scholarly journals Optimization of process conditions for catalytic alkylation of isomeric cresols with cyclohexene

2012 ◽  
Vol 47 (2) ◽  
pp. 153-160
Author(s):  
Mohammad Kamruzzaman ◽  
Ashequl Alam Rana ◽  
Manoranjan Saha

Alkylation of isomeric cresols with cyclohexene in presence of perchloric acid as catalyst was studied and cyclohexyl cresols obtained in high yield. The effects of the variation of reaction parameters such as temperature, molar ratio of cresol to cyclohexene, amount of perchloric acid and time of reaction were investigated. The yield of the products increased with the increase of each of the above-mentioned parameters. Optimum yield (97.6% for cyclohexyl m-cresol; 95.4% for 2-cyclohexyl-4-methylphenol and 91.2% for cyclohexyl o-cresol) of the products were obtained under the reaction conditions of a temperature of 140ºC; an 8-6:1 molar ratio of cresol to cyclohexene, a 5% by weight perchloric acid of cresol, a 2 h time of addition of cyclohexene and a 2 h time of stirring of the reaction mixture. Considering the yields of cyclohexyl cresols and ease of purifications, the above mentioned conditions were accounted as optimum for the alkylation of isomeric cresols with cyclohexene in the presence of perchloric acid.   DOI: http://dx.doi.org/10.3329/bjsir.v47i2.11446   Bangladesh J. Sci. Ind. Res. 47(2), 153-160, 2012  

2012 ◽  
Vol 60 (2) ◽  
pp. 195-198 ◽  
Author(s):  
Md. Ashaduzzaman ◽  
A. M. Sarwaruddin Chowdhury ◽  
Manoranjan Saha

Cyclohexylcresols were synthesized in high yield by the alkylation of cresols with cyclohexanol in the presence of perchloric acid as catalyst. The effects of the variation of temperature, molar ratio of cresol to cyclohexanol, time of reaction and amount of catalyst on the reactions were also extensively studied. The products were confirmed by spectral means and physicochemical constants.DOI: http://dx.doi.org/10.3329/dujs.v60i2.11503 Dhaka Univ. J. Sci. 60(2): 195-198, 2012 (July)


2012 ◽  
Vol 60 (2) ◽  
pp. 199-202
Author(s):  
Md. Ashaduzzaman ◽  
Dipti Saha ◽  
Manoranjan Saha

2-Cycloalkyl-4-chlorophenols were synthesized in high yield by the alkylation of p-chlorophenol with cyclopentanol and cyclohexanol in the presence of perchloric acid as catalyst. The effects of the variation of temperature, molar ratio of p-chlorophenol to cycloalcohols, time of reaction and amount of catalyst on the reactions were also studied.DOI: http://dx.doi.org/10.3329/dujs.v60i2.11504 Dhaka Univ. J. Sci. 60(2): 199-202, 2012 (July)


2012 ◽  
Vol 60 (1) ◽  
pp. 79-85
Author(s):  
Mohammad Kamruzzaman ◽  
Ashequl Alam Rana ◽  
Md Zahangir Alam ◽  
Manoranjan Saha

Alkylation of o-cresol with cyclohexene in the presence of perchloric acid as catalyst was studied statistically with a three-factored experimental design. Factorial design was employed to study the effects of single factors and the effects of their interactions on the yield of alkylation. Reaction temperature, molar ratio of o-cresol to cyclohexene and amount of perchloric acid were considered as the major variables. A mathematical model was derived to calculate the predicted yield of alkylation of o-cresol with cyclohexene in the presence of perchloric acid under certain reaction conditions and cyclohexyl o-cresol was obtained in high yield. The adequacy of the suggested model was checked up and the discrepancies between the experimental and calculated values did not exceed 1.52%. An optimum yield (89.5%) of the product was obtained under the reaction conditions of a temperature of 140º C; a 6:1 molar ratio of ocresol to cyclohexene and a 5% by weight perchloric acid of o-cresol.DOI: http://dx.doi.org/10.3329/dujs.v60i1.10342  Dhaka Univ. J. Sci. 60(1): 79-85 2012 (January)


2017 ◽  
Vol 79 (7) ◽  
Author(s):  
Ida Nurhazwani Abd Rahman ◽  
Fatin Myra Abd Manan ◽  
Nur Haziqah Che Marzuki ◽  
Naji A. Mahat ◽  
Nursyafreena Attan ◽  
...  

Being the prevailing approach for producing esters such as butyl butyrate, the use of chemical route has been linked to numerous disadvantages. Hence, a green alternative method for higher yield production of butyl butyrate by esterification reaction utilizing Novozyme 435 as biocatalysts in a solvent-less system may prove useful. Such approach can be further improved by optimizing the relevant reaction parameters using the Response Surface Methodology by the Box-Benkhen Design attempted in this present study. The reaction parameters evaluated were: substrate molar ratio, time and temperature, and the response of each parameter was measured as percentage conversion yield. Using the Design Expert 7.1.6 optimization functions, the two sets of optimum conditions selected viz. [i] molar ratio butyric acid:butanol 1:3.93, 9.93 h at 56.09°C and [ii] molar ratio butyric acid:butanol 1:3.35, 9.79 h at 53.90°C had afforded the highest yield of butyl butyrate i.e. 99.62% and 99.55%, respectively. The ester product obtained from the reaction were confirmed as butyl butyrate by FTIR and GC. Therefore, the results substantiated the applicability of the RSM prediction technique as well as efficacy of Novozyme 435 as biocatalysts in the high yield solvent-less synthesis of butyl butyrate, adhering to the philosophy of Green Chemistry.


1989 ◽  
Vol 54 (9) ◽  
pp. 2375-2385 ◽  
Author(s):  
Peter Gemeiner ◽  
Eva Hrabárová ◽  
Magdaléna Zacharová ◽  
Albert Breier ◽  
Milan J. Beneš

Hydrophobization of bead cellulose is described, carried out by its alkylation with 1,2-epoxy-3-phenoxypropane under the conditions of acid (perchloric acid, borontrifluoride diethyl etherate) and basic (sodium hydroxide) catalysis. Reaction conditions (temperature, reaction time, molar ratio of reactants) have been determined, allowing the hydrophobization of bead cellulose to be carried out to the largest possible extent while maintaining its spherical shape. The nonstoichiometric mechanism suggested for the adsorption of amphiphilic adsorptives on bead 2-hydroxy-3-phenoxypropyl-cellulose (HPP-C) was checked by means of adsorption of six proteins. It was found that the surface of the hydrophobic segment of the adsorbent must be sufficiently large to be able to come in touch with the hydrophobic region of the protein through its multiple residues. In such cases the partitioning of the protein between the hydrophobic segment present as a liquid-like film and the surrounding solution becomes the predominant step of the adsorption. This adsorption mechanism is also reflected in zonal chromatography on bead HPP-C, as no displacement phenomena could be observed in any of the six proteins used. Retention of these proteins has been affected to a decisive extent by the degree of hydrophobization of HPP-C.


2011 ◽  
Vol 55-57 ◽  
pp. 312-316
Author(s):  
Qi Wang ◽  
Guo Zheng ◽  
Jian Jie Ai ◽  
Xue Jing Wei

High yield diglycerin borate(DGB) have been synthesized by the raw materials glycerol and boric acid in this paper. The structure of the products was characterized by FTIR and11B NMR. The yield of the products was discussed by reaction conditions that were material ratio, reaction temperature, reaction pressure etc. and then the optimum process conditions of preparing DGB was decided. In this condition, high yield DGB can be prepared which could reach more than 96%.


1970 ◽  
Vol 44 (1) ◽  
pp. 131-136 ◽  
Author(s):  
Manoranjan Saha ◽  
M Kabir Hossain ◽  
M Ashaduzzaman ◽  
Shams Tania Afroza Islam ◽  
Mirza Galib ◽  
...  

Alkylphenols have been synthesised in high yield by the alkylation of phenol with olefins (C6-C8) in the presence of sulphuric acid. The effects of the variation of temperature, molar ratio of phenol to olefin, time of reaction, concentraction and amount of sulphuric acid have also been studied on the reactions.Keywords: Alkylation, Phenol, Sulphuric Aciddoi: 10.3329/bjsir.v44i1.2722 Bangladesh J. Sci. Ind. Res. 44(1), 131-136, 2009  


2015 ◽  
Vol 1120-1121 ◽  
pp. 873-876
Author(s):  
Xiang Qun Xu ◽  
Nian Hong ◽  
Jie Yang ◽  
You Quan Zhong ◽  
Lin Cheng

To study the process conditions for preparing sultamicillin tosilate β-cyclodextrin inclusion.Method: Choose the usage ration of sultamicillin tosilate with β-cyclodextrin, the inclusion temperature and the time of reaction as the main factors, and use the inclusion yield as evaluated indicators and the process condition to conduct the L9 (34) orthogonal experiment Optimization Pack sultamicillin tosilate.Outcome: The optimum inclusion process condition: molar ratio of the sultamicillin tosilate with β-cyclodextrin is 1:8, inclusion temperature is 47°C, inclusion time is 40 minutes.Conclusion: The process condition of using β-cyclodextrin inclusion to inconcluse sultamicillin tosilate is feasible, effective, and of applicative value.


2011 ◽  
Vol 8 (s1) ◽  
pp. S33-S40 ◽  
Author(s):  
Noor Hafizah Arbain ◽  
Jumat Salimon

Biolubricant production of trimethylolpropane ester (ET) was conducted via esterification of fatty acid (FA) ofJatropha curcasoil with trimethylolpropane (TMP). The condition for this reaction was as follows: temperature was 150°C, time of reaction was 3 hours, molar ratio of FA: TMP was 4:1 and 2% wt/wt concentrated catalyst (based on weight of FA). Different catalyst was used in this reaction such as perchloric acid, sulfuric acid,p-toluenesulfonic acid, hydrochloric acid and nitric acid. The composition of ET was determined by Gas Chromatography (GC-FID). The ester group was confirmed by Fourier Transform Infrared Spectroscopy (FTIR) and the structure was confirmed by proton and carbon Nuclear Magnetic Resonance (1H-NMR and13C-NMR) spectra. 70% of ET was successfully synthesized using perchloric acid in this research. The pour point of the product was observed as low as –23°C, flash point is >300°C and viscosity index is 150.


2013 ◽  
Vol 634-638 ◽  
pp. 145-151
Author(s):  
Guo Qing Liu ◽  
Jian Wu ◽  
He An Luo

An innovative green process of producing ε-caprolactam (CPL) was proposed by integrating ammoximation and Beckmann rearrangement effectively. As a second part of the new process, two-phase (liquid-liquid) Beckmann rearrangement of cyclohexanone oxime to caprolactam was carried out using solution of oxime-cyclohexane as reactant instead of melting oxime in conventional route. The experimental results indicated that a relatively high yield of CPL can be achieved with much less oleum under milder reaction conditions in comparison with conventional technology. Furthermore, preliminary work on the quality of CPL, characterized by D value, was also performed. It was found that molar ratio of acid to oxime had a great impact on D value while the influences of other parameters were less important.


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