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Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt)

Received: 11 August 2021     Accepted: 20 August 2021     Published: 6 September 2021
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Abstract

Laboratory synthesis of IronIIchloride-FeCl2 at approximately 200[°C] to 250[°C] using hydrochloric acid-HCl-(33%) and fine iron filament (purity>99%) was done with respecting the reaction stoichiometric. A titration procedure with NaOH-0.05N was established and allowed to titrate the FeCl2 synthesized in solution. Thus, the mass yield against raw materials (Iron and HCl) was 67.22[%]. Then, this synthesized FeCl2 solution suffered an evaporation-crystallization-drying thermic treatment procedure which efficiency evaluated with NaOH-0.05N titration was up to 98[%]. Secondly, laboratory synthesis procedure of IronIIEthoxide-Fe(OEt)2 or FeO2C4H10 by reflux during 150[mn] at approximately 90[°C] to 115[°C] (maximally) using the previous synthesized FeCl2, sodium ethoxide-Na(OEt) and ethanol with pure hexane as solvent was carried out. The molar ratios (Iron/Ethanol) and (Ethanol/Hexane/Na(OEt)/Iron) were respectively (0.4775/1) and (1/2.5/0.96/0.4775) and permitted to acquire a heterogeneous phases which extraction with a washing-extracting mixed solvent; composed with Ethanol 90°-Pure Hexane-Toluene and another solvent composed only with Ethanol90°-Pure Hexane without ethanol such as the molar ratios of (Ethanol/Hexane), (Hexane/Toluene), (Ethanol/Toluene) and (Ethanol/Hexane)/Na(OEt) were respectively 1.27, 20.19, 26.55 and 14.02; followed by a crystallization procedure permitted to obtain pure IronIIEthoxide-Fe(OEt)2 liquid phases on top and solid grey graphite fine powders with eventually the FeCl2 representative-by-product on the bottom solution which concentrations were quantified and evaluated by a titration procedure using NaOH-0.05N and hexane as additive in titrated solution. It was noticed that the concentration of pure IronIIEthoxide-Fe(OEt)2 in liquid phases increased from the top to the bottom between respectively 1.458E-2 [mol/L] to 1.667E-1 [mol/L]. Then, an evaporation-crystallization procedure to concentrate the previous heterogeneous phases was established and carried out in order to crystalize a large part of the IronIIEthoxide-Fe(OEt)2 to the solid grey graphite fine powders, the mass yield quantified by the previous titration was up to 97[%]. The grey graphite fine powders was filtered and washed with a washing procedure using water and pure hexane such as (H2O/FeCl2) and (Hexane/H2O) molar ratios were respectively 221 and 14 which efficacy to retain alkenes-ethylene and to extract FeCl2 was very high respectively 99.15[%] and 97.07[%] as molars rates with 86.08[%] retention rate of Fe(OEt)2. Finally, the washed grey graphite fine powders suffered a thermic treatment which permitted to increase its purity 99.75[%] with 75[%] as porosity evaluated with acetone.

Published in American Journal of Applied Chemistry (Volume 9, Issue 5)
DOI 10.11648/j.ajac.20210905.11
Page(s) 123-130
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2021. Published by Science Publishing Group

Keywords

Ethanol-90°, Hydrochloric Acid-HCl, Hexane, IronIIchloride-FeCl2, IronIIEthoxide-Fe(OEt)2, Titrations, Evaporation, Crystallization

References
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[3] https://www.americanelements.com/iron-ethoxide-5058-42-4
[4] https://pubchem.ncbi.nlm.nih.gov/compound/22476984
[5] William L. Jolly, Modern Inorganic Chemistry, McGraw-Hill, 1984, p. 177.
[6] Paul. ARNAUD, Cours de chimie organique, 15th éd., Eds. Dunod 199O.
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[12] Nambinina Richard Randriana, Avotra Marson Randrianomenjanahary, Andry Tahina Rabeharitsara «Sodium Ethoxide Concentrated Solution Synthesis at Ambient Temperature Using Sodium Hydroxide and Ethanol-90 in Excess» World Journal of Applied Chemistry Volume 6, Issue 1, March 2021, Pages: 6-11 Received: Mar. 25, 2021; Accepted: Apr. 12, 2021; Published: Apr. 23, 2021.
[13] Bradley, Don C.; Mehrotra, Ram C.; Rothwell, Ian P.; Singh, A. (2001). Alkoxo and Aryloxo Derivatives of Metals. San Diego: Academic Press. ISBN 978-0-08-048832-5.
[14] Turova, Nataliya Y.; Turevskaya, Evgeniya P.; Kessler, Vadim G.; Yanovskaya, Maria I. (2002). The Chemistry of Metal Alkoxides. Dordrecht: Kluwer Academic Publishers. ISBN 9780792375210.
[15] Gulaim A. Seisenbaeva, Suresh Gohil, Evgeniy V. Suslova, Tatiana V. Rogova, Nataliya Y. Turova, Vadim G. Kessler “The Synthesis of Iron(III) Ethoxide Revisited: Characterization of the Metathesis Products of Iron(III) Halides and Sodium Ethoxide” Department of Chemistry Uppsala Sweden and Department of Chemistry, Moscow State University, Russia.
[16] Friedel, C.; Crafts, J. M. (1877) "Sur une nouvelle méthode générale de synthèse d'hydrocarbures, d'acétones, etc.," Compt. Rend., 84: 1392 & 1450.
[17] Price, C. C. (1946). "The Alkylation of Aromatic Compounds by the Friedel-Crafts Method". Org. React. 3: 1. doi: 10.1002/0471264180.or003.01. ISBN 0471264180.
[18] Zimmermann H, Walz R (2008). "Ethylene". Ullmann's Encyclopedia of Industrial Chemistry. Weinheim: Wiley-VCH. doi: 10.1002/14356007.a10_045.pub3. ISBN 978-3527306732.
[19] Research and Markets. "The Ethylene Technology Report 2016 - Research and Markets". www.researchandmarkets.com. Retrieved 19 June 2016.
[20] Rabearimihaja Phandry Nomena Ndjiva, Andry Tahina Rabeharitsara “Betacarotenes Dosage by Hydrofluoric Acid Solution and Validation of This New Process by SPC” - Chemical Process Engineering Department (E. S. P. A), Antananarivo University – Madagascar - American Journal of Applied Chemistry in Vol. 4, Issue Number 3, June 2016.
[21] Nambinina Richard Randriana, Avotra Marson Randrianomenjanahary, Andry Tahina Rabeharitsara, Trisodium Citrate Synthesis at Ambient Temperature Using Sodium Hydroxide Relatively in Excess and Citric Acid with Ethanol-90 as Solvent, American Journal of Applied Chemistry. Vol. 9, No. 3, 2021, pp. 83-89. doi: 10.11648/j.ajac.20210903.14.
[22] Nambinina Richard Randriana, Avotra Marson Randrianomenjanahary, Andry Tahina Rabeharitsara, “Trisodium Citrate Synthesis at Ambient Temperature Using Sodium Hydroxide Relatively in Excess and Citric Acid with Ethanol-90 as Solvent”, American Journal of Applied Chemistry Volume 9, Issue 3, June 2021, Pages: 83-89 Received: Jun. 6, 2021; Accepted: Jun. 18, 2021; Published: Jun. 25, 2021.
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    Nambinina Richard Randriana, Avotra Marson Randrianomenjanahary, Andry Tahina Rabeharitsara. (2021). Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt). American Journal of Applied Chemistry, 9(5), 123-130. https://doi.org/10.11648/j.ajac.20210905.11

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    Nambinina Richard Randriana; Avotra Marson Randrianomenjanahary; Andry Tahina Rabeharitsara. Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt). Am. J. Appl. Chem. 2021, 9(5), 123-130. doi: 10.11648/j.ajac.20210905.11

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    Nambinina Richard Randriana, Avotra Marson Randrianomenjanahary, Andry Tahina Rabeharitsara. Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt). Am J Appl Chem. 2021;9(5):123-130. doi: 10.11648/j.ajac.20210905.11

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  • @article{10.11648/j.ajac.20210905.11,
      author = {Nambinina Richard Randriana and Avotra Marson Randrianomenjanahary and Andry Tahina Rabeharitsara},
      title = {Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt)},
      journal = {American Journal of Applied Chemistry},
      volume = {9},
      number = {5},
      pages = {123-130},
      doi = {10.11648/j.ajac.20210905.11},
      url = {https://doi.org/10.11648/j.ajac.20210905.11},
      eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.ajac.20210905.11},
      abstract = {Laboratory synthesis of IronIIchloride-FeCl2 at approximately 200[°C] to 250[°C] using hydrochloric acid-HCl-(33%) and fine iron filament (purity>99%) was done with respecting the reaction stoichiometric. A titration procedure with NaOH-0.05N was established and allowed to titrate the FeCl2 synthesized in solution. Thus, the mass yield against raw materials (Iron and HCl) was 67.22[%]. Then, this synthesized FeCl2 solution suffered an evaporation-crystallization-drying thermic treatment procedure which efficiency evaluated with NaOH-0.05N titration was up to 98[%]. Secondly, laboratory synthesis procedure of IronIIEthoxide-Fe(OEt)2 or FeO2C4H10 by reflux during 150[mn] at approximately 90[°C] to 115[°C] (maximally) using the previous synthesized FeCl2, sodium ethoxide-Na(OEt) and ethanol with pure hexane as solvent was carried out. The molar ratios (Iron/Ethanol) and (Ethanol/Hexane/Na(OEt)/Iron) were respectively (0.4775/1) and (1/2.5/0.96/0.4775) and permitted to acquire a heterogeneous phases which extraction with a washing-extracting mixed solvent; composed with Ethanol 90°-Pure Hexane-Toluene and another solvent composed only with Ethanol90°-Pure Hexane without ethanol such as the molar ratios of (Ethanol/Hexane), (Hexane/Toluene), (Ethanol/Toluene) and (Ethanol/Hexane)/Na(OEt) were respectively 1.27, 20.19, 26.55 and 14.02; followed by a crystallization procedure permitted to obtain pure IronIIEthoxide-Fe(OEt)2 liquid phases on top and solid grey graphite fine powders with eventually the FeCl2 representative-by-product on the bottom solution which concentrations were quantified and evaluated by a titration procedure using NaOH-0.05N and hexane as additive in titrated solution. It was noticed that the concentration of pure IronIIEthoxide-Fe(OEt)2 in liquid phases increased from the top to the bottom between respectively 1.458E-2 [mol/L] to 1.667E-1 [mol/L]. Then, an evaporation-crystallization procedure to concentrate the previous heterogeneous phases was established and carried out in order to crystalize a large part of the IronIIEthoxide-Fe(OEt)2 to the solid grey graphite fine powders, the mass yield quantified by the previous titration was up to 97[%]. The grey graphite fine powders was filtered and washed with a washing procedure using water and pure hexane such as (H2O/FeCl2) and (Hexane/H2O) molar ratios were respectively 221 and 14 which efficacy to retain alkenes-ethylene and to extract FeCl2 was very high respectively 99.15[%] and 97.07[%] as molars rates with 86.08[%] retention rate of Fe(OEt)2. Finally, the washed grey graphite fine powders suffered a thermic treatment which permitted to increase its purity 99.75[%] with 75[%] as porosity evaluated with acetone.},
     year = {2021}
    }
    

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  • TY  - JOUR
    T1  - Laboratory Synthesis and Titrations of IronIIchloride-FeCl2 and IronII Ethoxide-Fe(OEt)2 Using Ethanol-90° - Hexane and Sodium Ethoxide-Na(OEt)
    AU  - Nambinina Richard Randriana
    AU  - Avotra Marson Randrianomenjanahary
    AU  - Andry Tahina Rabeharitsara
    Y1  - 2021/09/06
    PY  - 2021
    N1  - https://doi.org/10.11648/j.ajac.20210905.11
    DO  - 10.11648/j.ajac.20210905.11
    T2  - American Journal of Applied Chemistry
    JF  - American Journal of Applied Chemistry
    JO  - American Journal of Applied Chemistry
    SP  - 123
    EP  - 130
    PB  - Science Publishing Group
    SN  - 2330-8745
    UR  - https://doi.org/10.11648/j.ajac.20210905.11
    AB  - Laboratory synthesis of IronIIchloride-FeCl2 at approximately 200[°C] to 250[°C] using hydrochloric acid-HCl-(33%) and fine iron filament (purity>99%) was done with respecting the reaction stoichiometric. A titration procedure with NaOH-0.05N was established and allowed to titrate the FeCl2 synthesized in solution. Thus, the mass yield against raw materials (Iron and HCl) was 67.22[%]. Then, this synthesized FeCl2 solution suffered an evaporation-crystallization-drying thermic treatment procedure which efficiency evaluated with NaOH-0.05N titration was up to 98[%]. Secondly, laboratory synthesis procedure of IronIIEthoxide-Fe(OEt)2 or FeO2C4H10 by reflux during 150[mn] at approximately 90[°C] to 115[°C] (maximally) using the previous synthesized FeCl2, sodium ethoxide-Na(OEt) and ethanol with pure hexane as solvent was carried out. The molar ratios (Iron/Ethanol) and (Ethanol/Hexane/Na(OEt)/Iron) were respectively (0.4775/1) and (1/2.5/0.96/0.4775) and permitted to acquire a heterogeneous phases which extraction with a washing-extracting mixed solvent; composed with Ethanol 90°-Pure Hexane-Toluene and another solvent composed only with Ethanol90°-Pure Hexane without ethanol such as the molar ratios of (Ethanol/Hexane), (Hexane/Toluene), (Ethanol/Toluene) and (Ethanol/Hexane)/Na(OEt) were respectively 1.27, 20.19, 26.55 and 14.02; followed by a crystallization procedure permitted to obtain pure IronIIEthoxide-Fe(OEt)2 liquid phases on top and solid grey graphite fine powders with eventually the FeCl2 representative-by-product on the bottom solution which concentrations were quantified and evaluated by a titration procedure using NaOH-0.05N and hexane as additive in titrated solution. It was noticed that the concentration of pure IronIIEthoxide-Fe(OEt)2 in liquid phases increased from the top to the bottom between respectively 1.458E-2 [mol/L] to 1.667E-1 [mol/L]. Then, an evaporation-crystallization procedure to concentrate the previous heterogeneous phases was established and carried out in order to crystalize a large part of the IronIIEthoxide-Fe(OEt)2 to the solid grey graphite fine powders, the mass yield quantified by the previous titration was up to 97[%]. The grey graphite fine powders was filtered and washed with a washing procedure using water and pure hexane such as (H2O/FeCl2) and (Hexane/H2O) molar ratios were respectively 221 and 14 which efficacy to retain alkenes-ethylene and to extract FeCl2 was very high respectively 99.15[%] and 97.07[%] as molars rates with 86.08[%] retention rate of Fe(OEt)2. Finally, the washed grey graphite fine powders suffered a thermic treatment which permitted to increase its purity 99.75[%] with 75[%] as porosity evaluated with acetone.
    VL  - 9
    IS  - 5
    ER  - 

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Author Information
  • Polytechnics Engineer School Vontovorona-Chemical Process Engineering Department, Antananarivo University, Antananarivo, Madagascar

  • Polytechnics Engineer School Vontovorona-Chemical Process Engineering Department, Antananarivo University, Antananarivo, Madagascar

  • Polytechnics Engineer School Vontovorona-Chemical Process Engineering Department, Antananarivo University, Antananarivo, Madagascar

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