Hidrodesulfurisasi tiofen menggunakan katalis CoMo H Zeolit Y
MUSTA, Rustam, Prof. Dra. Wega Trisunaryanti, M.S., Ph.D.Eng
2009 | Tesis | S2 Ilmu Kimia
Telah dilakukan penelitian terhadap reaksi hidrodesulfurisasi (HDS) tiofen menggunakan katalis CoMo/H-zeolit Y. Katalis dipreparasi dari NH4Y kemudian di oven pada temperatur 115oC selama 1 jam untuk menghilangkan kandungan air lalu dikalsinasi pada temperatur 550oC selama 2 jam untuk menguapkan amonia. Pengembanan logam CoMo dilakukan dengan metode koimpregnasi, di mana HY(10 g) dicampur dalam larutan (NH4)6Mo7O24.4H2O dalam 24 mL aquabides dan 3 mL amonia. Campuran ini kemudian dicampurkan lagi dengan Co(NO3)2.6H2O dalam 24 mL aquabides dan 3 mL amonia. Sampel hasil lalu disaring dan dikeringkan. Sampel yang telah kering tersebut selanjutnya dikalsinasi sambil dialiri gas N2 pada temperatur 550oC selama 2 jam, dioksidasi dengan dialiri gas O2 selanjutnya direduksi dengan dialiri gas H2 masing-masing pada temperatur 400oC selama 2 jam. Karakterisasi katalis untuk analisis keberadaan gugus NH3 dilakukan dengan spektofotometer infra red (IR), kristalinitas dengan X-ray diffraction (XRD) serta uji keasaman dengan absorpsi basa NH3 menggunakan metode gravimetri. Kadar logam teremban pada zeolit ditentukan dengan atomic absorption spectroscopy (AAS). Proses hidrodesulfurisasi (HDS) tiofen dilakukan dalam reaktor sistem batch dengan variasi temperatur 200, 250, 300, 350, 400 oC dan variasi laju alir gas pembawa (H2) 40, 55, 70, 85, 100 mL/menit. Produk cair dianalisis dengan gas chromatography mass spectrometry (GCMS). Konversi produk gas dihitung berdasarkan persentase berat produk gas terhadap umpan. Hasil karakterisasi katalis CoMo/H-zeolit Y aktif dengan spektra IR mempelihatkan hilangnya amonia yang ditunjukkan dengan menurunnya intensitas peak pada bilangan gelombang 1404,18 dan hilangnya peak pada bilangan gelombang 3186,40. XRD menunjukkan peningkatan kristalinitas di mana kristalinitas NH4Y Hydrodesulfurization reaction (HDS) of tiofen using catalyst CoMo/H-zeolite Y has been done. Catalyst was prepared from NH4Y-zeolite then heated 115oC for 1 h to eliminate water then calcined at 550oC for 2 h to evaporate ammonia, produced HY-zeolite (HYZ) sample. Impregnation of CoMo metals on the HYZ sample was done by co-impregnation method, where the HYZ (10 g) was mixed with (NH4)6MO7O24.4H2O in 24 mL aquabidest and 3 mL of ammonia then stirred of 60oC for 2 h. This mixture was then mixed with Co(NO3)2.6H2O in 24 mL aquabidest and 3 mL of ammonia then stirred of 60oC for 2 h. The resulting sample was filtered and dried. The dried sample was then calcined under N2 stream at temperature of 550oC for 2 h, followed by oxidized with O2 then reduced with H2 stream at temperature 400oC for 2 h, respectively produced CoMo/HY catalyst. Characterization of the catalyst included analysis of NH3 groups was done with by infra red spectrofotometry (IR), the crystallinity with X-ray diffraction (XRD) and the acidity was calculated with NH3 absorption by gravimetry method, metal content on the catalyst was determined by atomic absorption spectroscopy (AAS). Hidrodesulfurization (HDS) of tiophene was done in batch reactor system under the various temperature of 200, 250, 300, 350, 400 oC and various of H2 flow rate at 40, 55, 70, 85, 100 mL/min. The liquid product was analysed with gas chromatography mass spectrometry (GCMS). The gas product conversion was calculated based on weight percentage of gas product to tiophene. IR result of CoMo/HY catalyst showed that disappeared ammonia was after heating. The XRD date indicated the increase of catalyst crystallinity as the following: NH4Y< died NH4Y < HY< CoMo/HY. CoMo/HY catalyst has average acidity = 6,87 mmol/g where as the HY has average acidity = 7,66 mmol/g. The metal content in the HY was 8023 and 7681 ppm, for Co and Mo respectively . Result of GCMS analyzed showed the existence tiofen peak at retention time of 3,764 min. Maximum gas conversion at temperature 350oC = 82.07% (b/b) with k = 49.56 min-1.
Kata Kunci : Katalis CoMo,H,zeolit Y,Hidrodesulfurisasi,Tioven,Konversi gas