A facile post-synthetic modification of ordered mesoporous carbon to get efficient catalysts for the formation of acetins

Gościańska, Joanna; Malaika, Anna

doi:10.1016/j.cattod.2019.02.049

Cited by 27 publications

(23 citation statements)

References 54 publications

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“…This result is promising when compared to earlier studies using acetic acid. The results of Okoye et al [ 18 ], Goscianska and Mailakal [ 22 ], Kakasaheb et al [ 23 ], and Marwan et al [ 24 ] exhibited triacetin selectivity of 43, 22, 15, and 8.3% with very high glycerol conversion (>95%) over different catalysts, which were lower under relatively similar reaction conditions than our earlier study. However, the triacetin selectivity reported by Rezayat and Ghaziaskar [ 19 ] and Liu et al [ 20 ] were much higher, as indicated earlier above, albeit under extreme conditions.…”

Section: Introductionsupporting

confidence: 54%

“…This was further confirmed by the pore size distribution ( Figure 6 b) centered between 30 and 50 Å [ 41 , 45 ]. The surface area and pore volume of the catalyst reduced after sulfonation optimization from 484 to 217 m 2 /g and from 0.327 to 0.164 cm 3 /g, respectively ( Table 2 ), suggesting blockage of some pores arising from successful sulfonation process [ 22 , 43 ]. The increase in pore size of the catalyst may permit easy diffusion of the products out of the pores, which may be a contributing factor in the excellent performance of the catalyst in acetylation [ 34 ].…”

Section: Resultsmentioning

confidence: 99%

“…Kulkarni et al reported GC of 99.1%, MA, DA, and TA selectivity of 22, 57, and 21%, respectively, and at optimum conditions of 100 °C, 1:10 G/AA mole ratio, 5 wt % catalyst, and a reaction time of 3 h using a sulfated CeO 2 –ZrO 2 mixed-oxide catalyst. Using a composite of treated sucrose-based carbon with a silica template (SBA-15), 95% GC and selectivity of 19, 59, and 22% MA, DA, and TA, respectively, were reported at optimum conditions of 110 °C, a 1:9 G/AA mole ratio, and 0.7 g but at a higher reaction time of 6 h [ 22 ]. Okoye et al also reported the use of sulfonated glycerol-based carbon as a catalyst with 99% GC, a selectivity of 12, 45, and 43% MA, DA, and TA, respectively, and at optimum conditions of 110 °C, a 1:3 G/AA mole ratio, 2 wt % glycerol, and a 3 h reaction time, respectively.…”

Section: Resultsmentioning

confidence: 99%

“…Temperature-programmed desorption-ammonia (TPD-NH 3 ) analysis was carried out on a Thermo Finnigan TPD/R/O 1100 series instrument equipped with a thermal conductivity detector (TCD) to measure the total acid site and their distribution. The elemental sulfur was determined using the CHNS analyzer (EA1112 Thermo Finnigan FLASH, Delft, Netherlands) and the sulfonic acid density also estimated from it with the assumption that all the sulfur present in the samples were due to sulfonic acid groups as reported in the literature [ 22 , 60 ]. Thermogravimetric analysis (TGA) was carried out with a thermal gravimetric analyzer (Mettler, Toledo 851e, Greifensee, Switzerland) equipped with differential thermogravimetric in the temperature range of 50 to 600 °C at 10 °C min −1 under nitrogen gas flow at 50 mL/min.…”

Section: Methodsmentioning

confidence: 99%

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Optimization and Characterization of Mesoporous Sulfonated Carbon Catalyst and Its Application in Modeling and Optimization of Acetin Production

et al. 2020

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In this study, an optimized mesoporous sulfonated carbon (OMSC) catalyst derived from palm kernel shell biomass was developed using template carbonization and subsequent sulfonation under different temperatures and time conditions. The OMSC catalyst was characterized using acid-base titration, elemental analysis, XRD, Raman, FTIR, XPS, TPD-NH3, TGA-DTA, SEM, and N2 adsorption–desorption analysis to reveal its properties. Results proved that the OMSC catalyst is mesoporous and amorphous in structure with improved textural, acidic, and thermal properties. Both FTIR and XPS confirmed the presence of -SO3H, -OH, and -COOH functional groups on the surface of the catalyst. The OMSC catalyst was found to be efficient in catalyzing glycerol conversion to acetin via an acetylation reaction with acetic acid within a short period of 3 h. Response surface methodology (RSM), based on a two-level, three-factor, face-centered central composite design, was used to optimize the reaction conditions. The results showed that the optimized temperature, glycerol-to-acetic acid mole ratio, and catalyst load were 126 °C, 1:10.4, and 0.45 g, respectively. Under these optimum conditions, 97% glycerol conversion (GC) and selectivities of 4.9, 27.8, and 66.5% monoacetin (MA), diacetin (DA), and triacetin (TA), respectively, were achieved and found to be close to the predicted values. Statistical analysis showed that the regression model, as well as the model terms, were significant with the predicted R2 in reasonable agreement with the adjusted R2 (<0.2). The OMSC catalyst maintained excellent performance in GC for the five reaction cycles. The selectivity to TA, the most valuable product, was not stable until the fourth cycle, attributable to the leaching of the acid sites.

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Section: Introductionsupporting

confidence: 54%

Section: Resultsmentioning

confidence: 99%

Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

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Optimization and Characterization of Mesoporous Sulfonated Carbon Catalyst and Its Application in Modeling and Optimization of Acetin Production

et al. 2020

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“…Such materials are featured by well-developed specific surface area, large pore volume, and very good mechanical, thermal, and chemical stability. It allows for a wide range of post-synthetic modifications/functionalizations to proceed, for example, via grafting [ 15 ], impregnation [ 16 ], and sulfonation [ 17 ], but mostly through diverse oxidation [ 18 , 19 , 20 ]. Different oxidizing agents at varied temperatures enrich OMCs’ surface in additional functional groups [ 21 ].…”

Section: Introductionmentioning

confidence: 99%

Design of Paracetamol Delivery Systems Based on Functionalized Ordered Mesoporous Carbons

et al. 2020

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The oxidized ordered mesoporous carbons of cubic and hexagonal structure obtained by two templating methods (soft and hard) were applied for the first time as delivery systems for paracetamol—the most common antipyretic and analgesic drug in the world. The process of carbon oxidation was performed using an acidic ammonium persulfate solution at 60 °C for 6 h. The functionalization was found to reduce the specific surface area and pore volume of carbon materials, but it also led to an increasing number of acidic oxygen-containing functional groups. The most important element and the novelty of the presented study was the evaluation of adsorption and release ability of carbon carriers towards paracetamol. It was revealed that the sorption capacity and the drug release rate were mainly affected by the materials’ textural parameters and the total amount of surface functional groups, notably different in pristine and oxidized samples. The adsorption of paracetamol on the surface of ordered mesoporous carbons occurred according to different mechanisms: donor–acceptor complexes and hydrogen bond formation. The adsorption kinetics was assessed using pseudo-first- and pseudo-second-order models. The regression results indicated that the adsorption kinetics was more accurately represented by the pseudo-second-order model. Paracetamol was adsorbed onto the carbon materials studied following the Langmuir type isotherm. The presence of oxygen-containing functional groups on the surface of ordered mesoporous carbons enhanced the amount of paracetamol adsorbed and its release rate. The optimal drug loading capacity and expected release pattern exhibited oxidized ordered mesoporous carbon with a hexagonal structure obtained by the hard template method.

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Synthesis of ethyl levulinate from cellulose over a double acid site catalyst

Huang

Hao

2021

J of Chemical Tech & Biotech

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BACKGROUND: A novel double acid site solid catalyst (Al-OCS-0.1) having an ordered mesoporous structure was synthesized by grafting sulfonic acid groups on an oxidized ordered mesoporous carbon (OOMC) support and loading 10% Al 2 (SO 4 ) 3 .RESULT: Assessments using Field emission scanning electron microscopy, Transmission electron microscopy and X-ray diffraction showed that the OMC structure remained unchanged after the chemical modification and Al 2 (SO 4 ) 3 loading. The Brunauer-Emmett-Teller surface area and average pore size of Al-OCS-0.1 decreased to 181 m 2 g −1 and 7.1 nm after loading Al 2 (SO 4 ) 3 , respectively. Ammonia temperature-programmed desorption (NH 3 -TPD) and Pyridine adsorption infrared spectroscopy (Py-IR) demonstrated that Al-OCS-0.1 had abundant Brønsted and Lewis acid sites. The ammonia desorption of Al-OCS-0.1 increased from 2.0 to 7.2 mmol g −1 after loading Al 2 (SO 4 ) 3 .CONCLUSION: The Al-OCS-0.1 was used to catalyze the synthesis of ethyl levulinate from cellulose in ethanol and gave an extremely high yield of 50.8 mol% after 5 h at 200 °C.

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A facile post-synthetic modification of ordered mesoporous carbon to get efficient catalysts for the formation of acetins

Cited by 27 publications

References 54 publications

Optimization and Characterization of Mesoporous Sulfonated Carbon Catalyst and Its Application in Modeling and Optimization of Acetin Production

Optimization and Characterization of Mesoporous Sulfonated Carbon Catalyst and Its Application in Modeling and Optimization of Acetin Production

Design of Paracetamol Delivery Systems Based on Functionalized Ordered Mesoporous Carbons

Synthesis of ethyl levulinate from cellulose over a double acid site catalyst

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