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United States Patent Office Patented Apr 3,130,147 United States Patent Office Patented Apr. 21, 1964 2 ponent as described above, be employed for reforming or 3,130,147 hydrocracking operations. Another reaction employing ZRCONUM-AJMNUMA - POSPHRUS CATA LYST AND WETHOY FOR PREPARNG THE a catalyst of the above dual-function type is a desulfuriza SAME, EMPLOYED FOR THE CRACEKENG OF tion reaction in which hydrocarbon fractions containing HYDRO CAR3CNS combined sulfur are subjected to mild hydrogenating con Francis G. Bwyer, Daiayware Township, Canadea County, ditions in the presence of an acidic catalyst to effect the and Sylvander C. Eastwood, Woodbary, N.J., assigliors hydrogenation and desulfurization of molecules to pro to Socoay Mobil Gi Conigaay, Inc., a coregration of duce hydrogen sulfide and the corresponding hydrocarbon. New York The dual-function type catalyst may be prepared by inti No Drawing. Fied Sept. 18, 1961, Ser. No. 138,563 mately combining the acidic composite described herein 7 Cairns. (C. 208-114) O with a dehydrogenation component comprising a heavy This invention relates to an acidic catalytic composite metal of groups V through VII of the periodic table or a and to a method for manufacture thereof. More particul compound thereof. Examples of suitable metals for such larly, the present invention is directed to an acidic catalyst purpose are platinum, palladium, nickel, cobalt, iron, consisting essentially of an oxygen-containing combina 5 manganese, chromium, molybdenum, tungsten, vanadium tion of aluminum, zirconium and phosphorus and to a and copper. Certain combinations of these metals pro method for preparing said catalyst. duce synergistic effects such as combinations of cobalt It has heretofore been known to prepare catalytic com and moiybdenum, nickel and tungsten, and chromium and posites of alumina and zirconia. Such composites have copper. been produced, for example, by reacting a solution of an 20 One of the principal objects of the present invention is aluminum salt and an alkali metal zirconium carbonate. the provision of an acidic catalyst consisting essentially It has also been known to prepare metal phosphate cata of any oxygen-containing combination of aluminum, zir lysts, particularly applicable for use in polymerization re conium, and phosphorus. Another object is to afford a actions, by treating suitable porous adsorbent materials method for producing hydrosols of such composition with phosphoric acid. 25 characterized by a short gelation time. A still further ob The present invention is directed to a new acidic cata ject is the provision of a process for manufacturing cogels lyst useful in hydrocarbon conversion processes utilizing consisting essentially of an oxygen-containing combination an acid-acting catalyst, such as isomerization, polym of alurhinum, zirconium, and phosphorus by forming a erization, alkylation and cracking. Also, the catalyst hydrogel of such composition which, after aging, may be described herein may effectively serve as the acidic com 30 washed free of water-soluble matter and dried to form ponent of a dual-function catalyst comprising an acid a porous adsorbent catalytic product. acting component and a dehydrogenation component. The above and other objects which will be apparent to Such latter type catalysts are useful in hydrocarbon con those skilled in the art are achieved in accordance with version operations such as hydrocracking and reforming. the present invention wherein composites consisting es In one embodiment, the present invention provides Sentially of an oxygen-containing combination of alu for a process for the manufacture of an acidic catalyst minum, zirconium and phosphorus are prepared by re by reacting, in aqueous solution, a water-soluble aluminum acting, in aqueous solution, a water-soluble salt of zir compound, a water-soluble zirconium compound and a conium, a water-soluble salt of aluminum, and a water water-soluble oxyacid of phosphorus or salt thereof to soluble oxyacid of phosphorus or salt of such acid to yield an acidic hydrosol in which the atomic ratio of 40 yield a sol which sets to an all-embracing hydrogel in aluminum to zirconium is between about 0.1 and about which the atomic ratio of aluminum to zirconium is be 10 in which the atomic ratio of the combined content of tween about 0.1 and about 10, and in which the atomic aluminum and zirconium to phosphorus is between about ratio of the combined content of aluminum and zirconium 0.1 and about 10, permitting the resulting hydrosol to set to phosphorus is between about 0.1 and about 10. The to a hydrogel, aging the hydrogel in an aqueous solution hydrogel so obtained, is thereafter aged in a solution of of an alkali metal or ammonium sait of an acid char a weak acid ammonium or alkali metal salt and subse acterized by a dissociation constant of less than about quently contacted with such aqueous treating solutions 1.7Xi 02, washing the aged hydroge! free of water as are desired for density control, base-exchange, impreg soluble matter and drying the washed hydrogel. nation or the like; water-washed free of soluble matter In another embodiment, the invention provides for an 50 and dried. The resulting product is thereafter calcined acidic catalyst consisting essentially of an oxygen-con generally at a temperature between about 800 F. and taining combination of aluminum, zirconium and phos about 1400 F. phorus prepared by the foregoing method. Hydrogels prepared by the process described herein are In still another embodiment, the invention comprises generally characterized by a gelation time of not more an acidic catalyst consisting essentially of an oxygen 55 than 2 hours although it is to be realized that hydrogels containing combination of aluminum, zirconium and phos having a longer time of set when desired may also be phorus wherein the atomic ratio of aluminum to zirconium produced by the present method. The method of this is between about 0.1 and about 10 and in which the atomic invention is particularly adaptable for the production of ratio of the combined aluminum and zirconium content hydrogels characterized by a time of set of less than about 60 20 seconds which hydrogels are capable of being formed to phosphorus is between about 0.1 and about 10. into spheroidal particles upon introducing the hydrosol in In yet another embodiment, the invention provides for the form of globules into a water-immiscible medium and a dual function catalyst wherein the above acidic com maintaining the hydrosol globules in the medium until ponent is intimately combined with a dehydrogenation they set to globules of hydrogel. component, comprising a heavy metal constituent, for 65 The essential compounds required for forming inor example, metals or compounds of metals of groups V ganic Oxygen-containing cogels of aluminum, zirconium through VIII of the periodic table. and phosphorus in accordance with the present process The catalyst described herein is thus applicable for use include a water-soluble aluminum salt, a water-soluble in numerous hydrocarbon conversion reactions. The zirconium salt and a water soluble oxyacid of phosphorus catalyst may be employed by itself, for example, in effect 70 or a Salt thereof. These compounds may be intimately ing isomerization, polymerization, alkylation and crack mixed, in aqueous solution, in any desired manner to ing or may, in combination with a dehydrogenation com yield a resulting hydrosol. The solutions may be con 3,130,147 4. tacted by flowing streams thereof together under con pounds. The present composites have been found to ditions of rapid flow such as in a mixing nozzle. Addi be particularly useful as acidic catalysts in promoting tional components may, if so desired, be introduced at acid catalyzed reactions such as cracking, isomerization, this stage by dissolving a suitable. compound of the de polymerization, and alkylation when used alone. The sired component in one of the hydrosol forming solutions catalyst described herein may also be used as one com or by mixing a stream of a compound of such desired ponent of a dual-function catalyst wherein it is present as component with the streams of the reactants. The an acidic component and intimately combined either by water-soluble aluminum salt employed may include any suitable mechanical admixture or by impregnation with of the readily available water-soluble salts of this metal a dehydrogenation component as described hereinabove. and, particularly, the salts of mineral acids such as the O The following examples will serve to illustrate the sulfate, chloride and nitrate. Likewise, the water-soluble catalyst of the invention, its method of preparation and zirconium salt employed may include any of the readily its use in hydrocarbon conversion. available zirconium salts such as zirconium tetrachloride, zirconium tetraiodide, zirconium sulfate, zirconyl bromide, Example 1 zirconyl chloride, and zirconyl iodide. The water-solu 5 A hydrosol was prepared by mixing 6629 grams of ble oxyacid of phosphorus or salt thereof may include, an aqueous solution containing 128 grams of AlO3 as by way of example, orthophosphoric acid, pyrophos Al2(SO4)3 and 622 grams ZrO2 as Zr(SO4)2.4H2O with phoric acid, and metaphosphoric acid, phosphorus acid 3870 grams of a solution containing 1158 grams of so and hypophosphorus acid and salts of said acids, particu dium hexametaphosphate. The resulting sol set to a larly, the alkali metal and ammonium salts which may 20 firm, all-embracing hydrogel having a pH of less than be monobasic, dibasic or tribasic salts of the specified 1 in about 10 minutes. The hydrogel was broken up acids including, for example, sodium tripolyphosphate into cubes and aged in a 10 percent weight aqueous solu and sodium hexametaphosphate. tion of ammonium acetate for 16 hours at 160 F. After The quantity and concentration of the reactant solu aging, the gel was water-washed for 24 hours to remove tions employed is, in accordance with the invention, 25 soluble salts and thereafter dried in superheated steam controlled to afford a resulting gel product in which the at 250 F.
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