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Vanadium Contribution to the Surface Modification of Titanium Silicalite for Conversion of Benzene to Phenol Mulyatun, Mulyatun; Prasetyoko, Didik
IPTEK The Journal for Technology and Science Vol 22, No 2 (2011)
Publisher : Institut Teknologi Sepuluh Nopember

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.12962/j20882033.v22i2.58

Abstract

Vanadium oxide supported on the surface of titanium silicalite was investigated in benzene hydroxylation to determine its activity as heterogeneous catalyst. Effect of vanadium loading on structure and activity of titanium silicalite was investigated. On the basis of X-ray diffraction and infrared spectroscopy techniques, it was found that the titanium structure was remained on the modified catalyst. The catalytic activity of the modified catalyst was observed to be higher than that of parent catalyst.
Structural Characterization of Tungsten Oxides Supported on Titanium Silicalite Prasetyoko, Didik; Ramli, Zainab; Endud, Salasiah; Nur, Hadi
IPTEK The Journal for Technology and Science Vol 19, No 2 (2008)
Publisher : Institut Teknologi Sepuluh Nopember

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.12962/j20882033.v19i2.150

Abstract

Titanium silicalite (TS-1) is known as an active material catalyst in the epoxidation reaction. In this study, tungsten oxides (WO3) with various loading amount have been supported on the TS-1 to increase of the catalytic activity of the TS-1 material. The solids structure and property were investigated by X-ray diffraction (XRD), temperature programmed reduction (TPR), ultra violet-visible diffuse reflectance (UV-Vis-DR) and infrared (IR) spectroscopy and scanning electron microscopy (SEM) techniques. The results showed that the structure of TS-1 is not collapsed after impregnation of WO3. It was also found that tungsten species have interacted with the silanol groups on the surface of TS-1.
Synthesis and Characterization of Low Loading MoO3/Ts-1 Catalyst Indrayani, Suci; Prasetyoko, Didik
IPTEK The Journal for Technology and Science Vol 19, No 4 (2008)
Publisher : Institut Teknologi Sepuluh Nopember

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.12962/j20882033.v19i4.144

Abstract

Abstract⎯Molybdenum oxide (MoO3) have been introduced to titanium silicalite (TS-1) by impregnation methode and have been characterized with X-ray diffraction (XRD), infrared spectroscopy, nitrogen and pyridine adsorption. The results show that TS-1 and XMoO3/TS-1 have orthorhombic structure and MFI framework structure type. 0,5% MoO3/TS-1, dan 1% MoO3/TS-1 catalyst have not been yet Brønsted acid site, while Brønsted acidity increased from 2% MoO3/TS-1 to 4% MoO3/TS-1 respectively.
Activities of Heterogeneous Acid-Base Catalysts for Fragrances Synthesis: A Review Hartati, Hartati; Santoso, Mardi; Triwahyono, Sugeng; Prasetyoko, Didik
Bulletin of Chemical Reaction Engineering & Catalysis 2013: BCREC Volume 8 Issue 1 Year 2013 (SCOPUS Indexed)
Publisher : Department of Chemical Engineering - Diponegoro University

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (71.575 KB) | DOI: 10.9767/bcrec.8.1.4394.14-33

Abstract

This paper reviews various types of heterogeneous acid-base catalysts for fragrances preparation. Catalytic activities of various types of heterogeneous acid and base catalysts in fragrances preparation, i.e. non-zeolitic, zeolitic, and mesoporous molecular sieves have been reported. Generally, heterogeneous acid catalysts are commonly used in fragrance synthesis as compared to heterogeneous base catalysts. Heteropoly acids and hydrotalcites type catalysts are widely used as heterogeneous acid and base catalysts, respectively. © 2013 BCREC UNDIP. All rights reservedReceived: 20th January 2013; Revised: 31st March 2013; Accepted: 1st April 2013[How to Cite: Hartati, H., Santoso, M., Triwahyono, S., Prasetyoko, D. (2013). Activities of Heterogeneous Acid-Base Catalysts for Fragrances Synthesis: A Review. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1): 14-33. (doi:10.9767/bcrec.8.1.4394.14-33)][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4394.14-33] | View in  |
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 MIPA Universitas Jember

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (473.394 KB)

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 2θ = 23o and at small angle (2θ < 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 μm. Keywords: Pore structure, morphology, mesoporous ZSM-5, aging time
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 (71.575 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 2θ 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 (71.575 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 of UiO-66 Using Solvothermal Method at High Temperature Rahmawati, Ika Diah; Ediati, Ratna; Prasetyoko, Didik
IPTEK Journal of Proceedings Series Vol 1 (2014): International Seminar on Applied Technology, Science, and Arts (APTECS) 2013
Publisher : Institut Teknologi Sepuluh Nopember

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.12962/j20882033.v1i1.417

Abstract

UiO-66 solids have been synthesized using solvothermal method in which reaction mixtures of zirconium tetrachloride (ZrCl4) and 1,4-benzenedicarboxylic acid (BDC) in N-N-dimethylformamide (DMF) were heated at 140 °C for 6, 12, 24, 36, 48, 72 and 144 hours, respectively. The weight of reaction products, in the form white powder, increased with the increase in heating time up to 72 hours, then decreased. Characterization results using XRD showed that the diffractogram of the solid obtained at heating time of 6 h had the same pattern to that of reported UiO-66, characterized by a main peak with a high intensity at 2θ of 7.3°, as well as other characteristic peaks with lower intensity at 2θ of 8.4°; 25.6° and 30.6°. The longer the heating time (12 and 24 h), the lower the intensity of the main peak. When the reaction mixtures were heated for 36 h or longer, the obtained solid diffractograms showed that the main peak intensity at 2θ of 7.3° was lower than the second peak, and new peaks appeared at 2θ of 13.8°; 15.8° and 17.5°. SEM micrographs showed that the solid synthesized for 6 h was in the form of clusters of square morphology, whereas solids synthesized for 72 h showed needle-like surface morphology
Crystal Growth of IRMOF-3 (Isoreticular Metal-Organic Frameworks-3) Synthesized using Solvothermal Method Deka, Pemta Tia; Ediati, Ratna; Prasetyoko, Didik
IPTEK Journal of Proceedings Series Vol 1 (2014): International Seminar on Applied Technology, Science, and Arts (APTECS) 2013
Publisher : Institut Teknologi Sepuluh Nopember

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.12962/j20882033.v1i1.416

Abstract

IRMOF-3 crystals have been synthesized using solvothermal method by reacting zinc nitrate hexahydrate with 2-amino-1,4-benzenedicarboxylic acid in NN-dimethylformamide ( DMF ) at 100 °C for 18, 24, 48, 72, 120 and 144 h to observe crystal growth . The obtained crystals were characterized using X - ray Diffraction ( XRD ) , SEM ( Scanning Electron Microscopy ) and Scanning Electron Microscopy - Energy Dispersive X-ray ( SEM - EDX ). Diffractograms of crystals synthesized at heating times of 24 and 48 hours showed major peaks at 2θ of 6.8; 9.6 and 13.7, which are the characteristic peaks of an IRMOF-3 crystal. The size of IRMOF-3 crystals observed using SEM increased with the increase in heating time up to 48 h, then decreased at heating times of 72, 120 and 144 h. The largest IRMOF-3 crystal is of cube shape with a particle size of 500 µm. The weight of the resulting crystals increased with the increase in heating time, then remained constant after 72 h.
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 | 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