Clean Synthesis of 2-Methylglycidol over a Novel Titanosilica Catalyst - Ti-MWW under Autogenic Pressure

Author(s):  
Anna Fajdek ◽  
Agnieszka Wróblewska ◽  
Eugeniusz Milchert

In this work the epoxidation of methallyl alcohol (MAA) with 30 wt% H2O2 over the Ti-MWW catalyst has been studied. The significant parameters for the MAA epoxidation were established as temperature (20-120°C), the molar ratio of MAA/H2O2 (1:1-5:1), methanol (solvent) concentration (5-90 wt%), Ti-MWW catalyst concentration (0-5.0 wt%), reaction time (5-300 min) and intensity of stirring (0-500 rpm). The process of MAA epoxidation was carried out the most effective at temperature of 100°C, the molar ratio of MAA/H2O2=1:1, methanol concentration of 40 wt%, the catalyst concentration of 2 wt%, the reaction time of 15 min and with the stirring intensity over 350 rpm. These the best technological parameters (mild and relatively safe) allow to obtain the selectivity of transformation to 2MG 37 mol%, the MAA conversion 52 mol%, and the selectivity of transformation to organic compounds in relation to H2O2 consumed 48 mol%.

2014 ◽  
Vol 554 ◽  
pp. 500-504 ◽  
Author(s):  
Farid Nasir Ani ◽  
Ahmed Bakheit Elhameed

This paper investigated the three critical reaction parameters including catalyst concentration, microwave exit power and reaction time for the transesterification process of jatropha curcas oil using microwave irradiation. The work is an attempt to reduce the production cost of biodiesel. Similar quantities of methanol to oil molar ratio 6:1 and calcium oxide as a heterogeneous catalyst were used. The results showed that the best yield percentage 96% was obtained using 300W microwave exit power, 8 %wt CaO and 7 min. The methyl ester FAME obtained was within the standard of biodiesel fuel.


2017 ◽  
Vol 2017 ◽  
pp. 1-9 ◽  
Author(s):  
Nichaonn Chumuang ◽  
Vittaya Punsuvon

The present study was performed to optimize a heterogeneous calcium methoxide (Ca(OCH3)2) catalyzed transesterification process assisted with tetrahydrofuran (THF) as a cosolvent for biodiesel production from waste cooking oil. Response surface methodology (RSM) with a 5-level-4-factor central composite design was applied to investigate the effect of experimental factors on the percentage of fatty acid methyl ester (FAME) conversion. A quadratic model with an analysis of variance obtained from the RSM is suggested for the prediction of FAME conversion and reveals that 99.43% of the observed variation is explained by the model. The optimum conditions obtained from the RSM were 2.83 wt% of catalyst concentration, 11.6 : 1 methanol-to-oil molar ratio, 100.14 min of reaction time, and 8.65% v/v of THF in methanol concentration. Under these conditions, the properties of the produced biodiesel satisfied the standard requirement. THF as cosolvent successfully decreased the catalyst concentration, methanol-to-oil molar ratio, and reaction time when compared with biodiesel production without cosolvent. The results are encouraging for the application of Ca(OCH3)2 assisted with THF as a cosolvent for environmentally friendly and sustainable biodiesel production.


2012 ◽  
Vol 15 (2) ◽  
Author(s):  
Agnieszka Wróblewska

AbstractsAs a result of phenol hydroxylation, two useful products can be received: hydroquinone and pyrocatechol. In this work the hydroxylation of phenol with hydrogen peroxide over the Ti-MWW catalyst has been studied. Optimization studies were performed by application of a statistical experimental design method utilizing a rotatable-uniform design. The influence of five parameters on the course of this process was examined: temperature (120-150°C), molar ratio of phenol/hydrogen peroxide (0.5-1.5), acetonitrile - solvent content (20- 50 wt%), catalyst - Ti-MWW content (8-18 wt%) and reaction time (60-120 min). The process description was based on four response functions: the conversion of phenol to organic compounds, the yield of pyrocatechol, the yield of hydroquinone and the conversion of phenol to tars. The most favourable parameters for the process of phenol hydroxylation were as follows: temperature 147-150°C, molar ratio of phenol/hydrogen peroxide 0.5-0.6, acetonitrile content 21-24 wt%, Ti-MWW content 10.3-10.6, reaction time 221-236 min. In summary, these the most favourable parameters allow one to obtain pyrocatechol with the yield of 18 mol%, hydroquinone with the yield of 20 mol%, at the conversion of phenol to organic compounds 38 mol% in relatively mild and safe conditions. These results also showed that Ti-MWWcatalyst can be a good substitute for TS-1 catalyst.


2016 ◽  
Vol 18 (4) ◽  
pp. 9-14 ◽  
Author(s):  
Marika Walasek ◽  
Agnieszka Wróblewska

Abstract This work presents the studies on the epoxidation of allyl-glycidyl ether (AGE) over the Ti-SBA-15 catalyst. In these studies an aqueous hydrogen peroxide was used as an oxidizing agent and as a solvent methanol was applied. The studies on the influence the following parameters: temperature (20–80°C), molar ratio of AGE/H2O2 (1:1.5–5:1), methanol concentration (10–90 wt%), catalyst content (1–9 wt%) and reaction time (15–240 min.) were carried out and the most favourable values of these parameters were chosen (temperature 80°C, molar ratio of AGE/H2O2 = 5:1, methanol concentration 30 wt%, catalyst content 3 wt% and the reaction time 240 min.). At these conditions the functions describing the process reached the following values: the selectivity of diglycidyl ether (DGE) 9.2 mol%, the conversion of AGE 13.9 mol% and the efficiency of H2O2 conversion 89.9 mol%.


2018 ◽  
Vol 2018 ◽  
pp. 1-7 ◽  
Author(s):  
Tanat Chokpanyarat ◽  
Vittaya Punsuvon ◽  
Supakit Achiwawanich

The novel three-dimensionally ordered macroporous (3DOM) CaO/SiO2, 3DOM CaO/Al2O3, and 3DOM Ca12Al14O32Cl2 catalysts for biodiesel transesterification were prepared by sol-gel method. The 3DOM catalysts were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Fourier transform infrared spectroscopy (FTIR). The hierarchical porous structure was achieved; however, only 3DOM CaO/Al2O3 and 3DOM Ca12Al14O32Cl2 catalysts were used for transesterification due to high amount of active CaO. Various parameters such as methanol to oil molar ratio, catalyst concentration, reaction time, and their influence on the biodiesel production were studied. The result showed that 99.0% RPO conversion was achieved using the 3DOM Ca12Al14O33Cl2 as a catalyst under the optimal condition of 12 : 1 methanol to oil molar ratio and 6 wt.% catalyst with reaction time of 3 hours at 65°C.


Author(s):  
Agnieszka Wróblewska

Abstract This work presents the studies on the optimization of the process of phenol hydroxylation over the Ti-MWW catalyst. The medium of the reaction was only water introduced into the rector with the 30 wt% hydrogen peroxide (oxidizing agent) and formed during the reaction from the hydrogen peroxide. For the mathematical optimization the rotatable-uniform design was used. The main investigated technological parameters were: the temperature, the molar ratio of phenol/hydrogen peroxide, the catalyst content and the reaction time. The course of the main functions describing the process were presented in the form of layer drawings. The analysis of the layer drawings allowed to establish the most beneficial parameters for this process. Studies have shown that in water solution it is best to conduct phenol hydroxylation process at: the temperature of 93-100oC, phenol/hydrogen peroxide molar ratio 0.9-1, catalyst concentration 3-3.5 wt% and during the reaction time of 55-60 minutes. Under these conditions, it is possible to achieve phenol conversion of 85 mol%, selectivity of transformation to organic compounds in relation to phenol consumed 50 mol% and the yield of hydroquinone about 19 mol%. The phenol hydroxylation method, presented in this article, is a preferred alternative to conventional solutions, as it is more environmentally and cost-effective, taking into account consumption of raw materials and energy.


2020 ◽  
Vol 20 (4) ◽  
pp. 887 ◽  
Author(s):  
Nor Faeqah Idrus ◽  
Robiah Yunus ◽  
Zurina Zainal Abidin ◽  
Umer Rashid ◽  
Norazah Abd Rahman

Pentaerythritol tetraoleate esters synthesized from high oleic palm oil methyl ester (POME) have potential as biolubricant base stock. In the present study, the chemical transesterification of POME and pentaerythritol (PE) using sodium methoxide as a catalyst was conducted under vacuum. The effect of operating variables such as reaction temperature, catalyst concentration, the molar ratio of POME to PE, vacuum pressure, and stirring rate on the yield of PE tetraoleate was examined. The ideal conditions for the reaction were at a temperature of 160 °C, 1.25% (w/w) catalyst concentration, the molar ratio of POME to PE at 4.5:1, vacuum pressure at 10 mbar, and stirring speed at 900 rpm. PE tetraoleate with a yield of 36% (w/w), was successfully synthesized under this condition within 2 h of reaction time.


2020 ◽  
Vol 997 ◽  
pp. 93-101
Author(s):  
Mohd Nurfirdaus Mohiddin ◽  
A.A. Saleh ◽  
Amarnadh N.R. Reddy ◽  
Sinin Hamdan

Heterogeneous catalyst has been viewed as a promising catalyst for biodiesel production. This study employed Turritella terebra (TT) shell as a source for synthesizing heterogeneous CaO catalyst for biodiesel production via transesterification by utilizing chicken fat as a feedstock. The TT shell CaO catalyst was characterized and its catalytic performance was studied. The spectrographic methods that include FTIR, SEM, PSA, and BET-BJH were employed for characterization of the synthesized CaO. The TT shell CaO catalyst optimally produced chicken fat biodiesel (CFB) with reaction parameters at catalyst concentration of 4 wt%, chicken fat to methanol molar ratio of 1:12, reaction temperature of 60°C, and reaction time of 90 min. The optimal yield was 94.03% and the TT shell CaO catalyst still yield 79.19% of CFB on the fifth cycle of reaction. This study has implied that TT shell is a feasible and attractive renewable source of heterogeneous CaO catalyst for biodiesel production.


2021 ◽  
Vol 29 (4) ◽  
Author(s):  
Ratna Dewi Kusumaningtyas ◽  
Haniif Prasetiawan ◽  
Radenrara Dewi Artanti Putri ◽  
Bayu Triwibowo ◽  
Siti Choirunisa Furi Kurnita ◽  
...  

Nyamplung seed (Calophyllum inophyllum L.) oil is a prospective non-edible vegetable oil as biodiesel feedstock. However, it cannot be directly used in the alkaline catalysed transesterification reaction since it contains high free fatty acid (FFA) of 19.17%. The FFA content above 2% will cause saponification reaction, reducing the biodiesel yield. In this work, FFA removal was performed using sulfuric acid catalysed esterification to meet the maximum FFA amount of 2%. Experimental work and response surface methodology (RSM) analysis were conducted. The reaction was conducted at the fixed molar ratio of nyamplung seed oil and methanol of 1:30 and the reaction times of 120 minutes. The catalyst concentration and the reaction temperature were varied. The highest reaction conversion was 78.18%, and the FFA concentration was decreased to 4.01% at the temperature of 60℃ and reaction time of 120 minutes. The polynomial model analysis on RSM demonstrated that the quadratic model was the most suitable FFA conversion optimisation. The RSM analysis exhibited the optimum FFA conversion of 78.27% and the FFA content of 4%, attained at the reaction temperature, catalyst concentration, and reaction time of 59.09℃, 1.98% g/g nyamplung seed oil, and 119.95 minutes, respectively. Extrapolation using RSM predicted that the targeted FFA content of 2% could be obtained at the temperature, catalyst concentration, and reaction time of 58.97℃, 3%, and 194.9 minutes, respectively, with a fixed molar ratio of oil to methanol of 1:30. The results disclosed that RSM is an appropriate statistical method for optimising the process variable in the esterification reaction to obtain the targeted value of FFA.


2009 ◽  
Vol 12 (13) ◽  
pp. 69-76
Author(s):  
Huong Thi Thanh Le ◽  
Tan Viet Le ◽  
Tan Minh Phan ◽  
Hoa Thi Viet Tran

In this study, biodiesel was produced from fat of tra catfish by methanolysis reaction with KOH/y-A12O3 heterogenous catalyst. This research was carried out using response surface methodology (RSM) based on four-variable central composite design (CCD) with a = 1,54671. The transesterification process variables and their investigated ranges were methanol/fat molar ratio (X1: 7/1 - 9/1), catalyst concentration (X2: 5%-7%), reaction time (X3: 60 min - 120 min), and reaction temperature (X4: 55 °C - 65 °C). The result show the biodiesel yield could be reach up to 92,8 % using the following optimized reaction condition: molar ratio of methanol/fat at 8,26/1, catalyst concentration of 5,79 %, reaction time of 96 min, and reaction temperature at 59,6 °C.


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