Rheological Modification for Asphaltic Materials Using a Mixture (Poly carbonate: Poly Methyl Methacrylate) and Microwave Radiation

Obtaining asphalt that suits the nature of the countries it is used in, is of great importance. Asphalt constitutes an important component in the paving of roads, mastic and flattening substance. This study was included the modification of the asphaltic material by the use of a mixture of polycarbonate and polymethyl methacrylate after crushed to obtain low molecular weight. The study included two paths: In the first asphaltic materials was treated with different percentages of a mixture in the presence of anhydrous aluminium chloride (0.06%of weight) as a catalyst for this reaction. The mixture was heated at 150° for 30 minutes. In the second path, the process of mixing was performed with the existence of a 360 watt microwave radiation for 15 minutes. The process of mixing was repeated in the presence of sulphur (1% of weight) instead of anhydrous aluminium chloride and under the same conditions. Properties of the original and modified asphalts were determined, and this included the measurement of ductility, penetration, softening point, penetration index and calculating the percentage of separated asphaltenes. Additionally, Marshal test, chemical Immersion test and aging were measured for some of the samples. Good samples that can suit Iraq's climate were obtained from this study.

Synthesis of 3-Ferrocenyl Isocoumarins

The derivatives of 3-ferrocenyl isocoumarin were synthesized by the condensation of substituted homothphalic anhydride with ferrocene using phosphoric acid or anhydrous aluminium chloride as cyclising agent. Substituted homophthalic acid did not condense with ferrocene so homophthalic acids were converted into their anhydride and then allowed to react with ferrocene in the presence of polyphosphoric acid or in the presence of anhydrous aluminium chloride using dichloromethane as the solvent to give 3-ferrocenyl isocoumarins. 7-Methoxy, 6-methyl, 5,7-dihydroxy, 6,7-dimethoxy and 5,7-dimethoxy derivatives of 3-ferrocenyl isocoumarin were synthesized. All the compounds were characterised by melting point determination, elemental and spectral analysis.

Development of a mathematical model for alkylation of m-cresol with α-methylstyrene using anhydrous aluminium chloride

Alkylaromatic compounds such as alkylphenols are the most wide spread and efficient material due to its broad practical utilization in different arenas including antioxidants, stabilizers for fuels, lubricating oils, polymeric materials and so on. In this work, (2-phenylpropan-2-yl) m-cresol with high yield was prepared from the reaction between m-cresol and _-methylstyrene in the presence of anhydrous aluminium chloride catalyst. Plackett-Burman design was applied for screening significant variables, such as, temperature, molar ratio of m-cresol to _-methylstyrene, time of reaction and amount of catalyst etc. to determine an optimum condition for the production of (2-phenylpropan-2-yl) m-cresol. Moreover, a 23 Yates pattern factorial design was used to develop a mathematical model to predict the yield of alkylation of m-cresol with _-methylstyrene. Analyses of the results revealed that temperature, molar ratio and amount of catalyst were the main effective variables. The products were characterized by FT-IR, UV-visible and 1H NMR spectroscopy. The adequacy of the suggested model was checked up. The experimental yields exhibited good agreement with the predicted yields designed by the mathematical model. Hence, (2-phenylpropan-2-yl) m-cresol has the potential to be used as an industrially important compound in various applications. Bangladesh J. Sci. Ind. Res.54(3), 195-202, 2019

Alkylation of Ethylbenzene with Cyclohexylchloride: A Statistical Study

A mathematical model was developed for the alkylation of ethylbenzene with cyclohexyl chloride in the presence of anhydrous aluminium chloride as a catalyst using the Yates Pattern experimental design. The variables chosen for the study were temperature, molar ratio of ethylbenzene to cyclohexyl choloride and amount of anhydrous aluminium chloride. The critical response was the yield of cyclohexylethylbenzene. Main effects as well as interaction effect of molar ratio of ethylbenzene to cyclohexyl chloride and amount of catalyst were statistically significant. The adequacy of the suggested model was checked.DOI: http://dx.doi.org/10.3329/dujs.v60i1.10340 Dhaka Univ. J. Sci. 60(1): 71-76 2012 (January)

SYNTHESIS OF C-METHYL-4,10,16,22-TETRAMETHOXYCALIX[4]ARENE FROM PHENOL USING BF3-METHANOL AS THE CATALYST

C-Methyl 4,10,16,22-tetramethoxycalix[4]arene has been synthesized from phenol. The reaction performed consisted of methylation of phenol, acetylation of methyl phenyl ether, reduction of p-methoxyacetophenone, and cyclization of p-methoxy-(1-hydroxyethyl)benzene to form C-methyl-4,10,16,22-tetramethoxycalix[4]-arene using BF3-methanol as the acid catalyst. Methylation of phenol was done by reacting phenol with solution of NaOH to generate sodium phenoxide salt. This mixture was strirred at reflux for 0.5 hours. Dimethyl sulphate was added and the reflux was continued for 2,5 hours. The product obtained was methyl phenyl ether, which was found as a colorless liquid in 99.0% yield. Acetylation of methyl phenyl ether was carried out in chloroform using acetic anhydride as the acetylating agent and anhydrous aluminium chloride as the catalyst. The addition of acetic anhydride and anhydrous aluminium chloride was done in two portions. The first portion was 0.967 g of acetic anhydride and 1.4 g of anhydrous aluminium chloride. The second portion was 0.54 g of acetic anhydride and 0.6 g of anhydrous aluminium chloride. The product obtained was found as a reddish yellow liquid in 69.6% yield. Reduction of p-methoxyacetophenone as the acetylation product was done using NaBH4 in ethanol at reflux for 2.5 hours. From this reaction, p-methoxy-(1-hydroxyethyl)benzene was obtained as a brown viscous liquid in 44.9% yield. Cyclization of p-methoxy(1-hydroxyethyl)benzene was done using BF3-methanol as the acid catalyst for two days at room temperature. The product obtained from this cyclization was found as a brown very viscous liquid in 87.3% yield. Identification of reaction products were carried out using Infra Red (IR) Spectrophotometer, Proton Nuclear Magnetic Resonance (1H NMR) spectrometer and Gas Chromatography-Mass spectroscopy (GC-MS). Keywords: synthesis, calix[4]arene, cyclization, and catalyst.

Synthesis and Properties of Linear Chloroacetylated Polystyrene

Polystyrene (PS) was synthesized by emulsion polymerization. The linear chloroacetylated PS was prepared high effectively by Friedel-Crafts acetylation of PS using chloroacetyl chloride and anhydrous aluminium chloride as chloroacetylation reagent and catalysts, respectively. The structure of chloroacetyl group is similar to that of chloromethyl group. In this method, carcinogenic compound (chloromethyl ether etc.) was avoided and the reactions of secondary cross link and multi-substitute could be eliminated. The resultant polymers were characterized by Fourier transform infrared spectrometery (FTIR) and thermogravimetric analysis. The effects of reaction conditions on chloroacetylation were studied, and the optimum reaction conditions were obtained. Chloroacetyl group was introduced into benzene ring of PS because of the appearance of the absorption peaks at 1695cm-1 (due to C=O bonds) and 644cm-1 (due to C-Cl bonds) in the FTIR spectrum. The thermal stability of the chloroacetylated PS was decreased with increasing chloroacetyl group. Moreover, there were two decomposing stages. The glass transition temperature of chloroacetylated PS increased with substitution value increasing. The effects of the reaction conditions such as reaction temperature, the solvent amount and the concentration of chloroacetyl chloride and anhydrous aluminium chloride on the chloroacetylation of PS were obvious. The certain loading can be controlled when it is lower than the maximum loading of chloroacetylated PS. The reaction condition is gentle and the operation is safe, simple and economical so that Friedel-Crafts acetylation of PS is an ideal reaction method.