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United States Patent (19) (11) 3,899,444 Stephens (45) Aug

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United States Patent (19) (11) 3,899,444 Stephens (45) Aug United States Patent (19) (11) 3,899,444 Stephens (45) Aug. 12, 1975 54 EXHAUST GAS CATALYST SUPPORT 75) Inventor: Ruth E. Stephens, Royal Oak, Mich. Primary Examiner-Carl F. Dees Attorney, Agent, or Firm-Donald L. Johnson; Robert 73) Assignee: Ethyl Corporation, Richmond, Va. A. Linn; Joseph D. Odenweller 22 Filed: Dec. 22, 1972 (21) Appl. No.: 317,831 57 ... ' ABSTRACT A thermally stable and attrition resistant catalyst sup Related U.S. Application Data port consisting essentially of an alumina coating on an 63 Continuation-in-part of Ser. No. 224,240, Feb. 7, inert substrate. The alumina coating has a rare earth 1972. metal oxide substantially uniformly distributed throughout. Catalyst compositions utilizing this sup 52 U.S. Cl.............. 252/455 R; 252/462; 252/463; port, processes for preparing both support and cata 252/471; 423/213.5 lyst, and a method of treating internal combustion en (51) Int. Cl..... B01j 11/40; B01j 1 1/06; B01j 1 1/32 gine exhaust gases and preventing crystallization of 58) Field of Search........ 252/462, 463, 455 R, 457; alumina are disclosed. Catalysts consisting essentially 423/213.5 of an alumina matrix containing rare earth metal oxide and a catalytic metal oxide are also disclosed. The 56 References Cited atom ratio of rare earth metal to aluminum in the sup UNITED STATES PATENTS port is 1:5.7-25. The atom ratio of catalytic metal to 3,284,370 1 1/1966 Clifford et al...................... 252/462 rare earth metal to aluminum in the catalysts is 3,554,929 1/1971 Aarons................................ 252/462 1:0.8-1.4:8-20. 3,741,725 6/1973 Graham ... ... 423/213.5 3,781,406 12/1973 Roth et al....................... 252/462 X 42 Claims, No Drawings 3,899,444 2 EXHAUST GAS CATALYST SUPPORT an effective catalyst should exhibit the following prop This application is a continuation-in-part of applica erties: tion Ser. No. 224,240, filed Feb. 7, 1972. a. Catalyst should be effective at a relatively low tem perature so that it will function soon after the en BACKGROUND OF THE INVENTION 5 gine has started, i.e., it must have a short warm-up This invention relates to an improved method for period or a low activation temperature. preparing stabilized alumina catalyst supports. More b. It should be highly efficient in oxidizing exhaust particularly, it relates to the use of novel and inexpen hydrocarbons and carbon monoxide. sive materials to prepare a stabilized activated alumina c. It should have a long life, i.e., catalyst support which when used with suitable metal O 1. It should not be easily poisoned. containing catalysts has been found to be especially ef 2. It should withstand at least 800°C. likely to de fective in the oxidation of automotive exhaust gases. velop during operation. Even more specifically, this invention relates to the use 3. It should not be abraded by the frequent shaking of alumina to which is added a rare earth metal com and occasional shocks characteristic of a pulsat pound thereby forming an activated, stabilized catalyst 15 ing exhaust gas stream. support when calcined at elevated temperatures. Rare Extensive research in this field has revealed that earth metals are also known as Lanthanide Series met many catalysts will effectively oxidize the carbon mon als and include metals having an atomic number from oxide and hydrocarbons contained in the exhaust gas 57 through 71, but more generally from 57 through 63. from internal combustion engines. However, these cat It has been well known that alumina is an excellent 20 alysts have uniformly failed to be economically feasible support for catalysts in a wide range of chamical reac in automotive catalytic converters due to their short tions. In fact, in many cases alumina has been shown to life. have catalytic activity of its own and will therefore A primary reason for short catalyst life is the trans often enchance the activity of the catalyst it is support formation of the alumina support from an amorphous ing. It is further known that the activity of an alumina 25 or lower crystalline state (e.g., gamma, eta) to a highly supported catalyst will be dependent on the surface crystalline state by either thermal or chemical means. area. It is advantageous to retain a maximum surface In the more crystalline state, the catalyst is subject to area when the alumina is calcined. At very high tem fracture along the crystal's grain boundary, resulting in peratures phase changes occur which convert the desir powdering, dusting, and eventually loss of catalyst. The able eta or gamma phases into the less desirable theta 30 formation of more crystalline material can be caused or alpha phases, resulting in a great drop in the surface by phase transformation of the amorphous or transi aca. tional alumina to crystalline a-alumina through action According to U.S. Pat. No. 3,291,564, it is known to of heat over a period of time. Further, the interaction use potassium, cesium, or barium compounds to stabi of alumina with catalyst metals forming metal alumi lize the alumina support and prevent loss of surface 35 nates also results in crystalline structures. In fact, many area and phase changes at high temperature. of the more active oxidation catalysts, particularly cop According to British Pat. No. 1,231,276, potassium, per, not only interact with alumina to form aluminates calcium, and particularly barium, stabilize alumina, but but also promote formation of highly crystalline alu only when the active catalyst is impregnated in an inter mina phases. After formation of such crystalline struc mediate zone between the surface and the carrier core. 40 tures, thermal and mechanical shock loss of catalyst by Catalysts consisting essentially of an alumina support attrition and hence shortened life. containing rare earth metal oxides are disclosed in U.S. Thus, it is an object of this invention to provide a cat Pat. Nos. 3,483,138 and 3,545,917. These catalysts dif alyst support which is thermally stable and attrition re fer from the presently claimed catalyst supports in that sistant. A further object is to provide a thermally stable the present supports have the alumina-rare earth metal and attrition resistant catalyst composition suitable for oxide composition as a coating on an inert substrate or use in the exhaust gas of an internal combustion engine. core. Also, the present support compositions have a de A still further object of this invention is to provide a fined atom ratio of rare earth metal to aluminum in the process for producing a thermally stable and attrition coating. resistant catalyst support and catalyst. Another object Laminar catalysts having an alumina core with a first of this invention is to provide a method of lowering the layer of Lanthanide Series metal oxide and an outer noxious constituents of engine exhaust gas such as car layer of copper oxide are disclosed in U.S. Pat. No. bon monoxide, hydrocarbons and nitrogen oxides con 3,226,340. These catalysts differ from the presently tained in internal combustion engine exhaust gases claimed catalysts in that the rare earth metal oxide and using the thermally stable and attrition resistant sup copper oxide are disclosed to be in discrete lamina and, 55 port and catalyst composition provided. Another ob hence, do not have an alumina matrix containing a cat ject is to provide a method of preventing crystallization alytic metal and a rare earth metal. of alumina at high temperature. Other patents relating to rare earth metal catalysts are U.S. Pat. Nos. 3,453,333; 2,152,908; 2,148, 129; SUMMARY OF THE INVENTION 2,129,733; 3,395,004; 3,284,370; 3,153,635; and 60 The above and other objects are accomplished by 2,945,057. providing a catalyst support composition consisting es The extremely severe conditions which prevail in the sentially of an inert substrate or core coated with an catalytic oxidation of carbon monoxide and hydrocar alumina containing from about 1 to about 45 weight bons contained in the exhaust gases from internal com is percent based on said alumina of a rare earth metal bustion engines set unusually severe criteria for such oxide uniformly distributed throughout said alumina catalysts, and this makes the selection of an effective coating. In the preferred embodiments to be described catalyst extremely difficult. It is generally agreed that later the atom ratio of rare earth metal to aluminum in 3,899,444 3 4 said alumina coating is 1 to about 5.7-25. Preferred composition consisting essentially of an inert substrate rare earth metal oxides are lanthanum oxide, neodym coated with an alumina selected from amorphous and ium oxide, and praseodymium oxide and mixtures transitional alumina, said alumina coating containing thereof. from about 1 to about 45 weight per cent based on said In a further aspect of this invention there is provided alumina coating of a rare earth metal oxide uniformly a method of retarding change in the crystalline phase distributed throughout said alumina coating. More in alumina on heating to elevated temperatures, for ex preferably, the rare earth metal oxide is present in an ample, about 900°C., said method comprising incorpo amount to provide an atom ratio of rare earth metal to rating uniformly throughout said alumina a rare earth aluminum of 1 to 5.7-25 in said coating. A more pre metal oxide in an amount of from about 1 to about 45 10 ferred range is 1 to 8-20. weight per cent based on said alumina and, more pref The alumina coating can be either amorphous or erably, an amount that provides an atom ratio of rare transitional alumina which are well known and com earth metal to aluminum of 1 to about 5.7-25.
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