scholarly journals Two-Stage Conversion of High Free Fatty AcidJatropha curcasOil to Biodiesel Using Brønsted Acidic Ionic Liquid and KOH as Catalysts

2014 ◽  
Vol 2014 ◽  
pp. 1-9 ◽  
Author(s):  
Subrata Das ◽  
Ashim Jyoti Thakur ◽  
Dhanapati Deka
Keyword(s):  
Ionic Liquid ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Two Stage ◽  
Second Stage ◽  
Stage Conversion ◽  
Acidic Ionic Liquid ◽  
Brønsted Acidic Ionic Liquid ◽  
Optimum Reaction ◽  
Stage Process

Biodiesel was produced from high free fatty acid (FFA)Jatropha curcasoil (JCO) by two-stage process in which esterification was performed by Brønsted acidic ionic liquid 1-(1-butylsulfonic)-3-methylimidazolium chloride ([BSMIM]Cl) followed by KOH catalyzed transesterification. Maximum FFA conversion of 93.9% was achieved and it reduced from 8.15 wt% to 0.49 wt% under the optimum reaction conditions of methanol oil molar ratio 12 : 1 and 10 wt% of ionic liquid catalyst at 70°C in 6 h. The ionic liquid catalyst was reusable up to four times of consecutive runs under the optimum reaction conditions. At the second stage, the esterified JCO was transesterified by using 1.3 wt% KOH and methanol oil molar ratio of 6 : 1 in 20 min at 64°C. The yield of the final biodiesel was found to be 98.6% as analyzed by NMR spectroscopy. Chemical composition of the final biodiesel was also determined by GC-MS analysis.

Effects of Microwave and Additional Co–Solvents on Two–Stage Waste Cooking Oil to Biodiesel Conversion

2012 ◽  
Vol 209-211 ◽  
pp. 1136-1141
Author(s):  
Ming Chien Hsiao ◽  
Yung Hung Chang ◽  
Li Wen Chang
Keyword(s):  
Reaction Time ◽  
Reaction Temperature ◽  
Waste Cooking Oil ◽  
Molar Ratio ◽  
Phase System ◽  
Reaction Conditions ◽  
Two Stage ◽  
Second Stage ◽  
Cooking Oil ◽  
Standard Value

This paper introduced a better solution to accelerating the production of biodiesel from waste cooking oil by using suitable acidic and alkaline catalysts in a two-stage catalytic reaction. Next, a co-solvent named tetrahydrofuran (THF), which significantly increased mixing level of the reactants in the mixture of vegetable oil and methanol, was added to form a single phase system. The whole system was then put into a microwave oven to support heat for the transesterification of biodiesel to shorten the reaction time. Reaction conditions of the first stage were methanol to oil molar ratio of 9:1, catalyst amount 1wt%, reaction temperature 60 oC and reaction time 7.5 minutes. In the second stage, for the transesterification, reaction conditions were methanol to oil molar ratio 12:1, catalyst loadings 1 wt%, reaction temperature 60 oC and reaction time 1.5 minutes. Finally, the conversion rate of biodiesel after the nine-minute reaction time was 97.38% which was higher than the EU EN14214 standard value of 96.5%.

scholarly journals PREPARATION OF [AcMI] HSO4 AND USING AS CATALYST FOR ESTERIFICATION

2011 ◽  
Vol 14 (4) ◽  
pp. 61-73
Author(s):  
Thu Ngoc Ha Le ◽  
Thach Ngoc Le
Keyword(s):  
Ionic Liquid ◽  
Chloroacetic Acid ◽  
Molar Ratio ◽  
Hydrogen Sulfate ◽  
Reaction Conditions ◽  
Brønsted Acidic Ionic Liquid ◽  
Acidic Sites ◽  
Concentrated Sulfuric Acid ◽  
Zwitter Ion ◽  
Optimal Reaction

New Bronsted acidic ionic liquid, 1-carboxymethyl-3-methylimidazolium hydrogen sulfate [AcMI]HSO4, has two acidic sites -COOH and HSO4 -. It has been synthesized by three steps. First, 1-carboxymethyl-3-methylimidazolium chloride [AcMI]Cl was prepared by alkylation of 1- methylimidazole with chloroacetic acid (molar ratio is 1.5:1) under microwave irradiation in 6 min (84 % isolated yield). Then, zwitter ion 1-carboxylatmethyl-3-methylimidazolium was obtained by using Ag2O to remove ion chloride Cl- from [AcMI]Cl. At last, concentrated sulfuric acid (98 %) was added into zwitter ion to give 1-carboxymethyl-3-methylimidazolium hydrogen sulfate (yield 96 %). This ionic liquid used as a recyclabe catalyst for the esterification of isopropanol and chloroacetic acid. The optimal reaction conditions were obtained as follows: isopropanol: chloroacetic acid:[AcMI]HSO4 are 1.3:1:0.2, reaction time for 10 min at 60 oC under microvave irradiation. The yield of isopropyl chloroacetate was 86 %. This ionic liquid was removed from ester easily, recovered and recycled without loss of activity.

Alkylation of Phenol with Cyclohexanol Catalyzed by Acidic Ionic Liquid

2011 ◽  
Vol 233-235 ◽  
pp. 188-193 ◽  
Author(s):  
Hai Bing Yu ◽  
Jun Nan ◽  
Jing Cheng Zhang ◽  
Jian Zhou Gui
Keyword(s):  
Ionic Liquid ◽  
Catalytic Activity ◽  
Reaction Time ◽  
Reaction Temperature ◽  
Reactant Ratio ◽  
Temperature Reaction ◽  
Reaction Conditions ◽  
Acidic Ionic Liquid ◽  
Optimum Reaction

Alkylation of phenol with cyclohexanol catalyzed by acidic ionic liquid has been investigated. The influences of reaction temperature, reaction time, reactant ratio (mol ratio of phenol to cyclohexanol), the amount and the recycle of ionic liquid on catalytic activity were studied. The conversion of phenol and the selectivity of paracyclohexylphenol were 75.5% and 61.6%, respectively, under optimum reaction conditions. The ionic liquid was utilized repeatedly over three times without remarkable loss of catalytic activity．

Catalysis Investigation of PET Depolymerization with Brønsted Acidic Ionic Liquid under Microwave Irradiation

2014 ◽  
Vol 893 ◽  
pp. 23-26 ◽  
Author(s):  
Na Liu ◽  
Yong Shuai Ma ◽  
Ke Wen Shu ◽  
Bo Wu ◽  
Dong Zhang
Keyword(s):  
Ionic Liquid ◽  
Reaction Time ◽  
Microwave Irradiation ◽  
Reaction Temperature ◽  
Orthogonal Experiment ◽  
Main Reaction ◽  
Reaction Conditions ◽  
Acidic Ionic Liquid ◽  
Brønsted Acidic Ionic Liquid ◽  
Catalyst Dosage

The catalytic effect of Brønsted acidic ionic liquid for PET hydrolysis reaction under microwave irradiation has been investigated through orthogonal experiment in this article, and the influence of main reaction conditions has also been studied. The results shown that the influence level sequence of reaction factors was: catalyst kind > reaction time > reaction temperature > catalyst dosage. According to a further study of catalyst dosages influence on PET depolymerization degree, the optimal reaction condition was finally concluded as below: [Hexanemi [HSO4] used as catalyst, catalyst dosage: 0.01 mol/2 g PET, reaction time: 210 min, reaction temperature: 195 °C.

1, 1’-Sulfinyldiethylammonium Bis (Hydrogen Sulfate) as a Recyclable Dicationic Ionic Liquid Catalyst for the Efficient Solvent-free Synthesis of 3, 4-Dihydropyrimidin-2(1H)-ones via Biginelli Reaction

2020 ◽  
Vol 23 (2) ◽  
pp. 157-167
Author(s):  
Zainab Ehsani-Nasab ◽  
Ali Ezabadi
Keyword(s):  
Ionic Liquid ◽  
Biginelli Reaction ◽  
Aromatic Aldehydes ◽  
Solvent Free ◽  
Hydrogen Sulfate ◽  
One Pot ◽  
Acidic Ionic Liquid ◽  
Brønsted Acidic Ionic Liquid ◽  
Solvent Free Conditions ◽  
Dicationic Ionic Liquid

Objective: A facile and efficient method for synthesis of 3, 4-dihydropyrimidin-2(1H)-ones via Biginelli reaction catalyzed by a novel dicationic Brönsted acidic ionic liquid, [(EtNH2)2SO][HSO4]2, has been successfully developed. Material and Method:: 3, 4-Dihydropyrimidin-2(1H)-ones were synthesized through one-pot condensation of aromatic aldehydes, ethyl acetoacetate, and urea under solvent-free conditions using [(EtNH2)2SO][HSO4]2 as a novel catalyst. The progress of the reaction was monitored by thin-layer chromatography (ethyl acetate / n-hexane = 1 / 5). The products have been characterized by IR, 1H NMR, 13C NMR, and also by their melting points. Results: In this research, a library of dihydropyrimidinone derivatives was synthesized via Biginelli reaction under solvent-free conditions at 120oC using [(EtNH2)2SO][HSO4]2 as a catalyst. Various aromatic aldehydes, as well as heteroaromatic aldehydes, were employed, affording good to high yields of the corresponding products and illustrating the substrate generality of the present method. In addition, the prepared dicationic Brönsted acidic ionic liquid can be easily recovered and reused. Conclusion: 1, 1’-Sulfinyldiethylammonium bis (hydrogen sulfate), as a novel dicationic ionic liquid, can act as a highly efficient catalyst for the synthesis of 3, 4-dihydropyrimidin-2(1H)-ones under solvent-free conditions.

Synthesis and Characterization of a Novel Ionic Liquid Based on N,N,N,N-tetramethylethylenediamine and its Application in the Synthesis of 1,8-dioxo-octahydro Xanthenes

2018 ◽  
Vol 21 (7) ◽  
pp. 526-532 ◽  
Author(s):  
Zahra Abdi Piralghar ◽  
Mohammad Mahmoodi Hashemi ◽  
Ali Ezabadi
Keyword(s):  
Ionic Liquid ◽  
Chlorosulfonic Acid ◽  
Solvent Free ◽  
Aryl Aldehydes ◽  
Acidic Ionic Liquid ◽  
Brønsted Acidic Ionic Liquid ◽  
Solvent Free Conditions ◽  
Aryl Aldehyde ◽  
High Yields

Aim and Objective: In this work, we synthesized and characterized a novel Brönsted acidic ionic liquid from the reaction of N, N, N’, N’-tetramethylethylenediamine with chlorosulfonic acid and explored its catalytic activity in 1, 8-dioxo-octahydroxanthenes synthesis. Materials and Methods: Dimedone, aryl aldehydes, and the ionic liquid as the catalyst were reacted under solvent-free conditions. The progressive of the reaction was monitored by a thin layer of chromatography (ethyl acetate/n-hexane = 1/5). All products were characterized as the basis of their spectra data and melting point by comparison with those reported in the literature. Results: The prepared ionic liquid was successfully applied in the synthesis of 1, 8-dioxooctahydroxanthenes in good to high yields on the reaction of aryl aldehyde and dimedone at 120oC under solvent-free conditions. Conclusion: This research demonstrates that the catalyst is impressive for 1, 8-dioxo-octahydroxanthenes synthesis under solvent-free conditions.

scholarly journals Two-Stage Biodiesel Synthesis from Used Cooking Oil with a High Acid Value via an Ultrasound-Assisted Method

Energies ◽  
2021 ◽  
Vol 14 (12) ◽  
pp. 3703
Author(s):  
Ming-Chien Hsiao ◽  
Wei-Ting Lin ◽  
Wei-Cheng Chiu ◽  
Shuhn-Shyurng Hou
Keyword(s):  
Acid Value ◽  
Molar Ratio ◽  
Optimal Conditions ◽  
Two Stage ◽  
Cooking Oil ◽  
High Acid ◽  
Used Cooking Oil ◽  
Biodiesel Synthesis ◽  
Stage Process ◽  
Ultrasound Assisted

In this study, ultrasound was used to accelerate two-stage (esterification–transesterification) catalytic synthesis of biodiesel from used cooking oil, which originally had a high acid value (4.35 mg KOH/g). In the first stage, acid-catalyzed esterification reaction conditions were developed with a 9:1 methanol/oil molar ratio, sulfuric acid dosage at 2 wt %, and a reaction temperature of 60 °C. Under ultrasound irradiation for 40 min, the acid value was effectively decreased from 4.35 to 1.67 mg KOH/g, which was decreased to a sufficient level (<2 mg KOH/g) to avoid the saponification problem for the subsequent transesterification reaction. In the following stage, base-catalyzed transesterification reactions were carried out with a 12:1 methanol/oil molar ratio, a sodium hydroxide dosage of 1 wt %, and a reaction temperature of 65 °C. Under ultrasound-assisted transesterification for 40 min, the conversion rate of biodiesel reached 97.05%, which met the requirement of EN 14214 standard, i.e., 96.5% minimum. In order to evaluate and explore the improvement of the ultrasound-assisted two-stage (esterification–transesterification) process in shortening the reaction time, additional two-stage biodiesel synthesis experiments using the traditional mechanical stirring method under the optimal conditions were further carried out in this study. It was found that, under the same optimal conditions, using the ultrasound-assisted two-stage process, the total reaction time was significantly reduced to only 80 min, which was much shorter than the total time required by the conventional method of 140 min. It is worth noting that compared with the traditional method without ultrasound, the intensification of the ultrasound-assisted two-stage process significantly shortened the total time from 140 min to 80 min, which is a reduction of 42.9%. It was concluded that the ultrasound-assisted two-stage (esterification–transesterification) catalytic process is an effective and time-saving method for synthesizing biodiesel from used cooking oil with a high acid value.

Study on the Synthesis of Isoamyl Acetate Catalyzed by Strong Acidic Cation Exchange Resin

2011 ◽  
Vol 396-398 ◽  
pp. 2411-2415 ◽  
Author(s):  
Ping Lan ◽  
Li Hong Lan ◽  
Tao Xie ◽  
An Ping Liao
Keyword(s):  
Acetic Acid ◽  
Reaction Time ◽  
Cation Exchanger ◽  
Cation Exchange Resin ◽  
Isoamyl Acetate ◽  
Molar Ratio ◽  
Esterification Reaction ◽  
Reaction Conditions ◽  
Optimum Reaction

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.

Lipase-Catalyzed Acyl-L-Carnitines Synthesis in [Bmim]PF6 Ionic Liquid

2009 ◽  
Vol 5 (1) ◽  
Author(s):  
Jin-qiang Tian ◽  
Qiang Wang ◽  
Zhong-yuan Zhang
Keyword(s):  
Ionic Liquid ◽  
Lipase Activity ◽  
Molecular Sieves ◽  
Reaction Medium ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Optimal Reaction ◽  
Better Than

In order to significantly improve the biosynthesis of acyl-L-carnitines catalyzed by lipase, there must be an efficient and suitable reaction medium that is not only polar but also hydrophobic. [Bmim]PF6, which satisfies the above two requirements, was applied as the medium. The optimal reaction conditions were: for isovaleryl-L-carnitine, 0.22aW, 200mg molecular sieves, 60ºC, 4:1 of molar ratio (fatty acid:L-carnitine), 150rpm and 60h; for octanoyl-L-carnitine and palmitoyl-L-carnitine, 0.22aW, 250 mg molecular sieves, 5:1 of molar ratio (fatty acid:L-carnitine), 200rpm, 48h, 60ºC (octanoyl-L-carnitine) and 65ºC (palmitoyl-L-carnitine). Their overall yields could reach 59.14%, 90.79% and 98.03%, respectively. The yields of isovaleryl-L-carnitine, octanoyl-L-carnitine and palmitoyl-L-carnitine in [Bmim]PF6 were 16.21%, 73.67% and 44.22 % more than those in acetonitrile, respectively. [Bmim]PF6 as the medium was better than acetonitrile. It could not only enhance the yields of acyl-L-carnitines, but also protect the lipase activity.

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