysatoren geleitet wurde. Trägergase waren He oder H2, denen O2 beigemischt wurde; auf diese Weise wurde den Katalysatoren auch NOx angeboten. Die angegebenen Umsätze sind auf reines NO bezogen. Der untersuchte Temperaturbereich geht von Zimmertemperatur bis 425° C.The preparation and action of the new catalysts are shown in the examples below. Pure NO was used, which was mixed in pulses or continuously with a carrier gas and passed over the catalytic converters. Carrier gases were He or H 2 to which O 2 was added; in this way, NO x was also offered to the catalytic converters. The stated conversions are based on pure NO. The examined temperature range goes from room temperature to 425 ° C.
Durch die Einwirkung von Stickoxiden oder Sauerstoff auf die reinen MPc entstehen neue Substanzen mit einer gewissen Phasenbreite. Sie unterscheiden sich in ihrem IR-Spektrum und im Temperaturbereich ihrer Beständigkeit eindeutig und deutlich von den bislang beschriebenen »Einlagerungsverbindungen« oder »Addukten«. Am ehesten lassen sie sich als verbrückte Strukturen mit Nitrito- oder Nitrato- bzw. Oxy- oder Peroxy-Gruppen beschreiben. Im Folgenden werden sie vereinfacht als MPc-Oxy-Katalysator bzw. als MPc-Nitrato-Katalysator bezeichnet. Die BET-Oberflächen liegen üblicherweise zwischen 1 und 14 mVg. Sie können durch die in der heterogenen Katalyse üblichen Methoden beträchtlich vergrößert werden. Aufgrund der thermischen Stabilität der neuen Katalysatoren können die neuen Substanzen bis zu Temperaturen von 55O0C eingesetzt werden.The action of nitrogen oxides or oxygen on the pure MPc creates new substances with a certain phase width. They clearly differ in their IR spectrum and in the temperature range of their resistance from the "intercalation compounds" or "adducts" described so far. They can best be described as bridged structures with nitrite or nitrato or oxy or peroxy groups. In the following, they are simply referred to as MPc-Oxy-Catalyst or MPc-Nitrato-Catalyst. The BET surface areas are usually between 1 and 14 mVg. They can be increased considerably by the methods customary in heterogeneous catalysis. Due to the thermal stability of the new catalysts, the new substances can be used up to temperatures of 55O 0 C.
Beispiele
Beispiel 1(MnPc)Examples
Example 1 (MnPc)
Chemisch reines MnPc ist kaum aktiv. Der MnPc-Oxy-Katalysator wird durch Sublimation von MnPc in Gegenwart von O2 erhalten. Ober 125 mg MnPc-Oxy-Katalysator werden im HrStrom bei 395° C 5,6 mg NO geleitet (Reaktionszeit 7,5 Sekunden). Es tritt ausschließlich Zerfall des NO ein, der konstante Umsatz beträgt 4%.Chemically pure MnPc is hardly active. The MnPc oxy catalyst is obtained by subliming MnPc in the presence of O 2 . 5.6 mg NO are passed over 125 mg MnPc oxy catalyst in a stream of Hr at 395 ° C. (reaction time 7.5 seconds). Only decomposition of the NO occurs, the constant conversion is 4%.
Nach weiterer O2-Aktivierung durch Überleiten eines Inertgas-O2-Gemisches (O2-Anteil 5%) bei Temperaturen oberhalb von 20O0C (Mindesteinwirkzeit 600 Sekunden) steigt der Umsatz im H2-Strom auf 54%. Der Anteil an MnPc:Oxy-Katalysator im MnPc und dementsprechend die Aktivität sind also mehr als VerzehnfachtAfter further O 2 activation by passing a inert gas-O 2 mixture (O 2 content 5%) at temperatures above 20O 0 C (minimum contact 600 seconds) increase the sales in the H 2 stream to 54%. The proportion of MnPc : Oxy catalyst in MnPc and, accordingly, the activity are more than tenfold
Beispiel 2(MnPc)Example 2 (MnPc)
Ober !25 mg MnPc-Oxy-Katalysator, erhalten entsprechend Beispiel 1, werden im He-Strom bei 380°C 5,2 mg NO geleitet (Reaktionszeit 5 Sekunden). Der Umsatz beträgt 3%.About 25 mg of MnPc oxy catalyst, obtained according to Example 1, are added at 380 ° C. in a stream of He 5.2 mg NO passed (reaction time 5 seconds). The conversion is 3%.
Die Beispiele machen deutlich, daß der MnPc-Oxy-Katalysator, gewonnen durch entsprechende Behandlung von MnPc mit O2, eine hohe Aktivität besitzt und nur den Zerfall der Stickoxide ohne Ammoniak-Bildung katalysiertThe examples make it clear that the MnPc oxy catalyst, obtained by appropriate treatment of MnPc with O 2 , has a high activity and only catalyzes the decomposition of the nitrogen oxides without the formation of ammonia
20 Beispiel 3(CoPc) 20 Example 3 (CoPc)
Werden über 250 mg reines CoPc (erhalten durch Sublimation unter Inertgas) bei 416°C im H2-Strom 0,85 mg NO geleitet (Reaktionszeit 7,5 Sekunden), so beträgt der Umsatz nur 6%o. Durch Einwirken von 85 mg NO oberhalb 300° C (Einwirkzeit 150 Sekunden) wird aus CoPc teilweise der CoPC-Nitrato-Katalysator gebildet. Bei 410°C werden im HrStrom für 0,3, 3,0 und 30,0 mg NO (Reaktionszeit 0,5 Sekunden/mg NO) jeweils Umsätze von 11% erzielt.If over 250 mg of pure CoPc (obtained by sublimation under inert gas) at 416 ° C in the H 2 stream 0.85 mg of NO are passed (reaction time 7.5 seconds), the conversion is only 6% o. By exposure to 85 mg NO above 300 ° C (exposure time 150 seconds), the CoPC nitrate catalyst is partially formed from CoPc. At 410 ° C, conversions of 11% are achieved in the HrStrom for 0.3, 3.0 and 30.0 mg NO (reaction time 0.5 seconds / mg NO).
Beispiel 4(CoPc)Example 4 (CoPc)
Über 500 mg entsprechend Beispiel 3 mit NO behandeltes CoPc werden bei 425° C im He-Strom 1,0,10,0 und 20,0 mg NO geleitet (Reaktionszeit 2 Sekunden/mg NO). Ein NO-Zerfall tritt nur in Spuren auf.Over 500 mg of CoPc treated with NO according to Example 3 are 1,0,10,0 and at 425 ° C. in a He stream 20.0 mg NO passed (reaction time 2 seconds / mg NO). NO decay occurs only in traces.
Aus dem Vergleich der Beispiele 3 und 4 ergibt sich, daß Stickoxide vom CoPc-Nitrato-Katalysator in Gegenwart von H2 gut zu H2O und N2 reduziert werden, indes der Zerfall nur unwesentlich istA comparison of Examples 3 and 4 shows that nitrogen oxides are effectively reduced to H 2 O and N 2 by the CoPc-Nitrato catalyst in the presence of H 2 , while the decomposition is only insignificant
35 Beispiel 5(NiPc) 35 Example 5 (NiPc)
Reines NiPc, erhalten durch Sublimation unter Intertgas, ist nahezu inaktiv, sowohl beim Zerfall wie bei der Reduktion.Pure NiPc, obtained by sublimation under inert gas, is almost inactive, both during decay and during Reduction.
Aus 250 mg NiPc wird durch Einwirkung von 95 mg NO oberhalb 250° C im H2-StTOm (Mindesteinwirkzeit 150 Sekunden) NiPc-Nitrato-Katalysator hergestellt. Er bewirkt im HrStrom einen Umsatz von 19,5% bei 380°C (Reaktionszeit 0,5 Sekunden/mg NO), einziges Stickstoffprodukt ist N2.From 250 mg NiPc, the action of 95 mg NO above 250 ° C in the H 2 -StTOm (minimum exposure time 150 seconds) produces NiPc nitrate catalyst. In the HrStrom it causes a conversion of 19.5% at 380 ° C (reaction time 0.5 seconds / mg NO), the only nitrogen product is N 2 .
Beispiel 6(NiPc)Example 6 (NiPc)
Werden an 250 mg NiPc-Nilrato-Katalysator (vgl. Beispiel 5) bei 367°C 0,45 mg NO im H2-Strom zur Reaktion gebracht (Reaktionszeit 2 Sekunden/mg NO), wird NO hauptsächlich zu NH3 reduziert, der Umsatz beträgt 32%. If 0.45 mg NO is brought to reaction in the H 2 stream on 250 mg NiPc-Nilrato catalyst (cf. Example 5) at 367 ° C. (reaction time 2 seconds / mg NO), NO is mainly reduced to NH 3 , which Conversion is 32%.
Beispiel 7(NiPc) soExample 7 (NiPc) see above
Über 500 mg NiPc-Nitrato-Katalysator entsprechend Beispiel 5 werden bei 400° C im He-Strom 0,85 mg NO geleitet (Reaktionszeit 2 Sekunden/mg NO). Der Umsatz für den NO-Zerfall liegt unter 3%o.Over 500 mg of NiPc nitrate catalyst according to Example 5, 0.85 mg of NO are added at 400 ° C. in a stream of He conducted (reaction time 2 seconds / mg NO). The conversion for the NO decomposition is below 3% o.
Die Beispiele5 bis 7 zeigen, daß NiPc-Nitrato-Katalysator ein sehr aktiver Katalysator ist, bei dem der NO-Zerfall untergeordnet, die Umsätze der Reduktion indes erheblich sind.Examples 5 to 7 show that NiPc nitrate catalyst is a very active catalyst in which the NO decay is subordinate to the reduction, but the sales are considerable.
Beispiel 8(CuPc)Example 8 (CuPc)
An 500 mg reinem CuPc beträgt der Umsatz bei 425°C bei Einsatz von 0,9,9,0 und 18,0 mg NO (Reaktionszeit 4 Sekunden/mg NO) jeweils nur 5%o.On 500 mg of pure CuPc, the conversion at 425 ° C is when 0.9,9.0 and 18.0 mg NO are used (reaction time 4 seconds / mg NO) each only 5% o.
Beispiel 9(CuPc)Example 9 (CuPc)
Chemische Behandlung des reinen CuPc mit NO bei Temperaturen oberhalb von 300° C (Einwirkzeiten mindestens 300 Sekunden) erhöht den Umsatz: Bei 425°C werden an 250 mg CuPc-Nitrato-Katalysator im HrStrom bei Einsatz von 0,25 mg NO Umsätze von 2 bis 3% festgestellt (Reaktionszeit 0,5 Sekunden/mg NO); N H3 ist nicht nachweisbar.Chemical treatment of the pure CuPc with NO at temperatures above 300 ° C (exposure times at least 300 seconds) increases the conversion: at 425 ° C 250 mg CuPc-Nitrato-catalyst are im HrStrom when using 0.25 mg NO conversions of 2 to 3% determined (reaction time 0.5 seconds / mg NO); N H3 is not detectable.
Beispiele 8 und 9 zeigen, daß CuPc-Nitrato-Katalysator zwar kein sehr aktiver aber in der ausschließlichen ■Examples 8 and 9 show that CuPc nitrate catalyst, although not a very active one, is exclusive
Bildung von N2 und H2O ein sehr selektiver Reduktionskatalysator istFormation of N 2 and H 2 O is a very selective reduction catalyst
Höhere Effizienz und vollständige Beseitigung von NO bei gegebenenfalls gleichzeitiger Senkung der Reaktionstemperaturen läßt sich durch die üblichen Maßnahmen der Festbettkatalyse (z. B. Vergrößerung der Menge, Bettlänge und Oberfläche bzw. volle Ausnutzung der Temperaturstabilität der Katalysatoren bis 550°C) 5 erreichen.Higher efficiency and complete elimination of NO with, if necessary, simultaneous lowering of the reaction temperatures can be achieved by the usual measures of fixed bed catalysis (e.g. increasing the Amount, bed length and surface area or full utilization of the temperature stability of the catalysts up to 550 ° C) Reach 5.
Beispiel 10(CoPc)Example 10 (CoPc)
4 g durch Sublimation erhaltenes CoPc werden durch Mahlen in ihrer BET-Oberfläche auf das fünffache des ίο Wertes entsprechend Beispiel 3 gebracht und bei 3500C mit 180 mg NO behandelt (Mindesteinwirkzeit 300 Sekunden). Der Umsatz bei 412° C beträgt jetzt 98%.4 g obtained by sublimation CoPc be brought by milling in its BET surface area five times the ίο value corresponding to Example 3, and at 350 0 C and 180 mg NO-treated (a minimum contact 300 seconds). The conversion at 412 ° C. is now 98%.
Claims (2)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19772743031 DE2743031C2 (en) | 1977-09-24 | 1977-09-24 | Catalytic converters for the elimination of nitrogen oxides in exhaust gases |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
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DE19772743031 DE2743031C2 (en) | 1977-09-24 | 1977-09-24 | Catalytic converters for the elimination of nitrogen oxides in exhaust gases |
Publications (2)
Publication Number | Publication Date |
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DE2743031A1 DE2743031A1 (en) | 1979-04-05 |
DE2743031C2 true DE2743031C2 (en) | 1984-11-22 |
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Family Applications (1)
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DE19772743031 Expired DE2743031C2 (en) | 1977-09-24 | 1977-09-24 | Catalytic converters for the elimination of nitrogen oxides in exhaust gases |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3522637C1 (en) * | 1985-06-25 | 1986-10-02 | Friedrich Prof. Dr.rer.nat. 2000 Hamburg Steinbach | Catalyst for removing nitrogen oxides, carbon monoxide and / or residual hydrocarbons from exhaust gases |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3121478C2 (en) * | 1981-05-29 | 1986-05-22 | Heiner Dipl.-Chem. Dr. 8000 München Eckert | Process for the optionally selective reduction of unsaturated C, C, C, N, N, N and N, O bonds or of C-halogen or acyl groups |
DE3634553A1 (en) * | 1986-10-10 | 1988-04-21 | Didier Werke Ag | USE OF MANGANE NUMBERS OR MANGANEOUS DEEP SEA ORES IN CATALYSTS TO REDUCE NITROGEN OXIDES IN EXHAUST GAS |
DE3917900A1 (en) * | 1989-06-01 | 1990-12-06 | Steinbach Friedrich | USE OF A CARRIER-BASED TRANSITION METAL PHTHALOCYANINE CATALYST TO REMOVE ORGANIC COMPOUNDS CONTAINING OXYGEN AND / OR NITROGEN FROM EXHAUST GASES |
-
1977
- 1977-09-24 DE DE19772743031 patent/DE2743031C2/en not_active Expired
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE3522637C1 (en) * | 1985-06-25 | 1986-10-02 | Friedrich Prof. Dr.rer.nat. 2000 Hamburg Steinbach | Catalyst for removing nitrogen oxides, carbon monoxide and / or residual hydrocarbons from exhaust gases |
WO1987000077A1 (en) * | 1985-06-25 | 1987-01-15 | Friedrich Steinbach | Catalytic device for eliminating nitrogen oxides, carbon monoxide and/or residual hydrocarbons contained in exhaust gases |
Also Published As
Publication number | Publication date |
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DE2743031A1 (en) | 1979-04-05 |
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