Patent GB-1319544-A (GB)
Title: Process for the preparation of catalysts containing crystalline aluminosilicate zeolite
IPC: B01J29/08
Filed: 1970-05-14
Abstract: 1319544 Zeolite-containing hydrocarbon cracking catalysts KONINKLIJKE ZWAVELZUURFABRIEKEN 14 May 1970 [18 June 1969] 23457/70 Heading B1E [Also in Division C5] Hydrocarbon cracking catalyst containing crystalline aluminosilicate zeolite, silica and an oxide of at least one metal selected from Groups IIA, IIIA and IVA is prepared by a process comprising the steps of (a) adding mineral acid to an aqueous alkaline solution containing alkali metal silicate thereby to gel silica therefrom, (b) adding to the resulting mixture at least one solution containing a compound of at least one metal selected from Groups IIA, IIIA and IVA, (c) hydrolysing such compound(s), (d) washing the resulting precipitate, for example to an alkali metal content of less than 0.1 weight per cent (dry basis) and (e) drying, preferably spray drying, the washed precipitate, for example at a temperature of from 105 to 600‹C, there being added, either to the silicate-containing solution before step (a) or to the mixture of mineral acid and silicate-containing solution resulting from step (a) prior to gellation of silica therefrom, an aqueous suspension containing crystalline aluminosilicate zeolite which has had its alkali metal content reduced by at least one ion exchange and thereafter has been thermally treated, for example by heating in an inert medium at a temperature of from 120 to 900‹C. The zeolite, which may be natural or synthetic and selected from mordenite and Zeolites X, Y, L, D, T and K-G, may have been ion exchanged with ions selected from hydrogen ions, ammonium ions, alkaline earth metal ions and rare earth metal ions; the zeolite-containing suspension may contain dissolved alkaline earth metal and/or rare earth metal salt(s). Gelling of silica from the alkali metal silicate solution may be effected by a procedure comprising mixing part of the mineral acid and part of the silicate solution, allowing gelling to occur and adding, to the resulting mixture, the remainder of the acid and then the remainder of the silicate solution. The compound(s) of metal(s) selected from Groups IIA, IIIA and IVA may be chosen to provide catalyst comprising a binary co-gel of silica and beryllia, magnesia, alumina, titania or thoria or a ternary co-gel of silica and alumina-magnesia, alumina-zirconia, alumina-thoria or magnesia-zirconia, silica constituting preferably from 55 to 99 weight per cent (dry basis) of such gel; a preferred co-gel consists of silica and alumina which may be derived by the sequential addition, to the mixture comprising zeolite and silica gel, of aluminium sulphate solution and of sodium aluminate solution. As exemplified, thermallytreated rare earth metal-exchanged zeolite Y (Examples 1, 2, 3 and 5) or zeolite X (Example 4), sulphuric acid, sodium silicate, aluminium sulphate and sodium aluminate are used in the preparation of catalyst by a procedure comprising spray drying and subsequent treatment of the spray dried product with steam at a temperature of 700‹C or 750‹C, the catalyst being regenerated after use by oxidative burn-off in air to remove coke deposited thereon. Reference has been directed by the Comptroller to Specification 3414525.