Transesterification Temperature Research Articles

Optimization of Grafted Fibrous Polymer as a Solid Basic Catalyst for Biodiesel Fuel Production

Grafted fibrous polymer with quaternary amine groups could function as a highly-efficient catalyst for biodiesel fuel (BDF) production. In this study, the optimization of grafted fibrous polymer (catalyst) and transesterification conditions for the effective BDF production was attempted through a batch-wise transesterification of triglyceride (TG) with ethanol (EtOH) in the presence of a cosolvent. Trimethylamine was the optimal quaternary amine group for the grafted fibrous catalyst. The optimal degree of grafting of the grafted fibrous catalyst was greater than 170%. The optimal transesterification conditions were as follows: The optimal molar quantity of quaternary amine groups, transesterification temperature, molar ratio of TG and EtOH, and primary alkyl alcohol were 0.8 mmol, 80°C, 1:200, and 1-pentanol, respectively. The grafted fibrous catalyst could be applied to BDF production using natural oils. Furthermore, the grafted fibrous catalyst could be used repeatedly after regeneration involving three sequential processes, i.e., organic acid, alkali, and alcohol treatments, without any significant loss of catalytic activity.

Influence of nitrogen fertilization on physical and chemical properties of fatty acid methyl esters from Brassica napus oil

Biodiesel is a biodegradable fuel that originates from a variety of oleaginous raw materials, although most studies have been traditionally based on vegetable oils. Rapeseed (Brassica napus) is the raw material most widely used in the production of biodiesel in temperate climate, i.e. central Europe, due to its physical properties and the content of oleic acid of its oil. However, this plant needs nitrogen fertilization at different stages of growth to achieve an optimal oilseed production, thus increasing costs. For this reason, the aim of this work was to find out the importance of nitrogen fertilization through the study of its influence on the physicochemical properties of both rapeseed oil and its biodiesel. Rapeseed variety “Lucia” was used to carry out this research. The oil from each sample of rapeseed was extracted using mechanical processing (cold pressed) and analyzed according to European standards. Results indicate some differences on the acid value and fatty acid composition among the samples of oil depending on the level of nitrogen fertilization. With respect to the fatty acid composition, the sample 0–0 (no nitrogen fertilization) showed a decrease on oleic acid compared to the rest of samples. With the aid of an experimental design, the optimum transesterification parameters were also determined. Results indicate that the temperature of the reaction and KOH increased for the sample 0–0, while less amount of methanol-to-oil ratio was needed. Finally the most important physical and chemical properties of biodiesel were analyzed. It may be concluded that nitrogen fertilization influences oil properties. Moreover, despite of the saving during the cultivation, when the crops are not fertilized there is a rise in biodiesel production costs due to an increase of the reaction transesterification temperature and KOH needs, besides the reduction in seeds production.

Room temperature transesterification of soybean oil to biodiesel catalyzed by rod-like Ca SiO+2 solid base

Rod-like CaxSiOx + 2 catalysts were synthesized by using one-pot hydrothermal method. Catalysts calcined at 550 °C were used in the transesterification reaction of soybean oil with methanol. Under methanol reflux condition, FAME yields of 82% and 95% were achieved on Ca4SiO6 in a reaction time of 1 and 2 h, separately. Also, the FAME yields on different CaxSiOx + 2 catalysts were correlated with their basic properties. Besides, a FAME yield of ca. 80% can be achieved under room temperature over Ca4SiO6 catalyst.

New Denatonium Benzoate/tin Heterogeneous Catalyst to Obtain Biodiesel via Low Temperature Transesterification Process(LTTP)

Biodiesel was synthesized using waste chicken oil and ethyl alcohol as reactives as well as denatonium benzoate and tin particles as catalysts in 500 mL three neck flask. The reaction mixtures were mechanically stirred at 200 rpm during 15 minutes at 30, 40, 50, y 60 º C, after that the products were filtered trough a 400 m mesh an then casted in a separating funnel in order to obtain two layers corresponding to glycerol and Biodiesel. The tin catalyst particles were observed by optical microscopy. The biodiesel and glycerol were characterized using refractive index, pH, Fourier transformer infrared spectrometry (FTIR), while the viscosity was determined in a Brookfield viscosimeter and density using a picnometer. The results suggest that at a low concentration of denatonuim benzoate (7 ppm) the reaction will occur only if tin is present at all test temperatures. The pH of biodiesel obtained was 6, similar to petrodiesel used commonly in diesel motors.

Transesterification of edible and non-edible oils over basic solid Mg/Zr catalysts

A series of Mg–Zr catalysts with varying Mg to Zr ratios was prepared by co-precipitation method. These catalysts were characterized by BET surface area, X-ray diffraction, X-ray photo electron spectroscopy and temperature programmed desorption of CO 2. The catalytic activity of these catalysts was evaluated for the room temperature transesterification of both edible and non-edible oils to their corresponding fatty acid methyl esters. The catalyst with Mg/Zr (2:1 wt./wt.%) exhibited exceptional activity towards transesterification reaction within short reaction time. The effects of different reaction parameters such as catalyst to oil mass ratio, reaction temperature, reaction time and methanol to oil molar ratio were studied to optimize the reaction conditions. The reasons for the observed activity of these catalysts are discussed in terms of their basicity and other physico-chemical properties.

Increased yields in biodiesel production from used cooking oils by a two step process: Comparison with one step process by using TGA

Short chain alcohol esters of fatty acids can be used as diesel fuel. In this study, one step and two step base catalyzed room temperature transesterification reaction of used cooking oil was compared. In the two step base catalyzed process, for 1000 g of used cooking oil 4.2 g NaOH and 140 ml MeOH was used in the first step and 1.8 g NaOH and 60 ml MeOH was used in the second step. All reactions were done at 25 °C; the effects of water content and suspended particles on the yield were studied. The yields were easily determined by Thermo Gravimetric Analysis (TGA) instead of the usual Gas chromatography (GC) and the viscosity of products was measured by Ubbelohde type viscosimeter. It was found that two step processes gives a better yield (96%) than the one step process (86%).

Processing characteristics of PET/PEN blends, part 2: Rheology and degradation kinetics

AbstractBlends and copolyesters of poly(ethylene terephthalate)/poly(ethylene 2,6‐naphthalene dicarboxylate), PET/PEN, have shown promise in high performance container applications. In the first part of this series on the processing characteristics of PET/PEN blends, we investigated the applicability of reaction kinetics to predict the critical transesterification temperature during processing and the influence of the equilibrium melting point of the miscible blends on the critical transesterification temperature. In the present work, we have studied both the rheology and degradation kinetics of the blends as a function of material composition. Melt viscosity loss was measured as a function of time and temperature. Activation energies for degradation were calculated from experimental data. Results show that blends containing a minimum of 10% PEN by weight are as stable as PEN in terms of thermal and thermal‐oxidative degradation. Addition of low amounts of PEN to PET causes a depression in melt viscosity. A critical composition of 10% PEN by weight is required before an increase in blend viscosity is observed. © 2003 Wiley Periodicals, Inc. Adv Polym Techn 22: 147–154, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.10045

Processing characteristics of PET/PEN blends, part 1: Extrusion and transesterification reaction kinetics

AbstractBlends of poly(ethylene terephthalate)/poly(ethylene 2,6‐naphthalene dicarboxylate) (PET/PEN) have exhibited properties that are of commercial interest to the packaging industry. Melt processing of PET with PEN results in transesterification reactions. The blend properties are controlled by the kinetics of these reactions. The chemical kinetics equations have been modified to predict theoretical processing temperatures required for different blend compositions to achieve critical levels of transesterification. These values are found to be in close agreement with the experimentally observed values obtained for blends processed in a twin‐screw extruder. The critical transesterification temperature is dependent on the equilibrium melting point of the miscible blend and the nature of the PET and PEN resins used for preparing the blend. © 2003 Wiley Periodicals, Inc. Adv Polym Techn 22: 137–146, 2003; Published online in Wiley InterScience (www.interscience.wiley.com). DOI 10.1002/adv.10044

Synthesis and characterisation of fully aromatic lactamimide-containing polyesters

Three novel aromatic naphthalene-lactamimide monomers were synthesised and polymerised via high temperature transesterification in melt to produce fully aromatic lactamimide-containing polyesters. Molecular modelling of the synthesised polymers showed that they should possess better solubility compared to the respective polyimides due to the more flexible polymer chain. Some of the synthesised polymers are soluble in chloroform and show medium molecular weight. Polymers were found to be rather thermostable exhibiting T 10 up to 510°C. Aromatic polylactamimides did not show strong photoemission, probably due to Loose-Bolt quenching, however, the third order non-linear optical susceptibilities of the polymers were up to 9. 1 × 10 -11 esu, which is 5 times that of polylactamimides bearing aliphatic substituents and comparable with those of polydiacetylenes, polyanilines and polythiophenes known for their non-linear optical properties.

Polymers from coumarins, 2. Design and synthesis of novel main‐ and side‐chain coumarin‐containing polymers

AbstractTwo novel coumarin‐containing monomers, 3,3′‐bis(ethoxycarbonyl)‐6,6′‐bicoumarin (3) and 7‐[(2‐norbornenyl)methoxy]coumarin (7), were prepared and characterized. They give polymers with Mw up to 350 000 and are soluble in common organic solvents. Polymers were prepared by high temperature transesterification reaction (poly‐3) and metathesis polymerization (poly‐7). Poly‐10 was prepared by direct activated polymidation of 6‐aminocoumarin‐3‐carboxylic acid (10). All polymers are amorphous with glass transition Tg of 121 and 64°C for poly‐3 and poly‐7, respectively. High optical quality films can be prepared by solution casting, and in the case of poly‐3 fibers can be drawn from the melt. All polymers show strong photoemission in the region from violet (poly‐7) to blue‐green (poly‐10) (410–510 nm). An electroluminescent device was fabricated from poly‐3 with turn‐on voltage of 4 V.

Determination of fatty acid composition of amaranthus species

AbstractFatty acid compositions of the seed oils from eighteen vareties of amaranthus species have been determined after room temperature transesterification. Consistent with earlier studies, wide variations in the fatty acid composition are reported, and appear to be agronomically related. All variaties show significant levels (2–5%) of squalene and a combined linoleic acid and olaic acid occurrence of between 70–‐80%. This study represents the frist reported fatty acid composition of grain amaranthus cultivated in West Africa.

Allyl esters and allyl epoxy esters from crambe oil

AbstractRoom temperature transesterification of crambe oil with allyl alcohol gave allyl esters previously prepared by hydrolysis of the oil and reesterification of the mixed acids at elevated temperatures. Treating the esters with m‐chloroperbenzoic acid in the presence of sodium bicarbonate resulted in the selective epoxidation of ethylenic bonds and suppression of side reactions. Bifunctional allyl epoxy esters produced in 88% overall yield by this method contain 5.08% oxirane oxygen and an unsaturation equivalent to 91% allyl group; they are prospective monomers for various types of polymerization.

A Simple and Rapid Method for the Preparation of Methyl Esters of Fats in Milligram Amounts for Gas Chromatography

A method is described which allows the transesterification of 0.5–1 milligram of milk fat and a fraction of a milligram of a wide range of natural fats. The method insures complete recovery of both short chain and unsaturated fatty acid methyl esters, and also permits the use of a reasonable sensitivity of the gas-chromatograph to insure base line stability. The tranesterifying reagent used consists of 15% methanolic sodium methoxide solution 0.5 N, 60% petroleum ether and 25% diethyl ether which forms a one phase system at room temperature. Twenty-five μL of this reagent is used for room temperature transesterification of up to 4mg fat. The reaction mixture is diluted with 25μL of petroleum ether before injection into the gas-chromatograph. The method was checked by TLC for completion of transesterification and the transesterifying capacity of the reagent. Several fats, lard, cocoa butter, corn oil and tripalmitin gave satisfactory results, indicating the applicability of the method for all milk fat fractions and a wide range of natural fats. The fatty acid composition of a milk fat sample from methyl esters prepared by the present method compared very well with those of the sealed tube method, (deMan 1964). The weight response factors for milk fat major fatty acid methyl esters were determined.