反応 #1973896
ord-8fc8dc0d77d247f4987441317360e075
反応方程式
反応条件
後処理
- 1workup.ADDITIONwhile mixing the slurry
実験手順
Initially, iron sulfate heptahydrate was prepared from iron powder and sulfuric acid. 100 g of iron powder were added to 7.6 liters of deionized water in a 22 liter round bottomed flask. Separately, 86 ml of concentrated H2SO4 was mixed with 500 ml of deionized water to prepare a sulfuric acid solution. The sulfuric acid solution was added dropwise over a period of 2 hours to the iron powder slurry while mixing the slurry. The slurry was stirred overnight after completion of addition of the sulfuric acid solution to the slurry to form a solution of iron sulfate heptahydrate. After stirring, the solution was heated between 30-45° C. for 3 hours and gas evolution was observed. The warm iron sulfate solution was then added over a period of 1 hour to a stirred solution, under nitrogen, containing 398 g of (NH4)2MoS4 in 7.6 liters of deionized water. The iron sulfate solution was added to the (NH4)2MoS4 solution by pumping the iron sulfate solution through a 2.75″×0.020″ outer diameter injector nozzle immersed in the (NH4)2MoS4 solution. After addition of the iron sulfate solution to the (NH4)2MoS4 solution was completed, the mixture was stirred under nitrogen at ambient temperature (28° C.) for a period of 2 hours. The mixture was then allowed to settle overnight. The solids were then separated from the mixture using a continuous centrifuge. The separated solids were washed with deionized water, then dried by azeotropic distillation. 526 grams of solid catalyst were recovered. Semi-quantitative fluorometry (XRF) indicated that the catalyst contained, on a mass basis, 17.6% Fe, 37.8% Mo, 44.5% S, and 0.04% Ni. The catalyst material was particulate and had a particle size distribution with a mean particle size of 213 μm as determined by laser diffractometry using a Mastersizer S made by Malvern Instruments. The BET surface area of the catalyst was measured and found to be 301 m2/g. The pore volume of the catalyst was found to be 0.311 cm3/g and the mean pore diameter was found to be from 20 to 150 angstroms. X-ray diffraction and Raman IR spectroscopy confirmed that at least a portion of the catalyst had an iron tetrathiomolybdate structure in which iron, sulfur, and molybdenum were arranged as shown in Formula (XII) above.