scholarly journals Catalytic Activity of Maghnite-H+ in the Synthesis of Polyphenylmethylsiloxane under Mild and Solvent-free Conditions

2017 ◽  
Vol 62 (2) ◽  
pp. 195 ◽  
Author(s):  
Djamal Eddine Kherroub ◽  
Mohammed Belbachir ◽  
Saad Lamouri ◽  
Larbi Bouhadjar ◽  
Karim Chikh
Keyword(s):  
Molecular Mass ◽  
Maximum Yield ◽  
Xrd Analysis ◽  
Operating Conditions ◽  
Polymer Chains ◽  
Average Molecular Mass ◽  
Solvent Free Conditions ◽  
Different Temperatures ◽  
Ir Analysis ◽  
Cationic Ring Opening Polymerization

In this study, a new and easy strategy was discussed for the purpose of synthesizing of a polymer of phenylmethylcyclosiloxane type (PPMS). The cationic ring opening polymerization of triphenyltrimethylcyclotrisiloxane (D3Ph,Me) was initiated by a solid, efficient and environmentally-friendly catalyst called Maghnite-H+. Maghnite-H+ is a natural clay composed essentially of montmorillonite, it is activated with an acid treatment by replacing the interlayer ions by protons, that results to the increase of the basal space, this may be confirmed by XRD analysis. The reaction was carried out without solvent at different temperatures and for different periods of time, using also several catalyst contents. Subsequently, the operating conditions were opted in order to obtain a maximum yield of the linear polymer and a high average molecular mass as well. The structure of polymers obtained was confirmed by IR analysis. 1H NMR and 13C NMR analyzes were used to follow the crosslinking of polymer chains over time. The thermal behavior was investigated by DSC analysis. The average molecular mass and the polydispersity indices were determined by GPC.

scholarly journals Green Polymerization of Hexadecamethylcyclooctasiloxane Using an Algerian Proton Exchanged Clay Called Maghnite-H+

2018 ◽  
Vol 13 (1) ◽  
pp. 36 ◽  
Author(s):  
Djamal Eddine Kherroub ◽  
Mohammed Belbachir ◽  
Saad Lamouri
Keyword(s):  
Molecular Mass ◽  
Interlayer Spacing ◽  
Reaction Engineering ◽  
Operating Conditions ◽  
Solid Catalyst ◽  
Chemical Methods ◽  
Average Molecular Mass ◽  
Environment Friendly ◽  
Hydronium Ions ◽  
The Impact

The purpose of this study was to synthesize polydimethylsiloxanes by heterogeneous catalysis, based on the polymerization of the hexadecamethylcyclooctasiloxane (D8) by an environment-friendly solid catalyst (Maghnite-H+). Maghnite-H+ is a natural Algerian clay of the montmorillonite type, prepared by activation with sulfuric acid, the impact of this activation was observable in the XRD spectrum, by the increase in the interlayer spacing (d001) resulting from the intercalation of hydronium ions between layers. The molecular structure of the obtained polymer was determined by different chemical methods of analysis such as IR, 1H NMR, and 13C NMR. The thermal behavior of the polysiloxane obtained was confirmed by DSC. In order to achieve the best possible yield and at the same time to get a polymer of high molecular mass, the operating conditions have been set at t = 8 h and T = 70 °C after the reaction was repeated several times. The average molecular mass and the polydispersity index were measured by GPC. A reaction mechanism has been suggested to show the action of the Maghnite-H+ during the reaction. Copyright © 2018 BCREC Group. All rights reservedReceived: 8th March 2017; Revised: 27th July 2017; Accepted: 1st August 2017; Available online: 22nd January 2018; Published regularly: 2nd April 2018How to Cite: Kherroub, D.E., Belbachir, M., Lamouri, S. (2018). Green Polymerization of Hexadecamethylcyclooctasiloxane Using an Algerian Proton Exchanged Clay Called Maghnite-H+. Bulletin of Chemical Reaction Engineering & Catalysis, 13 (1): 36-46 (doi:10.9767/bcrec.13.1.993.36-46) 

Synthesis and Evaluation of Levulinic Ester as Biodiesel Additives

2020 ◽  
Vol 71 (8) ◽  
pp. 21-26
Author(s):  
Elena-Emilia Oprescu ◽  
Cristina-Emanuela Enascuta ◽  
Elena Radu ◽  
Vasile Lavric
Keyword(s):  
Maximum Yield ◽  
Strength Distribution ◽  
Point Of View ◽  
Reaction Parameters ◽  
X Ray ◽  
Ethyl Levulinate ◽  
Ft Ir ◽  
Ir Analysis ◽  
Biodiesel Blend ◽  
Acid Strength Distribution

In this study, the SO42-/TiO2-La2O3-Fe2O3 catalyst was prepared and tested in the conversion of fructose to ethyl levulinate . The catalyst was characterized from the point of view of the textural analysis, FT-IR analysis, acid strength distribution, X-ray powder diffraction and pyridine adsorption IR spectra. The influence of the reaction parameters on the ethyl levulinate yield was study. The maximum yield of 37.95% in levulinate esters was obtained at 180 �C, 2 g catalyst and 4 h reaction time. The effect of ethyl levulinate addition to diesel-biodiesel blend in different rates, i.e, 0.5, 1, 2.5, 5 (w.t %) on density, kinematic viscosity and flash point was evaluated and compared with the European specification.

Synthesis of Dihydropyrimidinones (DHPMs) and Hexahydro Xanthene Catalyzed by 1,4-Diazabicyclo [2.2.2] Octane Triflate Under Solvent-Free Condition

2019 ◽  
Vol 16 (5) ◽  
pp. 776-786 ◽  
Author(s):  
Deepa ◽  
Geeta D. Yadav ◽  
Mohd J. Aalam ◽  
Pooja Chaudhary ◽  
Surendra Singh
Keyword(s):  
Ethyl Acetoacetate ◽  
Biginelli Reaction ◽  
Solvent Free ◽  
Efficient Catalyst ◽  
Solvent Free Condition ◽  
Solvent Free Conditions ◽  
Xanthene Derivatives ◽  
Different Temperatures ◽  
Flash Column Chromatography ◽  
Biginelli Condensation

Objective:DABCO salts were evaluated as catalysts for the Biginelli reaction between 4- methoxybenzaldehyde, urea and ethyl acetoacetate under solvent-free conditions. 1,4-Diazabicyclo [2.2.2] octane triflate was found to be a simple, inexpensive, highly efficient catalyst for Biginelli reaction for a variety aromatic aldehyde with urea and ethyl acetoacetate at 80°C afforded corresponding 3,4-dihydropyrimidinones in 50-99% yields after 30-120 minutes. 1,3-Cyclohexadione was used in place of ethyl acetoacetate in the absence of urea this methodology is giving hexahydro xanthene derivatives in good to excellent yields after 3-4 hours.Methods:DABCO salt 4 (5 mol%), 4-methoxybenzaldehyde (0.73 mmol) and urea (0.73 mmol) were stirred for 10 minutes at 80°C, then ethyl acetoacetate (1.5 equiv.) was added and reaction mixture was stirred at 80°C for specified time. The resulting solution was stirred continuously and progress of the reaction was followed by TLC. The crude reaction mixture was purified by flash column chromatography on silica gel (hexane/ethyl acetate (1:2)) to give pure desired product.Results:Reaction conditions of the Biginelli reaction were optimized using 4-methoxybenzaldehyde (0.73 mmol), urea (0.73 mmol), and ethyl acetoacetate (5 equiv.) as model substrates catalyzed by 1,4-Diazabicyclo [2.2.2] octane triflate (5 mol%) in a different solvents, screening of different catalysts and different temperatures. Neat condition was found to be the best for the Biginelli condensation and corresponding 3,4- dihydropyrimidinones was obtained in good to excellent yields. When the reaction was carried out with benzaldehyde derivatives and cyclohexane-1,3-dione in place of ethyl acetoacetate in the absence of urea, solely corresponding hexahydro xanthene derivatives were obtained in 61-91% yields.Conclusion:In conclusion, we have applied salts of 1,4-Diaza-bicyclo [2.2.2] octane as catalysts in the Biginelli condensation and corresponding 3,4-dihydropyrimidinones were obtained in 50- 99% yields under solvent free conditions. This methodology is having advantages like simple work-up; low loading of catalyst and reaction was performed at moderate temperature under solvent-free conditions.

Extraction of polyethylene glycols with dicarbolide solutions in nitrobenzene

1990 ◽  
Vol 55 (8) ◽  
pp. 1959-1967 ◽  
Author(s):  
Petr Vaňura ◽  
Pavel Selucký
Keyword(s):  
Polyethylene Glycol ◽  
Molecular Mass ◽  
Extraction Constant ◽  
Metal Extraction ◽  
Polyethylene Glycols ◽  
Relative Molecular Mass ◽  
Published Data ◽  
Average Molecular Mass ◽  
Peg 400 ◽  
Extraction Constants

The extraction of polyethylene glycol of average molecular mass 400 (PEG 400) with dicarbolide solution in nitrobenzene and of longer-chain polyethylene glycol, of average molecular mass 1 500 (PEG 1 500), with chlorinated dicarbolide solution in nitrobenzene was studied. During the extraction of PEG 400, the polyethylene glycol solvates the Horg+ ion in the organic phase giving rise to the HLorg+ species (L is polyethylene glycol). The obtained value of the extraction constant Kex(HLorg+) = 933 is consistent with published data of metal extraction. Extraction of PEG 1 500 was treated applying the simplified assumption that the thermodynamic behaviour of PEG 1 500 is the same as that of n molecules of polyethylene glycol with relative molecular mass 1 500/n, each solvating one cation. For this model, the value of n = 3.2 ± 1.1 and the values of the extraction constants of the HL1/n,org+ and HL2/n,org+ species were obtained by using the adapted program LETAGROP. This value of n is consistent with published extraction data in the presence of polyethylene glycol with a relative molecular mass from 200 to 1 000.

Electrogeneration of Conducting Poly(α-tetrathiophene). Effect of Solution Stirring and Detection of Linear Oligomers

2003 ◽  
Vol 68 (7) ◽  
pp. 1326-1344 ◽  
Author(s):  
Francesc Estrany ◽  
Ramon Oliver ◽  
Esther García ◽  
Esther Gualba ◽  
Pere-Lluís Cabot ◽  
...  
Keyword(s):  
Ion Pairs ◽  
Polymer Chains ◽  
Polymerization Process ◽  
Anodic Process ◽  
Cathodic Peak ◽  
Linear Chains ◽  
Monomer Solution ◽  
Ir Analysis ◽  
Microscopy Images ◽  
Tof Ms

The anodic oxidation of α-tetrathiophene on Pt was studied in a 1.0 mM monomer solution in 0.1 M LiClO4 in 45:35:20 acetonitrile/ethanol/DMF. Three consecutive oxidation peaks were detected by cyclic voltammetry, along with a cathodic peak related to the reduction of electroactive polarons formed during the first anodic process. Uniform, adherent, insoluble and black polymer films were obtained by chronoamperometry at 1.000 V vs Ag|AgCl corresponding to the first oxidation-polymerization process. Stirring of monomer solution promotes the production of polymer, favoring the oxidation of polymer chains with the incorporation of more doping ClO4- ions and ion pairs of Li+ClO4- in their monomeric units. The conductivity of the polymer obtained under stirring was three orders of magnitude higher than that synthesized from a quiescent solution. The scanning electron microscopy images also showed much more uniform films under stirring. This behavior points to the existence of less crosslinking in the polymer and the production of longer linear chains when the solution is stirred. IR analysis of these materials confirmed the formation of crosslinked chains with predominance of β-β linkages. Short linear oligomers such as the dimer, trimer and tetramer were detected in all polymers by MALDI-TOF-MS, thus showing a radical polycondensation as initial electropolymerization mechanism. A larger proportion of linear oligomers is formed under solution stirring.

scholarly journals Nanomechanical Molecular Mass Sensing Using Suspended Microchannel Resonators

Sensors ◽  
2021 ◽  
Vol 21 (10) ◽  
pp. 3337
Author(s):  
Alberto Martín-Pérez ◽  
Daniel Ramos ◽  
Javier Tamayo ◽  
Montserrat Calleja
Keyword(s):  
Molecular Mass ◽  
Mass Density ◽  
Applied Pressure ◽  
Atomic Mass ◽  
Liquid Sample ◽  
Mass Sensing ◽  
Average Molecular Mass ◽  
Fluid Properties ◽  
Molecular Masses ◽  
Microchannel Resonators

In this work we study the different phenomena taking place when a hydrostatic pressure is applied in the inner fluid of a suspended microchannel resonator. Additionally to pressure-induced stiffness terms, we have theoretically predicted and experimentally demonstrated that the pressure also induces mass effects which depend on both the applied pressure and the fluid properties. We have used these phenomena to characterize the frequency response of the device as a function of the fluid compressibility and molecular masses of different fluids ranging from liquids to gases. The proposed device in this work can measure the mass density of an unknown liquid sample with a resolution of 0.7 µg/mL and perform gas mixtures characterization by measuring its average molecular mass with a resolution of 0.01 atomic mass units.

scholarly journals Experimental Comparison of Innovative Composite Sorbents for Space Heating and Domestic Hot Water Storage

Crystals ◽  
2021 ◽  
Vol 11 (5) ◽  
pp. 476
Author(s):  
Vincenza Brancato ◽  
Larisa G. Gordeeva ◽  
Angela Caprì ◽  
Alexandra D. Grekova ◽  
Andrea Frazzica
Keyword(s):  
Silica Gel ◽  
Xrd Analysis ◽  
Complete Characterization ◽  
Operating Conditions ◽  
Hot Water ◽  
Experimental Comparison ◽  
Space Heating ◽  
Calorimetric Analysis ◽  
Domestic Hot Water ◽  
Composite Sorbents

In this study, the development and comparative characterization of different composite sorbents for thermal energy storage applications is reported. Two different applications were targeted, namely, low-temperature space heating (SH) and domestic hot water (DHW) provision. From a literature analysis, the most promising hygroscopic salts were selected for these conditions, being LiCl for SH and LiBr for DHW. Furthermore, two mesoporous silica gel matrixes and a macroporous vermiculite were acquired to prepare the composites. A complete characterization was performed by investigating the porous structure of the composites before and after impregnation, through N2 physisorption, as well as checking the phase composition of the composites at different temperatures through X-ray powder diffraction (XRD) analysis. Furthermore, sorption equilibrium curves were measured in water vapor atmosphere to evaluate the adsorption capacity of the samples and a detailed calorimetric analysis was carried out to evaluate the reaction evolution under real operating conditions as well as the sorption heat of each sample. The results demonstrated a slower reaction kinetic in the vermiculite-based composites, due to the larger size of salt grains embedded in the pores, while promising volumetric storage densities of 0.7 GJ/m3 and 0.4 GJ/m3 in silica gel-based composites were achieved for SH and DHW applications, respectively.

scholarly journals Cefquinome Controlled Size Submicron Particles Precipitation by SEDS Process Using Annular Gap Nozzle

2017 ◽  
Vol 2017 ◽  
pp. 1-8 ◽  
Author(s):  
Kefeng Xiao ◽  
Weiqiang Wang ◽  
Dedong Hu ◽  
Yanpeng Qu ◽  
Zhihui Hao ◽  
...  
Keyword(s):  
Particle Size ◽  
Xrd Analysis ◽  
Solution Concentration ◽  
Operating Conditions ◽  
Submicron Particles ◽  
Optimal Operating ◽  
Surface Appearance ◽  
Precipitation Temperature ◽  
Annular Gap ◽  
Feeding Speed

An annular gap nozzle was applied in solution enhanced dispersion by supercritical fluids (SEDS) process to prepare cefquinome controlled size submicron particles so as to enhance their efficacy. Analysis results of orthogonal experiments indicated that the concentration of solution was the primary factor to affect particle sizes in SEDS process, and feeding speed of solution, precipitation pressure, and precipitation temperature ranked second to fourth. Meanwhile, the optimal operating conditions were that solution concentration was 100 mg/mL, feeding speed was 9 mL/min, precipitation pressure was 10 MPa, and precipitation temperature was 316 K. The confirmatory experiment showed that D50 of processed cefquinome particles in optimal operating conditions was 0.73 μm. Moreover, univariate effect analysis showed that the cefquinome particle size increased with the increase of concentration of the solution or precipitation pressure but decreased with the increase of solution feeding speed. When precipitation temperature increased, the cefquinome particle size showed highest point. Moreover, characterization of processed cefquinome particles was analyzed by SEM, FT-IR, and XRD. Analysis results indicated that the surface appearance of processed cefquinome particles was flakes. The chemical structure of processed cefquinome particles was not changed, and the crystallinity of processed cefquinome particles was a little lower than that of raw cefquinome particles.

CHARACTERIZATION OF HYDROXYAPATITE/TI6AL4V COMPOSITE POWDER UNDER VARIOUS SINTERING TEMPERATURE

2015 ◽  
Vol 75 (7) ◽  
Author(s):  
Amir Arifin ◽  
Abu Bakar Sulong ◽  
Norhamidi Muhamad ◽  
Junaidi Syarif
Keyword(s):  
Mechanical Properties ◽  
Composite Powder ◽  
Sintering Temperature ◽  
Physical And Mechanical Properties ◽  
Xrd Analysis ◽  
X Ray Diffraction ◽  
Different Temperatures ◽  
Two Phases ◽  
Work Interaction

Hydroxyapatite (HA) has been widely used in biomedical applications due to its excellent biocompatibility. However, Hydroxyapatite possesses poor mechanical properties and only tolerate limited loads for implants. Titanium is well-known materials applied in implant that has advantage in mechanical properties but poor in biocompatibility. The combination of the Titanium alloy and HA is expected to produce bio-implants with good in term of mechanical properties and biocompatabilty. In this work, interaction and mechanical properties of HA/Ti6Al4V was analyzed. The physical and mechanical properties of HA/Ti6Al4V composite powder obtained from compaction (powder metallurgy) of 60 wt.% Ti6Al4V and 40 wt.% HA and sintering at different temperatures in air were investigated in this study. Interactions of the mixed powders were investigated using X-ray diffraction. The hardness and density of the HA/Ti6Al4V composites were also measured. Based on the results of XRD analysis, the oxidation of Ti began at 700 °C. At 1000 °C, two phases were formed (i.e., TiO2 and CaTiO3). The results showed that the hardness HA/Ti6Al4V composites increased by 221.6% with increasing sintering temperature from 700oC to 1000oC. In contrast, the density of the composites decreased by 1.9% with increasing sintering temperature. 

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