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United States Patent (19) 11) 4411,818 Reuter Et Al

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United States Patent (19) 11) 4411,818 Reuter Et Al United States Patent (19) 11) 4411,818 Reuter et al. 45) Oct. 25, 1983 (54 REACTIVATION OF 56) References Cited WANADUM-CONTAINING OXIDATION U.S. PATENT DOCUMENTS CATALYSTS 3,474,041 10/1969 Kerr ................................ 252/411 R 75 Inventors: Peter Reuter, Ludwigshafen; Kurt 4,007,136 2/1977 Blechschmitt et al. ............. 252/476 Blechschmitt, Schifferstadt; Friedrich 4,035,399 7/1977 Yokoyama .......................... 549/248 Wirth, Ludwigshafen, all of Fed. 4,036,783 7/1977 Blechschmitt et al. ............. 252/46 Rep. of Germany 4,123,442 10/1978 Bakshi ................................. 252A16 FOREIGN PATENT DOCUMENTS 73) Assignee: BASF Aktiengesellschaft, Fed. Rep. 2436009 2/1976 Fed. Rep. of Germany . of Germany 2510994 9/1976 Fed. Rep. of Germany . 368229 1/1973 U.S.S.R. .............................. 549/248 21 Appl. No.: 348,198 Primary Examiner-P. E. Konopka Attorney, Agent, or Firm-Keil & Witherspoon 22 Filed: Feb. 12, 1982 57 ABSTRACT (30) Foreign Application Priority Data A process for reactivating avanadium-containing oxi Mar. 4, 1981 (DE) Fed. Rep. of Germany ....... 3.08101 dation catalyst, wherein the catalyst is treated first at from 100 to 600' C., with a volatile phosphorus com 51) Int. Cl. ........................ B01J 23/92; B01J 21/20; pound in the presence of an oxygen-containing gas, and B01J 27/28; C07D 307/89 then at from 50 to 600 C. with sulfur trioxide or a 52 U.S.C. ...................................... 502/35; 260/369; mixture of a volatile sulfur compound and an oxygen 549/248; 549/257; 549/258; 549/259; 502/37 containing gas. 58) Field of Search ..................... 252/41 R, 416, 415; 549/248 4 Claims, No Drawings 4,411,818 2 Although German Published Application DAS No. REACTIVATION OF VANADIUM-CONTAINING 1,468,816 discloses that oxidation catalysts containing OX DATION CATALYSTS vanadium and phosphorus can be reactivated by the addition of phosphites, the novel process is not sug The present invention relates to a process for reacti 5 gested by this procedure since the advantageous results vating vanadium-containing oxidation catalysts. These of the process of the invention are not obtained when catalysts are conventionally used for the preparation of the catalyst is treated with the phosphorus compound carboxylic acids, carboxylic acid anhydrides or qui or the sulfur compound alone, or when the substances nones by oxidation of saturated or unsaturated aliphatic are employed for treatment in the reverse sequence. or aromatic hydrocarbons. The oxidation is carried out O Suitable volatile phosphorus compounds are those industrially in the vapor phase, using air, in a fixed bed which are volatile at the temperatures of the reactiva or fluidized bed reactor. tion according to the invention, examples being phos Vanadium-containing catalysts which have become phines, eg. trimethylphosphine, phosphine oxides, eg. important for large-scale industrial processes are, for trimethylphosphine oxide, hydrogen phosphide, phos example, those used for the preparation of phthalic 15 phorus oxides, eg. phosphorus pentoxide, phosphates or anhydride (PA) from o-xylene or naphthalene, of ma phosphites, eg. CP(OCH2)3CH3)3, phosphorus halides, leic anhydride (MA) from benzene or saturated or un eg. phosphorus trichloride, phosphorus oxyhalides, eg. saturated aliphatic hydrocarbons of 4 to 6 carbon atoms, phosphorus oxychloride, or phosphorus sulfohalides. or of anthraquinone from diphenylmethane compounds. In addition to sulfur trioxide, preferred volatile sulfur Catalysts of this type which contain vanadium, for ex compounds are those which are converted under the ample in the form of vanadium pentoxide, together with reactivation conditions, with air or another oxygen titanium dioxide, and whose active material also con containing gas, or with a catalyst, completely or in part tains other active constituents, for example the oxides of into sulfur trioxide, for example sulfur dioxide, hydro cesium, rubidium, phosphorus or antimony, are de gen sulfide, mercaptans, eg. ethylmercaptan, carbon scribed, for example, in German Laid-Open Applica 25 disulfide, elementary sulfur, sulfur halides, eg. sulfur tions DOS Nos. 2,436,009 or 2,510,994. dichloride, and sulfur oxyhalides, eg. thionyl chloride. These vanadium-containing catalysts have the disad Particularly good results are obtained when triphen vantage that they undergo a continuous loss of activity ylphosphine is used as the phosphorus compound and during operation. To maintain an adequate conversion, SO3 or SO2 as the sulfur compound. it is therefore necessary to employ increasingly severe 30 The novel process is particularly suitable for reacti reaction conditions. This can be effected, for example, vating vanadium-containing catalysts used for the oxi by increasing the reaction temperature, lowering the dation of o-xylene or naphthalene to PA. Such catalysts throughput of air, or decreasing the loading, of the air which are described, for example, in German Laid or of the carrier gas, with the hydrocarbon to be oxi Open Application DOS No. 2,510,994, are supported dized. 35 catalysts consisting of an inert carrier and a catalytically The loss in yield associated therewith, or the decrease active material which is applied onto the carrier, con in capacity, finally becomes so great that the catalyst tains, for example, from 1 to 30% by weight of vana can no longer be used economically and must be re dium pentoxide and from 70 to 99% by weight of tita placed. This is an expensive procedure, since the plant 40 nium dioxide, and can also contain small amounts, for has to be shut down for weeks, giving rise to loss of example up to 5% by weight, of other activators, eg. production. Additionally, the catalysts are expensive. rubidium oxide, cesium oxide, phosphorus pentoxide Attempts have therefore been made to counteract the and antimony trioxide. deactivation of the catalysts by continually adding acti For the production of PA, a catalyst of this type is vating substances to the catalyst. Sulfur dioxide is 45 conventionally placed in a tube oven whose tubes have added, for example, in the oxidation of o-xylene to give a diameter of from 18 to 40 mm and a length of from 1.0 PA. Without continual addition of these activators, the to 4.0 m, and are surrounded by a salt melt, kept at from catalyst loses activity even more rapidly, and the oper 340' to 450° C., for regulating the temperature. The ating conditions have to be rapidly made more severe to gaseous mixture of air and the hydrocarbon to be oxi maintain the desired results. Some or all of the activa 50 dized is passed through the tube oven. tor, eg. SO2, leaves the plant unchanged and therefore The novel reactivation process is carried out, for pollutes the environment; its removal from the waste example, as follows: the air or another oxygen-contain gases leaving the plant is very expensive. ing gas is preheated to from 20 to 500 C., advanta It is an object of the present invention to provide a geously from 100 to 300 C., the phosphorus com process for reactivating completely or partially deacti 55 pound is then added to the gas, and the mixture is passed vated vanadium-containing catalysts, which makes it over the catalyst in a tube reactor. The catalyst is heated unnecessary continually to add activators while the to 100°-600 C., advantageously to 200-500° C., by the catalyst is in use, and makes it possible to maintain high heat transfer medium circulating through the reactor yields and throughputs in the catalytic oxidation. tubes. The amount of phosphorus compound used pro We have found that this object is achieved by the 60 vides from 1.0 to 10,000, advantageously from 10 to process according to the invention, in which the reacti 1,000, mg of phosphorus per 100 g of catalytic material vation of a vanadium-containing oxidation catalyst is in the catalyst. The amount of air laden with the phos effected as follows: the catalyst is treated first at from phorus compound, or of the carrier gas, is from 0.01 to 100 to 600 C., with a volatile phosphorus compound 8.0, advantageously from 0.1 to 5.0, m3 (S.T.P.) per in the presence of an oxygen-containing gas, and then at 65 hour per 100 g of catalytic material. The mixture of the from 50' to 600 C. with sulfur trioxide or a mixture of phosphorus compound and the air or carrier gas con a volatile sulfur compound and an oxygen-containing tains from 0.01 to 10,000, advantageously from 0.1 to gas. 1,000, mg of phosphorus per m of gas. 4411,818 3 4. In a particularly advantageous embodiment of the The amount of gas mixture passed over the catalyst is invention, the phosphorus compound required for acti from 0.5 to 8.0, advantageously from 1.0 to 6, m3 vating the catalyst is added during operation, ie. during (S.T.P.) per hour. The concentration of o-xylene can be the oxidation of, for example, o-xylene with air, since it up to 150g per m3 (S.T.P.) of gas mixture. is thus not necessary to interrupt the production of PA, The concentration of SO3, SO2 or a suitable sulfur and particularly rapid and good activation is obtained. compound in the air or in the carrier gas, which can also For this purpose, the liquid orgaseous phosphorus com be laden with o-xylene, can be varied within wide lim pound is added to the carrier gas before the latter is its. The procedure is advantageously carried out using passed into the reactor. The phosphorus compound can an excess of air or carrier gas, particularly when the also be dissolved in liquid o-xylene and added together O latter is laden with o-xylene. therewith to the air.
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