Use of Zirconium Phosphate-Sulphate as Acid Catalyst for Synthesis of Glycerol-Based Fuel Additives

In the present work, zirconium phosphates and mixed zirconium phosphate–sulphate acid catalysts have been investigated in the acetylation of glycerol in order to obtain acetins as fuel additives. The following catalysts with chemical composition, Zr3(PO4)4, Zr(SO4)2, Zr2(PO4)2SO4, Zr3(PO4)2(SO4)3 and Zr4(PO4)2(SO4)5 have been prepared and characterized by acid capacity measurements, BET, XRD, FT-IR, XPS. The surface chemical composition in terms of P/Zr and S/Zr atomic ratios was monitored in the fresh and used catalysts. Zr3(PO4)2(SO4)3 and Zr4(PO4)2(SO4)5 showed the highest acidity associated with the synergic effect of two main crystalline phases, Zr2(PO4)2SO4 and Zr(SO4)2·4H2O. The reactions of glycerol acetylation were carried out by using a mass ratio of catalyst/glycerol equal to 5 wt% and molar ratio acetic acid/glycerol equal to 3:1. The glycerol conversion versus time was investigated over all the prepared samples in order to identify the best performing catalysts. Over Zr3(PO4)2(SO4)3 and Zr4(PO4)2(SO4)5 full glycerol conversion was achieved in 1 h only. Slightly lower conversion values were registered for Zr3(PO4)4 and Zr2(PO4)2SO4, while Zr(SO4)2 was the worst catalyst. Zr4(PO4)2(SO4)5 was the most selective catalyst and was used for recycling experiments up to five cycles. Despite a modest loss of activity, a drastic decrease of selectivity to tri- and diacetin was observed already after the first cycle. This finding was attributed to the leaching of sulphate groups as detected by XPS analysis of the spent catalyst.

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β-Cyclodextrin-Calcium Complex Intercalated Hydrotalcites as Efficient Catalyst for Transesterification of Glycerol

Catalysts ◽

10.3390/catal11111307 ◽

2021 ◽

Vol 11 (11) ◽

pp. 1307

Author(s):

Guanhao Liu ◽

Jingyi Yang ◽

Xinru Xu

Keyword(s):

Value Added ◽

Nitrogen Adsorption ◽

Collision Probability ◽

Molar Ratio ◽

Glycerol Carbonate ◽

Efficient Catalyst ◽

Glycerol Conversion ◽

Ft Ir ◽

Adsorption Desorption ◽

Basic Strength

β-cyclodextrin derivative intercalated MgAl-hydrotalcites (β-CD-Ca/LDH) was synthesized to convert glycerol into high value-added glycerol carbonate(GC) by transesterification of dimethyl carbonate (DMC) and glycerol in this paper. β-cyclodextrin-metal complexes and β-CD-Ca/LDH was characterized by XRD, FT-IR, SEM, XPS and nitrogen adsorption-desorption. The enrichment of organic reactants in the hydrophobic cavity of β-cyclodextrin improved the collision probability of reactants. The intercalation of β-cyclodextrin-calcium complex (β-CD-Ca) increased the pore size and basic strength of catalyst. The experiment results showed that the glycerol conversion was 93.7% and the GC yield was 91.8% catalyzed by β-CD-Ca/LDH when the molar ratio of DMC and glycerol was 3:1, the catalyst dosage was 4 wt.%, the reaction temperature was 75 °C and the reaction time was 100 min while the glycerol conversion was 49.4% and the GC yield was 48.6% catalyzed by MgAl-LDH under the same conditions.

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Catalytic Synthesis of Butyraldehyde Glycol Acetal with H4SiW12O40/MCM-48

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.531.312 ◽

2012 ◽

Vol 531 ◽

pp. 312-315 ◽

Cited By ~ 2

Author(s):

Ming Bo Xu ◽

Jie Yang ◽

Yong Kui Huang ◽

Shui Jin Yang

Keyword(s):

Reaction Time ◽

Molecular Sieve ◽

Catalytic Synthesis ◽

Molar Ratio ◽

Impregnation Method ◽

Mass Ratio ◽

Optimum Conditions ◽

Environmental Friendly ◽

Ft Ir ◽

Catalyst Dosage

A novel environmental friendly catalyst，H4SiW12O40/MCM-48, was prepared by impregnation method. The catalysts were characterized by means of XRD and FT-IR. The synthesis of butyraldehyde glycol acetal catalyzed by H4SiW12O40/MCM-48 was studied with butyraldehyde and glycol as reactants. H4SiW12O40/MCM-48 was an excellent catalyst for the synthesizing butyraldehyde glycol acetal and Keggin structure of H4SiW12O40 kept unchanged after being impregnated on surface of the molecular sieve support. Effects of n(butyraldehyde)∶n(glycol), catalyst dosage, cyclohexane(water-stripped reagent ) and reaction time on yields of the product were investigated. The optimum conditions had been found, that is, molar ratio of butyraldehyde to glycol is1:1.4，mass ratio of catalyst used to the reactants is 0.4% and reaction time is 45 min. Under these conditions, the yield of butyraldehyde glycol acetal can reach 73.3%.

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Interesterification for biofuel synthesis over HJ-2# caly-supported SO42-/ZrO2 solid acid catalyst

E3S Web of Conferences ◽

10.1051/e3sconf/202129001033 ◽

2021 ◽

Vol 290 ◽

pp. 01033

Author(s):

Dong Lixin ◽

Zhang Xueqiong ◽

Chen Jing ◽

Hao Yinan ◽

Pang Liwen ◽

...

Keyword(s):

Soybean Oil ◽

Solid Acid ◽

Solid Acid Catalyst ◽

Maximum Yield ◽

Acid Catalyst ◽

Acid Sites ◽

Preparation Condition ◽

Molar Ratio ◽

Impregnation Method ◽

Ft Ir

This study makes use of soybean oil to produce biodiesel using SO42-/ZrO2-HJ-2# caly solid acid catalyst (SZ-HJ-2#). It was through coprecipitation and impregnation method that the catalyst was prepared which was then characterized by means of FE-SEM, XRD, EDS, BET, FT-IR, ICP-MS, NH3-TPD and XPS. The catalytic property of the synthesized catalyst was determined by using it to produce biodiesel from soybean oil. A study was carried out to find the effect of the different preparation condition of catalyst affecting the process. For SZ-HJ-2#, Optimized condition of 0.5 mol/L(zirconium salt solution), 1.5 mol/L (the concentration of sulfuric acid impregnating solution) and 450℃(calcination temperature). Optimized conditions of 8.32:1 methanol to soybean oil molar ratio and catalytic loading of 1 wt% at 55℃ with a stirring rate of 500 rpm for a reaction duration of 10 h gave a maximum yield of 89.6 wt%. Moreover, the further investigation indicated the catalytic activities were closely related to the ratio of Brönsted acid sites and intensity on catalysts. Besides, the excellent performance of the catalyst during recycling was shown by conducting reusability study.

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Synthesis of Hydrotalcites from Waste Steel Slag with [Bmim]OH Intercalated for the Transesterification of Glycerol Carbonate

Molecules ◽

10.3390/molecules25194355 ◽

2020 ◽

Vol 25 (19) ◽

pp. 4355

Author(s):

Guanhao Liu ◽

Jingyi Yang ◽

Xinru Xu

Keyword(s):

Ionic Liquid ◽

Dimethyl Carbonate ◽

Steel Slag ◽

Catalytic Performance ◽

Molar Ratio ◽

Glycerol Carbonate ◽

Glycerol Conversion ◽

Before And After ◽

Ft Ir ◽

The Stability

Ca-Mg-Al hydrotalcites were prepared by coprecipitation from Type S95 steel slag of Shanghai Baosteel Group as supports of ionic liquid in this paper. Five basic ionic liquids [Bmim][CH3COO], [Bmim][HCOO], [Bmim]OH, [Bmim]Br and ChOH were prepared and their catalytic performance on the synthesis of glycerol carbonate by transesterification between dimethyl carbonate and glycerol was investigated. The characterization results indicated that [Bmim]OH is the best ionic liquid (IL) for the transesterification reaction of glycerol carbonate. The hydrotalcites before and after intercalation by ionic liquid were characterized by XRD, FTIR, SEM, EDS and the IL were characterized by FT-IR, 13C-NMR and basicity determination via the Hammett method. The analysis results implied that the dispersion of [Bmim]OH in hydrotalcites reduced the alkali density appropriately and facilitated the generation of glycerol carbonate. The yield of glycerol carbonate and the conversion rate of glycerol reached 95.0% and 96.1%, respectively, when the molar ratio of dimethyl carbonate and glycerol was 3:1, the catalyst dosage was 3 wt%, the reaction temperature was 75 °C and the reaction time was 120 min. The layered structure of hydrotalcites increased the stability of ionic liquid intercalated in carriers, thus the glycerol conversion and the GC yield still remained 91.9% and 90.5% in the fifth reaction cycle.

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Biodiesel Production From Waste Palm Oil Using Palm Empty Fruit Bunch-Derived Novel Carbon Acid Catalyst

Journal of Energy Resources Technology ◽

10.1115/1.4038380 ◽

2017 ◽

Vol 140 (3) ◽

Cited By ~ 5

Author(s):

P. G. I. Thushari ◽

S. Babel

Keyword(s):

Palm Oil ◽

Alternative Energy ◽

Acid Methyl Ester ◽

Acid Catalyst ◽

Biodiesel Production ◽

Molar Ratio ◽

Empty Fruit Bunch ◽

X Ray ◽

Ft Ir ◽

Carbon Acid

Production of biodiesel from waste palm oil (WPO) can provide alternative energy and at the same time reduce the problems created by disposal of WPO. In this study, a novel, inexpensive, and environmental benign carbon acid catalyst is prepared by direct in situ concentrated H2SO4 impregnation of palm empty fruit bunch (PEFB) powder and employed for biodiesel production using WPO. The structure and the physiochemical properties of the prepared catalyst (PEFB-DS-SO3H) are analyzed by acid-base back titration data, energy dispersive X-ray spectroscopy (scanning electron microscopy (SEM)-EDS), SEM, Fourier transform infrared (FT-IR) spectroscopy, X-ray photoelectron spectroscopy (XPS), and using N2 adsorption and desorption isotherm data. It is observed that the catalyst has a unique amorphous structure with total acid density of 5.40 mmolg−1, surface area of 5.5 m2g−1, and 0.31 cm3g−1 pore volume. In addition, FT-IR, XPS, and EDS results confirm a successful sulfonation during the catalyst preparation. It is found that fatty acid methyl ester (FAME) yield increases with increasing methanol:oil (molar ratio) and reaction time up to an optimum value. The highest biodiesel yield of 91% is reported under reaction conditions of 5 wt % catalyst, 14:1 methanol: oil (molar ratio), at 65–70 °C after 14 h in an open reflux system. Results show that the catalyst can be reused for four consecutive cycles without significant loss of catalytic activity. Fuel properties of the produced biodiesel are compatible with the international fuel standards for biodiesel.

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Al-alginate as acid catalyst for FAME synthesis using electrolysis process

E3S Web of Conferences ◽

10.1051/e3sconf/20184301002 ◽

2018 ◽

Vol 43 ◽

pp. 01002

Author(s):

Rudy Syah Putra ◽

Tasyrifatur Rahma

Keyword(s):

Solid Acid Catalyst ◽

Acid Methyl Ester ◽

Acid Catalyst ◽

Molar Ratio ◽

Esterification Reaction ◽

High Catalytic Activity ◽

Ir Spectrometry ◽

Electrolysis Process ◽

Used Cooking Oil ◽

Ft Ir

A novel solid acid catalyst, which was prepared from sodium alginate and aluminum chlorides and characterized by SEM-EDS, XRD and FT-IR spectrometry. The catalyst was used for the synthesis of fatty acid methyl ester (FAME) via (trans)esterification reaction using electrolysis process. Purity and FAME components of biodiesel were measured by GC-MS. The results showed that the aluminum-alginate prepared in a cheap and easy way exhibited high catalytic activity. FAME conversion from used-cooking oil was obtained by 93.82% in the presence of 10 wt.% of catalyst dosage upon refluxing for 4 h of methanol and oil in a molar ratio of 6:1.

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Lamellar zirconium phosphates to host metals for catalytic purposes

Dalton Transactions ◽

10.1039/c7dt03717a ◽

2018 ◽

Vol 47 (9) ◽

pp. 3047-3058 ◽

Cited By ~ 5

Author(s):

Daniel Ballesteros-Plata ◽

Antonia Infantes-Molina ◽

Elena Rodríguez-Aguado ◽

Pilar Braos-García ◽

Enrique Rodríguez-Castellón

Keyword(s):

Zirconium Phosphate ◽

Noble Metals ◽

Molar Ratio ◽

Zirconium Phosphates

In the present study a porous lamellar zirconium phosphate heterostructure (PPH) formed from zirconium(iv) phosphate expanded with silica galleries (P/Zr molar ratio equal to 2 and (Si + Zr)/P equal to 3) was prepared to host noble metals.

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SO3H-functionalized Zeolite-Y as an Efficient Nanocatalyst for the Synthesis of Nbenzimidazole- 2-aryl-4-thiazolidinones and tri-substituted Imidazoles

Current Organic Synthesis ◽

10.2174/1570179417666200115170019 ◽

2020 ◽

Vol 17 (2) ◽

pp. 117-130 ◽

Cited By ~ 1

Author(s):

Mehdi Kalhor ◽

Zohre Zarnegar ◽

Zahra Seyedzade ◽

Soodabeh Banibairami

Keyword(s):

Zeolite Y ◽

Internal Standard ◽

Acid Catalyst ◽

Aromatic Aldehydes ◽

Reaction Rates ◽

Ambient Conditions ◽

Catalytic Method ◽

Efficient Catalyst ◽

Bet Analysis ◽

Ft Ir

Background: SO3H-functionalized zeolite-Y was prepared and used as a catalyst for the synthesis of 2-aryl-N-benzimidazole-4-thiazolidinones and tri-substituted imidazoles at ambient conditions. Objective: The goals of this catalytic method include excellent yields and high purity, inexpensive procedure and ease of product isolation, the use of nontoxic and heterogeneous acid catalyst, shorter reaction times and milder conditions. Materials and Methods: NMR spectra were recorded on Brucker spectrophotometer using Me4Si as internal standard. Mass spectra were recorded on an Agilent Technology 5975C VL MSD with tripe-axis detector. FTIR spectra were obtained with KBr disc on a galaxy series FT-IR 5000 spectrometer. The surface morphology of nanostructures was analyzed by FE-SEM (EVO LS 10, Zeiss, Carl Zeiss, Germany). BET analysis were measured at 196 °C by a Japan Belsorb II system after the samples were vacuum dried at 150°C overnight. Results: The NSZ was characterized by FT-IR, FESEM, EDX, XRF, and BET. The catalytic activity of NSZ was investigated for synthesis of 1,3-tiazolidin-4-ones in H2O/Acetone at room temperature. Moreover, NSZ was used for synthesis of tri-substituted imidazoles at 60 °C via solvent-free condensation. Different kinds of aromatic aldehydes were converted to the corresponding of products with good to excellent yields. Conclusion: Sulfonated zeolite-Y was as an efficient catalyst for the preparation of N-benzimidazole-2-aryl-1,3- thiazolidin-4-ones and 2,4,5-triaryl-1H-imidazoles. High reaction rates, elimination toxic solvent, simple experimental procedure and reusability of the catalyst are the important features of this protocol.

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Continuous Integrated Process of Biodiesel Production and Purification—The End of the Conventional Two-Stage Batch Process?

Energies ◽

10.3390/en14020403 ◽

2021 ◽

Vol 14 (2) ◽

pp. 403

Author(s):

Matea Bačić ◽

Anabela Ljubić ◽

Martin Gojun ◽

Anita Šalić ◽

Ana Jurinjak Tušek ◽

...

Keyword(s):

Extraction Efficiency ◽

Deep Eutectic Solvent ◽

International Standards ◽

Biodiesel Production ◽

Molar Ratio ◽

Process Conditions ◽

Integrated Process ◽

Free Glycerol ◽

Mass Ratio ◽

Glycerol Content

In this research, optimization of the integrated biodiesel production process composed of transesterification of edible sunflower oil, catalyzed by commercial lipase, with simultaneous extraction of glycerol from the reaction mixture was performed. Deep eutectic solvents (DESs) were used in this integrated process as the reaction and extraction media. For two systems, choline chloride:glycerol (ChCl:Gly) and choline chloride:ethylene glycol (ChCl:EG), respectively, the optimal water content, mass ratio of the phase containing the mixture of reactants (oil and methanol) with an enzyme and a DES phase (mass ratio of phases), and the molar ratio of deep eutectic solvent constituents were determined using response surface methodology (RSM). Experiments performed with ChCl:Gly resulted in a higher biodiesel yield and higher glycerol extraction efficiency, namely, a mass ratio of phases of 1:1, a mass fraction of water of 6.6%, and a molar ratio of the ChCl:Gly of 1:3.5 were determined to be the optimal process conditions. When the reaction was performed in a batch reactor under the optimal conditions, the process resulted in a 43.54 ± 0.2% yield and 99.54 ± 0.19% glycerol extraction efficiency (t = 2 h). Unfortunately, the free glycerol content was higher than the one defined by international standards (wG > 0.02%); therefore, the process was performed in a microsystem to enhance the mass transfer. Gaining the same yield and free glycerol content below the standards (wG = 0.0019 ± 0.003%), the microsystem proved to be a good direction for future process optimization.

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Biofoam of Spittlebug, Poophilus costalis (Walker): Preferential Sites, Temperature Regulation, Chemical Composition and Antimicrobial Activity

Insects ◽

10.3390/insects12040340 ◽

2021 ◽

Vol 12 (4) ◽

pp. 340

Author(s):

Kitherian Sahayaraj ◽

Balakrishnan Saranya ◽

Samy Sayed ◽

Loko Yêyinou Laura Estelle ◽

Koilraj Madasamy

Keyword(s):

Antimicrobial Activity ◽

Chemical Composition ◽

High Performance ◽

Host Plants ◽

Ground Level ◽

College Campus ◽

The Other ◽

Mimosa Pudica ◽

Ft Ir ◽

Gas Chromatography Mass Spectroscopy

The foam produced by nymphs of Poophilus costalis on eleven different host plants belonging to eight families on St. Xavier’s College campus in India was studied over five months. The chemical composition and antimicrobial activity of these biofoams were investigated. The results revealed that P. costalis preferred Theporsia purpurea and Mimosa pudica for laying their eggs and producing foam, over the other tested plants. P. costalis produce their foam on either nodes or internodes on monocotyledons (30%) (p < 0.05), whereas on dicotyledons, they produce more foam on the stems (63.8%) than on the leaves (6.2%) (p < 0.01). The number of nymphs in each piece of foam from P. costalis varied from 1 to 3 (mean = 1.8 per plant). They produced their foam (5.7 to 45.2 cm) from the ground level on a plant. The length and breadth of a piece of foam ranged from 1.0 to 3.9 cm and 0.6 to 4.7 cm, respectively. The foam tended to be cooler than the environment. Qualitative profiling showed that the foam consists of carbohydrates, including maltose; trypsin; amino acids; protease. The foam was also analyzed using a spectrophotometer, Fourier transform infrared spectroscopy (FT-IR), gas chromatography–mass spectroscopy (GC-MS), and high-performance liquid chromatography (HPLC). The antimicrobial activity of the biofoam was the greatest against Staphylococcus aureus, the growth of which was reduced by 55.9 ± 3.9%, suggesting that the foam could be used as an antimicrobial product. However, no activities were observed against Fusarium oxysporum and Candida albicans.

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