DE597515C - Process for the preparation of hydrocarbons from gases containing carbon oxides and hydrogen - Google Patents

Process for the preparation of hydrocarbons from gases containing carbon oxides and hydrogen

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Publication number
DE597515C
DE597515C DEG78657D DEG0078657D DE597515C DE 597515 C DE597515 C DE 597515C DE G78657 D DEG78657 D DE G78657D DE G0078657 D DEG0078657 D DE G0078657D DE 597515 C DE597515 C DE 597515C
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Prior art keywords
hydrocarbons
hydrogen
preparation
containing carbon
gases containing
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Expired
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DEG78657D
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German (de)
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Dr Alfred Braune
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STICKSTOFFWERKE
Gewerkschaft Victor
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STICKSTOFFWERKE
Gewerkschaft Victor
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Priority to DEG78657D priority Critical patent/DE597515C/en
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
    • C07C1/04—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon monoxide with hydrogen
    • C07C1/0425—Catalysts; their physical properties
    • C07C1/043—Catalysts; their physical properties characterised by the composition
    • C07C1/0435—Catalysts; their physical properties characterised by the composition containing a metal of group 8 or a compound thereof
    • C07C1/044—Catalysts; their physical properties characterised by the composition containing a metal of group 8 or a compound thereof containing iron
    • 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
    • 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
    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • B01J27/06—Halogens; Compounds thereof
    • B01J27/08—Halides
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
    • C07C1/04—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon monoxide with hydrogen
    • C07C1/0425—Catalysts; their physical properties
    • C07C1/043—Catalysts; their physical properties characterised by the composition
    • C07C1/0435—Catalysts; their physical properties characterised by the composition containing a metal of group 8 or a compound thereof
    • 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
    • B01J23/90—Regeneration or reactivation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
    • C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
    • C07C2523/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals of the platinum group metals
    • C07C2523/42—Platinum
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
    • C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
    • C07C2523/74—Iron group metals
    • C07C2523/745—Iron
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
    • C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
    • C07C2523/74—Iron group metals
    • C07C2523/75—Cobalt
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
    • C07C2523/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of the iron group metals or copper
    • C07C2523/74—Iron group metals
    • C07C2523/755—Nickel
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • C07C2527/06—Halogens; Compounds thereof
    • C07C2527/08—Halides
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Catalysts (AREA)

Description

Verfahren zur Darstellung von Kohlenwasserstoffen aus kohlenoxyd-und wasserstoffhaltigen Gasen Die vorliegende Erfindung betrifft ein Verfahren zur Darstellung von Kohlenwasserstoffen aus kohlenoxyd- und wasserstoffhaltigen Gasen. Als Katalysatoren für derartige Umsetzungen sind außer Metallen, wie Chrom, Mangan, Wolfram, Uran, Kupfer, Silber oder Mischungen derselben oder ihrer Oxyde, hauptsächlich die Metalle der Eisengruppe vorgeschlagen worden, gegebenenfalls auch Metalle der Platingruppe. Je nach der Art des verwendeten Katalysators und den sonstigen Reaktionsbedingungen entstehen hierbei entweder vorwiegend sauerstoffhaltige Verbindungen, wie. Alkohole, Ketone usw., oder in stärkerem Maße flüssige bzw. gasförmige Kohlenwasserstoffe.Process for the preparation of hydrocarbons from carbon oxide and Hydrogen-Containing Gases The present invention relates to a method of preparation of hydrocarbons from gases containing carbon oxides and hydrogen. As catalysts in addition to metals such as chromium, manganese, tungsten, uranium, Copper, silver, or mixtures thereof or their oxides, chiefly the metals the iron group has been proposed, possibly also metals of the platinum group. Depending on the type of catalyst used and the other reaction conditions either predominantly oxygen-containing compounds arise here, such as. Alcohols, Ketones etc., or to a greater extent liquid or gaseous hydrocarbons.

Es ist bekannt, daß man die ölbildende Wirkung der Katalysatoren durch bestimmte Beimischungen erhöhen kann. Zu diesem Zweck hat man bisher Sauerstoffverbindungen der Alkalien, insbesondere deren Oxyde bzw. It is known that the oil-forming effect of the catalysts can increase through certain admixtures. Oxygen compounds have hitherto been used for this purpose of alkalis, especially their oxides or

Hydroxyde oder Carbonate angewandt. Mit derartig aktivierten Katalysatoren werden jedoch unter Verwendung von kohlenoxyd-und wasserstoffhaltigen Gasen teile gewonnen, die einen erheblichen Sauerstoffgehalt von etwa 20 Cyo aufweisen. Sie enthalten also beträchtliche Mengen Alkohole, Aldehyde, Säuren, Ketone usw.Hydroxides or carbonates applied. With such activated catalysts However, parts are made using gases containing carbon dioxide and hydrogen obtained, which have a significant oxygen content of about 20 Cyo. she therefore contain considerable amounts of alcohols, aldehydes, acids, ketones, etc.

Man hat auch schon einen Zusatz von Alkalichlorid zu derartigen Katalysatoren vorgeschlagen, ohne daß sich jedoch hierbei eine befriedigende Ausbeute an Kohlenwasserstoffen ergibt. Alkali metal chloride has also been added to such catalysts proposed without, however, a satisfactory yield of hydrocarbons results.

Andererseits hat man für die Zwecke der Methanolsynthese bereits Katalysatoren vorgeschlagen, die in der Hauptsache aus Oxyden der Metalle der zweiten Gruppe des periodischen Systems, wie Zink oder Magnesium, in Mischung mit Oxyden anderer Metalle (Chrom, Nickel, Kobalt usw.) bestehen, denen Erdalkalihalogenide zugesetzt sind. On the other hand, one already has for the purposes of methanol synthesis Catalysts proposed, which mainly consist of oxides of the metals of the second Group of the periodic table, such as zinc or magnesium, mixed with oxides Other metals (chromium, nickel, cobalt, etc.) consist of alkaline earth halides are added.

Es wurde nun gefunden, daß ein Zusatz von Halogeniden der Erdalkalien in geringen Mengen zu einem aus Metallen der Eisen-oder Platingruppe bestehenden Grundkatalysator die Bildung von Kohlenwasserstoffen erheblich begünstigt. It has now been found that the addition of halides of alkaline earths in small amounts to one consisting of metals of the iron or platinum group Basic catalyst significantly favors the formation of hydrocarbons.

Bei Verwendung der neuen Katalysatoren entstehen fast ausschließlich Kohlenwasserstoffe vom Äthylen- bzw. Äthantyp. 85 °l0 dieser Kohlenwasserstoffe sieden innerhalb einer Grenze von 40 bis 2000 C. Die Ausbeute an Kohlenwasserstoffen, berechnet auf die angewandte Kohlenoxydmenge, ist erheblich höher als bei den bekannten Verfahren. When using the new catalytic converters, almost exclusively Hydrocarbons of the ethylene or ethane type. 85 ° l0 of these hydrocarbons boil within a limit of 40 to 2000 C. The yield of hydrocarbons, calculated on the amount of carbon dioxide used, is considerably higher than with the known ones Procedure.

Der Sauerstoffgehalt des neuen Reaktionsproduktes beträgt höchstens 20/0.The oxygen content of the new reaction product is at most 20/0.

Bei Anwendung der bisher vorgeschlagenen, alkalisch reagierenden Aktivatorzusätze zum Grundkatalysator entstehen ferner nicht unerhebliche Mengen Säuren, und zwar wasserlösliche sowohl wie wasserunlösliche. When using the previously proposed, alkaline reacting Activator additives to the basic catalyst also result in not inconsiderable amounts Acids, both water-soluble and water-insoluble.

Bei Anwendung der Halogenide der Erdalkalien sind Säuren weder in dem Öl noch in der wasserlöslichen Schicht nachzuweisen.When using the halides of the alkaline earths are Acids cannot be detected either in the oil or in the water-soluble layer.

Außerdem besitzt das gebildete Öl keinerlei Löslichkeit in Wasser, während die mit den bisherigen Zusätzen erzeugten Öle nach den vorliegenden Literaturangaben eine Wasserlöslichkeit bis zu 10% aufweisen, die hauptsächlich auf die Anwesenheit von Alkoholen zurückzuführen ist.In addition, the oil formed has no solubility in water, while the oils produced with the previous additives according to the available literature have a water solubility up to 10%, mainly due to the presence is due to alcohol.

Ferner zeigt sich, daß die Anwendung der genannten Erdalkalisalze unter sonst gleichen Bedingungen die Neigung-der Eisenmetalle, Kohlenoxyd unter Kohlenstoffabscheidung zu zersetzen, weitgehend vermindert. Diese sonst stets auftretende Kohlenstoffabscheidung auf dem Katalysator mindert seine Wirksamkeit= sehr schnell herab. Die neue Arbeitsweise gewährleistet eine wesentlich längere Lebensdauer des Katalysators. It is also shown that the use of the alkaline earth metal salts mentioned all other things being equal, the inclination of ferrous metals, carbon oxide below Decompose carbon deposition, largely diminished. This always occurs Carbon deposition on the catalyst reduces its effectiveness = very quickly down. The new way of working ensures that the Catalyst.

Eine weitere unangenehme Begleiterscheinung bei der Herstellung von Kohlenwasserstoffen aus koblenoxyd- und wasserstoffhaltigen Gasen, die man bei den bisher bekannten Arbeitsweisen in Kauf nehmen mußte, ist die Entstehung von paraffinartigen Verbindungen, die den Katalysator einhüllen und inaktiv machen und außerdem zu einem Zusammenbacken des Katalysators führen. Bei Anwendung der oben beschriebenen Zusätze wird die Entstehung dieser Verbindungen sehr verringert, die Neigung des Katalysators zum Zusammenbacken vermindert und infolgedessen ebenfalls eine längere Lebensdauer des Katalysators erzielt. Während beispielsweise der Katalysator bei Anwendung alkalisch reagierender Zusätze bereits nach 48 Stunden Betriebsdauer auf rund 20% seinerAnfangsleistung zurückgeht, ist derselbe Katalysator bei Anwendung von Calciumchlorid als Aktivator noch nach drei tagen im Besitze seiner vollen Leistungsfähigkeit. Another unpleasant side effect in the production of Hydrocarbons from gases containing carbon dioxide and hydrogen, which are found in the previously known working methods had to be accepted, is the emergence of paraffin-like Compounds that envelop the catalyst and make it inactive and also to one Lead caking of the catalyst. When using the additives described above the formation of these compounds is greatly reduced, the tendency of the catalyst for caking and consequently also a longer service life of the catalyst achieved. For example, while the catalyst is alkaline when used reacting additives to around 20% of their initial performance after 48 hours of operation decreases is the same catalyst when using calcium chloride as an activator even after three days in full capacity.

Beispiel Als Ausgangsmaterial zur Herstellung des Katalysators wird Eisenoxyduloxyd verwandt, das mit Wasserstoff bei etwa 500 bis I000 at reduziert wird. 100 g des so erhaltenen metallischen Eisens, das eine große Oberfläche aufweist, werden nun mit einer Lösung, welche 0,1 bis 10% (zweckmäßigerweise 2,5 %) CaCl2, bezogen auf das Eisen, enthält, zur trocknung gebracht. Der so behandelte Katalysator wird in ein Kontaktrohr eingeführt und über denselben ein Gas, das Kohlenoxyd und Wasserstoff im richtigen Verhältnis, beispielsweise 1:2, enthält, geleitet. Man arbeitet zweckmäßig mit einem Druck von etwa 100 at, jedoch kann dieser auch niedriger oder höher liegen. Die Temperatur wählt man nicht über 300 bis 3500 C bei einem stündlichen Gasdurchsatz von etwa 1000 1 und folgender Zusammensetzung des Ausgangsgases: 0,8 % CO2, 31,0% CO, 66,8 01, H2, I,4 Olo N2. Example As starting material for the production of the catalyst is Related to iron oxide, which reduces with hydrogen at about 500 to 1000 at will. 100 g of the metallic iron thus obtained, which has a large surface area, are now with a solution, which 0.1 to 10% (expediently 2.5%) CaCl2, based on the iron it contains, dried. The catalyst thus treated is introduced into a contact tube and over the same a gas, the carbon oxide and Hydrogen in the correct ratio, for example 1: 2, is passed. Man works expediently with a pressure of about 100 at, but this can also be lower or higher. The temperature is not chosen above 300 to 3500 C for one hourly gas throughput of about 1000 1 and the following composition of the starting gas: 0.8% CO2, 31.0% CO, 66.8 01, H2, I, 4 Olo N2.

Es werden rund 40% des als Kohlenoxyd eingebrachten Kohlenstoffes als Kohlenwasserstoffe erhalten. Diese Kohlenwasserstoffe von wasserhellem Aussehen haben folgende Konstanten: d20=0,720.Around 40% of the carbon introduced as carbon dioxide is used obtained as hydrocarbons. These hydrocarbons have a water-white appearance have the following constants: d20 = 0.720.

Siedebeginn 420 C. Beginning of boiling 420 C.

Es gehen über bis 100°C ........... 40 bis 60%, - 150°C........... 66 - 80%, - 200°C........... 85 - 95%. It goes over to 100 ° C ........... 40 to 60%, - 150 ° C ........... 66 - 80%, - 200 ° C ........... 85 - 95%.

Elementarzusammensetzung : C 84,2% : 88,16%, H 14,6% : 15,23%, O 1,2% : 0,61%. Elemental composition: C 84.2%: 88.16%, H 14.6%: 15.23%, O 1.2%: 0.61%.

Die Löslichkeit der Kohlenwasserstoffe in konzentrierter Schwefelsäure beträgt 15 bis 20 0/0. Es handelt sich also vorwiegend um Kohlenwasserstoffe von Benzincharakter.The solubility of hydrocarbons in concentrated sulfuric acid is 15 to 20 0/0. So it is mainly about hydrocarbons of Petrol character.

Eine besondere Eigenschaft des Katalysators ist die, daß bei Einhaltung der richtigen Temperatur bei der Synthese nur wenig Kohlensäure und Methan entsteht, wie aus nachfolgender Endgasanalyse hervorgeht: CO2................ 1,9%, CnH2n ............. 1,9%, CO ................ 25,5%, H2 ................ 62,4%, C2H6............... 2,2%, CH4 ............... 4,5%, N2 ................ 1,6%. A special property of the catalyst is that if it is adhered to at the right temperature, the synthesis produces little carbonic acid and methane, as can be seen from the following end gas analysis: CO2 ................ 1.9%, CnH2n ............. 1.9%, CO ................ 25.5%, H2 ......... ....... 62.4%, C2H6 ............... 2.2%, CH4 ............... 4.5%, N2 ................ 1.6%.

Das Gas ist, wie ersichtlich, ohne weiteres zum nochmaligen überleiten über den Kontakt zu verwenden. As can be seen, the gas can be passed over again without further ado to use via the contact.

Claims (1)

PATENTANSPRUCH: Verfahren zur Darstellung von Kohlenwasserstoffen aus kohlenoxyd- und wasserstoffhaltigen Gasen unter Verwendung von Katalysatoren der achten Gruppe desperiodischen Systems, wieEisen, Nickel, Kobalt, Platin bzw. Mischungen oder Legierungen dieser Metalle, dadurch gekennzeichnet, daß der lediglich aus den genannten Metallen bestehende Katalysator zur Aktivierung eine geringe Beimischung von Halogeniden der Erdalkalien enthält. PATENT CLAIM: Process for the preparation of hydrocarbons from gases containing carbon oxide and hydrogen using catalysts the eighth group of the periodic system, such as iron, nickel, cobalt, platinum or Mixtures or alloys of these metals, characterized in that the only Catalyst consisting of the metals mentioned for activation, a small admixture of halides of alkaline earths.
DEG78657D 1931-01-29 1931-01-29 Process for the preparation of hydrocarbons from gases containing carbon oxides and hydrogen Expired DE597515C (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE975335C (en) * 1937-04-15 1961-11-09 Basf Ag Process for the conversion of carbon oxide with hydrogen in the presence of iron catalysts
EP0016851A1 (en) * 1978-09-20 1980-10-15 The Dow Chemical Company Process for producing olefins from carbon monoxide and hydrogen

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE975335C (en) * 1937-04-15 1961-11-09 Basf Ag Process for the conversion of carbon oxide with hydrogen in the presence of iron catalysts
EP0016851A1 (en) * 1978-09-20 1980-10-15 The Dow Chemical Company Process for producing olefins from carbon monoxide and hydrogen

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