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United States Patent (19) 11) 4,415,440 Roberts Et Al

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United States Patent (19) 11) 4,415,440 Roberts Et Al United States Patent (19) 11) 4,415,440 Roberts et al. 45 Nov. 15, 1983 (54) CRACKING CATALYST IMPROVEMENT 4,025,458 5/1977 McKay ............................... 252/416 WITH GALLUM COMPOUNDS 4,111,845 9/1978 McKay .............. ... 252/455 Z 4,115,249 9/1978 Blanton, Jr. et al ... 252/455 Z. 75 Inventors: John S. Roberts; Dwight L. McKay; 4,175,057 11/1979 Davies et al. ....................... 252/455 Brent J. Bertus, all of Bartlesville, 4,198,320 4/1980 Chester et al. ... 252/455 Z Okla. 4,238,367 12/1980 Bertus et al. ... ... 252/455 Z 4,255,287 3/1981 Bertus et al. ... ... 252/455 Z. 73 Assignee: Phillips Petroleum Company, 4,256,564 3/1981 Roberts et al. ...................... 208/120 Bartlesville, Okla. 4,259,175 3/1981 McArthur ..... ... 208/113 4,279,735 7/1981 Bertus et al. ........................ 208/120 21 Appl. No.: 415,953 4,283,274 8/1981 Bertus et al. .. 208/52 CT 22) Fied: Sep. 8, 1982 4,289,608 9/1981 McArthur ........................... 208/21 4,295,955 10/1981 Tu .............. 208/52 CT 4,325,847 4/1982 Lim et al. ... ... 252/455 Z Related U.S. Application Data 4,334,979 6/1982 Bertus et al. ........................ 208/120 62 Division of Ser. No. 259,390, May 1, 1981. 4,337,144 6/1982 Yoo ................................ 208/52 CT 51 Int. Cl. ....................... C10G 11/04; C10G 1 1/18 FOREIGN PATENT DOCUMENTS 52) U.S. Cl. ................................ 208/120; 208/52 CT 53.3169 11/1978 United Kingd 58) Field of Search ............... 208/120, 52 CT, 251 R A nited Kingdom . 56) References Cited Primary Examiner-Delbert E. Gantz Assistant Examiner-Anthony McFarlane U.S. PATENT DOCUMENTS 2,90,419 8/1959 Brill ..................................... 208/119 (57) ABSTRACT 3,130,007 4/ E. B. - - - is, 2. Gallium compounds are usefully employed to modify 3,297,5653,242,069 3/19l/1967 Garwoodadrow etet al.al. ....................................... ;; hydrocarbon cracking catalysts. 3,431,219 3/1969 Argauer ........... ... 208/120 3,926,78l 12/1975 Gale .................................... 208/117 21 Claims, No Drawings 4,415,440 1. 2 It is another object of this invention to provide a CRACKING CATALYST IMPROVEMENT WITH process for cracking hydrocarbons wherein the delete GALLUM COMPOUNDS rious effects caused by metals on the cracking catalyst are at least mitigated. BACKGROUND OF THE INVENTION 5 These and other objects of the present invention will This application is a divisional of co-pending applica be more fully explained in the following detailed disclo tion Ser. No. 259,390, filed May 1, 1981. sure of the invention and the appended claims. The present invention relates to catalysts. In another aspect, the present invention relates to hydrocarbon SUMMARY OF THE INVENTION cracking catalysts. In still another aspect, the invention 10 In accordance with the present invention, a catalyst relates to restoring the selectivity of hydrocarbon composition comprises a zeolite-modified cracking cat cracking catalysts. In yet another aspect, the invention alyst having deposited thereon a treating agent selected relates to cracking a hydrocarbon feedstock. from gallium and a compound of gallium. Contaminants, for example, nickel, vanadium, and Further, according to the invention, a contaminated iron are found in significant concentrations in hydrocar 15 cracking catalyst previously employed for the catalytic bon feedstocks such as, for example, heavy oil fractions cracking of hydrocarbons is improved by contacting and in lower quality crude oils. These contaminants the cracking catalyst with gallium or a compound have a detrimental effect on the catalysts employed to thereof. convert these oils into gasoline and other valuable pe Still further in accordance with the invention, a hy troleum products, making processing of these oils eco 20 drocarbon feedstock is catalytically cracked employing nomically unattractive. Unfortunately, because of lim the above described catalyst composition. ited supplies of oils containing low levels of contami DETAILED DESCRIPTION OF THE nants, it is necessary to employ metals contaminated oils INVENTION in hydrocarbon processes, such as catalytic cracking 25 It has been discovered that the adverse effects of processes. nickel, vanadium and iron on a cracking catalyst can be The contaminants found in feedstocks to cracking mitigated by contacting the cracking catalyst with a processes become deposited on the cracking catalyst. treating agent selected from gallium and gallium com The deposition on the catalyst of, for example, nickel, pounds. The treating agent can be selected from most vanadium and iron, causes a decrease in the activity of 30 any source of gallium such as elemental gallium, inor the cracking catalyst to convert the hydrocarbon feed ganic gallium compounds, and organic gallium com stock into cracked products, including gasoline. The pounds. Suitable inorganic gallium compounds include selectivity of the cracking catalyst for cracking the salts, for example, gallium nitrate, gallium sulfate, gal feedstock into gasoline as manifested by the portion of lium oxide, gallium hydroxide, gallium phosphide, gal cracked products comprising gasoline is also decreased. 35 lium nitride, gallium sulfide, gallium selenide, sodium The production of undesirable products, for example, gallate, calcium gallate, gallium antimonide, or gallium hydrogen and methane, which must be compressed, compounds that have the empirical formula GaM(- necessitating additional equipment; and coke, which is SO4)2, where M is NH4+ or a member of Group IA of deposited on the catalyst and must be burned off, requir the periodic table, as found at page 83 of the Handbook ing additional equipment and "off time', during which of Chemistry and Physics, 54th edition (1973-74), pub the catalyst is not employed for cracking, is signifi lished by the Chemical Rubber Company Press, Cleve cantly increased. land, Ohio. Less preferred, because of the corrosive Because of these problems, the industry often re effect of halogens on process equipment, are halogen places cracking catalysts contaminated by more than containing gallium salts, for example, GX3 or Ga(X- about 3,000 parts per million (ppm) of vanadium equiva 45 O3)3, where X is selected from the group Cl, Br and I, lents and iron. As used herein, the term vanadium Suitable organic compounds can be represented gener equivalents is the measure of the combined parts by ally by the formula GaR3 wherein R is an organic moi weight of vanadium and four times the nickel per mil ety. Included within this group are the salts of carbox lion parts by weight of cracking catalyst including the ylic acids, (R'COO)3Ga wherein R is hydrogen or a weight of nickel, vanadium and iron on the cracking 50 hydrocarbyl radical having from 1 to about 20 carbon catalyst. There is thus a need for a cracking process atoms. Examples of suitable carboxyl compounds in suitable for use with contaminated feedstocks and con clude gallium formate, gallium acetate, gallium propio taminated cracking catalysts. There is also a need for a nate, gallium butyrate, gallium decanoate, gallium stea cracking catalyst which avoids at least some of the rate, gallium citrate, gallium lactate, gallium malate, detrimental effects caused by deposits thereon of con 55 gallium oxalate, and the like. Polybasic carboxylates, taminants selected from nickel, vanadium and iron. such as gallium citrate, gallium malonate, and gallium There is also a need for a process of treating a contami oxalate can also be utilized. Other suitable organic com nated cracking catalyst to increase its selectivity for pounds are for example, gallium tris(hydrocarbyl ox producing gasoline boiling range type products. ide)s-Ga(OR")3-wherein R" preferably contains one to about 20 carbon atoms and can be an alkyl, alkenyl, OBJECTS OF THE INVENTION cycloalkyl, or aryl radical, or a combination of radicals It is thus an object of the present invention to provide such as alkaryl, aralkyl, alkylcycloalkyl, and the like. a method for restoring the selectivity of a contaminated Examples of suitable oxyhydrocarbyl compounds are cracking catalyst. gallium methoxide, gallium isopropoxide, gallium tert It is a further object of this invention to provide an 65 butoxide, gallium phenoxide, gallium decyloxide, and improved cracking catalyst wherein decreased catalyst the like. Other suitable organic compounds are for ex selectivity caused by contaminants such as nickel, vana ample, gallium alkyls-GaR"3-where R' can be an dium and iron on the cracking catalyst is mitigated. alkyl group containing 1-20 carbon atoms, preferably 4,415,440 3 4. 1-5 carbon atoms. Examples of suitable hydrocarby catalyst of between 5:1,000 to 500:1,000. Most prefera compounds are triethylgallium, tributylgallium, diethyl bly, the added gallium is in an amount sufficient to pentylgallium, and the like. It is recognized that these impart to the cracking catalyst a ratio of weight of compounds are pyrophoric and must be treated accord added gallium to vanadium equivalents of between ingly. R', R', and R' can be substituted with, for exam about 20:1,000 to about 200:1,000, because treated ple, halogen, sulfur, phosphorus or nitrogen. For exam cracking catalysts having weight added gallium:- ple, sulfur containing compounds such as gallium dialk vanadium equivalents ratios within this range have been yldithio-carbamates and gallium xanthates are suitable. tested with good results. Also, gallium compounds containing both phosphorus The present invention has particular utility for in and sulfur, for example, gallium dihydrocarbyl dithio O proving the cracking characteristics of cracking cata phosphates, such as those represented by the formula lysts having deposited thereon 3,000 ppm and greater of GaS2P(OR")23 wherein R" is as defined before, are vanadium equivalents. Untreated cracking catalysts suitable. Of course, mixtures of any of the above com have usually developed undesirable cracking behavior. pounds may be utilized. The gallium containing treating at a contamination level of 3,000 vanadium equivalents.
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