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Boron-Promoted Reducible Metal Oxide and Methods for Their Use

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Boron-Promoted Reducible Metal Oxide and Methods for Their Use Europaisches Patentamt J European Patent Office © Publication number: 0 253 522 B1 Office europeen des brevets EUROPEAN PATENT SPECIFICATION © Date of publication of patent specification: 16.10.91 © Int. Cl.5: C07C 2/84, C07C 5/48, B01J 23/34, C01G 45/02 © Application number: 87305522.2 © Date of filing: 22.06.87 Boron-promoted reducible metal oxide and methods for their use. © Priority: 23.06.86 US 877574 Proprietor: ATLANTIC RICHFIELD COMPANY 515 South Flower Street © Date of publication of application: Los Angeles California 90071 (US) 20.01.88 Bulletin 88/03 Inventor: Gastinger, Robert G. © Publication of the grant of the patent: 4502 School Lane 16.10.91 Bulletin 91/42 Brookhaven Pennsylvania 19015(US) Inventor: Jones, Andrew C. © Designated Contracting States: 24 Clearbrook Road BE DE FR NL Newton Square Pennsylvania 19073(US) Inventor: Sofranko, John A. © References cited: 452 Summit House EP-A- 0 183 225 West Chester Pennsylvania 19382(US) US-A- 4 285 835 US-A- 4 443 649 US-A- 4 523 049 © Representative: Cropp, John Anthony David et US-A- 4 568 789 al MATHYS & SQUIRE 10 Fleet Street London, EC4Y 1AY(GB) CD CM CM in in CM Note: Within nine months from the publication of the mention of the grant of the European patent, any person may give notice to the European Patent Office of opposition to the European patent granted. Notice of opposition CL deemed have been filed until the opposition fee LU shall be filed in a written reasoned statement. It shall not be to has been paid (Art. 99(1 ) European patent convention). Rank Xerox (UK) Business Services EP 0 253 522 B1 Description This invention relates to hydrocarbon conversion processes employing reducible metal oxide composi- tions and producing hydrocarbon product, coproduct water and reduced metal oxide One particular 5 application of this invention is a method for converting methane to higher hydrocarbons. Another particular application of this invention is a process for the oxidative dehydrogenation of hydrocarbons, especially a process for the oxidative dehydrogenation of paraffinic hydrocarbons to the corresponding mono-olefins. A central aspect of the presently claimed invention is the catalyst composition employed in such hydrocarbon conversion processes and which comprises a boron promoted reducible oxide of manganese w optionally in combination with alkaline earth metals or both alkaline earth metals and alkali metals. Recently, it has been discovered that methane may be converted to higher hydrocarbons by a process which comprises contacting methane and an oxidative synthesizing agent at synthesizing conditions (e.g., at a temperature selected within the range from about 500° to about 1000° C). Oxidative synthesizing agents are compositions having as a principal component at least one oxide of at least one metal which J5 compositions produce C2+ hydrocarbon products, co-product water, and a composition comprising a reduced metal oxide when contacted with methane at synthesizing conditions. Reducible oxides of several metals have been identified which are capable of converting methane to higher hydrocarbons. In particular, oxides of manganese, tin, indium, germanium, lead, antimony, bismuth, praseodymium, terbium, cerium, iron and ruthenium are most useful. See commonly-assigned U.S. Patent Numbers 4,443,649 (Mn); 20 4,444,984 (Sn); 4,443,648 (In); 4,443,645 (Ge); 4,443,647 (Pb) ; 4,443,646 (Bi); 4,499,323 (Pr) ; 4,499,324 (Ce); and 4,593,139 (Ru). Commonly-assigned U.S. Patent Number 4,554,395 discloses and claims a process which comprises contacting methane with an oxidative synthesising agent under elevated pressure (2-100 atmospheres) to produce greater amounts of C3 + hydrocarbon products. 25 Commonly-assigned U.S. Patent Number 4,560,821 discloses and claims a process for the conversion of methane to higher hydrocarbons which comprises contacting methane with particles comprising an oxidative synthesizing agent which particles recirculate between two physically separate zones~a methane contact zone and an oxygen contact zone. As noted, the reaction products of such processes are mainly ethylene, ethane, other light hydrocar- 30 bons, carbon oxides, coke and water. It would be beneficial to these oxidative synthesis processes to reduce selectivities to carbon oxides and coke. Hydrocarbon conversion processes employing the composition of this invention are characterized by relatively severe reaction conditions and by the formation of coproduct water. Thus, hydrothermal stability at elevated temperatures (e.g., 500 to 1000° C) is an important criterion for the compositions. Moreover, uses 35 contemplated for the present compositions require catalysts which are rugged, attrition-resistant, and stable at high temperatures. It is also desirable that the compositions are able to operate effectively for relatively long periods while cycling between oxidized and reduced states. The present invention thus also provides rugged, stable, attrition-resistant oxidant compositions suitable for hydrocarbon conversion processes, especially for processes characterised by the formation of by- 40 product water. Of particular interest is the process for converting methane to higher hydrocarbons with the formation of by-product water and the process for the oxidative dehydrogenation of hydrocarbons, especially of paraffinic hydrocarbons to form the corresponding mono-olefins. 45 SUMMARY OF THE INVENTION It has now been found that hydrocarbon conversions (especially the conversion of methane to higher hydrocarbons) wherein a hydrocarbon feed is contacted at elevated temperatures with a solid comprising a reducible oxide of manganese, is improved when the contacting is conducted in the presence of a 50 promoting amount of at least one member of the group consisting of boron and compounds thereof. According to the present invention, there is provided a method for converting methane to higher hydrocarbon products which comprises contacting a gas comprising methane at synthesising conditions with a solid composition consisting essentially of a reducible oxide of Mn which oxide when contacted with methane at synthesising conditions is reduced and produces higher hydrocarbon products and water, and a 55 promoting amount of at least one boron component selected from boron and compounds of boron and wherein the atomic ratio of said reducible oxide (expressed as Mn) to said boron component (expressed as B) is greater than 1 :1 but not greater than 5:1 . The invention also provides a method of dehydrogenating dehydrogenatable hydrocarbons at oxidative EP 0 253 522 B1 free of dehydrogenation conditions with said solid composition with the proviso that it is substantially catalytically effective iron. The invention further provides a hydrocarbon conversion method which comprises contacting a effective hydrocarbon feedstock with said solid composition which is substantially free of catalytically iron, water and reduced 5 said method being characterised by the production of hydrocarbon product, coproduct metal oxide. As indicated above, in certain embodiments of this invention, the catalyst compositions are charac- terised by the substantial absence of catalytically effective iron, to distinguish known oxidative dehydro- genation catalysts based on the use of Mn ferrites. 10 One class of catalyst compositions useful in this invention comprises: (1) at least one reducible oxide of manganese (2) at least one member of the group consisting of boron and compounds thereof, and (3) at least one member of the group consisting of oxides of alkaline earth metals. A related class of catalyst compositions further comprises at least one alkali metal or compound thereof. rubidium and 75 Alkali metals are selected from the group consisting of lithium, sodium, potassium, cesium. Lithium, sodium and potassium, and especially lithium and sodium, are preferred alkali metals. Alkaline earth metals are selected from the group consisting of magnesium, calcium, strontium and from barium. Presently preferred members of this group are magnesium and calcium. Compositions derived magnesia have been found to be particularly effective catalytic materials. mixed oxides of sodium, 20 Further classes of catalysts compositions within the scope of this invention are magnesium, manganese and boron characterized by the presence of the crystalline compound NaB2Mg+Mn20x wherein x is the number of oxygen atoms required by the valence states of the other elements, said compound having a distinguishing x-ray diffraction pattern. In its most active form, the has compound is believed to correspond to the formula NaB2Mg*Mn20n. While this crystalline compound found that still 25 been found to be associated with highly effective oxidant compositions, it has further been better results are obtained when the oxidant is characterised by both: (1) the presence of crystalline compound NaB2Mg*Mn20x and (2) a stoichiometric excess of Mn relative to at least one of the other elements of the crystalline compound. In currently preferred oxidants of this type, a stoichiometric excess of Mn relative to B is provided. In a still more specific preferred embodiment excess amounts of Na and Mg, amount 30 as well as Mn, are present in the mixed oxide composition relative to the amounts required by the of boron present to satisfy the stoichiometry of the compound NaB2Mg4Mn20x. The present invention also provides, as a catalyst composition suitable for use in this invention, a of Li composition comprising a reducible oxide of manganese, at least one
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