PILARISASI ANION TETRATITANAT STRUKTUR LAYER OLEH SPESIES POLIKATION ZIRKONIUM (IV)

Pilarisasi spesies zirkonium(IV) ke dalam anion tetratitanat struktur layer (Ti4O9 2-) berhasil dilakukan melalui 3 tahap: 1). pertukaran kation K+ pada kalium tetratitanat dengan H+ dari HCl menjadi hidrogen tetrtatitanat, 2). interkalasi butilamonium ke dalam layer anion tetratitanat dan 3). pertukaran kation butilamonium dengan kation spesies zirkonium(IV). Prosedur tersebut lebih dikenal sebagai metode Chimie Douce. Spesies polikation Zr(IV) diperoleh dengan cara melarutkan kristal ZrOCl2.8H2O dalam pelarut air pada kondisi berbagai pH lingkungan reaksi yaitu 0,1; 0,9 dan 1,8). Padatan yang dihasilkan dikarakterisasi dengan difraktometer sinar-X (XRD). Secara khusus, analisis kadar Ti dan Zr dalam padatan yang dihasilkan pada pH lingkungan reaksi = 0,9 dengan spektrometer pendar sinar-X. Pilarisasi spesies Zr(IV) ke dalam anion tetratitanat struktur layer ditunjukkan bahwa spesies kationik Zr(IV) yang terpilar pada antar layer anion tetratitanat (Ti4O9 2-) pada kondisi pH lingkungan reaksi: 0,1; 0,9 dan 1,8 terdiri dari tiga jenis spesies yaitu [Zr(H2O)8]4+, [Zr(OH)(H2O)7]3+ dan [Zr(OH)2(H2O)6]2+. Spesies [Zr(OH)(H2O)7]3+ mendominasi pada pH = 0,9 dan berkurang dominasinya pada pH yang lebih rendah (pH = 0,1). Pada pH yang lebih tinggi (pH = 1,8) dominasi dari kluster [Zr(OH)(H2O)7]3+ berkurang, dan muncul kluster lain yaitu [Zr(OH)2(H2O)6]2+. Rumus molekul yang mungkin padatan yang dihasilkan pada pH lingkungan = 0,9 dalam kondisi major didasarkan data spektrometer pendar sinar-X: [Zr(OH)(H2O)7]0,089H1,911 Ti4O9.x H2O

PILLARIZATIONOF LAYERED TETRATITANATES ANION BYZIRCONIUM(IV) POLYCATION SPECIES Pilarisasi Layer Anion Tetratitanat o/eh Spesies Polikation Zirkonium(lV)

ABSTRACT Pilfaring layered tetratitanates anion by zirkonium(lV) polycation species has been realized by three steps: 1). cationexchange of potasium tetratitanates, 2). intercalation of n-butylamine compound in layered hydrogen tetratitanates and 3). intercalation of zirconium(IV) polycation species by mixing butylamine-intercalated tetratitanates with an aqueous solution of ZrOC12.8H20at pH various: 0.1, 0.9 and 1.8. The procedure was carried out by Chimie Douce method. The structures oftitanates and the products which had undergone ft exchange and intercalated by n-butylamine and zirkonium(IV) polycation spesies were investigated by.X-rays Diffractometer(XRD) and X-rays Fluorescence (XRF). It was found in the research that [Zr(H20)ef+, [Zr(OH)(H20M3+or [Zr(OHMH20)B!+types have presented in the [nterlayerof the products. At pH = 0.1 and 0.9, [Zr(OH)(H20hf.+ type was pillared more dominated in layered tetratitanates than [Zr(H20)ef+ type. At pH 1.8, it was signaled that [Zr(OH)(H20)r+ and [Zr(OHMH20)B!+ types intercalated in layered tetratitanates. Keywords: tetratitanates, intercalation, zirconium(IV) species, Chimie Douc

OLIGOMERIC CHROMIUM(III) POLICATION SPECIES-PILLARED LAYERED TETRATITANATES ANION

Intercalation of oligomeric chromium(III) polycation species in layered tetratitanates was prepared by three steps: 1) ion-exchange of H+ for K+ in potasium tetratitanates, 2) intercalation of n-alchylamine (n-propylamine, n-butylamine, n-amylamine, and n-hexylamine) compounds in layered hydrogen tetratitanates by adding an aqueous solution of  5M n-alchylamine to  hydogen titanates with stiring at room temperature,  and 3) intercalation of oligomeric chromium(III) polycation species by mixing butylamine-intercalated tetratitanates with an aqueous solution of CrCl3.6H2O at pH various. The procedure was carried out by Chimie Douce method. The results showed that all of n-alchylamine-intercalated tetratitanates crystallize on monoclinic crystal system with the Bravais lattice C. The hight intensity of the first peaks (200)  indicated that butylamine and amylamine-intercalated tetratitanates have a remarkably high crystallinity without impurities phase. The interlayered distance (d) and  the lattice parameter projected along a increase with increasing the amount of C-atoms in n-alchylamine. At pH=1.3, [CrCl(H2O)5]2+ or [CrCl2(H2O)4]+ species was pillared more efective in layered tetratitanates than [Cr(H2O)6]3+ spesies and just one spesies, Cr(H2O)6]3+ at  pH=1.7. On the contrary, [Cr(OH)(H2O)5]2+ or [Cr(OH)2(H2O)4]+ was  intercalated more effevtive than [Cr(H2O)6]3+ species  at pH=5.3.   Keywords: tetratitanates, intercalation, oligomeric chromium(III) species, Chimie Douce

PILLARIZATION OF LAYERED TETRATITANATES ANION BY ZIRCONIUM(IV) POLYCATION SPECIES

Pillaring layered tetratitanates anion by zirkonium(IV) polycation species has been realized by three steps: 1). cation-exchange of potasium tetratitanates, 2). intercalation of n-butylamine compound in layered hydrogen tetratitanates and 3). intercalation of zirconium(IV) polycation species by mixing butylamine-intercalated tetratitanates with an aqueous solution of ZrOCl2.8H2O at pH various: 0.1, 0.9 and 1.8. The procedure was carried out by Chimie Douce method. The structures of titanates and the products which had undergone H+ exchange and intercalated by n-butylamine and zirkonium(IV) polycation spesies were investigated by X-rays Diffractometer (XRD) and X-rays Fluorescence (XRF). It was found in the research that [Zr(H2O)8]4+, [Zr(OH)(H2O)7]3+ or [Zr(OH)2(H2O)6]2+ types have presented in the interlayer of the products. At pH = 0.1 and 0.9, [Zr(OH)(H2O)7]3+ type was pillared more dominated in layered tetratitanates than [Zr(H2O)8]4+ type. At pH 1.8, it was signaled that [Zr(OH)(H2O)7]3+ and [Zr(OH)2(H2O)6]2+ types intercalated in layered tetratitanates.   Keywords: tetratitanates, intercalation, zirconium(IV) species, Chimie Douc

CRYSTALLIZATION AND CHARACTERIZATION OF CHROMIUM-CONTAINING SILICALITE-1

Chromium-containing silicalite-1, designed CrS-1, was synthesized by the hydrothermal method and characterized by XRD and FTIR techniques. The objectives of the research are to study the synthesis of CrS-1 and investigate the effect of crystallization temperatures and times toward its character. All samples of CrS-1 crystallized in orthorhombic structure and Pnma space group. The phase observed in the XRD patterns of CrS-1 synthesized from 150 to 190 oC for 11 days showed only MFI-type phase. The CrS-1 prepared under static condition for 1 day at 150 oC indicated -SiO2 phase, on the contrary, the samples conditioned for 2 to 8 days at 150 oC are only MFI phase.   Keywords: Crystallization, synthesis, chromium silicate CrS-1, incorporation