scholarly journals Mixed-Metal Oxide Catalyst for Liquid Phase Benzene Alkylation

Author(s):  
M. Alhassan ◽  
U. Z. Faruq ◽  
A. Galadima

Development of cheaper, active and more ecofriendly heterogeneous acid catalyst is a challenge mitigating the petrochemical industries. CuO-MoO3/ZrO2 solid catalyst was prepared by impregnation using suitable precursor materials supported over zirconia. Upon calcination at 450°C for 2 h and activation (by soaking in 2M H2SO4 for 30 minutes), available techniques were employed for the characterization. The available oxides and minerals in the catalyst were revealed by the XRF and XRD profiles respectively. The catalyst crystallite size (131.6nm) was obtained using the Bragg’s equation from the latter. Thermal analysis showed three weight loss stages between (49.25-152.06°C), (152.06-559.47°C) and (559.47-752.0°C ) while presence of sulphate and zirconia oxides was revealed by the FTIR analysis due to appearance of absorption bands around 1225-980cm-1 and 700-600cm-1 respectively. The catalyst (1wt%) was tested for alkylation in a continuous stirred reactor at 80°C using variable (2:1, 4:1 and 10:1) benzene to 1-decene molar ratios. The effects of reaction time and molar ratios on the selectivity, conversion and yield were determined. The alkylation results showed that the catalyst is highly selective to 1-decylbenzene as low amount of side products was obtained. The product yield and conversion increased with reaction time and benzene /1-decene molar ratio while selectivity decreased with increase in benzene /1-decene molar ratio with time.

2021 ◽  
Vol 2 (1) ◽  
Author(s):  
Mohammed Takase ◽  
Paul Kwame Essandoh ◽  
Rogers Kipkoech

AbstractSodium molybdate (Na2MoO4) has been synthesized and investigated as a heterogeneous solid catalyst for biodiesel from Camelina sativa seed oil. Transesterification reactions occurred under atmospheric conditions with relatively, low temperature short reaction time and normal pressure. The prepared catalyst was characterised by means of SEM, TGA, UV, XRD and FTIR. The properties of the biodiesel were compared with international standards. The transesterification reaction was very efficient with the optimum yield higher than 95% at methanol to oil molar ratio of 17:1, catalyst amount of 6%, reaction temperature of 60 °C and reaction time of 2.5 h. The molybdate complex had a high Lewis acidity and most certainly act as alcohol O–H bond leading to a transient species which has high nucleophilic character. The catalyst was easily recovered and after being washed for three times, showed capacity of recyclability for another catalytic reaction of five cycles with similar activity. The properties of the biodiesel were comparable to international standards.


Materials ◽  
2019 ◽  
Vol 12 (18) ◽  
pp. 2995 ◽  
Author(s):  
Alex de Nazaré de Oliveira ◽  
Erika Tallyta Leite Lima ◽  
Deborah Terra de Oliveira ◽  
Rômulo Simões Angélica ◽  
Eloisa Helena de Aguiar Andrade ◽  
...  

A new prepared catalyst, 12-molybdophosphoric acid (HPMo) anchored to the mesoporous aluminosilicate AlSiM, synthesized from Amazon kaolin, was characterized and used as a heterogeneous acid catalyst for the production of eugenyl acetate by acetylation of eugenol with acetic anhydride. The effect of various reaction parameters, such as catalyst concentration, eugenol/acetic anhydride molar ratio, temperature and reaction time, was studied to optimize the conditions of maximum conversion of eugenol. The kinetics studies showed that in eugenol acetylation, the substrate concentration follows a first order kinetics. The results of activation energy was 19.96 kJ mol−1 for HPMo anchored to AlSiM. The reuse of the catalyst was also studied and there was no loss of catalytic activity after four cycles of use (from 99.9% in the first cycle to 90% in the fifth cycle was confirmed), and an excellent stability of the material was observed. Based on catalytic and kinetic studies, HPMo anchored to AlSiM is considered an excellent catalyst.


2019 ◽  
Vol 9 (21) ◽  
pp. 4488
Author(s):  
Amri ◽  
Gómez ◽  
Balea ◽  
Merayo ◽  
Srasra ◽  
...  

Glycerol remains a bottleneck for the biodiesel industry as well as an opportunity from the biorefinery perspective, having a notable reactivity as a platform chemical. In particular, glycerol ketals can be envisaged as oxygenates for fuel formulation. In this study, we have focused on the green synthesis of glycerol ketals by reacting glycerol with acyclic (acetone, butanone) and cyclic (cyclohexanone) ketones in the presence of an acid activated clay Tunisian AC in homogeneous systems under quasi-solventless conditions. These reactions were followed by on-line Fourier Transform Infrared Spectroscopy (FTIR) (namely, ReactIR 10). Firstly, the contacting time was selected studying the activity, stability and chemical characteristics of a set of catalysts. The 1-h activated clay AC was further characterized by X-Ray diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electronic Microscopy with Energy Dispersive Spectroscopy (SEM/EDS). Finally, the effect of the main operational variables (catalyst concentration, reagents molar ratio, time and temperature) were checked and we reflected on adequate second-order kinetic models with partial first-order deactivation.


Catalysts ◽  
2020 ◽  
Vol 10 (2) ◽  
pp. 164 ◽  
Author(s):  
Zuchra Helwani ◽  
Muliadi Ramli ◽  
Edy Saputra ◽  
Bahruddin Bahruddin ◽  
Delvi Yolanda ◽  
...  

In this work, calcium oxide (CaO) extracted from eggshell impregnated with magnetite (Fe3O4) is prepared successfully and it had been applied on transesterification of palm oil off-grade. Prior experiment, the eggshells material are powdered and calcined at 900 °C then impregnated with Fe3O4 and recalcined. The obtained Fe3O4/CaO catalyst is characterized using X-ray diffraction and Braunaeur–Emmet–Teller (BET) surface area. The influence of various parameters including recalcined time and temperature are investigated. The prepared catalyst is tested for transesterification of palm oil off-grade to produce biodiesel in which the optimal conditions of a methanol/palm oil off-grade molar ratio of 10:1, the catalyst weight of 6%, the reaction temperature of 70 °C, and the reaction time of 2 h. The transesterification product was analyzed using GC-MS, which showed the biodiesel yield of 90% at the recalcined temperature of 600 °C and reaction time of 2 h. It has been noted that the catalyst activity is achieved when the moderate recalcination temperature is applied and the disordered structure of the catalyst is maintained. This study also confirms that CaO impregnated with Fe3O4 could be a solid catalyst for the biodiesel synthesis through transesterification reaction of palm oil off-grade.


Author(s):  
Xueyang Li ◽  
Jiao Zhang ◽  
Yunfei Song ◽  
Yanhong Ji ◽  
Mohammad Younas ◽  
...  

AbstractIn this work, the esterification of glycerol with acetic acid (HOAc) was investigated under sulfonated polyphenylene sulfide non-woven fabric (SPSF) as a solid catalyst. The effects of the amount of catalyst, reaction temperature, molar ratio of glycerol to HOAc and the reaction time on the esterification were studied in detail. It was found that SPSF has good catalytic activity and stability. Under the reaction conditions of the molar ratio of glycerol/HOAc of 1:6 (glycerol 0.1 mol), the reaction temperature of 110 °C, the amount of catalyst of 3 g, and the reaction time of 2 h, the glycerol conversion and the selectivity to diacetin (DAG) reached upto 96 and 56.1%, respectively. Reusability test of SPSF showed that no significant declination in the glycerol conversion and the selectivity was observed after five reaction cycles. The experimental results proved the esterification of glycerol with HOAc by SPSF a promising and green process.


2016 ◽  
Vol 22 (4) ◽  
pp. 445-452 ◽  
Author(s):  
Joana Dias ◽  
Pedro Leite ◽  
Maria Alvim-Ferraz ◽  
Manuel Almeida

The present study evaluated the recycling of crude glycerol as source of catalyst for biodiesel production. For that purpose, two sets of experiments were conducted. In the first set (A), biodiesel was synthesized by conventional methanolysis of sunflower oil using NaOH as catalyst at 65?C during 1 h and varying catalyst concentration (0.4 - 1.2 wt.%) or methanol to oil molar ratio (6:1-12:1). The second set (B) was performed by replicating the conditions of set A and considering the use of crude glycerol as source of catalyst. The evaluation of excess methanol and catalyst distribution in the crude products was performed. For both sets of experiments, product yield and quality (viscosity and purity) were determined. Methanol was predominantly in the glycerol phase (54 - 68%), with negligible effect of variation in catalyst concentration and higher percentages found when higher methanol to oil molar ratios were used, due to a higher polarity of this phase. In most cases, catalyst was predominantly in the crude glycerol (53 wt.% in average) and no clear relation was found between catalyst distribution and the different reaction conditions studied. The results from set A showed a clear influence of catalyst concentration in biodiesel conversion and a minor effect of methanol to oil molar ratio. The best conditions were 6:1 methanol to oil molar ratio and 0.6 wt.% of catalyst leading to a product yield of 95.1 wt.%, a purity of 99.3% and a viscosity of 4.59 mm2s-1. The second set of experiments showed different trends and variability compared to the first one and the results indicated that catalyst might be altered during glycerol storage. It was found an effect of methanol to oil molar ratio in reaction conversion with the highest purity (96.9 wt.%) being obtained when the highest molar ratio was used (12:1) possibly due to the reduced mass transfer limitations. Overall, the results clearly show the potential of using crude glycerol as source of catalyst, avoiding the use of new catalyst and allowing a more sustainable biodiesel production.


Author(s):  
I Nengah Simpen ◽  
I Made Sutha Negara ◽  
Sofyan Dwi Jayanto

Biodiesel production from waste cooking oil in two steps reaction of esterification and transesterification is low efficient, due to twice methanol consumption and need more reaction time. Optimizing reaction conditions of CaO as a matrix of solid catalyst prepared from crab shell (green CaO) and modified by K2O/TiO2 for converting waste cooking oil to biodiesel have been carried out. Catalytic process of waste cooking oil to biodiesel took place in one step reaction of esterification and transesterification. The research result showed that optimum conditions in its one step reaction such as methanol to oil molar ratio was 9:1, amount of CaO/K2O-TiO2 catalyst to oil was 5% and reaction time of 60 minutes with biodiesel yield was 88.24%. Physical and chemical properties of biodiesel which produced from one step reaction of esterification and transesterification of waste cooking oil were suitable with Indonesian National Standard (SNI-04-7182-2006) namely density at 40oC of 850 kg/m3, kinematic viscosity at 40oC of 3.32 cSt, water content of 0.046%, iodine number of 59.25 g I2/100g and acid value of 0.29 mg KOH/g. Gas chromatography-mass spectrometry (GC-MS) analysis of biodiesel formed fatty acid methyl esters from conversion of waste cooking oil.


2021 ◽  
Vol 899 ◽  
pp. 726-732
Author(s):  
Fatma I. Gasimova ◽  
Zaur Z. Aghamali̇yev ◽  
Gulshan J. Gasanova ◽  
Chingiz K. Rasulov

The present study deals with the investigation of catalytic cycloalkylation reactions of phenol with 1-methylcyclopentene. KU-23 and aluminum phenolate were used as catalysts for the process. The effect of kinetic parameters (temperature, duration, molar ratios of the initial components and the amount of catalyst) on the yield and selectivity of methylcyclopentyl phenols obtained as a result of scientific research was investigated. As a result, effective conditions were found for the production of para- and ortho-, ortho- (1-methylcyclopentyl) phenols with high yield and selectivity. It was determined that high yield of target product in the presence of phenol, 1-methylcyclopentene and catalyst KU-23, was 71.2% for phenol and selectivity for target product - 92.8% is obtained under the following conditions of cycloalkylation reaction: temperature 110°C, reaction time-5 hours, molar ratio phenol to methylcyclopentene-1 : 1, the amount of catalyst-10% according to the phenol taken. The cycloalkylation reaction of phenol with 1-methylcyclopentene in the presence of aluminum phenolate catalyst was carried out in an autoclave in a nitrogen environment and effective conditions were found: temperature 260°C, reaction time - 5 hours, molar ratio of phenol to 1-methylcyclopentene 1: 2, amount of catalyst 20% according to the phenol taken. Under these conditions, the yield of the target product is 44.3% for the phenol taken, and the selectivity is 87.6% for the target product. The chemical structures of the synthesized para- and ortho-, ortho- (1-methylcyclopentyl) phenols were confirmed by IR-, 1H and NMR spectroscopy, and physicochemical parameters were determined.


2020 ◽  
Vol 7 (1) ◽  
pp. 191592
Author(s):  
Shehu-Ibrahim Akinfalabi ◽  
Umer Rashid ◽  
Imededdine Arbi Nehdi ◽  
Thomas Shean Yaw Choong ◽  
Hassen Mohamed Sbihi ◽  
...  

The optimum conditions to produce palm fatty acid distillate (PFAD)-derived-methyl esters via esterification have been demonstrated with the aid of the response surface methodology (RSM) with central composite rotatable design in the presence of heterogeneous acid catalyst. The effect of four reaction variables, reaction time (30–110 min), reaction temperature (30–70°C), catalyst concentration (1–3 wt.%) and methanol : PFAD molar ratio (3 : 1–11 : 1), were investigated. The reaction time had the most influence on the yield response, while the interaction between the reaction time and the catalyst concentration, with an F -value of 95.61, contributed the most to the esterification reaction. The model had an R 2 -value of 0.9855, suggesting a fit model, which gave a maximum yield of 95%. The fuel properties of produced PFAD methyl ester were appraised based on the acid value, iodine value, cloud and pour points, flash point, kinematic viscosity, density, ash and water contents and were compared with biodiesel EN 14214 and ASTM D-6751 standard limits. The PFAD methyl ester was further blended with petro-diesel from B0, B3, B5, B10, B20 and B100, on a volumetric basis. The blends were characterized by TGA, DTG and FTIR. With an acid value of 0.42 (mg KOH g −1 ), iodine value of 63 (g.I 2 /100 g), kinematic viscosity of 4.31 (mm 2 s −1 ), the PFAD methyl ester has shown good fuel potential, as all of its fuel properties were within the permissible international standards for biodiesel.


2012 ◽  
Vol 550-553 ◽  
pp. 400-403 ◽  
Author(s):  
Xue Nan Sun ◽  
Li Cui ◽  
Tong Kuan Xu ◽  
Da Zhi Wang

Benzaldehyde 1, 2-propanediol acetal was synthesized from benzaldehyde and 1, 2-propanediol in the presence of ionic liquid [HMIM]HSO4. The effect of the amount of catalyst, reaction time, reaction temperature, and the molar ratio of raw materials agent on the product yield was investigated respectively. Experimental results demonstrate that ionic liquid [HMIM]HSO4is a good catalyst for preparation of benzaldehyde 1, 2-propanediol acetal. Results showed the optimal reaction conditions are as follows: the mole ratio of benzaldehyde to 1, 2-propanediol is 1:1.3, the amount of catalyst is 3.0g, the reaction temperature is 343K, and the reaction time is 4h. The achieved yield of acetal is 78. 7%.


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