scholarly journals Esterification of Benzyl Alcohol with Acetic Acid over Mesoporous H-ZSM-5

Author(s):  
Desy Tri Kusumaningtyas ◽  
Didik Prasetyoko ◽  
Suprapto Suprapto ◽  
Sugeng Triwahyono ◽  
Aishah Abdul Jalil ◽  
...  

In this study, the performance of mesoporous ZSM-5 has been studied on the esterification of acetic acid (AA) with benzyl alcohol (BA). The mesoporous ZSM-5 catalyst has been synthesized with the variation of aging time i.e. 6, 12, and 24 hours at the same temperature, 70 °C. The cation exchange of Na-ZSM-5 to H-ZSM-5 was performed before the catalytic activity test. The acidity type and amount of solids were determined by FT-IR spectroscopy using pyridine as a probe molecule. The characterization by pyridine adsorption showed that at a higher mesoporous surface area, the number of Lewis acid was increased. The highest mesoporous surface area, Lewis, and Brönsted acid sites were obtained by sample which has the lowest crystallinity, i.e. 255.78 m2/g, 0.2732 mmol/g, and 0.20612 mmol/g, respectively. Influence of mesoporous volume was studied on the catalytic activity of the mesoporous ZSM-5 in the esterification reaction. Conversion of acetic acid in the esterification reaction for samples of    HZ-6, HZ-12, and HZ-24 were obtained by titration methods, i.e. 39.59, 36.39, and 32.90 %, respectively. Hence, the reaction temperature of 393 K, molar ratio 1:4 (AA:BA) and catalyst loading 5 % were selected as an optimum reaction parameters. Copyright © 2017 BCREC Group. All rights reservedReceived: 21st November 2016; Revised: 1st February 2017; Accepted: 18th February 2017How to Cite: Kusumaningtyas, D.T., Prasetyoko, D., Suprapto, Triwahyono, S., Jalil, A.A., Rosidah, A. (2017). Esterification of Benzyl Alcohol with Acetic Acid over Mesoporous H-ZSM-5. Bulletin of Chemical Reaction Engineering & Catalysis, 12 (2): 243-250 (doi:10.9767/bcrec.12.2.806.243-250)Permalink/DOI: http://dx.doi.org/10.9767/bcrec.12.2.806.243-250 

2011 ◽  
Vol 396-398 ◽  
pp. 2411-2415 ◽  
Author(s):  
Ping Lan ◽  
Li Hong Lan ◽  
Tao Xie ◽  
An Ping Liao

Isoamyl acetate was synthesized from isoamylol and glacial acetic acid with strong acidic cation exchanger as catalyst. The effects of reaction conditions such as acid-alcohol ratio, reaction time, catalyst dosage to esterification reaction have been investigated and the optimum reaction conditions can be concluded as: the molar ratio of acetic acid to isoamylol 0.8:1, reaction time 2h, 25 % of catalyst (quality of acetic acid as benchmark). The conversion rate can reach up to 75.46%. The catalytic ability didn’t reduce significantly after reusing 10 times and the results showed that the catalyst exhibited preferably catalytic activity and reusability.


2017 ◽  
Vol 743 ◽  
pp. 355-359
Author(s):  
Svetlana A. Popova ◽  
Irina Yu. Chukicheva

[bnmim]HSO4 and [bnpy]HSO4 are active and environmentally friendly catalysts for the acetylation of camphene with acetic acid. The reaction provides isobornyl acetate with 100% selectivity and 72-86% yield. The effect of temperature, molar ratio camphene/acetic acid, and catalyst loading were investigated. The catalyst can be reused four times without loss of activity. Isobornyl acetate is an important fine chemical and has been used in the field of fragrance, medicine, organic synthesis and cosmetics [1]. It is an intermediary in the synthesis of camphor [2]. Usually it is prepared by an acid-catalized reaction of camphene with acetic acid or acetic anhydride. But this process has serious drawbacks such as the corrosion of equipment, non-recyclability of the catalyst and serious environmental pollution. In the face of increasing environmental requirements, the use of such catalysts becomes unacceptable. Therefore many studies have recently focused on the development of "clean" (green) processes for the production of terpene derivatives with high selectivity. For this purpose, heteropolyacids [3, 4], zeolites [5, 6], solid acid catalysts [7, 8], ion-exchange resin [9-11] were used as catalysts for synthesizing terpene esters. However, these catalysts have drawbacks such as a large ratio of catalyst/substrate, fast deactivation and a selectivity that leaves much to be desired. In the recent years ionic liquids (IL) have been investigated by many researchers as catalysts for different reactions. Due to its low volatility, negligible vapor pressure, reasonable thermal stability, outstanding recyclability and reusability, ionic liquids may be a viable alternative to widely applicable catalysts in the processes of modern synthetic chemistry, the green chemistry [12]. The improvement of the versatility of ionic liquids was achieved by creating acidic functionalized ionic liquids and combining the properties of a reagent and solvent [13]. A number of such ionic liquids were synthesized and successfully applied in the esterification reaction [14-17]. Received that the structure of the IL cation determines the direction of the rearrangement of terpene, whereas the nature of the anion affects the selectivity of the reaction [18, 19]. In the present work, we report the acetylation of camphene with acetic acid catalyzed by imidazolium and pyridinium ionic liquids (Scheme 1). The influence of various reaction parameters, such as the temperature, the molar ratio of camphene/acetic acid and catalyst loading, on the activity of the most active catalyst is also studied.


2021 ◽  
Vol 1036 ◽  
pp. 130-136
Author(s):  
Ting Qun Tan ◽  
Lei Geng ◽  
Yan Lin ◽  
Yan He

In order to prepare carbon nanotubes with high specific surface area, small diameter, low resistivity, high purity and high catalytic activity, the Fe-Mo/Al2O3 catalyst was prepared based on the microreactor. The influence of different Fe/Al molar ratios on the catalyst and the carbon nanotubes prepared was studied through BET, SEM, TEM and other detection methods. Studies have shown that the pore structure of the catalyst is dominated by slit pores at a lower Fe/Al molar ratio. The catalytic activity is the highest when the Fe/Al molar ratio is 1:1, reaching 74.1%. When the Fe/Al molar ratio is 1:2, the catalyst has a higher specific surface area, the maximum pore size is 8.63 nm, and the four-probe resistivity and ash content of the corresponding carbon nanotubes are the lowest. The higher the proportion of aluminum, the higher the specific surface area of the catalyst and the carbon nanotubes, and the finer the diameter of the carbon nanotubes, which gradually tends to relax. The results show that when the Fe/Al molar ratio is 1:2, although the catalytic activity of the catalyst is not the highest, the carbon nanotubes prepared have the best performance.


2015 ◽  
Vol 13 (3) ◽  
pp. 389-393 ◽  
Author(s):  
Emine Sert

Abstract Within the framework of green chemistry, catalysts should be met different criteria such as biodegradability, recyclability, flammability, non-toxicity and low price. Acidic deep eutectic solvent (DES) have been synthesized for this purpose, by mixing para-toluene sulfonic acid and choline chloride. The catalytic activity of DES was studied in the esterification of acrylic acid with n-butanol. The usage of DES as catalyst is simple, safe and cheap. The effects of temperature, catalyst loading, n-butanol/acrylic acid molar ratio on the conversion of acrylic acid were performed. The batch reactor experiments were carried out at temperatures of 338, 348, 358 and 368 K, molar ratio of butanol to acrylic acid of 1, 2,3 and catalyst loading of 10, 15, 20 and 90 g/L. 90.2% of acrylic acid conversion was achieved at a temperature of 358 K and catalyst loading of 20 g/L. Reusability of DES was investigated. Reusability and catalytic activity makes DES efficient as catalyst.


2007 ◽  
Vol 5 (3) ◽  
pp. 715-726 ◽  
Author(s):  
Emil Muresan ◽  
Spiridon Oprea ◽  
Theodor Malutan ◽  
Mihai Vata

AbstractThe esterification reaction of palmitic acid with epichlorohydrin catalyzed by an anionic macroporous resin was studied. Purolite A-500 resin proved to be a very effective catalyst in the synthesis of 3-chloro-2-hydroxypropyl palmitate. The effects of certain parameters such as speed of agitation, catalyst particle size, catalyst loading, temperature, initial molar ratio between reactants on the rate of reaction were studied. It was found that the overall rate is intrinsically kinetically controlled. The structure of synthesized ester was confirmed by FTIR and 1H NMR analyses.


2019 ◽  
Vol 8 (1) ◽  
pp. 128-134 ◽  
Author(s):  
Emine Kaya Ekinci ◽  
Nuray Oktar

Abstract A series of active and selective MCM-41 supported catalysts have been successfully prepared and used for bioderived glycerol esterification with acetic acid to produce fuel additives. In the synthesis of MCM-41, an acidic hydrothermal synthesis route was used, and silicotungstic acid (STA) and zirconia (ZrO2) were added to the catalyst structure by wet impregnation. X-ray diffraction, nitrogen adsorption-desorption methods, scanning electron microscopy with energy-dispersive spectroscopy, and inductively coupled plasma-mass spectrometry analysis were used for characterizations of the catalysts. Diffuse reflectance infrared Fourier transform spectroscopy analyses of pyridine-adsorbed catalysts owns Lewis and Brønsted acidity hosting in one, which promotes the esterification reaction of glycerol into glycerol esters with high selectivity. Esterification of glycerol reactions were performed at temperature intervals of 105°C–200°C, with an amount of catalyst equal to 0.5 g, and glycerol/acetic acid molar ratio of 1:6 in a stirred autoclave reactor operated batchwise. STA and ZrO2-impregnated MCM-41 catalysts showed better performance with a complete glycerol conversion and high selectivity to triacetin.


Author(s):  
Kailas L. Wasewar ◽  
Shyambabu Patidar ◽  
Vijay K. Agarwal ◽  
Ajit Rathod ◽  
Shriram S. Sonawane ◽  
...  

The most common reaction system studied for the application of pervaporation (PV) is an esterification reaction between alcohol and acid in the presence of a catalyst. In present paper, performance of pervaporation reactor (PVR) for esterification of acetic acid with ethanol was studied. Model equations were developed for reaction and separation in PVR. Model results were validated with experimental results and excellent comparison was obtained. The effect of various parameters such as: reactant ratio, ratio of effective membrane area to volume of reacting mixture, catalyst concentration and flux on the performance of PVR were discussed. The optimum conditions were obtained as: membrane area to volume of reacting mixture = 2 m-1, reactant ratio = 1.5, catalyst concentration = 50 g/l for esterification of acetic acid with ethanol in PVR. The model presented can also be used for the other esterification reactions. The described model allows the evolution of the reaction time necessary to achieve a given conversion. The process parameters: temperature, catalyst concentration, initial molar ratio of acid to alcohol, the ratio of the effective membrane area to the volume of reacting mixture can be changed in order to attain the optimum operating conditions of the pervaporation-esterification coupling operating.


2013 ◽  
Vol 781-784 ◽  
pp. 190-193
Author(s):  
Mei Xu ◽  
Hua Yuan ◽  
Wei Liu ◽  
Jian Wang ◽  
Feng Zhen Yang

The synthesis of isoamyl acetate with ammonium 9-molybdate manganese heteropolyacid salt supported activated carbon as catalyst was studied. The optimum reaction conditions are obtained as follows: isoamyl alcohol to acetic acid molar ratio = 1.646, the weight of catalyst is 40% of total weigh, m (acidulate catalyst)=0.2g, m (water carrying reagent toluene) = 3ml, reaction time is about 63 minutes. Selectivity is 100% and conversion rate is 89.48%.


2020 ◽  
Vol 15 (2) ◽  
pp. 514-524
Author(s):  
Laddawan Tumkot ◽  
Armando T. Quitain ◽  
Tetsuya Kida ◽  
Navadol Laosiripojana ◽  
Artiwan Shotipruk ◽  
...  

In this study, the esterification reaction of oleic acid (OA) with methanol was investigated in the presence of a sulfonated hydrothermal carbon-based catalyst under microwave irradiation. The reaction conditions were optimized using response surface methodology based on a central composite design. Three following variables were studied: methanol to OA molar ratios (2.5:1–7.5:1), reaction time (50–70 min) and catalyst loading (2–5 wt.%) to provide a statistical model with the coefficient of regression (R2) of 0.9407. Based on the model, the optimum OA conversion of 95.6% was predicted at 5.8:1 methanol to OA molar ratio, 60 min and 3.05 wt.% catalyst loading. The experimental validation indicated that the model gave a good prediction of OA conversion (2.8% error). Furthermore, the reaction was found to be reasonably described by the pseudo-first order kinetics. The dependency of the reaction rate constant on temperatures gave a value of the activation energy of 64 kJ/mol. Copyright © 2020 BCREC Group. All rights reserved 


2021 ◽  
Vol 17 (1) ◽  
pp. 13-21
Author(s):  
Shofiyya Julaika ◽  
Agus Farid Fadli ◽  
Widiyastuti Widiyastuti ◽  
Heru Setyawan

Solid acid catalyst is a promising alternative to the counterpart homogeneous acid for esterification reaction from the viewpoint of reusability and environmental concerns. This work aims to develop sulfonated mesoporous silica-carbon composite as solid acid catalyst for the esterification. The catalyst was synthesized from sodium silicate as the silica precursor and polyethylene glycol (PEG) as both carbon precursor and template via a sol-gel route in an aqueous system. Then, it was carbonized to produce mesoporous silica-carbon composite. Using the proposed method, the surface area of the silica-carbon composite could reach as high as 1074.21 m2/g. Although the surface area decreased to 614.02 m²/g when it was functionalized with sulfonate groups, the composite had a high ionic capacity of 5.3 mEq/g and exhibited high catalytic activity for esterification reaction of acetic acid with ethanol. At a reaction temperature of 80 °C, the acetic acid conversion reached 76.55% in 4 h. In addition, the catalyst had good reusability, which can be comparable with the commercial catalyst Foltrol F-007. It appears that the sulfonated silica-carbon composite prepared from sodium silicate using PEG as the carbon source a promising candidate as catalyst for esterification and the related area. Copyright © 2021 by Authors, Published by BCREC Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0). 


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