Synthesis and characterization of bio catalyst prepared from dairy waste for lactic acid esterification

Author(s):  
Amol A. Bhusari ◽  
Bidyut Mazumdar ◽  
Ajit P. Rathod

Abstract Dairy byproduct is known for its valuable chemical and nutritional content possessing high market potential. Notwithstanding, it is tractable to exploit its utilization. The waste generated is organic and having huge energy potential. The objective of current research is to synthesize novel catalyst from a dairy based solid waste called Ghee Residue by chemical activation process and deploy it for the production of iso-butyl lactate. Surface identity of catalyst was furnished using Brunauer-Emmet Teller (BET) method and Fourier Transform Infrared Spectroscopy (FTIR). Effect of variables like reaction time, temperature of reaction and loading of catalyst on lactic acid conversion were studied. In addition to this, reaction kinetics modelling was performed using 2nd order pseudo-homogeneous approach. It was inferred that, both internal as well as external resistance of mass transfer could not offer any influence on overall rate of reaction in this esterification. Optimum condition for esterification reaction was at 368 K with 3% catalyst loading giving the highest conversion around 74%. The energy of activation for the present system using synthesized catalyst was 41.5 kJ/mol and found to be lower in comparison with the other catalysts. Although, the activity of GRC declined gradually less than 10% from the activity of the several reaction cycle.

2021 ◽  
Vol 1020 ◽  
pp. 224-230
Author(s):  
Meng Jun Zheng ◽  
Hsin Chi Tseng ◽  
Bo Yao Chiu ◽  
Wei Cheng Hung ◽  
Richard S. Horng

Esterification reaction of lactic acid with butanol to produce butyl lactate and its optimal conditions were investigated. Cyclohexane was used as entrainer to remove water to promote reaction yield. Catalyst of NaHSO4 was also used to increase reaction rate. Reaction parameters of butanol/lactic acid ratio, cyclohexane/lactic acid ratio, catalyst amount, and reaction time were optimized using Response Surface Methodology (RSM). Results showed that the butanol/lactic acid ratio was the most significant factor for esterification yield while interactions between butanol/lactic acid ratio and cyclohexane/lactic acid ratio, butanol/lactic acid ratio, and reaction time were less significant. The correlation coefficient between predicted values and experiment values was 0.985. The optimal conditions for the experiment are: ethanol/lactic acid ratio 5:1, cyclohexane/lactic acid ratio 1:1, catalyst loading 1.5%, and incubation period 3 hours. The esterification yield reaches 99.8% under these conditions.


2019 ◽  
Vol 16 (6) ◽  
pp. 913-920 ◽  
Author(s):  
Israel Bonilla-Landa ◽  
Emizael López-Hernández ◽  
Felipe Barrera-Méndez ◽  
Nadia C. Salas ◽  
José L. Olivares-Romero

Background: Hafnium(IV) tetrachloride efficiently catalyzes the protection of a variety of aldehydes and ketones, including benzophenone, acetophenone, and cyclohexanone, to the corresponding dimethyl acetals and 1,3-dioxolanes, under microwave heating. Substrates possessing acid-labile protecting groups (TBDPS and Boc) chemoselectively generated the corresponding acetal/ketal in excellent yields. Aim and Objective: In this study. the selective protection of aldehydes and ketones using a Hafnium(IV) chloride, which is a novel catalyst, under microwave heating was observed. Hence, it is imperative to find suitable conditions to promote the protection reaction in high yields and short reaction times. This study was undertaken not only to find a novel catalyst but also to perform the reaction with substrates bearing acid-labile protecting groups, and study the more challenging ketones as benzophenone. Materials and Methods: Using a microwave synthesis reactor Monowave 400 of Anton Paar, the protection reaction was performed on a raging temperature of 100°C ±1, a pressure of 2.9 bar, and an electric power of 50 W. More than 40 substrates have been screened and protected, not only the aldehydes were protected in high yields but also the more challenging ketones such as benzophenone were protected. All the products were purified by simple flash column chromatography, using silica gel and hexanes/ethyl acetate (90:10) as eluents. Finally, the protected substrates were characterized by NMR 1H, 13C and APCI-HRMS-QTOF. Results: Preliminary screening allowed us to find that 5 mol % of the catalyst is enough to furnish the protected aldehyde or ketone in up to 99% yield. Also it was found that substrates with a variety of substitutions on the aromatic ring (aldehyde or ketone), that include electron-withdrawing and electrondonating group, can be protected using this methodology in high yields. The more challenging cyclic ketones were also protected in up to 86% yield. It was found that trimethyl orthoformate is a very good additive to obtain the protected acetophenone. Finally, the protection of aldehydes with sensitive functional groups was performed. Indeed, it was found that substrates bearing acid labile groups such as Boc and TBDPS, chemoselectively generated the corresponding acetal/ketal compound while keeping the protective groups intact in up to 73% yield. Conclusion: Hafnium(IV) chloride as a catalyst provides a simple, highly efficient, and general chemoselective methodology for the protection of a variety of structurally diverse aldehydes and ketones. The major advantages offered by this method are: high yields, low catalyst loading, air-stability, and non-toxicity.


Materials ◽  
2021 ◽  
Vol 14 (11) ◽  
pp. 2951
Author(s):  
Mirosław Kwiatkowski ◽  
Jarosław Serafin ◽  
Andy M. Booth ◽  
Beata Michalkiewicz

This paper presents the results of a computer analysis of the effect of activation process temperature on the development of the microporous structure of activated carbon derived from the leaves of common polypody (Polypodium vulgare) via chemical activation with phosphoric acid (H3PO4) at activation temperatures of 700, 800, and 900 °C. An unconventional approach to porous structure analysis, using the new numerical clustering-based adsorption analysis (LBET) method together with the implemented unique gas state equation, was used in this study. The LBET method is based on unique mathematical models that take into account, in addition to surface heterogeneity, the possibility of molecule clusters branching and the geometric and energy limitations of adsorbate cluster formation. It enabled us to determine a set of parameters comprehensively and reliably describing the porous structure of carbon material on the basis of the determined adsorption isotherm. Porous structure analyses using the LBET method were based on nitrogen (N2), carbon dioxide (CO2), and methane (CH4) adsorption isotherms determined for individual activated carbon. The analyses carried out showed the highest CO2 adsorption capacity for activated carbon obtained was at an activation temperature of 900 °C, a value only slightly higher than that obtained for activated carbon prepared at 700 °C, but the values of geometrical parameters determined for these activated carbons showed significant differences. The results of the analyses obtained with the LBET method were also compared with the results of iodine number analysis and the results obtained with the Brunauer–Emmett–Teller (BET), Dubinin–Radushkevich (DR), and quenched solid density functional theory (QSDFT) methods, demonstrating their complementarity.


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.


Author(s):  
Nawwarah Mokti ◽  
Azry Borhan ◽  
Siti Nur Azella Zaine ◽  
Hayyiratul Fatimah Mohd Zaid

The use of an activating agent in chemical activation of activated carbon (AC) production is very important as it will help to open the pore structure of AC as adsorbents and could enhance its performance for adsorption capacity. In this study, a pyridinium-based ionic liquid (IL), 1-butylpyridinium bis(trifluoromethylsulfonyl) imide, [C4Py][Tf2N] has been synthesized by using anion exchange reaction and was characterized using few analyses such as 1H-NMR, 13C-NMR and FTIR. Low-cost AC was synthesized by chemical activation process in which rubber seed shell (RSS) and ionic liquid [C4Py][Tf2N] were employed as the precursor and activating agent, respectively. AC has been prepared with different IL concentration (1% and 10%) at 500°C and 800°C for 2 hours. Sample AC2 shows the highest SBET and VT which are 392.8927 m2/g and 0.2059 cm3/g respectively. The surface morphology of synthesized AC can be clearly seen through FESEM analysis. A high concentration of IL in sample AC10 contributed to blockage of pores by the IL. On the other hand, the performance of synthesized AC for CO2 adsorption capacity also studied by using static volumetric technique at 1 bar and 25°C. Sample AC2 contributed the highest CO2 uptakes which is 50.783 cm3/g. This current work shows that the use of low concentration IL as an activating agent has the potential to produce porous AC, which offers low-cost, green technology as well as promising application towards CO2 capture.


2009 ◽  
Vol 155 (3) ◽  
pp. 800-809 ◽  
Author(s):  
Jing Ma ◽  
Minhua Zhang ◽  
Lianyu Lu ◽  
Xin Yin ◽  
Jing Chen ◽  
...  

Catalysts ◽  
2019 ◽  
Vol 9 (1) ◽  
pp. 67 ◽  
Author(s):  
Muhammad Hossain ◽  
Md Siddik Bhuyan ◽  
Abul Md Ashraful Alam ◽  
Yong Seo

The aim of this research was to synthesize, characterize, and apply a heterogeneous acid catalyst to optimum biodiesel production from hydrolyzed waste cooking oil via an esterification reaction, to meet society’s future demands. The solid acid catalyst S–TiO2/SBA-15 was synthesized by a direct wet impregnation method. The prepared catalyst was evaluated using analytical techniques, X-ray diffraction (XRD), Scanning electron microscopy (SEM) and the Brunauer–Emmett–Teller (BET) method. The statistical analysis of variance (ANOVA) was studied to validate the experimental results. The catalytic effect on biodiesel production was examined by varying the parameters as follows: temperatures of 160 to 220 °C, 20–35 min reaction time, methanol-to-oil mole ratio between 5:1 and 20:1, and catalyst loading of 0.5%–1.25%. The maximum biodiesel yield was 94.96 ± 0.12% obtained under the optimum reaction conditions of 200 °C, 30 min, and 1:15 oil to methanol molar ratio with 1.0% catalyst loading. The catalyst was reused successfully three times with 90% efficiency without regeneration. The fuel properties of the produced biodiesel were found to be within the limits set by the specifications of the biodiesel standard. This solid acid catalytic method can replace the conventional homogeneous catalyzed transesterification of waste cooking oil for biodiesel production.


Materials ◽  
2019 ◽  
Vol 12 (9) ◽  
pp. 1377 ◽  
Author(s):  
Ruoke Ma ◽  
Xianxian Qin ◽  
Zhigao Liu ◽  
Yunlin Fu

Activated carbon fiber was prepared from liquefied wood by chemical activation with ZnCl2 (Z-LWACF) at different impregnation ratios, with a particular focus on its adsorption property, kinetic and isotherm. The characterization and properties of Z-LWACFs were investigated by nitrogen adsorption/desorption, X-ray photoelectron spectroscopy (XPS), methylene blue (MB) and iodine adsorption. Two activation process methods were employed to prepare Z-LWACF and contrasted with others fibers. The results showed that the Z-LWACF obtained by one-step ZnCl2 activation present higher yields and specific surface area than others fibers. Besides, the change of MB adsorption value at different impregnation ratios was consistent with pore structure distribution above 1.5 nm pore size, indicating that larger micropores (1.5 to 2 nm) and mesopores played a major role in the MB adsorption by Z-LWACF. The kinetics of MB adsorption process was found to follow the pseudo-second-order kinetic model and the adsorption rate was controlled by chemisorption. It was also found that MB adsroption by Z-LWACF belonged to monolayer adsorption and Z-LWACF was easy to adsorb MB.


2014 ◽  
Vol 875-877 ◽  
pp. 196-201 ◽  
Author(s):  
Mohd Faisal Taha ◽  
Ahmad S. Rosman ◽  
Maizatul S. Shaharun

The potential of rice husk-based activated carbon as an alternative low-cost adsorbent for the removal of Pb (II) ion from aqueous solution was investigated. Rice husk-based activated carbon was preparedviachemical activation process using NaOH followed by the carbonization process at 500°C. Morphological analysis was conducted using field-emission scanning electron microscope /energy dispersive X-ray (FESEM/EDX) on three samples, i.e. raw rice husk, rice husk treated with NaOH and rice husk-based activated carbon. These three samples were also analyzed for their C, H, N, O and Si contents using CHN elemental analyzer and FESEM/EDX. The textural properties of rice husk-based activated carbon, i.e. surface area (253 m2/g) and pore volume (0.17 cm2/g), were determined by N2adsorption. The adsorption studies using rice husk-based activated carbon as an adsorbent to remove Pb (II) ion from aqueous solution were carried out at a fixed initial concentration of Pb (II) ion (150 ppm) with varying adsorbent dose as a function of contact time at room temperature. The concentration of Pb (II) ion was determined by atomic absorption spectrophotometer (AAS). The removal of Pb (II) ion from aqueous solution increased from 35 % to 82 % when the amount of rice husk-based activated carbon was increased from 0.05 g to 0.30 g. The equilibrium data obtained from adsorption studies was found to fit both Langmuir and Freundlich adsorption isotherms.


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