• Search Research Projects
  • Search Researchers
  • How to Use
  1. Back to project page

1992 Fiscal Year Final Research Report Summary

Synthesis of Ultra-pure Higher n-Alkanes up to n-C_<160>H_<322> and Physical Properties of their Crystals

Research Project

Project/Area Number 03555191
Research Category

Grant-in-Aid for Developmental Scientific Research (B)

Allocation TypeSingle-year Grants
Research Field 高分子物性・高分子材料(含機械材料)
Research InstitutionKYUSHU UNIVERSITY

Principal Investigator

TAKAMIZAWA Kanichiro  Kyushu Univ., Fac. of Eng., Proc., 工学部, 教授 (10037707)

Co-Investigator(Kenkyū-buntansha) URABE Yoshiko  Kyushu Univ., Fac. of Eng., Assist., 工学部, 助手 (80037796)
Project Period (FY) 1991 – 1992
KeywordsHigher n-Alkane / Carboxylic Acid / Homologous Purity / Wurtz Condensation / Ketene Dimerization / Extended Chain Crystal / Folded Chain Crystal / High Temperature Capillary Gas Chromatography
Research Abstract

The Synthetic method to obtain ultra-pure higher n-alkanes (abbr. C_n, n: the number of carbon atoms in chain) was ketene dimarization from carboxylic acid, the starting materials which had been purified by preparative liquid chromatography for the odd n-alkanes. We confirmed that for the even n-alkanes , Wurtz condensation of monoiodoalkane (abbr. C_nI) was the most suitable method up to C102. But little progress has been made with the synthesis of C120 , C160 through Wurtz condensation from C60I and C80I respectively, as the depression in reaction activity with the chain length of C_nI become long. It is necessary to investigate the condition of this reaction.
In order to obtain more higher n-alkanes in the region that chain folding is found, Wurtz condensation of alpha,omega-diiodotetracontane was performed. That resulted in the mixture of H[(CH_2)_<40>]nH=1,2,3,4. The mixture of n-alkanes was first fractionated by adsorption column method, and was separated almost step-wise according to molecular weight up to C160. They were, furthermore purified by GPC on repeated runs.
The purity of the sample was examined by a Shimadzu capillary gas chromatogragh, GC-14AHF_<sc> equipped with data analyzer of C-R6A. The homologous impurity was proved to be quantitatively determined by the chromatography at a programmed-temperature operation up to 450゚C for C102,98.8%, C80 was 99.3%. Analysis of C160 couldn't done.
DSC measurements were done on C80,C102,C120 and C160 which were melt crystallized samples (chain extended crystals). Melting point of them were 109.6゚C, 115.7゚C, 119.7゚C and 125.0゚C, respectively. On the DSC thermogram of solution crystallized C160 was shown that melting of once-folded chain crystals was immediately followed by recrystallization (exotherm) in the extended chain form, which melted at a somewhat higher temperature. That the thickness of C160 crystals was about 10nm from observation by TEM, shows the formation of once-folded crystals.

  • Research Products

    (18 results)

All Other

All Publications (18 results)

  • [Publications] 高見沢 橄一郎: "n-アルカンの結晶化における高温構造の凍結" 九州大学大学院総合理工学研究科報告. 14. 181-188 (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.URABE: "The Effect of the Particle Size on the Anomalous Peaks observe with the DSC Measurements on Hep tacosane and Dopentacosane" Chemistry Letters. 1992. 2315-2318 (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] K.TAKAMIZAWA: "Application of a high pressure d.t.a.to study the pressure-glassification of polystyrene" Polymer,Communications. 33. 1333-1334 (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] K.TAKAMIZAWA: "A New Type of Refractometer for High-Temparature Use" Jpn.J.Appl.Phys.31. 2606-2609 (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 高見沢 橄一郎: "α,ωジハロゲノアルカンの結晶構造と双極子相互作用" 九州大学大学院総合理工学研究科報告. 13. 341-347 (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] A.TODA,: "Lateral habits of n-alkane single crystals" J.Mater.Sci.26. 2793-2796 (1991)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] Y.URABE: "The Determination of Homologous Purity of Higher n-Alkaneses up to Dohectane with Capillary Gas Chromatography" Polymer J.(1993)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] K.TAKAMIZAWA,: "The solubility limit of the solid solution for the systemes of long-chain symmetrical ketone in n-alkane matrix" Colloid & Polym.Sci.(1993)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] 高見沢 橄一郎 分担執筆: "融解現象「高分子機能材料」シリーズ第3巻" 高分子学会編 共立出版社, (1992)

    • Description
      「研究成果報告書概要(和文)」より
  • [Publications] K.Takamizawa: "Freezing-in of High Temperature Oblique Structures of Higher n-Alkanes on Crystallization." Eng.Sci.Rept.,Kyushu Univ. Vol.14 No.2. 181-188 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] Y.Urabe: "The Effect of the Particle Size on the Anomalous Peaks observed with the DSC Measurements on Henpentacontane and Dopentacontane." Chem.Lett.Vol.1992 No.12. 2315-2318 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] K.Takamizawa: "Application of a high pressure d.t.a. to study the pressure-Glassification of polystyrene." Polymer,Commun.Vol.33. 133-1334 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] K.Takamizawa: "A New Type of Refractometer for High-Temperature Use." Jpn.J.Appl.Phys.Vol.31. 2606-2609 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] K.Takamizawa: "Crystal Structures of a,w dihalogenoalkane and Effects of the Dipole Moments." Eng.Sci.Rept.,Kyushu Univ. Vol.13 No.4. 341-347 (1992)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] A.Toda: "Lateral habits of n-alkane single crystals." J.Mater.Sci.Vol.26. 2793-2796 (1991)

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] Y.Urabe: "The Determination of Homologous Purity of Higher n-Alkanes up to Dohectane with Capillary Gas Chromatography. (submitted)" Polym.J.

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] K.Takamizawa: "The solubility limit of the solid solution for the systems of long-chain symmetrical ketone in n-alkane matrix. (submitted)" Colloid & Polym.Sci.

    • Description
      「研究成果報告書概要(欧文)」より
  • [Publications] K.Takamizawa: The Soc.Polym.Sci.Jpn. Kyouritu Pub.Co.Melting Phenomena "Polymeric functional materials" Vol.3, (1992)

    • Description
      「研究成果報告書概要(欧文)」より

URL: 

Published: 1994-03-24  

Information User Guide FAQ News Terms of Use Attribution of KAKENHI

Powered by NII kakenhi