scholarly journals Novel Aryl-Imidazolium Ionic Liquids with Dual Brønsted/Lewis Acidity as Both Solvents and Catalysts for Friedel–Crafts Alkylation

2019 ◽  
Vol 9 (22) ◽  
pp. 4743 ◽  
Author(s):  
Che-Hsuan Yang ◽  
Jui-Cheng Chang ◽  
Tzi-Yi Wu ◽  
I-Wen Sun ◽  
Jun-Hao Wu ◽  
...  

Unique tunable aryl-imidazolium magnetic ionic liquids with dual functions as a solvent–catalyst and dual Brønsted–Lewis acidity (B-L MILs) are applied for Friedel–Crafts alkylation without additional solvents. The catalytic properties of these B-L MILs in the Friedel–Crafts alkylation of p-xylene with benzyl chloride are investigated. The various reaction parameters, including the catalyst dosage, reaction time, reaction temperature, molar ratio of reactants, and reusability, are discussed. The results show that the B-L MIL 5c has more excellent product selectivity (>99%) and reactant conversion (>99%) under the following optimum conditions (reaction temperature = 80 °C, reaction time = 0.5 h, molar ratio of p-xylene to benzyl chloride = 6:1, and catalyst 5c dosage = 1.0 mole %) than traditional catalysts reported in the previous literature. Specifically, due to the mesomeric effect between the FeCl4 anion and hydrogen atom at cationic moiety, the catalyst B-L MILs with the molar fraction of FeCl3 equal to 0.5 can be easily recovered and provide satisfactory catalytic activity after being re-used six times.

2013 ◽  
Vol 724-725 ◽  
pp. 1054-1061
Author(s):  
Zhi Hong Xiao ◽  
Ai Hua Zhang ◽  
Wei Wei Jiang ◽  
Hong Qin Zhang ◽  
Chang Zhu Li

In this study, the trench oil was processed by the technology of polyol pre-esterification and the bio-diesel was prepared using basic ionic liquid 1-methyl-3-butyl-imidazole hydroxide as a catalyst. The amount of ionic liquids, alcohol and oil molar ratio, reaction temperature and reaction time were investigated on the transesterification reaction. The results showed that the bio-diesel prepared conditions by trench oil are as follows: alcohol and oil molar ratio of 8:1, reaction temperature 70°C, reaction time 110min and the amount of catalyst for the quality of raw materials 3.0% oil. Under these conditions, fatty acid methyl ester was 95.7% conversion rate.


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.


2019 ◽  
Vol 19 (4) ◽  
pp. 849
Author(s):  
Nurul Atikah Amin Yusof ◽  
Nursyamsyila Mat Hadzir ◽  
Siti Efliza Ashari ◽  
Nor Suhaila Mohamad Hanapi ◽  
Rossuriati Dol Hamid

Optimization of the lipase catalyzed enzymatic synthesis of betulinic acid amide in the presence of immobilized lipase, Novozym 435 from Candida antartica as a biocatalyst was studied. Response surface methodology (RSM) and 5-level-4-factor central-composite rotatable design (CCRD) were employed to evaluate the effects of the synthesis parameters, such as reaction time (20–36 h), reaction temperature (37–45 °C), substrate molar ratio of betulinic acid to butylamine (1:1–1:3), and enzyme amounts (80–120 mg) on the percentage yield of betulinic acid amide by direct amidation reaction. The optimum conditions for synthesis were: reaction time of 28 h 33 min, reaction temperature of 42.92 °C, substrate molar ratio of 1:2.21, and enzyme amount of 97.77 mg. The percentage yield of actual experimental values obtained 65.09% which compared well with the maximum predicted value of 67.23%. The obtained amide was characterized by GC, GCMS and 13C NMR. Betulinic acid amide (BAA) showed a better cytotoxicity compared to betulinic acid as the concentration inhibited 50% of the cell growth (IC50) against MDA-MB-231 cell line (IC50 < 30 µg/mL).


Holzforschung ◽  
2007 ◽  
Vol 61 (5) ◽  
pp. 499-503 ◽  
Author(s):  
Shifa Wang

Abstract A light-colored rosin glycerol ester was synthesized from gum rosin and glycerol in the presence of a highly effective decolorizing agent. The effects of the type and dosage of the decolorizing agent and the reaction temperature and time on the yield, softening point, color, and acid number of the rosin glycerol ester were investigated. Experimental results showed that 4,4′-thio-bis(6-tert-butyl-3-methyl phenol) was the best decolorizing agent. It promoted esterification at an optimal dosage of 0.5% (based on the weight percentage of starting material rosin). Suitable conditions for esterification of rosin and glycerol were: reaction temperature, 260–270°C; reaction time, 6–8 h; and rosin/glycerol molar ratio, 2.5:1 (mol mol-1). The characteristics of the rosin glycerol ester obtained under these conditions were as follows: softening point, 90–94°C (ball and ring method); color, 1–2 (Gardner value); acid number, 7–8; and yield, >88% (based on the total weight of rosin and glycerol). The selected additive has a multifunctional effect involving bleaching, disproportionation, and catalysis.


2019 ◽  
Vol 953 ◽  
pp. 185-190
Author(s):  
Yong Li Peng ◽  
Ni An Zhuo ◽  
Can Zhang

A new phosphorus-containing flame-retardant curing agent PPDTA was synthesized from phenylphosphonic dichloride (PPD) and 3-amino-1,2,4-triazole (TA) in tetrahydrofuran solvent to improve the flame retardancy of epoxy resin. The structure of the compound was analyzed and confirmed by infrared spectroscopy. The effects of reaction time, reaction temperature and ratio of reactants on yield were studied by using three-factor three-level orthogonal experiment. The results show that the yield of PPDTA can reach 86.4%, when the reaction time is 10h, reaction temperature is 70 °Cand the molar ratio of TA to PPD is 2.2:1.


2013 ◽  
Vol 781-784 ◽  
pp. 526-530 ◽  
Author(s):  
Shao Ying Li ◽  
Chun Mei Niu ◽  
Hua Yu Zhong

Series of cationic cassia tora gum (CCTG) were synthesized using 3-chloro-2-hydroxypropyl trimethyl ammonium chloride (CHPTAC) as cationic etherifying agent, isopropanol-water solution as dispersing agent, in presence of sodium hydroxide under different reaction conditions. The optimum ratio for preparing the cationic cassia tora gum are that CHPTAC-CTG molar ratio is 0.6:1; NaOH-CHPTAC molar ratio is 1.3:1.The optimum conditions are that reaction temperature is 55°Cand reaction time is 3.5 h. The cold water solubility was improved apparently. The solution transmittance has corresponding relationship with the nitrogen content (N%) in the certain range, and the maximum transmittance is up to 87.2%. N% increased with the increase of reaction time and stable N% can be obtained in shorter reaction time at higher reaction temperature. The products were characterized by 13C-NMR. The heat resistance of CTG and CCTG were analyzed.


2012 ◽  
Vol 9 (2) ◽  
pp. 545-552 ◽  
Author(s):  
Yan-Hua Cai ◽  
Shun-Jiang Li

N-(benzoyl) stearic acid hydrazide was synthesized from benzoyl hydrazine and stearyl chloride which was deprived from stearic acid via acylation. The structure of the compound had been characterized by FT-IR,1H NMR, at the same time, the structure of N-(benzoyl) stearic acid hydrazide was optimized by the semiempirical method PM3. The influence of the reaction ratio, reaction time and reaction temperature to the yield ofN-(benzoyl) stearic acid hydrazide was investigated by orthogonal experiment, and the optimized reaction condition was molar ratio of benzoyl hydrazine: stearyl chloride 1:1, reaction time 6 h, reaction temperature 70°C, and the yield was 92.9%. The TGA thermal analysis of N-(benzoyl) stearic acid hydrazide showed that thermal stability ofN-(benzoyl) stearic acid hydrazide was affected by heating rate, and theN-(benzoyl) stearic acid hydrazide enhanced the tensile strength, modulus and elongation at break of Poly(L-lactic acid)(PLLA).


2013 ◽  
Vol 634-638 ◽  
pp. 628-631
Author(s):  
Yun Hui Long ◽  
Jun Ming Guo ◽  
Du Shu Huang ◽  
Gui Yang Liu

The catalytic synthesis of ethyl acetate from ethanol and acetic acid using Ti2SnC in liquid phase under the atmospheric pressure was studied. The influences of some factors such as catalyst usage, initial reactant molar ratio, reaction temperature and reaction time on acetic acid conversion rate of this reaction system were investigated. The acetic acid conversion rate of 88.12% is achieved while the molar ratio of alcohol and acid is 1:3.6, the amount of catalyst is 0.2000 g, the reaction temperature is 80 °C and the reaction time is 30min. The catalyst Ti2SnC is the ideal catalyst for synthesis of ethyl acetate for good catalytic performance, non-corrosive to equipment, easily separated from product and used repeatedly.


2012 ◽  
Vol 554-556 ◽  
pp. 1178-1182
Author(s):  
Hui Ling Cui ◽  
Yuan Dong Xu ◽  
Yu Jun Zhang ◽  
Hui Bo Song

The 1, 3-specific lipase of Lipozymetlim was used as catalyst to produce low calorie oil through the reaction of soybean oil with glycerol triacetate. The effects of catalyst using amount, molar ratio of the substrates, reaction temperature and reaction time on the product yields were investigated. The orthogonal experiment results showed that the optimal reaction conditions were the substrate molar ratio of 2:1, reaction temperature of 60 °C, reaction time of 24 h, and 10 % enzyme adding amount per gram of substrate. Under such conditions, the reaction yield was 79.56 %. After 5 times reuse of the enzyme, the yield still could reach 58.94 %. The calorific value of the product was measured by calorimetric method and the value was 35 027 J/g which was about 75 % of the corresponding value for soybean oil.


2012 ◽  
Vol 550-553 ◽  
pp. 1039-1042 ◽  
Author(s):  
Gui Rong Cao ◽  
Xue Yan Zhao ◽  
Rui Jie Xiao

In this paper, triphosgene respectively reacting with o-nitrophenyl aniline, m-nitrophenyl aniline and p-nitrophenyl aniline to synthesize corresponding isocyanates. The effects of reactants molar ratio, reaction time and reaction temperature on the yield were investigated. As a result, using 1,2-dichloroethane as reaction solvent, the optimum molar ratio of the three kinds of nitroaniline and triphosgene were all 2.5:1, the optimum reaction time of synthesis of o-nitrophenyl isocyanate, m-nitrophenyl isocyanate and p-nitrophenyl isocyanate respectively was 6h, 5.5h and 5h; the optimum reaction temperature of synthesis of the three kinds of nitrophenyl isocyanates were all 75°C. Under the optimal conditions, the yield of o-nitrophenyl isocyanate, m-nitrophenyl isocyanate and p-nitrophenyl isocyanate could respectively be 80.3%, 83.7% and 83.5%. The products were characterized by meltingtest, ebulliometry, IR, and HPLC


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