Process for regeneration of hydrogenation catalysts
The invention provides a process for regenerating a catalyst used for the hydrogenation of an aromatic species, consisting of several steps. First the system is purged with nitrogen, then air is metered in stepwise, and the addition of nitrogen is subsequently ended until only air is present.
1. A process for regenerating a catalyst used for the ring hydrogenation of an aromatic species, in at least one reactor, wherein the process comprises the following steps:
purging the at least one reactor in which the catalyst used is present with an inert gas, wherein the purging with an inert gas is commenced at a temperature of from 50 to 100° C.; followed by
stepwise addition of air to the inert gas during the purging of the reactor until the proportion of air in the total volume is between from 10% and 90% by volume; and then
a reduction in the amount of inert gas during the purging of the reactor until only air is flowing through the reactor,
wherein the temperature in the reactor during the regeneration is not more than 10° C. higher than the temperature at the reactor feed for the aromatic species, in the hydrogenation of the aromatic species,
wherein the catalyst comprises at least one transition metal selected from the group consisting of iron, ruthenium, nickel, rhodium, platinum, palladium, and mixtures thereof, on a support material selected from the group consisting of activated carbon, silicon carbide, aluminium oxide, silicon dioxide, aluminosilicate, titanium dioxide, zirconium dioxide, magnesium oxide, zinc oxide, and mixtures thereof.
2. The process according to claim 1 , wherein the temperature in the at least one reactor is monitored during the stepwise addition of air and/or during the reduction in the amount of inert gas.
3. The process according to claim 2 , wherein the temperature during the stepwise addition of air is not more than 20° C. higher than on commencement of the respective step of stepwise addition of air.
4. The process according to claim 2 , wherein the addition of air is stopped at least temporarily when the temperature during the stepwise addition of air is 20° C. above the temperature on commencement of the respective step of stepwise addition of air.
5. The process according to claim 4 , wherein inert gas is metered in during the stoppage.
6. The process according to claim 2 , wherein the temperature during the stepwise addition of air is not more than 15° C. higher than on commencement of the respective step of stepwise addition of air.
7. The process according to claim 2 , wherein the addition of air is stopped at least temporarily when the temperature during the stepwise addition of air is 15° C. above the temperature on commencement of the respective step of stepwise addition of air.
8. The process according to claim 2 , wherein the aromatic species is an aromatic ester.
9. The process according to claim 8 , wherein the aromatic ester is an ester of a benzenecarboxylic acid, of a benzenedicarboxylic acid, of a benzenetricarboxylic acid, or of a benzenetetracarboxylic acid.
10. The process according to claim 1 , wherein the purging of the at least one reactor with the inert gas is preceded by performance of the following steps:
decompressing the at least one reactor to a pressure of less than 10 bar;
displacing any remaining hydrogen from the at least one reactor by injecting an inert gas, to a pressure of more than 10 bar, and then decompressing the at least one reactor to a pressure of less than 10 bar.
11. The process according to claim 10 , wherein the injecting of an inert gas and the subsequent decompression is conducted at least twice.
12. The process according to claim 1 , wherein the duration for regenerating the catalyst is at least 24 hours.
13. The process according claim 1 , wherein the inert gas is selected from the group consisting of nitrogen, helium, neon, argon, carbon dioxide and mixtures thereof.
14. The process according to claim 1 , wherein the aromatic species is an aromatic ester.
15. The process according to claim 14 , wherein the aromatic ester is an ester of a benzenecarboxylic acid, of a benzenedicarboxylic acid, of a benzenetricarboxylic acid, or of a benzenetetracarboxylic acid.
16. The process according to claim 14 , wherein the aromatic ester is a C8- to C10-alkyl ester of phthalic acid or a C8- to C10-alkyl ester of terephthalic acid.
17. The process according to claim 1 , wherein the purging of the at least one reactor with the inert gas is preceded by performance of the following steps:
decompressing the at least one reactor to a pressure of less than 5 bar;
displacing any remaining hydrogen from the at least one reactor by injecting nitrogen, to a pressure of more than 15 bar, and then decompressing the at least one reactor to a pressure of less than 5 bar.
18. The process according to claim 1 , wherein the duration for regenerating the catalyst is at least 3 days.
19. The process according to claim 1 , wherein the purging of the at least one reactor with the inert gas is preceded by performance of the following steps:
decompressing the at least one reactor to a pressure of less than 7.5 bar; and
displacing any remaining hydrogen from the at least one reactor by injecting nitrogen to a pressure of more than 12.5 bar, and then decompressing the at least one reactor to a pressure of less than 7.5 bar.
20. The process according to claim 19 , wherein the injecting of nitrogen, and the subsequent decompression is conducted at least twice.