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||||||IIII USOO5504053A United States Patent (19) 11 Patent Number: 5,504,053 Chou Et Al ||||||IIII USOO5504053A United States Patent (19) 11 Patent Number: 5,504,053 Chou et al. 45 Date of Patent: Apr. 2, 1996 (54) ALKYLENE OXDE CATALYSTS HAVING FOREIGN PATENT DOCUMENTS ENHANCED ACTVTY AND/OR STABILITY 0247414 2/1984 European Pat. Off.. (75) Inventors: Pen-Yuan Chou; Madan M. Bhasin; 57-136941 8/1982 Japan. Hwaili Soo; Erind M. Thorsteinson, 2095242 9/1982 United Kingdom. all of Charleston, W. Va. OTHER PUBLICATIONS 73) Assignee: Union Carbide Chemicals & Plastics "Influence of Feed Water Vapor on the Selective Oxidation Technology Corporation, Danbury, of Ethylene over Silver Catalyst.' Applied Catalysis, 61: Conn. 265-74 (1990). Imamura, et al., "Effect of Samarium on the Thermal Sta 21 Appl. No.: 502,187 bility and Activity of the Mn/Ag Catalyst in the Oxidation of CO', J. of Catalysis, vol. 115, pp. 258-264 (1989). 22) Filed: Apr. 3, 1990 Lewis, "Decomposition of Silver Oxide by Autocatalysis', Z. Physik Chem, 52:310-326 (1905). Related U.S. Application Data Kendall, et al., "The Catalytic Influence of Foreign Oxides 63 Continuation-in-part of Ser. No. 340,242, Apr. 18, 1989, and on the Decomposition of Silver Oxide, Mercuric Oxide and a continuation-in-part of Ser. No. 340,390, Apr. 18, 1989. Barium Peroxide", J. Amer: Chem. Soc., vol.43, p. 2017 (1921). (51) Int. Cl. ............... B01J 23/50 Kripylo, et al., “Why Do Metal Oxide Dopings Stabilize the 52 U.S. C. .......................... 502/348; 502/208; 502/217; Dispersity of Silver Support Catalyst for the Selective 502/218: 502/322; 502/.324; 502/341; 502/344; Oxidation of Ethene', Chem. Techn., 38(5) (1985). 502/300; 549/536 Berger, et al., “Dependence of the Sintering of Polycrystal 58 Field of Search ..................................... 502/208, 218, line Silver on the Gas Atmosphere', Chem. Techn, 502/314, 324, 347, 348, 217,322, 341, 38(6):245-8 (1986). 344; 549/536 Primary Examiner-Anthony McFarlane (56) References Cited Attorney, Agent, or Firm J. B. Mauro U.S. PATENT DOCUMENTS 57 ABSTRACT 2,040,782 5/1936 van Peski.................................. 260/54 2,605,239 7/1952 Sears ....................................... 252/475 Catalysts for the production of alkylene oxide by the epoxi 2,615,900 10/1952 Sears, Jr. .............................. 260/348.5 dation of alkene with oxygen comprise a silver impregnated 2,769,016 10/1956 Lichtenwalter et al. ... 260/348.5 support containing a sufficient amount of manganese com 3,844,981. 10/1974 Cusumano .............................. 252/471 ponent to enhance at least one of activity and/or efficiency 3,962,285 6/1976 Cusumano ... ... 260/348.5 and/or stability as compared to a similar catalyst which does 4,007,135 2/1977 Hayden et al. ......................... 252A467 not contain manganese component. 4,761,394 8/1988 Lauritzen ................................ 502/348 4,766,105 8/1988 Lauritzen . ... 502/216 4,800,070 1/1989 Carlin et al. ......................... 423/210.5 39 Claims, No Drawings 5,504,053 1. 2 ALKYLENE OXDE CATALYSTS HAVING The carriers that have been employed are typically made ENHANCED ACTIVITY AND/OR STABILITY of inorganic materials, generally of amineral nature. In most cases, the preferred carrier is made of alpha-alumina, such as This patent application is a continuation-in-part of U.S. has been described in the patent literature: see for example, patent application Ser. Nos. 340,242 and 340,390, both filed U.S. Pat. Nos. 2,294,383; 3,172,893; 3,332,887; 3,423,328; Apr. 18, 1989, and both herein incorporated by reference. and 3,563,914. The carriers which are employed for the manufacture of most, if not all, commercially employed ethylene oxide FIELD OF THE INVENTION catalysts are produced by companies who do not produce 10 such catalysts. As a rule, the methods of making such This invention relates to silver-containing, supported carriers are trade secrets of significant value to the carrier catalysts for the epoxidation of alkene, especially ethylene, manufacturers. Consequently, the catalyst manufacturer can to the corresponding alkylene oxide, e.g., ethylene oxide, not know how the carrier is made. Critical to making a which contain a stability and/or efficiency and/or activity carrier which proves uniquely desirable for the manufacture enhancing amount of a manganese-containing component. of a successful catalyst can be a number of factors, such as 15 the purity and other physical/chemical properties of raw materials used to make the carrier and the method by which BACKGROUND OF THE INVENTION the carrier is made. The silver that is deposited on these carriers is thought to Ethylene oxide is commercially produced by the epoxi be in the form of small particles because that is all that can dation of ethylene over silver-containing catalyst at elevated 20 be seen by current microscopic techniques. The patent temperature. Considerable research efforts have been literature indicates that the size of the silver is a factor in the devoted to providing catalysts that increase the efficiency, or effectiveness of the catalyst and in most cases fine particle selectivity, of the process to ethylene oxide. silver is obtained utilizing the standard processes in the art; The manufacture of ethylene oxide by the reaction of see, for example, U.S. Pat. Nos. 2,554,459; 2,831,870; oxygen or oxygen-containing gases with ethylene in the 25 3,423,328 (specifies that silver particles of 150-400 Ang presence of a silver catalyst is an old and developed art. For stroms are employed); 3,702,259 (disclosed a preparation example, U.S. Pat. No. 2,040,782, patented May 12, 1936, procedure for forming silver particles less than 1 micron in describes the manufacture of ethylene oxide by the reaction diameter) and 3,758,418 (discloses silver particles having a of oxygen with ethylene in the presence of silver catalysts diameter less than 1000 Angstroms). Improvements in which contain a class of metal promoters. In U.S. Pat. No. 30 microscopic examinations of silver catalysts enable the Re.20,370, dated May 18, 1937, Leforte discloses that the observation that the particle size ranges to even smaller formation of olefin oxides may be effected by causing olefins values. to combine directly with molecular oxygen in the presence The deposition of silver onto the carrier can be achieved of a silver catalyst. From that point on, the prior art has by a number of techniques but the two techniques which are focused its efforts on improving the catatyst's efficiency in 35 most frequently employed involve, in one case, the impreg producing ethylene oxide. nation of the support with a silver solution followed by heat In characterizing this invention, the terms "conversion', treatment of the impregnated support to effect deposition of "selectivity", and "yield” are employed as defined in U.S. the silver on the support and, in the other case, the coating Pat. No. 3,420,784, patented Jan. 7, 1969, at column 3, lines 40 of the silver on the support by the precipitation of silver or 24-35 inclusive. This definition of "selectivity' is consistent the preformation of silver into a slurry such that the silver with that disclosed in U.S. Pat. No. 2,766,261 at column 6, particles are deposited on the support and adhere to the lines 5-22, and U.S. Pat. No. 3,144.916, lines 58-61. The support surface when the carrier or support is heated to definitions of "yield” and “conversion' have more varied remove the liquids present. These various procedures are meaning in the art and are not to be employed as defined, for 45 exemplified in various U.S. Pat. Nos. such as 2,773,844; example, in the aforementioned U.S. Pat. No. 2,766,261. 3,207,700; 3,501,407; 3,664,970 (see British Patent 754, The terms "efficiency” and "selectivity", as used throughout 593) and 3,172,893. the specification and claims are intended to be synonymous. The surface area provided by the support has been the Silver catalysts employed in the manufacture of ethylene subject of considerable interest in the development of silver oxide have undergone significant changes since their initial 50 catalysts. Disclosures concerning the surface area of the period of development. As reported by the art, silver par catalyst carrier can be found in U.S. Pat. No. 2,766,261 ticles were first deposited upon support materials with little (which discloses that a surface area of 0.002-10 m/gm is attention being paid to support properties, such as surface suitable); U.S. Pat. No. 3,172,893 which depicts a porosity area, pore volume and chemical inertness. As the art of 35–65% and a pore diameter of 80-200 microns); U.S. evolved, there developed special technologies related to 55 Pat. No. 3,725,307 which depicts a surface area of less than carriers or supports containing silver that were more effec 1 sq.m/gm and an average pore diameter of 10-15 microns): tive for the reaction of ethylene with oxygen to produce U.S. Pat. No. 3,664,970 (which utilizes a support having a ethylene oxide. Today, most supports for the silver catalyst minimum porosity of about 30%, at least 90% of the pores are shaped particulate materials which can be loaded in the having diameters in the range of 1-30 microns, and the interior of a reactor wherein the reacting gases and the 60 average of such diameters being in the range of 4-10 gaseous products of the reaction are capable of flowing in microns); and U.S. Pat. No. 3,563,914 which utilizes a and about these particulate materials to pass through the catalyst support having a surface area of less than 1 sq.m/ reactor and be recovered.
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