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In water; at 375℃; under 760.051 Torr; for 6h;Inert atmosphere; Flow reactor;
The dehydrocyclization activities of Zn?Cr?Ocatalysts calcined at different temperatures were performedat 375°C and atmospheric pressure in a fixedbedvertical quartz reactor (i.d = 8 mm, length =450 mm) placed in a two zone furnace operated in adown flow mode. In the first zone maintained at300°C the reaction mixture was preheated whereas inthe second zone containing the catalyst bed the reactortemperature was set at 375°C. Temperatures in theboth zones were monitored by a temperature controller-cum-programmer using a K-type thermocouple.Glycerol (Fluka) and EDA (SDFCL, India) wereused. Nitrogen (IOLAR-I grade, BOC, India) wasused as a carrier gas. The catalytic activities were measured using ?18/+23 sieved (BSS) particles. The carbonmass balance was done based on the inlet and outletconcentration of the organic moiety. Prior to thereaction, the calcined catalyst (about 0.2 g) wasreduced in a flow of 5percent H2 and 95percent Ar (30 mL min?1)at 400°C for 5 h. The catalytic activities were measuredunder strict kinetic control. An aqueous glycerol solution(20 wtpercent in H2O) was used with a glycerol to EDAmole ratio of 1 :1 , at a flow rate of 5 mL h?1 (10 mmolglycerol + 10 mmol EDA + 200 mmol H2O), alongwith N2 as a carrier gas at a flow rate of 1800 mL h?1.The feed mixture mole ratio is glycerol : EDA : H2O :N2= 1 : 1 : 20 : 8. The product mixture was analyzed bygas chromatograph (Shimadzu, GC-17A) via a flameionization detector (FID) using a ZB-5 capillary columnat a ramping rate of 10°C min?1 from 60 to280°C. The mass balance for all the measurements was>95percent. The samples were analyzed by GC-MS(QP5050A Shimadzu) using a ZB-5 capillary columnwith EI mode.
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