Patent GB-1264634-A (GB)
IPC: B01J23/96
Filed: 1969-07-10
Abstract: 1,264,634. Regeneration of deactivated catalyst. ENGELHARD MINERALS & CHEMICALS CORP. 10 July, 1969 [11 July, 1968], No. 34892/69. Heading B1E. A fixed bed of catalyst, which comprises noble metal of Group VIII, for example ruthenium, rhodium, palladium, osmium, iridium, platinum or a mixture thereof, supported on alumina derived by calcination of a hydrous alumina precursor containing a major proportion of alumina trihydrate and which has been deactivated by use in the treatment of hydrocarbons in the presence of molecular hydrogen so that carbonaceous material has been deposited thereon, is regenerated and reactivated by a method which comprises removing the carbonaceous material, for example by an oxidative burn-off in the presence of an oxygen-containing gas, for example at a temperature below 1000‹F, preferably of from 700 to 850‹F, and a pressure of from 100 to 500 pounds per square inch gauge, and thereafter contacting the catalyst, at a temperature of from 600 to 950‹F, successively with a first gaseous stream comprising oxygen, chlorine or chlorine-containing material, for example carbon tetrachloride, methylchloride, trichlorethylene or ethylenedichloride, in the vapour state and, optionally, water vapour until at least 0.2 per cent by weight of chlorine, based upon the total weight of Group VIII noble metal and alumina, has been added thereto and with a second gaseous stream comprising oxygen and water vapour but containing neither chlorine nor chlorine-containing material. After contact with the gaseous streams, the catalyst may contain from 0.4 to 1 per cent by weight of chlorine based on the total weight of Group VIII noble metal and alumina. Each gaseous stream contains oxygen in an amount such that the oxygen partial pressure thereof is from 3 to 100 pounds per square inch absolute. When the first gaseous stream contains water vapour, such gaseous stream contains water vapour in an amount such that the water vapour to chlorine mole ratio thereof is not greater than 10. Each gaseous stream (or, when the first gaseous stream does not contain water vapour, the second gaseous stream) contains water vapour in an amount such that the water vapour partial pressure thereof is not greater than 0.8 pounds per square inch absolute, the total amount of water vapour contacting the catalyst lying between defined limits which are dependent upon the exact temperature of the gaseous streams; the total amount of water vapour contacting the catalyst preferably does not exceed 4 per cent by weight, based on the catalyst, when the contact is effected at a temperature of 900‹F and preferably does not exceed 12 per cent by weight, based on the catalyst, when the contact is effected at a temperature of 700‹F. The first gaseous stream and/or the second gaseous stream may contain at least 100 parts per million by volume of water vapour. The catalyst is contacted with the first gaseous stream for a time preferably not greater than 4 hours and with the second gaseous stream for a time preferably greater than 2 hours, for example for at least 4 hours. Before or after removal of carbonaceous material therefrom or after contact with the gaseous streams, the catayst may be contacted, at a temperature of from 800 to 1000‹F and a pressure of from 100 to 500 pounds per square inch gauge, with an oxygencontaining gas. The alumina may have been prepared by calcination, for example at a temperature of from 700 to 1200‹F, of a precursor containing alumina trihydrate selected from bayerite, gibbsite and norstrandite (randomite); such precursor also may contain boehnite (alumina monohydrate) and/or amorphous hydrous alumina. The catalyst, which may contain gamma alumina or eta alumina and from 0.05 to 2 per cent by weight of platinum, may have a surface area of at least 150 m<SP>2</SP>/g, for example from 150 to 250 m<SP>2</SP>/g.