Zinc-Modified MCM-22 as Potential Solid acid Catalyst for Friedel–Crafts Alkylation Reaction

2013 ◽  
Vol 11 (1) ◽  
pp. 407-415 ◽  
Author(s):  
Sharad V. Lande ◽  
A. Sakthivel, ◽  
K. V. V. S. B. S. R. Murthy ◽  
Unnikrishnan Sreedharan ◽  
Jagannath Das ◽  
...  

Abstract In this paper, we report loading of ZnCl2 on microporous medium pore high surface area zeolite, which was achieved by incipient wetness method. The zinc-modified mobil composite material -22 (Zn-MCM-22) was systematically characterized by powder X-ray diffraction, N2 adsorption-desorption analysis, scanning electron microscopy and Fourier transform infrared spectroscopy. The acidity of the materials was studied by temperature programmed desorption of ammonia analysis. The well-characterized Zn-MCM-22 catalyst was investigated for the Friedel–Crafts alkylation of benzene by benzyl chloride in liquid phase medium. A systematic investigation of various operating parameters like effect of different temperature, catalyst loading and reactant molar ratio was carried out. The Zn-MCM-22 found to be promising, further the catalytic activity remains stable over several recycles.

2020 ◽  
Vol 12 (42) ◽  
pp. 47389-47396 ◽  
Author(s):  
Dinithi Rathnayake ◽  
Inosh Perera ◽  
Alireza Shirazi-Amin ◽  
Peter Kerns ◽  
Shanka Dissanayake ◽  
...  

2016 ◽  
Vol 79 (1) ◽  
Author(s):  
Nur Aainaa Syahirah Ramli ◽  
Nur Hidayah Zaharudin ◽  
Nor Aishah Saidina Amin

Levulinic acid (LA) is a versatile biomass-derived building block as it can be used for the synthesis of organic chemicals as alternative to the depleting fossil fuel resources. Levulinate esters, obtained from catalytic esterification of LA with alcohol, can be used in many applications such as fragrance and fuel additives. In this study, ion-exchange resins Amberlyst-15 was employed as solid acid catalyst for esterification of LA with methanol for methyl levulinate (ML) production. The effect of reaction time, catalyst loading, and molar ratio of LA to methanol, was investigated on LA esterification to ML at the reflux condition. The optimum ML yield of 82% was obtained from reaction conducted at reflux temperature for 5h, using 30% of Amberlyst-15 loading, and 1:20 of LA to methanol molar ratio. The reusability of Amberlyst-15 for ML production was examined for five successive reactions. In addition, Amberlyst-15 catalyst, employed in the esterification of LA with ethanol and 1-butanol for ethyl levulinate (EL) and butyl levulinate (BL), respectively, registered good performance. Yields of 71% and 55% have been obtained for EL and BL, respectively. Amberlyst-15 is a promising solid acid catalyst for production of biomass derived levulinate esters at mild process conditions. 


2020 ◽  
Vol 20 (6) ◽  
pp. 3496-3503
Author(s):  
Shuang Wang ◽  
Ling Wan ◽  
Leizhi Zheng ◽  
Xiaoqi Fu ◽  
Tingshun Jiang ◽  
...  

We present here a facile synthesis of SO2-4/ZrO2 solid superacid by impregnating the biscuit-like mesoporous ZrO2 nanoparticles prepared by an emulsion combustion method directly into H2SO4 solution. The obtained solid acid catalyst was characterized by means of X-ray powder diffraction, transmission and scanning electron microscopy, thermogravimetry, Brunner-Emmet-Teller measurement, and infrared analysis. Its catalytic performance was examined by alkylation of o-xylene with styrene. The optimal catalytic formulation, obtained from the investigation of experimental conditions, was determined to be 5 wt% of catalyst loading with initial o-xylene/styrene molar ratio of 5 under reaction temperature at 120 °C for 120 min, achieving a 100% styrene conversion and a 93.3% 1-phenyl-1-xylyl ethane selectivity. The biscuit-like SO2−4/ZrO2 solid acid exhibited high catalytic activity and selectivity and excellent structural stability. This synthetic strategy for preparing the mesoporous SO2−4 promoted ZrO2 solid superacid catalyst is generalized and expected to be applied to other metal oxides.


CrystEngComm ◽  
2020 ◽  
Vol 22 (38) ◽  
pp. 6275-6286
Author(s):  
Esun Selvam ◽  
Rajesh K. Parsapur ◽  
Carlos E. Hernandez-Tamargo ◽  
Nora H. de Leeuw ◽  
Parasuraman Selvam

Nano-zeolite with brain-coral morphology formed by self-organization of ultra-small nanospheres, exhibits micro/meso porosity with high surface area, distributed acid sites, and reduced diffusion resistance making it a promising solid acid catalyst.


2021 ◽  
Author(s):  
Bishwajit Changmai ◽  
Kalyani Rajkumari ◽  
diparjun das ◽  
Samuel Lalthazuala Rokhum

Synthesis and application of acid-functionalized mesoporous polymer catalyst for the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones via Biginelli condensation reaction under microwave irradiation is investigated. Several analytical techniques such as FT-IR, BET, TEM, SEM and EDX were employed to characterize the synthesized polymeric catalyst. High acidity (1.15 mmol g-1 ), high surface area (90.44 m2 g -1 ) and mesoporous nature of the catalyst effectively promoted the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones. Microwave irradiation shows higher yield (89-98 %) as compared to conventional heating (15-25 % yield) under our optimized reaction conditions such as 1:1:1.2 molar ratio of aldehyde/ethylacetoacetate/urea, catalyst loading of 6 wt.% (with respect to aldehyde), the temperature of 80 °C and microwave power of 50 W. The synthesized Biginelli products were fully characterized by 1H and 13C NMR. The reusability of the catalyst was investigated up to 5 successive cycles and it showed great stability towards the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones without any significant depreciation in yields.


Molecules ◽  
2021 ◽  
Vol 26 (9) ◽  
pp. 2519
Author(s):  
Arindam Modak ◽  
Akshay R. Mankar ◽  
Kamal Kishore Pant ◽  
Asim Bhaumik

Solid acid catalysts occupy a special class in heterogeneous catalysis for their efficiency in eco-friendly conversion of biomass into demanding chemicals. We synthesized porphyrin containing porous organic polymers (PorPOPs) using colloidal silica as a support. Post-modification with chlorosulfonic acid enabled sulfonic acid functionalization, and the resulting material (PorPOPS) showed excellent activity and durability for the conversion of fructose to 5-hydroxymethyl furfural (HMF) in green solvent water. PorPOPS composite was characterized by N2 sorption, FTIR, TGA, CHNS, FESEM, TEM and XPS techniques, justifying the successful synthesis of organic networks and the grafting of sulfonic acid sites (5 wt%). Furthermore, a high surface area (260 m2/g) and the presence of distinct mesopores of ~15 nm were distinctly different from the porphyrin containing sulfonated porous organic polymer (FePOP-1S). Surprisingly the hybrid PorPOPS showed an excellent yield of HMF (85%) and high selectivity (>90%) in water as compared to microporous pristine-FePOP-1S (yield of HMF = 35%). This research demonstrates the requirement of organic modification on silica surfaces to tailor the activity and selectivity of the catalysts. We foresee that this research may inspire further applications of biomass conversion in water in future environmental research.


2017 ◽  
Vol 68 (1) ◽  
pp. 101-107
Author(s):  
Song Il Kong ◽  
Danuta Matei ◽  
Diana Cursaru ◽  
Vasile Matei ◽  
Dragos Ciuparu

A series of solid acid catalyst of the Keggin-type 12-phosphotungstic acid, H3PW12O40, supported on ordered mesoporous silica MCM-41 were prepared by a simple and effective impregnation method. MCM-41 supports were synthesized in a relatively short time via a recently reported ultrasonic irradiation method. The synthesis sonication time has been systematically varied in order to investigate its influence on the structural order of the resulting materials. The prepared catalysts were characterized by nitrogen adsorption, X-ray diffraction, Raman spectroscopy and thermogravimetric analysis. The resulting materials exhibited hexagonally ordered meso structure, with high surface area of the order of several hundreds of m2g-1,relatively large pore volumes, with the pore diameter in the range of 2.19 to 2.41 nm and a corresponding pore wall thickness of over 1.67nm. The results have demonstrated that high quality MCM-41 materials can be synthesized via the ultrasonic irradiation in few tens of minutes, much shorter than the conventional synthesis methods. Despite their relatively high loading, all synthesized materials retained the characteristic MCM-41mesoporous structure after impregnation of the heteropolyacid active phase onto the inner pore surface, without crystallization, but preserving the Keggin structure as confirmed by Raman spectroscopy.


2021 ◽  
Author(s):  
Bishwajit Changmai ◽  
Kalyani Rajkumari ◽  
diparjun das ◽  
Samuel Lalthazuala Rokhum

Synthesis and application of acid-functionalized mesoporous polymer catalyst for the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones via Biginelli condensation reaction under microwave irradiation is investigated. Several analytical techniques such as FT-IR, BET, TEM, SEM and EDX were employed to characterize the synthesized polymeric catalyst. High acidity (1.15 mmol g-1 ), high surface area (90.44 m2 g -1 ) and mesoporous nature of the catalyst effectively promoted the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones. Microwave irradiation shows higher yield (89-98 %) as compared to conventional heating (15-25 % yield) under our optimized reaction conditions such as 1:1:1.2 molar ratio of aldehyde/ethylacetoacetate/urea, catalyst loading of 6 wt.% (with respect to aldehyde), the temperature of 80 °C and microwave power of 50 W. The synthesized Biginelli products were fully characterized by 1H and 13C NMR. The reusability of the catalyst was investigated up to 5 successive cycles and it showed great stability towards the synthesis of 3,4-Dihydropyrimidin-2(1H)-ones without any significant depreciation in yields.


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