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PORE STRUCTURE AND MORPHOLOGY CHARACTERIZATIONS OF MESOPOROUS ZSM-5 SYNTHESIZED AT VARIOUS AGING TIME Hartanto, Djoko; Purbaningtias, Tri Esti; Fansuri, Hamzah; Prasetyoko, Didik
Jurnal ILMU DASAR Vol 12 No 1 (2011)
Publisher : Fakultas Matematika dan Ilmu Pengetahuan Alam Universitas Jember

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Abstract

Mesoporous ZSM-5 has been successfully synthesized at various aging time of 6, 12 and 24 h. Mesoporous ZSM-5 was synthesized using cetyltrimethylammonium bromide (CTABr) as a template. Synthesis was carried out hydrothermally with aging and crystallization temperature at 60oC and 150oC. XRD patterns of the resulted material showed diffraction lines at 2? = 23o and at small angle (2? < 5o) which is characteristic of the structure of ZSM-5 and the existing of the mesoporous material. It was found that crystallinity of the sample increased at longer aging time. The result of nitrogen gas sorption analysis showed that all samples have pore size about 3,8 nm. The porosity of ZSM-5 decreased with shorter of aging time. ZSM-5 synthesized at 6 h aging time has the highest porosity of 72.57%. Aging time also affected the particle size, the longer the aging time, the smaller the particle size. The particle size was ranging 1.25 ? 1.0 ?m.
UKURAN PARTIKEL DAN KONFORMASI KRISTAL ZEOLIT-A HASIL SINTESIS DENGAN PENAMBAHAN TETRAPROPILAMMONIUM HIDROKSIDA (TPAOH) Widiastuti, Nurul; Thalib, Farhanah; Prasetyoko, Didik; Fansuri, Hamzah
Reaktor Volume 15, No.2, OKTOBER 2014
Publisher : Dept. of Chemical Engineering, Diponegoro University

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (684.131 KB) | DOI: 10.14710/reaktor.15.2.132-138

Abstract

Abstract PARTICLE SIZE AND CRYSTAL CONFORMATION OF SYNTHESIZED ZEOLITE-A WITH TETRAPROPYLAMMONIUM HYDROXIDE (TPAOH) ADDITION. The aims of this research is to study the effect of tetrapropylammonium hydroxide (TPAOH) concentration in the synthesis of zeolite A to its physical characteristics such as crystallinity, crystal conformation and average crystal size. The zeolite A was synthesized with composition 3.165 Na2O : 1.000 Al2O3: 1.926 SiO2: 128 H2O : x TPAOH where x was 0; 0.0385; 0.0577; 0.0770; 0.1540 and 4.1602. The zeolite was crystalized under hydrothermal condition in a stainless steel autoclave at 100°C for 5 hours. The resulting crystal was washed with distilled water until pH 8 and then dried in an oven at 80oC for 24 hours. FT-IR and XRD analysis results show that the synthesized zeolite A at x = 4.1602 has the lowest crystallinity. It is estimated due to the mass of TPAOH was four times higger than the mass of zeolite framework components (Si and Al). SEM and PSD (Particle Size Distribution) analysis results show that TPAOH concentration affected the crystal conformation and the average size of zeolite A particles. The formation of chained crystal conformation was caused by the electrostatic interactions between TPA+ and negatively charge of zeolite framework. In addition, the particel size of the synthesized zeolite A at x = 0.1540 was 2.024 µm which was smaller than the particel size of the synthesized zeolite A without TPAOH, which was 3.534 µm.  Keywords: average size of particles; crystal conformation; TPAOH; zeolite A  Abstrak Penelitian ini bertujuan untuk mempelajari pengaruh konsentrasi TPAOH (Tetrapropilamonium hidroksida) dalam sintesis zeolit A terhadap sifat fisikanya yang meliputi kekristalan, konformasi kristal dan ukuran rata-rata kristal yang terbentuk. Pada penelitian   ini   zeolit A   disintesis    dengan komposisi 3,165 Na2O : 1 Al2O3 : 1,926 SiO2 :128 H2O: x TPAOH. Konsentrasi TPAOH divariasikan dengan nilai x adalah 0; 0,0385; 0,0577; 0,0770; 0,1540 dan 4,1602. Metode hidrotermal digunakan dalam penelitian ini dengan kondisi suhu  hidrotermal 100°C dan waktu kristalisasi selama 5 jam dengan pH pencucian 8. Hasil karakterisasi menggunakan FT-IR (Fourier Transform ? Infrared Spectroscopy) dan XRD (X-Ray Diffraction)  menunjukkan bahwa zeolit A yang disintesis dengan x = 4,1602 memiliki kekristalan terendah. Hal ini diperkirakan terjadi karena masa TPAOH yang digunakan empat kali lebih besar daripada masa penyusun zeolit (Si dan Al). Berdasarkan hasil karakterisasi menggunakan SEM (Scanning Electron Microscopy) dan PSD (Particle Size Distribution), dapat diketahui bahwa TPAOH berpengaruh terhadap konformasi kristal dan rata-rata ukuran kristalnya.  Terbentuknya konformasi kristal seperti rantai disebabkan oleh adanya interaksi elektrostatik antara muatan positif pada TPA+ dan muatan negatif dari kerangka zeolit. Zeolit A yang disintesis dengan x = 0,1540 memiliki ukuran partikel rata-rata 2,024 µm yang lebih kecil dari daripada zeolit A tanpa TPAOH yaitu sebesar 3,534 µm. Kata kunci : ukuran partakel rata-rata; konformasi kristal; TPAOH; zeolite A  
PENGARUH KONSENTRASI TITANIUM DALAM TITANIUM SILIKALIT PADA VIBRASI GUGUS HIDROKSIL PERMUKAAN DENGAN MENGGUNAKAN TEKNIK SPEKTROSKOPI INFRAMERAH Prasetyoko, Didik; Ramli, Zainab; Endud, Salasiah; Nur, Hadi
Alchemy Jurnal Penelitian Kimia Vol 4, No 2 (2005)
Publisher : Alchemy Jurnal Penelitian Kimia

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Abstract

Padatan titanium silikat(TS1) yang mempunyai kandungan titanium berbeda telah disintesis dengan teknik hidrotermal. Struktur padatan dikarakterisasi dengan menggunakan teknik difraksi sinar X, spektroskopi inframerah dan Uvvis DR. Gugus hidroksil permukaan diamati dengan teknik spektroskopi inframerah setelah sampel dievakuasi pada suhu 400oC. Hasil menunjukkan adanya kaitan yang erat antara konsentrasi titanium tetrahedral,pergeseran puncak hidroksil permukaan dan jumlah titanol.
MODIFICATION OF TUREN BENTONITE WITH ALCL3 FOR ESTERIFICATION OF PALMITIC ACID Abdulloh, Abdulloh; Maryam, Siti; Aminah, Nanik Siti; Triyono, Triyono; Trisunaryanti, Wega; Mudasir, Mudasir; Prasetyoko, Didik
Bulletin of Chemical Reaction Engineering & Catalysis 2014: BCREC Volume 9 Issue 1 Year 2014 (SCOPUS Indexed, April 2014)
Publisher : Department of Chemical Engineering - Diponegoro University

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (728.293 KB) | DOI: 10.9767/bcrec.9.1.5513.66-73

Abstract

Natural Turen bentonite has been modified and applied as catalyst for palmitic acid esterification. Modification of natural Turen bentonite was conducted by cation exchange method using AlCl3 solution. Catalyst characterization was performed on X-ray Fluoroscence, X-ray Diffraction, nitrogen adsorption-desorption and infrared spectroscopy techniques. The catalytic activity test in the esterification reaction of palmitic acid with methanol was conducted by bath at 65 °C with a variation of reaction time of 1, 2, 3, 4 and 5 h. Catalytic activity has been observed qualitatively using GC-MS and quantitatively by changes in acid number. The analysis showed the formation of Al3+-bentonite. Observation on the elements has shown that the presence of calcium decreased from 10.2% to 4.17%, with an increase of aluminium content from 9.9% to 13%. Diffraction line at 2? 5.7379º became 5.6489º, along with changes in d-spacing of 15.3895 Å to 15.6319 Å. The surface area increased from 83.78 m2/g to 91.26 m2/g, while Brönsted acid sites increased from 10.2 µmol/g to 67.5 µmol/g and Lewis acid sites increased from 94.9 µmol/g to 132 µmol/g. Furthermore, Al3+-bentonite has showed as active catalyst in the esterification reaction of palmitic acid with palmitic acid with conversion of 78.78% for 5 h. © 2014 BCREC UNDIP. All rights reservedReceived: 24th September 2013; Revised: 31st December 2013; Accepted: 26th January 2014[How to Cite: Abdulloh, A., Maryam, S., Aminah, N.S., Triyono, T., Trisunaryanti, W., Mudasir, M., Prasetyoko, D. (2014). Modification of Turen?s Bentonite with AlCl3 for Esterification of Palmitic Acid. Bulletin of Chemical Reaction Engineering & Catalysis, 9 (1): 66-73. (doi:10.9767/bcrec.9.1.5513.66-73)][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.9.1.5513.66-73]
SYNTHESIS OF CAOZNO NANOPARTICLES CATALYST AND ITS APPLICATION IN TRANSESTERIFICATION OF REFINED PALM OIL Yulianti, Cicik Herlina; Ediati, Ratna; Hartanto, Djoko; Purbaningtias, Tri Esti; Chisaki, Yoshifumi; Jalil, Aishah Abdul; Che Ku Hitam, Che Ku Nor Liana; Prasetyoko, Didik
Bulletin of Chemical Reaction Engineering & Catalysis 2014: BCREC Volume 9 Issue 2 Year 2014 (SCOPUS Indexed, August 2014)
Publisher : Department of Chemical Engineering - Diponegoro University

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (524.493 KB) | DOI: 10.9767/bcrec.9.2.5998.100-110

Abstract

The CaOZnO nanoparticle catalysts with Ca to Zn atomic ratios of 0.08 and 0.25 have been successfully synthesized by co-precipitation method. The catalyst was characterized by X-ray Diffraction (XRD) analysis provided with Rietica and Maud software, Scanning Electron Microscopy (SEM) and Fourier Transform Infrared spectroscopy (FT-IR), and its properties was compared with bare CaO and ZnO catalysts. The phase composition estimated by Rietica software revealed that the CaO catalyst consists of CaO and CaCO3 phases. The estimation of the particle size by Maud software, showed that the particle size of all catalysts increased by the following order: ZnO. © 2014 BCREC UNDIP. All rights reservedReceived: 1st January 2014; Revised: 10th March 2014; Accepted: 18th March 2014[How to Cite: Yulianti, C.H., Ediati, R., Hartanto, D., Purbaningtias, T.E., Chisaki, Y., Jalil, A.A., Hitam, C.K.N.L.C.K., Prasetyoko, D., (2014). Synthesis of CaOZnO Nanoparticles Catalyst and Its Application in Transesterification of Refined Palm Oil. Bulletin of Chemical Reaction Engineering & Catalysis, 9 (2): 100-110. (doi:10.9767/bcrec.9.2.5998.100-110)][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.9.2.5998.100-110]
SYNTHESIS AND CHARACTERIZATION OF ZSM-5 MESOPOROUS WITH VARIATION RATIOS OF SiO2/Al2O3 Khalifah, Susi Nurul; Prasetyoko, Didik
Jurnal Zeolit Indonesia Vol 7, No 2 (2008)
Publisher : Jurnal Zeolit Indonesia

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Abstract

ZSM-5 Mesoporous with variation ratios of SiO2/Al2O3 20, 35, 50, and 100 have been successfully synthesized. Phase of mesoporous created using Cetyltrimethylammonium bromide (CTABr) templates. Crystal obtained has an acidity and higher thermal stability. Diffraction peaks typical of ZSM-5 appeared at 2θ = 7-9 ° and 2 θ = 23.02 °, while typical peak of mesoporous materi als appeared on 2θ
THE PHENOL HYDROXYLATION USING A MoO3/TS-1 CATALYST THAT CALCINED ON THE VARIOUS TEMPERATURE Farika, Anis; Akhlus, Syafsir; Prasetyoko, Didik
Jurnal Zeolit Indonesia Vol 9, No 2 (2010)
Publisher : Jurnal Zeolit Indonesia

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Abstract

MoO3/TS-1 catalyst has been proven have a higher catalityc activity rather than TS-1 on phenol hydroxylation reaction become a hydroquinone. Preparation catalyst using a impregnasi technique with ammonium molbidate as a precursor. Catalyst calcined at temperature 400-800°C and characterized by X-Ray Diffraction (XRD), pyridin adsorption, and hydrophilicity test. Calcinations temperature affects a catalyst characteristic and related to catalyst activity. MoO3/TS-1 catalyst has been calcined at temperature 400°C showed a higher hydrophilicity rather than TS-1, a faster speed reaction on phenol hydroxylation, and increasing of catalyst activity rather than initial catalyst, TS-1.
Condensation of Indole with Isatin over AlCl3/Mesoporous Aluminosilicate Purbaningtias, Tri Esti; Prasetyoko, Didik; Bahruji, Hasliza; Zein, Yusuf Muhammad; Triwahyono, Sugeng; Fadlan, Arief; Qoniah, Imroatul
Indonesian Journal of Chemistry Vol 15, No 1 (2015)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (365.91 KB) | DOI: 10.22146/ijc.21224

Abstract

Aluminium chloride immobilized on mesoporous aluminosilicate was investigated as catalysts in the condensation of isatin with indole. AlCl3/mesoporous aluminosilicate (AlCl3/AM) catalysts were prepared by impregnation of 1, 5, 10 and 15 wt% AlCl3 on the surface of mesoporous aluminosilicate. A maximum conversion of isatin was achieved using 15% AlCl3/AM catalyst whereas the highest selectivity of 68.97% towards trisindoline was obtained using pure AM. The activity of the catalysts was depended on their acid site number and surface area. The number of Brønsted acid and the surface area affected to the conversion of isatin while the total acidity and the number of Lewis acid influenced the selectivity.
SYNTHESIS OF ZEOLITE BETA DIRECTLY FROM RICE HUSK ASH: EFFECT OF REACTION COMPOSITION ON CRYSTALLINITY OF ZEOLITE BETA Prasetyoko, Didik; Ramli, Zainab; Endud, Salasiah; Hamdan, Halimaton; Sulikowski, Bogdan
Indonesian Journal of Chemistry Vol 6, No 1 (2006)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (258.267 KB) | DOI: 10.22146/ijc.21765

Abstract

White rice husk ash obtained from complete uncontrolled burning of rice husk contains more than 94% silica. The ash, which consists of crystalline silica of the type tridymite and a-crystobalite, was used directly as a source of silica in the synthesis of zeolite beta. The mole oxide ratio of the initial gel of 1.25-8Na2O: 10-120SiO2: Al2O3: 1-20TEA2O: 150-1000H2O was prepared and heated at 150°C in a static condition for 6 d. The solid phases formed were monitored by XRD technique. Influence of reaction mixture ratio in the initial gel to the crystalline products formed was studied. Results showed that the pure zeolite beta was formed in a certain range of reaction mixture, i.e.: 1.25-4Na2O : 15-45SiO2 : Al2O3 : 4-10TEA2O : 240-480H2O. The other ratio of reaction mixtures produced crystalline phases such as analcime, Na-P, mordenite, and gismondine, and non-reacted of a-crystobalite and tridymite. Keywords: rice husk ash, tridymite, a-crystobalite, zeolite beta, synthesis
CATALYTIC PERFORMANCES OF Fe2O3/TS-1 CATALYST IN PHENOL HYDROXYLATION REACTION Prasetyoko, Didik; Royani, Cholifah Endah; Fansuri, Hamzah; Ramli, Zainab; Nur, Hadi
Indonesian Journal of Chemistry Vol 10, No 2 (2010)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (392.369 KB) | DOI: 10.22146/ijc.21452

Abstract

Hydroxylation reaction of phenol into diphenol, such as hydroquinone and catechol, has a great role in many industrial applications. Phenol hydroxylation reaction can be carried out using Titanium Silicalite-1 (TS-1) as catalyst and H2O2 as an oxidant. TS-1 catalyst shows high activity and selectivity for phenol hydroxylation reaction. However, its hydrophobic sites lead to slow H2O2 adsorption toward the active site of TS-1. Consequently, the reaction rate of phenol hydroxylation reaction is tends to be low. Addition of metal oxide Fe2O3 enhanced hydrophilicity of TS-1 catalyst. Liquid phase catalytic phenol hydroxylation using hydrogen peroxide as oxidant was carried out over iron (III) oxide-modified TS-1 catalyst (Fe2O3/TS-1), that were prepared by impregnation method using iron (III) nitrate as precursor and characterized by X-ray diffraction, infrared spectroscopy, nitrogen adsorption, pyridine adsorption, and hydrophilicity techniques. Catalysts 1Fe2O3/TS-1 showed maximum catalytic activity of hydroquinone product. In this research, the increase of hydroquinone formation rate is due to the higher hydrophilicity of Fe2O3/TS-1 catalysts compare to the parent catalyst, TS-1.   Keywords: Fe2O3/TS-1, hydrophilic site, phenol hydroxylation