- Synthesis and characterization of calcium methoxide as heterogeneous catalyst for trimethylolpropane esters conversion reaction
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Trimethylolpropane (TMP) esters are potential biodegradable basestock for biolubricant. In order to attain environmental benignity, attention has been focused on utilizing heterogeneous catalysts for production of TMP esters. Alkaline homogeneous catalysts tend to react with free fatty acids to produce unwanted soap, thus reducing the overall product yield. This study had focused on the synthesis of calcium methoxide and investigating its potential as heterogeneous catalyst for the transesterification of TMP and palm oil methyl esters (POME) to TMP esters. The performance of synthesized calcium methoxide as a catalyst was examined by characterizing it through some instrumental techniques. X-ray diffraction (XRD) showed calcium methoxide has been successfully synthesized. Scanning electron microscopy (SEM) displayed thermally resistant surface structure with good porosity; BET showed high surface area; particle size analysis evidenced reasonable size of catalyst particles; and thermogravimetry (TGA) revealed good thermal stability of synthesized calcium methoxide. Moreover, the catalyst was found to possess mesoporous surface by pore size analysis through Barrett-Joyner-Halenda (BJH) method. The results of transesterification reaction indicated satisfactory catalytic activity of synthesized calcium methoxide and the TMP triesters yield obtained was 80.35% after 2 h, 87.48% after 4 h, 91.30% after 6 h and 92.38% after 8 h reaction time.
- Masood, Hassan,Yunus, Robiah,Choong, Thomas S.Y.,Rashid, Umer,Taufiq Yap, Yun H.
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- Study of challenging calcium alkoxides in solution by electrospray ionization mass spectrometry (Part 1)
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Electrospray ionization was applied on calcium alkoxides studying the most suitable operative conditions for their detection/identification. To reach this aim, calcium methoxide and ethylate were obtained by two different synthetic pathways, in order to understand their possible different aggregation states. The reaction mixture shows the presence of a supernatant and of a precipitate poorly soluble in most organic solvents. The purpose of this preliminary study is to understand the qualitative differences between the precipitated species and the ones in solution by analyzing both of them with the same analytical method. The electrospray ionization (ESI) operating conditions (voltages, temperatures, solvents) allow not only the detection of single species but also the study of clusters present in solution. Particular attention was paid to establishing the role of ESI conditions in the formation of the detected species. Experiments performed at different sprayer voltages (1 kV, 2 kV, 3 kV and 4 kV) proved that ESI does not perturbate the equilibria present in the original solution, demonstrating that the technique can be a useful tool to achieve information on this class of compounds. IM Publications LLP 2013 All rights reserved.
- Peruzzo, Valentina,Chiurato, Matteo Andrea,Tomasin, Patrizia,Traldi, Pietro,Favaro, Monica
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- New calcium alkoxides for consolidation of carbonate rocks. Influence of precursors' characteristics on morphology, crystalline phase and consolidation effects
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New ambient temperature liquid calcium alkoxides, [Ca(O(CH 2CH2O)3CH3)2] (1) and [Ca(O(CH2CH2O)3CH2CH 3)2] (2), together with [Ca(OCH2C(CH 3)3)2] (3), were synthesised by reaction of ammonia-activated calcium with the appropriate alcohol. Their potentiality as stone consolidant products was investigated and compared with those of other alkoxides: [Ca(OCH2CH3)2(CH3CH 2OH)4] (4), [Ca(OCH3)2] (5), [{Ca(OCH2CH2OCH3)2}9] (6), already described in the literature. Reaction of 1-3 with the atmosphere was studied, final products analysed and kinetic pathways investigated. The reaction produces CaCO3 and the vaterite/calcite ratios observed in the coatings generated from isopropyl alcohol solutions of 1-6 were found to considerably vary with the alkoxide precursor, which has a strong influence also on the morphology of the produced films. Furthermore, their efficiency as stone consolidants was tested by ultrasound measurements. The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2012.
- Ossola, Franco,Tomasin, Patrizia,De Zorzi, Chiara,El Habra, Naida,Chiurato, Matteo,Favaro, Monica
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- Comparison of homogeneous and heterogeneous catalysts in biodiesel production from Pongamia pinnata oil
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Biodiesel was prepared by transesterification of Pongamia pinnata (P. pinnata) oil using potassium hydroxide (KOH) as homogeneous catalyst and synthesized calcium methoxide [Ca(OCH3)2] as heterogeneous catalyst. The Ca(OCH3)2 was synthesized from quick lime and characterized by scanning electron microscopy, X-ray diffraction, attenuated total reflection fourier transform, energy dispersive X-ray spectroscopy and BET surface area analysis to evaluate its performance. The parameters affecting the fatty acid methyl ester (FAME) content such as catalyst concentration, methanol to oil molar ratio and reaction time were investigated. Under optimized reaction condition, it was found that the 99.5 % of FAME conversion using KOH catalyst was achieved with 11:1 of methanol to oil molar ratio, 1.50 % wt of catalyst amount and 1 h of reaction time. The Ca(OCH3)2 catalyst was obtained the 98.04 % of FAME conversion with 15:1 of methanol to oil molar ratio, 3 % wt of catalyst amount, 3 h of reaction time at 65 ± 0.5 °C of reaction temperature and 750 rpm of stirring rate on both catalysts. The result of the % FAME conversion, which determined by 1H NMR, suggested that Ca(OCH3)2 was the promising heterogeneous catalyst in replacing conventional homogeneous catalyst.
- Panpraneecharoen,Punsuvon,Puemchalad
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- Hydrothermal effect on synthesis, characterization and catalytic properties of calcium methoxide for biodiesel production from crude Jatropha curcas
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Hydrothermal synthesis is a well-suited approach for preparing bulk metal catalysts with high purity as it is cost-effective and easy to control in terms of temperature and time. In the current study, an effective catalyst for transesterification of high fatty acid content of crude Jatropha curcas oil (JCO) was appraised. Calcium methoxide (Ca(OCH3)2) has been successfully synthesized via a green and economical hydrothermal process at different synthesis times. CaO was used as a precursor as it is abundant, inexpensive and environmentally friendly. Ca(OCH3)2 can form on the surface of CaO and its active basic surface is very well developed. This facile experimental strategy without any surfactant or template produced porous Ca(OCH3)2 with a high surface area and high basicity, which leads to a superior catalytic reaction and is a promising alternative for short-reaction-time solid-based catalysts in biodiesel production in terms of excellent transesterification performance and long durability. The performance of synthesized Ca(OCH3)2 was examined by characterizing it using analytical techniques such as TG-DTA, XRD, BET, FT-IR, TEM and SEM. Ca(OCH3)2 catalysts had three types of morphologies, i.e. (a) irregular round shape particles, (b) a well arrangement of plate-like structures with rough surface and (c) a cluster of tiny plate-like architectures with smooth surfaces. The correlation between synthesis time, surface area and morphology of catalysts and the biodiesel yield was studied. Ca(OCH3)2 was able to maintain the FAME content above 86% after a fifth cycle, at optimum reaction conditions of 2 h reaction time, 12:1 methanol/oil molar ratio, 2 wt% catalyst loading and 65°C reaction temperature. Ca(OCH3)2 is a solid heterogeneous catalyst for the transesterification reaction of non-edible Jatropha curcas oil for biodiesel production. The catalyst can be separated easily from the reaction mixture and reused to give a consistent transesterification activity.
- Teo, Siow Hwa,Taufiq-Yap, Yun Hin,Rashid, Umer,Islam, Aminul
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- Method for preparing cyclopropylamine midbody cyclopropanecarboxylic acid methyl ester
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The invention discloses a method for preparing cyclopropylamine midbody cyclopropanecarboxylic acid methyl ester. First in a sealed reaction kettle, methanol is added dropwise into calcium carbide, togenerate calcium methoxide and acetylene; gamma-chloro methyl butyrate is added into calcium methoxide at 60-120 DEG C, the temperature is controlled to be constant in the reaction process, methanolgenerated in the process is collected, and the cyclopropanecarboxylic acid methyl ester is obtained through distillation. The method is simple in process, types of raw materials necessary for production are fewer, some of the raw materials can be reused, the yield is high, the quality is good, and the method is safe and environmentally friendly.
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Paragraph 0004; 0019-0032
(2018/03/26)
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- Process for the conversion of glycerol and catalytically active material suitable therefore
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The invention is directed to a process for the conversion of glycerol to produce di-glycerol or higher polyglycerols, which process comprises the steps of converting glycerol at a suitable temperature in the presence of a catalytically active material comprising calcium oxide having a basicity, defined as pKBH+, of between 11 and 15, and recovering di-glycerol and/or higher polyglycerols from the mixture thereby formed.
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Page/Page column 4
(2008/12/08)
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- Production of alcoholates
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A process that can be used for producing an alkali metal alcoholate such as sodium alcoholate or for removing a residual mixture containing alkali metal and alkaline earth metal from a vessel such as, for example, a tank car or storage tank used in manufacturing an alkali metal is disclosed. The process comprises contacting a mixture, which comprises an alkali metal and an alkaline earth metal, with an alcohol under a condition sufficient to produce an alkali metal alcoholate and alkaline earth metal alcoholate and, optionally, separating and recovering the alkali metal alcoholate.
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Page column 5-6
(2008/06/13)
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