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United States Patent (19) 11 Patent Number: 5,017,543 De Clippeleir Et Al

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United States Patent (19) 11 Patent Number: 5,017,543 De Clippeleir Et Al United States Patent (19) 11 Patent Number: 5,017,543 De Clippeleir et al. 45) Date of Patent: May 21, 1991 (54) PROCESS FOR THE PREPARATION OF A 56) References Cited DEHYDROGENATION CATALYST U.S. PATENT DOCUMENTS 75 Inventors: Georges E. M. J. De Clippeleir, 4,608,360 8/1986 Abrevaya et al. .............. 502/330 X Sint-Pieters-Leeuw, Belgium; 4,684,619 - 8/1987 Moore ................................. 502/330 Elizabeth Baumann Ofstad, Jar; 4,880,764 11/1989 Imai et al. ....................... 502/330 X Steinar Kvisle, Oslo, both of Norway FOREIGN PATENT DOCUMENTS Assignee: 73 Labofina, S.A., Brussels, Belgium 0020240 10/1980 European Pat. Off. ............ 502/328 Appl. No.: 21 519,183 Primary Examiner-W. J. Shine 22 Fed: May 3, 1990 Attorney, Agent, or Firm-Jim Wheelington; Michael Caddell; M. Norwood Cheairs w Related U.S. Application Data 57 ABSTRACT 62) Division of Ser. No. 310,261, Feb. 13, 1989, Pat. No. A process is described for the catalytic dehydrogena 4,962,265. tion of paraffinic hydrocarbons preferably having from 30 Foreign Application Priority Data 3 to 6 carbon atoms in the presence of a catalyst contain Feb. 11, 1988 BE Belgium ............................... 88OO157 ing at least one metal of the platinum group, a co Feb. 11, 1988 BE Belgium ............................... 88OO158 catalyst and a promoter, the noble metal of the platinum 51 Int. Cl......................... B01J 23/02; B01J 23/04; group being deposited into the alumina support in two B01J 23/58 steps, the first one being followed by a calcination and 52 U.S. C. .................................... 502/.328; 502/330; a reduction, the second one being followed by a calcina 502/.340, 502/341; 502/344 tion. 58) Field of Search ............... 502/.328,330, 340, 341, 502/.344 20 Claims, No Drawings 5,017,543 1. 2 a tin group metal, and an alkali or alkaline-earth metal PROCESS FOR THE PREPARATION OF A type promoter. DEHYDROGENATION CATALYST SUMMARY OF THE INVENTION This is a Division of co-pending application Ser. No. 5 The process of the present invention comprises the 07/310,261 filed on Feb. 13, 1989, now U.S. Pat. No. catalytic dehydrogenation of paraffinic hydrocarbons 4,962,265. in the presence of a catalyst, a co-catalyst and a pro moter wherein the co-catalyst contains at least one BACKGROUND OF THE INVENTION group IV A metal, the promoter is selected from alkali The present invention relates to a process for the 10 metals and alkaline-earth metals and the catalyst is pre catalytic dehydrogenation of hydrocarbons, such as pared by depositing a group VIII B or rhenium metal on paraffinic hydrocarbons. More particularly, the present a suitable support in two steps, the first step being fol invention concerns an improved process for the dehy lowed by calcination and reduction and the second step drogenation of paraffinic hYdrocarbons having from 3 being followed by calcination. to 6 carbon atoms. The present invention also relates to 15 the catalyst used to carry out the process. DETAILED DESCRIPTION OF THE The catalytic dehydrogenation of hydrocarbons has INVENTION been possible for many years and constitutes an impor The process of the present invention more preferably tant catalytic process in view of the increasing demand entails the catalytic dehydrogenation of paraffinic hy for dehydrogenated products which are of valuable use 20 drocarbons having from 3 to 6 carbon atoms by passing in various forms, such as gasolines having a high octane the paraffinic hydrocarbon over a catalyst containing an number, plastic materials and synthetic rubbers. alumina support at least one group VIII B or rhenium Moreover, in view of the increasing production of metal together with a group IV A metal co-catalyst and LPG (liquified petroleum gas), it seems particularly at least one alkali metal or alkaline-earth metal pro interesting to be able to convert a part of those paraf 25 moter. The dehydrogenation process is preferably car finic hydrocarbons into dehydrogenated products such ried out in the presence of the catalyst at a temperature as propylene which is of particular interest for the man between 400 and 800° C., under a pressure between ufacture of plastic materials. about 0.001 and 10 atm and at a weight hourly space The catalytic dehydrogenation of hydrocarbons is velocity between about 0.1 and 21. generally carried out in the presence of catalytic com 30 The catalyst contains a catalytically effective amount positions containing platinum deposited on a support. of at least one metal from the platinum (VIII B) qroup The catalytic compositions can also contain other cata or rhenium (preferably from about 0.1 to 2% by weiqht) lytically active metals such as tin or indium and promot a catalyatically effective amount of at least one metal ers based on alkaline or alkali-earth metals. from the tin (IVA) group as co-catalyst (preferably Such processes and catalytic composition have been 35 about 0.1 to 2% by weight) and an effective amount of described e.g. in U.S. Pat. Nos. 2,479,209, 2,602,772, at least one alkali or alkaline-earth metal as promoter 2,930,763, 3,531,543, 3,745,112, 3,892,657, 3,909,451 or (preferably about 0.5 to 5% by weight.) still in U.S. Pat. Nos. 4,329,258, 4,363,721 and 4,430,517. The catalyst is prepared by submitting the support Further, in most of these patents, it is also taught to containing the co-catalyst: - use a halogen in order to improve the yield of the dehy to a first treatment with a metal compound of the drogenation reaction. platinum group or rhenium, followed by a calcination in However, when the developed processes are applied air and by a reduction in the presence of hydrogen to the dehydrogenation of propane, the yield of the preferably at a temperature between about 450° and reaction at 600 C. does not exceed about 30 to 35%. 45 550° C.; This amount is 70 to 81% of the total theoretical con then to an intermediate treatment to deposit the pro version, taking into account the thermodynamic con moter, followed by a calcination, preferably at a tem straints. perature between about 380 and about 550° C.; There is, therefore, a need to provide a process for and finally to a second treatment with a metal com the dehyrogenation of paraffinic hydrocarbons with 50 pound of the platinum group or rhenium, followed by a improved yields. calcination preferably at a temperature not exceeding 525 C., OBJECT OF THE INVENTION It is preferred that the support be alumina and that the The object of the present invention is to provide an support and co-catalyst be calcined prior to being sub improved process for the dehydrogenation of hydrocar 55 mitted to the first treatment (preferably at a temperature bons. between about 450° and 550° C.). Another object of the present invention is to provide The process of the present invention can be applied to an improved dehydrogenation catalyst. the dehydrocyclization of hydrocarbons having at least A more specific object of the present invention is to 6 carbon atoms but is more preferably applied to the provide an improved process for the dehydrogenation dehydrogenation of paraffinic hydrocarbons having of paraffinic hydrocarbons having from 3 to 6 carbon from 3 to 6 carbon atoms, and particularly to the dehy atoms in the presence of a catalyst containing a platinum drogenation of propane and butanes. group or rhenium metal, a tin group metal and a pro The Applicants have unexpectedly found that by note. applying the process of the invention using the inven Another object of the present invention is to provide 65 tive catalyst it becomes possible to considerably in an improved process for the dehydrogenation of pro crease the yield of the dehydrogenation reaction when pane into propylene in the presence of an improved compared to the thermodynamic equilibrium, said yield catalyst containing a platinum group or rhenium metal, being apt to exceed 90% of theoretical yield when pro 5,017,543 3 4. pane is dehydrogenated at a temperature of about 600 at a temperature between about 450 and 550° C., during C. from about 1 to 4 hours. The metal of the platinum group or rhenium, as used The Applicant has found that this reduction step is herein, is preferably selected from the group consisting very important and has a beneficial effect on the yield of platinum, palladium, rhenium, iridium, rhodium, os during the dehydrogenation of paraffinic hydrocarbons mium, ruthenium or mixtures thereof, platinum being in the presence of this catalyst. most preferred. The metal of the tin group, as used Before carrying out a second treatment with the plati herein, is preferably selected from the group consisting num group or rhenium metal, the support is submitted of tin, germanium, lead or mixtures thereof, tin being to an intermediate treatment with a promoter. most preferred, which may be present as a compound The alkali or alkaline-earth metal is preferably well such as the oxide. The promoter can be an alkali metal dispersed on the support. The amount of alkali or alka selected from the group consisting of cesium, rubidium, line-earth metal compound present on the support is potassium, sodium, lithium or mixtures thereof, or an preferably between about 0.5 and about 5% by weight alkaline-earth metal selected from the group consisting more preferably between about 0.8 and 2.5% by weight of barium, strontium, calcium, magnesium or mixtures 5 expressed as metal. The preferred promoter is potas thereof, or even mixtures of alkali and alkaline-earth sium and the preferred amount deposited on the support metals, potassium being preferred; other promoters is an amount corresponding to about 0.8 to 2% by known generally to be efficient are also envisaged as weight expressed as metal.
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