scholarly journals STUDY ON THE CONCENTRATION EFFECT OF Nb2O5-ZAA CATALYST TOWARDS TOTAL CONVERSION OF BIODIESEL IN TRANSESTERIFICATION OF WASTED COOKING OIL

2010 ◽  
Vol 6 (3) ◽  
pp. 268-274
Author(s):  
Astuti Tri Padmaningsih ◽  
Wega Trisunaryanti ◽  
Iqmal Tahir

Study on the concentration effect of Nb2O5-ZAA catalyst towards total conversion of biodiesel has been conducted. The natural zeolite (ZA) was activated by dipping in NH4Cl solution and was calcined using N2 atmosphere at 500 °C for 5h to produce the ZAA sample. The Nb2O5-ZAA catalyst was made by mixing the activated natural zeolite (ZAA), Nb2O5 3 % (w/w) and oxalic acid 10 % (w/w) solution, until the paste was formed, followed by drying and calcining the catalyst for 3 h at 500 °C under N2 atmosphere. Catalyst characterizations were conducted by measuring acidity with NH3 gas using gravimetric method and porosimetric analysis using N2 gas adsorption based on the BET equation by surface area analyzer instrument. The Nb2O5-ZAA catalyst was then used as an acid catalyst in free fatty acid esterification reaction of wasted cooking oil in methanol medium with variation of catalyst concentration: 1.25%; 2.5%; 3.75% and 5% towards the weight of oil+methanol. The reaction was continued by transesterification of triglyceride in the used cooking oil using NaOH catalyst in methanol medium. For comparison, the esterification reaction using H2SO4 catalyst 1.25% towards the weight of oil+methanol has been conducted as well. Methyl ester (biodiesel) product was analyzed using Gas Chromatography (GC) and Gas Chromatography-Mass Spectrometry (GC-MS). The characters of biodiesel were analyzed using American Society for Testing and Materials (ASTM) method. The results showed that modification of ZAA by impregning Nb2O5 3% (w/w) increased the total catalyst acidity from 5.00 mmol/g to 5.65 mmol/g. The Nb2O5-ZAA catalyst has specific surface area of 60.61 m2/g, total pore volume of 37.62x10-3 cc/g and average pore radius of 12.41 Å. The Nb2O5-ZAA catalyst with concentration of 1.25%-5% produced higher total conversion of biodiesel than that of H2SO4 catalyst 1.25%. The Nb2O5-ZAA catalyst with concentration of 3.75% produced the highest total conversion of biodiesel, i.e. 76.76 %. Based on the ASTM data analysis, the product has a qualification as diesel fuel.   Keywords: biodiesel, transesterification, natural zeolite, niobium catalyst

2017 ◽  
Vol 5 (1) ◽  
pp. 1
Author(s):  
Hulyadi Hulyadi

NTB has a large zeolite potential with a zeolite content percentage of 190,405 tons. One area that has great potential is the Selong belanak Central Lombok precisely at coordinates 8o51'48.5 "S 116o10'62.0" E mull mullet. Utilization of zeolite Lombok area is only used as a mixture of animal feed because it has not done research on its potential. One potential zeolite is its ability as an absorbent. Alcohol fermentation has not been able to be an alternative as a solution to energy problems. Alcohol fermentation only produces alcohols of less than 30% purity. This is caused by acetic acid byproducts that make microbes in the fermentation process can not breed optimally. From these problems need to be performed zeolite characteristic for optimal utilization. The purpose of this research is to find out the characteristics of natural zeolite of Selong belanak Lombok as an adsorbent in purifying alcohol of fermentation. The method of this research is descriptive with data collecting technique performed by zeolite characterization including cation exchange capacity with Schollenberger method, surface area using methylene blue method, absorption using Iodometry titration method, zeolite water content using gravimetric method and alcohol concentration determined by specific gravity and instrument GC-MS. Based on the result of natural zeolite research, Selong belanak Lombok has characteristic with natural cation zeolite exchange capacity of Selong Belanaq Lombok for 14,0894 meq / 100 gram. The zeolite surface area is 16, 3537 m2 / gram. Absorption zeolite to iodium is relatively low at 2.9357%. water content obtained from natural zeolite Selong Belanaq Lombok is 7.74%. After use of various alcoholic distillate absorbent fermentation alcohol concentration was obtained 81.4%. Based on the findings of natural zeolite researchers mullet tubes need to be activated more optimally to produce alcohols with purity above 99%, as laden mixture material in gasoline. 


REAKTOR ◽  
2016 ◽  
Vol 16 (2) ◽  
pp. 72
Author(s):  
Nuryoto - Nuryoto ◽  
Hary Sulistyo ◽  
Wahyudi Budi Sediawan ◽  
Indra Perdana

Abstract MODIFIED  MORDENITE NATURAL ZEOLITE AS CATALYST FOR KETALIZATION AND ESTERIFICATION. The aims of this research was studied of  modified mordenite natural zeolite from Bayah effect by acidity and heating to change zeolite characteristics in orde to prepare as catalyst for glycerol ketalization and  acetit acid esterification by some reaction temperature variation. Natural zeolite which modified by precise treatment will be  produced of natural zeolite that ready for use as catalyst and has good perfomance. The characterization results showed that the best condition for modified mordenite natural zeolite of  Bayah achieved at sulfuric acid concentration of 6 N and heating temperature of 200oC, by surface area reached of 157.110 m2/g and cation exchanged capacity of 2.11 meq/ml. Modernite natural zeolite of Bayah has good performance indication as a catalyst, by the highest glycerol conversion of  70.10% at 60°C for the ketalization reaction, and for the esterification reaction, mordenit natural zeolit of Bayah able to acetit acid conversion of 11.72% at 70°C.   Keywords: characterization; esterification; glycerol; modified; ketalization Abstrak Penelitian ini bertujuan untuk untuk mempelajari pengaruh modifikasi dengan pengasaman dan pemanasan terhadap perubahan karakteristik zeolit alam mordenit dari Bayah guna persiapan sebagai katalisator pada reaksi ketalisasi gliserol dan esterifikasi asam asetat dengan beberapa variasi suhu reaksi. Zeolit alam yang termodifikasi dengan perlakuan yang tepat akan menghasilkan zeolit alam yang siap pakai, dan akan mampu menghasilkan performa yang baik. Hasil pengujian karakterisasi menunjukkan bahwa kondisi terbaik pada modifikasi zeolit alam mordenit Bayah dihasilkan pada konsentrasi pengasaman 6N H2SO4 dan suhu pengeringan 200oC dengan luas permukaan 157,110 m2/g dan kemampuan tukar kation sebesar 2,11 meq/ml. Zeolit alam mordenit Bayah menunjukkan performa yang baik sebagai katalisator dengan konversi gliserol tertinggi sebesar 70,10%  yang dicapai pada suhu 60oC pada reaksi ketalisasi, dan untuk reaksi esterifikasi,  zeolit alam mordenit Bayah mampu mengkonversi asam setat sebesar 11,72% pada suhu 70oC. Kata kunci: karakterisasi; esterifikasi; gliserol; modifikasi; ketalisasi


2010 ◽  
Vol 8 (3) ◽  
pp. 342-347 ◽  
Author(s):  
Wega Trisunaryanti ◽  
Suryo Purwono ◽  
Arista Putranto

Catalytic hydrocracking of waste lubricant oil into liquid fuel fraction using ZnO, Nb2O5, activated natural zeolite (ZAAH) and their modification has been investigated. The zeolite was produced in Wonosari, Yogyakarta. Activation of the zeolite was carried out by refluxing with HCl 3M for 30 min, produced the activated natural zeolite (ZAAH). The ZnO/ZAAH catalyst was prepared by impregnation of Zn onto the ZAAH by ion exchange method using salt precursor of Zn(NO3)2.4H2O. The Nb2O5/ZAAH catalyst was prepared by mixing the ZAAH sample with Nb2O5 and oxalic acid solution until the paste was formed. The impregnation of Zn onto Nb2O5/ZAAH was carried out using the same method to that of the ZnO/ZAAH catalyst resulted ZnO/Nb2O5-ZAAH catalyst. Characterization of catalyst includes determination of Zn metal by Atomic Absorption Spectroscopy (AAS), acidity by gravimetric method and catalyst porosity by Surface Area Analyzer (NOVA-1000). Catalytic hydrocracking was carried out in a semi-batch reactor system using ZnO, ZAAH, ZnO/ZAAH and ZnO/Nb2O5-ZAAH catalysts at 450 oC under the H2 flow rate of 15 mL/min. and the ratio of catalyst/feed = 1/5. The composition of liquid products was analyzed by Gas Chromatograpy (GC).The results showed that impregnation of ZnO and/or Nb2O5 on the ZAAH increased the acidity and specific surface area of catalyst. The products of the hydrocracking process were liquid, coke and gas. Conversion of liquid products was increased by the increase of catalyst acidity. The highest liquid product was produced by ZnO/Nb2O5-ZAAH catalyst, 52.97 wt-%, consist of gasoline, 38.87 wt-% and diesel, 14.10 wt-%.   Keywords: hydrocracking, waste lubricant oil, liquid fuel fraction


Author(s):  
Reza Yazdanpanah ◽  
Eshagh Moradiyan ◽  
Rouein Halladj ◽  
Sima Askari

Aim and Objective: The research focuses on recent progress in the production of light olefins. Hence, the common catalyst of the reaction (SAPO-34) deactivates quickly because of coke formation, we reorganized the mechanism combining SAPO-34 with a natural zeolite in order to delay the deactivation time. Materials and Methods: The synthesis of nanocomposite catalyst was conducted hydrothermally using experimental design. Firstly, Clinoptilolite was modified using nitric acid in order to achieve nano scaled material. Then, the initial gel of the SAPO-34 was prepared using DEA, aluminum isopropoxide, phosphoric acid and TEOS as the organic template, sources of Aluminum, Phosphor, and Silicate, respectively. Finally, the modified zeolite was combined with SAPO-34's gel. Results: 20 different catalysts due to D-Optimal design were synthesized and the nanocomposite with 50 weight percent of SAPO-34, 4 hours Crystallization and early Clinoptilolite precipitation showed the highest relative crystallinity, partly high BET surface area and hierarchical structure. Conclusion: Different analysis illustrated the existence of both components. The most important property alteration of nanocomposite was the increment of pore mean diameters and reduction in pore volumes in comparison with free SAPO-34. Due to low price of Clinoptilolite, the new catalyst develops the economy of the process. Using this composite, according to formation of multi-sized pores located hierarchically on the surface of the catalyst and increased surface area, significant amounts of Ethylene and Propylene, in comparison with free SAPO-34, were produced, as well as deactivation time that was improved.


Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 217
Author(s):  
Marin Ugrina ◽  
Martin Gaberšek ◽  
Aleksandra Daković ◽  
Ivona Nuić

Sulfur-impregnated zeolite has been obtained from the natural zeolite clinoptilolite by chemical modification with Na2S at 150 °C. The purpose of zeolite impregnation was to enhance the sorption of Hg(II) from aqueous solutions. Chemical analysis, acid and basic properties determined by Bohem’s method, chemical behavior at different pHo values, zeta potential, cation-exchange capacity (CEC), specific surface area, X-ray powder diffraction (XRPD), scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), as well as thermogravimetry with derivative thermogravimetry (TG-DTG) were used for detailed comparative mineralogical and physico-chemical characterization of natural and sulfur-impregnated zeolites. Results revealed that the surface of the natural zeolite was successfully impregnated with sulfur species in the form of FeS and CaS. Chemical modification caused an increase in basicity and the net negative surface charge due to an increase in oxygen-containing functional groups as well as a decrease in specific surface area and crystallinity due to the formation of sulfur-containing clusters at the zeolite surface. The sorption of Hg(II) species onto the sulfur-impregnated zeolite was affected by the pH, solid/liquid ratio, initial Hg(II) concentration, and contact time. The optimal sorption conditions were determined as pH 2, a solid/liquid ratio of 10 g/L, and a contact time of 800 min. The maximum obtained sorption capacity of the sulfur-impregnated zeolite toward Hg(II) was 1.02 mmol/g. The sorption mechanism of Hg(II) onto the sulfur-impregnated zeolite involves electrostatic attraction, ion exchange, and surface complexation, accompanied by co-precipitation of Hg(II) in the form of HgS. It was found that sulfur-impregnation enhanced the sorption of Hg(II) by 3.6 times compared to the natural zeolite. The leaching test indicated the retention of Hg(II) in the zeolite structure over a wide pH range, making this sulfur-impregnated sorbent a promising material for the remediation of a mercury-polluted environment.


2014 ◽  
Vol 660 ◽  
pp. 297-300
Author(s):  
Nor Hazwani Abdullah ◽  
Sulaiman Hassan

Waste cooking oil has always been an environment problem in food factories and one method of effect disposing this oil without effecting the environment is to convert it to fatty acid methyl ester (FAME) using small scale pilot plant. The conversion of waste cooking oil with sodium hydroxide as a catalyst in conversional process at 22kHz speed. The reaction of time, molar ratio, speed, catalyst and amount of catalyst will be effect in FAME quality. The quality of biodiesel define is total ester content using gas chromatography. Gas chromatography analysis is a one of technique for identification and quantitation of compounds in a biodiesel sample. From biodiesel sample can identification of contaminants and fatty acid methyl ester. In this research biodiesel sample were analyses using a gas chromatography-flame ionization detector ( Perkin Elmer GC Model Clarus 500) equipped with a DB-5 HT capillary column ( 0.53mm x 5 m) J&W Scientific. The analytic conditions for ester content were as follow by: column temperature used 2100C, temperature flame ionization detector (FID) of 2500C, pressure of 80kPa, flow carrier gas of 1ml/min, temperature injector of 2500C, split flow rate of 50ml/min, time for analysis 20 minute and volume injected of 1 μl. The ester content (C), expresses as a mass fraction in present using formula (EN 14103, 2003a) calculation. Conversion of triglyceride (TG) to FAME using conversional process obtained 96.54 % w.t with methanol to oil molar ratio 6:1, 1%w.t acid sulphuric and 1% w.t sodium hydroxide catalyst.


Clay Minerals ◽  
2011 ◽  
Vol 46 (2) ◽  
pp. 241-250 ◽  
Author(s):  
V. Lilkov ◽  
O. Petrov ◽  
V. Petkova ◽  
N. Petrova ◽  
Y. Tzvetanova

AbstractThis paper presents results from comparative thermogravimetric, calorimetric and pozzolanic activity analyses of five natural zeolite samples from Bulgaria, Slovakia, Philippines, USA and North Korea. The zeolites actively participate in the hydration processes of cement. Their activity in the early stage of hydration is based mainly on the large surface area of the particles while, in the later stages of activation, chemical reactions occur between the products of the hydration of cement and the soluble SiO2 that is present in the bulk of the zeolites. It has been shown that in all cement pastes which contain zeolite additives, the quantity of portlandite is lower than that in pure cement paste or is even totally absent. The amounts of hydration products are greater when 30% zeolite is used than when 10% zeolite is added (excluding the sample with chabazite). The lowest pozzolanic activity is shown by chabazite, which possessed the lowest SiO2/Al2O2 ratio.


2013 ◽  
Vol 14 (3) ◽  
pp. 219 ◽  
Author(s):  
Dwi Kartika ◽  
Senny Widyaningsih

Transesterification of waste cooking oil into biodiesel using KOH catalyst with and without esterification process usingactivated natural zeolite (ZAH) catalyst has been carried out. Activation of the zeolite was done by refluxing with HCl 6Mfor 30 min, followed calcining and oxydized at 500oC for 2 hours, consecutively. The transesterification without esterificationprocess were done using KOH catalyst 1% (w/w) from oil and methanol weight and oil/methanol molar ratio 1:6 at 60oC. Theesterification reaction was also done using ZAH catalyst then continued by transesterification using KOH catalyst inmethanol media. In order to study the effect of ZAH catalyst concentration at constant temperature, the catalysts werevaried, i.e. 0, 1, 2, and 3% (w/w). To investigate the effect of temperature, the experiments were done at various temperaturefrom 30, 45, 60, and 70oC at constant catalyst concentration. The conversion of biodiesel was determined by 1H-NMRspectrometer and physical properties of biodiesel were determined using ASTM standard methods. The results showedthat the transesterification using KOH catalyst without esterification produced biodiesel conversion of 53.29%. The optimumcondition of biodiesel synthesis via esterification process were reached at 60oC and concentration of ZAH catalyst of2% (w/w), that could give biodiesel conversion = 100.00%. The physical properties were conformed with biodiesel ASTM2003b and Directorate General of Oil and Gas 2006 specification.


2018 ◽  
Author(s):  
◽  
Elvis Tinashe Ganda

Thermochemical catalytic conversion of ethanol-waste cooking oil (eth-WCO) mixtures was studied over synthesised aluminosilicate catalysts HZSM-5, FeHZSM-5 and NiHZSM-5. The thermochemical reactions were carried out at temperatures of 400° and 450°C at a fixed weight hourly space velocity of 2.5 h-1 in a fixed bed reactor system. Successful conversion of the eth-WCO mixtures was carried out over the synthesised catalyst systems and in order to fully understand the influence of the catalysts, several techniques were used to characterise the synthesised materials which include XRD, SEM, EDS, BET techniques. Results of the catalyst characterisation showed that highly crystalline solid material had been formed as evidenced by the high relative crystallinity in comparison with the commercial HZSM-5 catalyst at 2θ peak values of 7°- 9° and 23°- 24°. The introduction of metals decreased the intensity of the peaks leading to lower values of relative crystallinity of 88% and 90% for FeHZSM-5 and NiHZSM-5, respectively. However this was even slightly higher than the commercial sample which had a value of 86% with respect to HZSM-5 synthesised catalyst taken as reference material. There was no significant change in XRD patterns due to the introduction of metal. Elemental analysis done with energy dispersive spectroscopy showed the presence of the metal promoters (Fe, Ni) and the Si/Al ratio obtained from this technique was 38 compared to the target ratio of 50 set out initially in the synthesis. From the SEM micrographs the morphology of the crystals could be described as regular agglomerated sheet like material. Surface area analysis showed that highly microporous crystals had been synthesised with lower external surface area values ranging from 57.23 m2/g - 100.82 m2/g compared to the microporous surface area values ranging from 195.96 m2/g to 212.51 m2/g. For all catalyst employed in this study high conversions were observed with values of over 93 %, almost total conversion was achieved for some samples with values as high as 99.6 % with FeHZSM-5 catalysts. Despite the high level of conversion the extent of deoxygenation varied with lower values recorded for FeHZSM-5 (25%WCO) at 400°C and NiHZSM-5 (75%WCO) at 450°C with oxygenated hydrocarbons of 19.5% and 19.33% respectively. The organic liquid product yield comprised mostly of aromatic hydrocarbon (toluene, p-xylene and naphthalene) decreased with the introduction of metal promoters with NiHZSM-5 producing higher yields than FeHZSM-5. For the pure waste cooking oil (WCO) feedstock the parent catalyst HZSM-5 had a liquid yield of 50% followed by NiHZSM-5 with 44% and lastly FeHZSM-5 had 40% at 400°C which may be seen to follow the pattern of loss of relative crystallinity. An increase in operating temperature to 450°C lowered the quantity of organic liquid product obtained in the same manner with the HZSM-5 parent catalyst still having the highest yield of 38% followed by Ni-HZSM-5 with 36% and Fe-HZSM-5 having a value of 30% for pure waste cooking oil feedstock which may be attributed to thermally induced secondary cracking reactions. For all catalyst systems with an increase in the content of waste cooking oil from 25% to 100% in the feed mixture there was a linearly increasing trend of the liquid product yield. HZSM-5 catalyst increased from 14% to 50% while FeHZSM-5 increased from 16% to 40% and NiHZSM-5 increased from 12% to 44% at a temperature setting of 400°C with lower values observed at 450°C.Results obtained in this study show the potential of producing aromatics for fuel and chemical use with highly microporous zeolite from waste material such as waste cooking oil forming part of the feedstock.


2010 ◽  
Vol 3 (2) ◽  
pp. 91-97 ◽  
Author(s):  
Eddy Heraldy ◽  
Hisyam SW ◽  
Sulistiyono Sulistiyono

Characterization and activation of Natural Zeolite from Ponorogo (ZAP) have been done to improve the quality of zeolite as porous material. Analysis of mineral composition is done using X-Ray Difraction (XRD), Fourier Transform-Infra Red (FTIR) Spectroscopy and metal analysis using Atomic Absorption Spectroscopy (AAS). Characterization of the activated zeolite covered about number of acidic sites, surface area, ratio Si/Al and metal composition (Na, Ca, K and Fe). Activated processes is done using various mineral acid, i.e HCl, HNO3, H2SO4 and HPO4 with each concentration at 1 M and 3 3 hours dipping. The result showed that ZAP has composition Ca-klinoptilolit (43.09 %), gismondin (17.57 %), modernit (4.21 %) and quartz (10.37 %). The most efectif of the acid to activate is HCl and is proved to absorp of Zn in waste water. The effect of chemical activation is increasing the ratio of Si/Al, increasing the surface area and reducing some metal composition.   Keywords: natural zeolite, chemical activation, porous material


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