DE870245C - Process for the activation of cobalt and / or nickel containing catalysts for the hydrogenation of carbons - Google Patents
Process for the activation of cobalt and / or nickel containing catalysts for the hydrogenation of carbonsInfo
- Publication number
- DE870245C DE870245C DER2391D DER0002391D DE870245C DE 870245 C DE870245 C DE 870245C DE R2391 D DER2391 D DE R2391D DE R0002391 D DER0002391 D DE R0002391D DE 870245 C DE870245 C DE 870245C
- Authority
- DE
- Germany
- Prior art keywords
- hydrogenation
- cobalt
- activation
- carbons
- containing catalysts
- 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
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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
- C07C1/0445—Preparation; Activation
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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
- 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
- B01J23/78—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 alkali- or alkaline earth metals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/15—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively
- C07C29/151—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases
- C07C29/153—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the catalyst used
- C07C29/156—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of oxides of carbon exclusively with hydrogen or hydrogen-containing gases characterised by the catalyst used containing iron group metals, platinum group metals or compounds thereof
-
- 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
Landscapes
- 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)
- Catalysts (AREA)
Description
Verfahren zur Aktivierung von Kobalt und/oder Nickel enthaltenden Katalysatoren für die Kohlenoxydhydrierung Für die Herstellung von Kobalt und/oder Nickel enthaltenden Katalysatoren für die Kohlenoxydhydrierung durch Fällungen wurden bisher ausschließlich Lösungen der Nitrate der genannten Metalle benutzt, wobei an die Reinheit der verwandten Nitrate ganz besondere Anforderungen gestellt werden, um die ausreichende Aktivität der fertigen Kontakte durch vorzügliche Beschaffenheit der Ausgangssubstanzen sicherzustellen.Process for activating cobalt and / or nickel containing Catalysts for the hydrogenation of carbohydrates For the production of cobalt and / or Nickel containing catalysts for the hydrogenation of caroxides by precipitation were made so far only solutions of the nitrates of the metals mentioned have been used, whereby Very special requirements are placed on the purity of the nitrates used, about the sufficient activity of the finished contacts due to their excellent condition ensure the starting substances.
Es wurde nun festgestellt, daß es nicht erforderlich ist, die Ausgangssubstanzen für die Kobalt und/oder Nickel enthaltenden Nitratlösungen in der bisher erforderlichen Reinheit zu verwenden, wenn die in üblicher Weise hergestellten Fällungen durch Waschen mit Alkalihydroxyden bzw. -carbonaten aktiviert werden. Der Aktivierung kann eine Waschung mit Wasser vorhergehen. Besonders günstige Ergebnisse werden erhalten, wenn die in üblicher Weise durchgeführte Fällung zunächst mit Wasser gewaschen, darauf aktiviert und anschließend der Überschuß des Alkalis durch nochmaliges Waschen mit Wasser beseitigt wird. Die zur Aktivierung der Kobalt- und Nickelfällungen dienenden Lösungen von Alkalihydroxyden und -carbonaten werden in einer Stärke von 1/20 n angewandt. It has now been found that it is not necessary to use the starting substances for the nitrate solutions containing cobalt and / or nickel in the amount previously required Use purity if the precipitates produced in the usual way Washing can be activated with alkali hydroxides or carbonates. The activation can be preceded by washing with water. Particularly favorable results will be obtained when the precipitation, carried out in the usual way, is first washed with water, then activated and then the excess of the alkali by washing again is eliminated with water. The activation of the cobalt and nickel precipitates Serving solutions of alkali hydroxides and carbonates are in a strength of 1/20 n applied.
Durch das nachstehend aufgeführte Beispiel wird nachgewiesen, welche Vorteile durch die Aktivierung der Fällung eines der genannten Metalle durch Waschen mit -Alkalilösung erhalten werden. The example below demonstrates which Advantages of activating the precipitation of one of the metals mentioned by washing can be obtained with alkali solution.
Beispiel Ein Kontakt mit 100 Teilen CO, I5 Teilen ThO2 und 200 TeilenKieselgur wird aus einer rohen ungereinigten Auflösung ausgebrauchter Kontaktmasse, die 40 g Co in Form von Nitrat enthält, durch Zusatz von Soda in einer Stärke von 100 g/l in der Hitze ausgefällt. Example A contact with 100 parts of CO, 15 parts of ThO2 and 200 parts of diatomaceous earth is made from a raw, uncleaned dissolution of spent contact mass, the 40th g Co in the form of nitrate, by adding soda at a strength of 100 g / l precipitated in the heat.
Die Behandlung des Niederschlages wird einmal durch Waschen mit Wasser ausgeführt, wobei auf 25 g Co 3 1 Wasser zur Anwendung gelangen (a).The treatment of the precipitate is once by washing with water carried out, with 3 1 water being used for 25 g of Co (a).
Im zweiten Falle werden auf 25 g Co zunächst 1 1 Wasser, darauf 1 1 1/20 n - K OH und anschließend 1 1 Wasser angewandt (b). Die Kontakte, die aus den derart behandelten Niederschlägen hergestellt werden, zeigen die folgende Wirksamkeit: O/, / Kontraktion Ausbeute / cbrt Gas nach 270 Stunden (a) 24 25 ccm Ö1 36 ccm Benzin 6I ccm Flüssigprodukte (b) 44 55 ccm Ö1 36 ccm Benzin 91 ccm Flüssigprodukte Es ist von anderer Seite vorgeschlagen worden, die Aktivitätserhöhung von Kontakten der Kohlenoxydhydrierung dadurch zu bewirken, daß der Kontakt mit Alkaliverbindungen in einer solchen Menge- imprägniert wird, daß er, auf die Metalle der Eisengruppe bezogen, weniger als rund 601o, vorzugsweise eine Menge von 0,4 bis o,6 0/o, an Alkalimetall enthält.In the second case, 1 liter of water is added to 25 g of Co, followed by 1 1 1/20 n - K OH and then 1 1 water applied (b). The contacts that made the precipitates treated in this way show the following effectiveness: O /, / contraction yield / cbrt gas after 270 hours (a) 24 25 cc oil 1 36 cc gasoline 6I cc liquid products (b) 44 55 cc oil 1 36 cc petrol 91 cc liquid products Es has been suggested by other sources to increase the activity of contacts to bring about the hydrogenation of carbohydrates by contact with alkali compounds in such an amount - is impregnated that it, on the metals of the iron group based, less than about 601o, preferably an amount of 0.4 to 0.60 / o Contains alkali metal.
Weiter wurde angegeben, daß allzu sorgfältiges Auswaschen des Carbonatniederschlages eines katalytisch wirksamen Metalls mit Wasser durch zu starke Erniedrigung des Alkaligehaltes einen ungünstigen Einfluß auf die Kontaktaktivität habe. Die nachstehenden Vergleichsversuche zeigen, daß die katalytische Wirksamkeit von Kontakten für die Kohlenoxydhydrierung nicht an die Menge des in ihnen enthaltenden Alkalis innerhalb eines gewissen Gebietes gebunden ist, sondern an die Art, in der die Herstellung der Kontakte durch Behandlung der Lösungen und der Fällungen mit Alkali durchgeführt wird, und daß des weiteren die Wirksamkeit der Kontakte nicht an das Vorhandensein bestimmter Mindestmengen von Alkali. geknüpft ist.It was also stated that the carbonate precipitate was washed out too carefully of a catalytically active metal with water due to excessive lowering of the Alkali content have an unfavorable influence on the contact activity. The following Comparative tests show that the catalytic effectiveness of contacts for Carbohydrate hydrogenation does not adhere to the amount of alkali contained in them within a certain area is bound, but to the way in which the manufacture the contacts are carried out by treating the solutions and the precipitates with alkali and that, furthermore, the effectiveness of the contacts does not affect the presence certain minimum quantities of alkali. is linked.
Es wurden zwei Kontakte in der folgenden Weise hergestellt: I48 ccm Co (N O2)2-Lösung = 25 g Co 20,2 ccm Th(NO3)4-Lösung = 3,75 g ThO2 wurden mit 330 ccm H20 verdünnt und zum Sieden erhitzt. Gleichzeitig wurden 750 ccm H20 mit 6I g NaCO3 zum Kochen gebracht und die siedende Co-Lösung unter starkem Rühren zugegeben. Hierauf wurden 25 g Kieselgur eingerührt. Two contacts were made in the following manner: 148 cc Co (N O2) 2 solution = 25 g Co 20.2 ccm Th (NO3) 4 solution = 3.75 g ThO2 were mixed with 330 ccm H20 diluted and heated to the boil. At the same time, 750 cc H20 with 6I Bring g NaCO3 to the boil and add the boiling Co solution with vigorous stirring. 25 g of kieselguhr were then stirred in.
Die Mutterlauge wurde abgenutscht. Kontakt 1 wurde mit 250 ccm heißem Wasser gewaschen. Kontakt 2 wurde heiß noch einmal mit 1 1 H2O, 1 1 1/20 n-K2 C Q und I1 H20 gewaschen. The mother liquor was filtered off with suction. Contact 1 became hot with 250 cc Water washed. Contact 2 got hot again with 1 1 H2O, 1 1 1/20 n-K2 C Q and I1 H20 washed.
Der Gehalt der getrockneten Kontakte an Alkalimetall betrug: I. o,o28 0/o bez. auf Co 2. 0,24 0/o bez. auf Co Die katalytische Prüfung ergab im Mittel-über 500 Stunden bei I85" folgende Werte: Kontraktion Ö1 Flüssige Produkte 1. 5 ovo 3 ccm 9 ccm 2. 64 ovo 71 ccm II3 ccm PATENTANSPRACHE I. Verfahren zur Herstellung von Kobalt und/ oder Nickel und hochadsorptive Trägerstoffe enthaltenden Kontakten für die Kohlenoxydhydrierung; dadurch gekennzeichnet, daß die Auswaschung der in den Ausgangssubstanzen enthaltenen und bei der Fällung gebildeten löslichen Bestandteile aus Fällungen, die in bekannter Weise aus Lösungen von Nitraten von katalytisch wirksamen Metallverbindungen mit löslichen Carbonaten erhalten werden, unter Anwendung einer Waschung mit Lösungen von Alkalihydroxyden bzw. -carbonaten von einer Konzentration von 1/20 n durchgeführt wird. The alkali metal content of the dried contacts was: I. o, o28 0 / o based on Co 2. 0.24 0 / o based on Co The catalytic test showed an average of about 500 hours at I85 "the following values: Contraction Ö1 Liquid products 1. 5 ovo 3 cc 9 cc 2. 64 ovo 71 cc II3 cc PATENT APPEAL I. Method of manufacture of contacts containing cobalt and / or nickel and highly adsorptive carriers for carbohydrate hydrogenation; characterized in that the leaching of the in Soluble constituents contained in the starting substances and formed during the precipitation from precipitations, which in a known manner from solutions of nitrates by catalytic effective metal compounds with soluble carbonates can be obtained using washing with solutions of alkali hydroxides or carbonates of one concentration of 1/20 n is carried out.
Claims (1)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DER2391D DE870245C (en) | 1939-04-16 | 1939-04-16 | Process for the activation of cobalt and / or nickel containing catalysts for the hydrogenation of carbons |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DER2391D DE870245C (en) | 1939-04-16 | 1939-04-16 | Process for the activation of cobalt and / or nickel containing catalysts for the hydrogenation of carbons |
Publications (1)
Publication Number | Publication Date |
---|---|
DE870245C true DE870245C (en) | 1953-03-12 |
Family
ID=7395978
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DER2391D Expired DE870245C (en) | 1939-04-16 | 1939-04-16 | Process for the activation of cobalt and / or nickel containing catalysts for the hydrogenation of carbons |
Country Status (1)
Country | Link |
---|---|
DE (1) | DE870245C (en) |
-
1939
- 1939-04-16 DE DER2391D patent/DE870245C/en not_active Expired
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