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Preparation of Polymer Standards with Uniform Molecular Weights and Their Application to the Studies of Polymer Structure and Properties

Research Project

Project/Area Number 07555293
Research Category

Grant-in-Aid for Scientific Research (A)

Allocation TypeSingle-year Grants
Section展開研究
Research Field 高分子合成
Research InstitutionOsaka University

Principal Investigator

HATADA Koichi  Fac.Eng.Sci., Osaka University, Prof., 基礎工学研究科, 教授 (60029402)

Co-Investigator(Kenkyū-buntansha) SAITO Muneo  JASCO Co., Researcher, 第二技術部, 部長(研究者)
NISHIURA Takafumi  Fac.Eng.Sci., Osaka University, Res.Assoc., 基礎工学研究科, 助手 (70243194)
UTE Koichi  Fac.Eng.Sci., Osaka University, Assoc.Prof., 基礎工学研究科, 助教授 (30176713)
KITAYAMA Tatsuki  Fac.Eng.Sci., Osaka University, Prof., 基礎工学研究科, 教授 (60135671)
Project Period (FY) 1995 – 1997
Project Status Completed (Fiscal Year 1997)
Budget Amount *help
¥14,500,000 (Direct Cost: ¥14,500,000)
Fiscal Year 1997: ¥800,000 (Direct Cost: ¥800,000)
Fiscal Year 1996: ¥1,600,000 (Direct Cost: ¥1,600,000)
Fiscal Year 1995: ¥12,100,000 (Direct Cost: ¥12,100,000)
KeywordsSupercritical Fluid Chromatography / Uniform Polymer / Monodisperse Polymer / Molecular Weight Distribution / Stereoregularity / Poly (methyl methacrylate) / Size Exclusion Chromatography / Stereocomplex / 単分散ポリマー / 分子量測定 / サイズ排除クロマトグラフィー / ポリアセタール
Research Abstract

(1) A Supercritical fluid chromatograph (SFC) equipped with an automatic fractionation system consisting of an automatic injector and six-way valve units was constructed to obtain uniform polymers efficiently. Using this SFC system, the individual homologues (uniform polymers) of isotactic and syndiotactic poly (methyl methacrylate) (PMMA), syndiotactic polystirene, poly (butyl isocyanate), poly(hexyl isocyanate), poly (D-lactide), and poly (L-lactide) were successfully isolated. The structure and purity of uniform polymers were analyzed by NMR and mass spectrometry.
(2) The glass transition temperature of uniform isotactic and syndiotactic PMMAs from 13mer to 50mer was determined as a function molecular weight. When the glass transition temperatures were plotted against the reciprocal of molecular weight, the data were well fitted by the linear relationship derived from the free-volume theory. The uniform isotactic PMMAs were highly crystalline, and the degree of crystallinity was foun … More d to exceed 92%.
(3) When uniform isotactic PMMAs with definite molecular weights were used as the molecular weight standards in gel permeation chromatography (GPC), the molecular weight distribution of non-uniform isotactic PMMA was able to be determined accurately. A small difference between isotactic and syndiotactic PMMA in hydrodynamic volume was clearly shown by the GPC analysis of uniform polymers.
(4) Solutions of uniform poly (hexyl isocyanate) s with numbers of repeating unit (n) from 10 to 30 in (-) -beta-pinene showed induced circular dichroism at the wavelength range where the absorption due to the backbone N-C linkage appears. Solvent-subtracted specific rotation decreased with increasing temperature, and increased monotonously with an increase in n. These chiroptical properties arise from an excess of one-handedness in the helical chain structure. Single crystals were grown from methanol solution of butyl isocyanate 12mer and the crystal structure was determined by X-ray analysis.
(5) End-functionalized stereoregular uniform PMMAswere obtained by SFC fractionation and used to construct uniform polymer architectures such as block, comb, and star polymers. Solution properties of the uniform comb nd star PMMs were also investigated. Less

Report

(4 results)
  • 1997 Annual Research Report   Final Research Report Summary
  • 1996 Annual Research Report
  • 1995 Annual Research Report
  • Research Products

    (51 results)

All Other

All Publications (51 results)

  • [Publications] Koichi Ute: "Glass Transition Temperature and Melting Temperature of Uniform Isotactic and Syndiotactic Poly(methyl methacrylate)s from 13mer to 50mer" Polymer. 36. 1415-1419 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute: "Stabilization of Oligo(butyl isocyanate) by Acetyl End-Capping" Polymer Journal. 27. 445-448 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute: "Controlled Synthesis of Isotactic and Symmetrical Poly-(methyl methacrylate) Directed toward Uniform Polymers with High Crystallinity" Polymer Journal. 27. 951-958 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Preparation of Uniform Stereoblock Poly(methyl methacrylate)" Polymer Journal. 28. 185-188 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Preparation and Solution Properties of Uniform Three-arm Star Poly(methyl methacrylate)" Polymer Bulletin. 36. 399-405 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Takafumi Nishiura: "Intra- and Intermolecular Stereocomplex Formation of Uniform Stereoblock Poly(methyl methacrylate)" Polymer Journal. 28. 1021-1023 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Tatsuki Kitayama: "Natural and Synthetic Uniform Polymers" Journal of Macromolecular Science-Pure and Applied Chemistry. A33. 1531-1540 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Preparation of a Uniform poly(methyl methacrylate) Macromonomer and Its Polymerization" Macromolecular Rapid Communication. 18. 37-43 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Uniform Poly(methyl methacrylate)s with Controlled Architecture" Trends in Polymer Science. 5. 223-229 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Toward Uniform Polymer Architecture Through Stereo-specific Living Polymerization and Chromatographic Separation Technique" Macromolecular Symposia. 118. 135-141 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute: "Fractionation of Polymer Homologs with Packed Column Supercritical Fluid Chromatography" Packed-Column Supercritical Fluid Chromatography. 349-368 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Uniform Polyolefin and Polymethacrylate" Macromolecular Symposia.

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Preparation of Uniform Stereoregular Polymer,Stereoblock Polymer and Copolymer of Methacrylate,and Their Stereo-complex Formation" Macromolecular Symposia.

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 右手 浩一: "「均一ポリマー」の調製とその構造・物性研究への展開" 海外高分子研究. 41. 128-133 (1995)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 右手 浩一: "分子量の最も大きい単分散高分子は?" 高分子. 45. 104-105 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 畑田 耕一: "均一ポリマーの化学" 高分子加工. 46. 2-10 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 右手 浩一: "超臨界流体クロマトグラフィーによる均一ポリマーの単離と高分子科学への応用" Jasco Report. 54-59 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 右手 浩一: "均一オリゴマーの単結晶-高分子立体化学の精密化をめざして" 高分子. 46. 749-750 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] 畑田 耕一: "立体規則性均一構造高分子の構築" 高分子論文集. 54. 661-673 (1997)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute, Nobuo Miyatake, Koichi Hatada: "Glass Transition Temperature and Melting Temperature of Uniform Isotactic and Syndiotactic Poly (methyl methacrylate) s from 13mer to 50mer" Polymer. 36. 1415-1419 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute, Toshiya Asai, Yoichi Fukunishi, Koichi Hatada: "Stabilization of Oligo (butyl isocyanate) by Acetyl End-Capping" Polym.J.27. 445-448 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute, Yumi Yamasaki, Masami Naito, Nobuo Miyatake, Koichi Hatada: "Controlled Synthesis of Isotactic and Symmetrical Poly (methyl methacrylate) Directed toward Uniform Polymers with High Crystallinity" Polym.J.27. 951-958 (1995)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Takafumi Nishiura, Tatsuki Kitayama, Koichi Ute, Shuji Hirotani: "Preparation of Uniform Stereoblock Poly (methyl methacrylate)" Polym.J.28. 185-188 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Takafumi Nishiura, Tatsuki Kitayama, Mayumi Tsubota: "Preparation and Solution Properties of Uniform Three-arm Star Poly (methyl methacrylate)" Polym.Bull.36. 399-405 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Takafumi Nishiura, Tatsuki Kitayama, Koichi Hatada: "Intra- and Intermolecular Stereocomplex Formation of Uniform Stereoblock Poly (methyl methacrylate)" Polym.J.28. 1021-1023 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Tatsuki Kitayama, Koichi Hatada: "Natural and Synthetic Uniform Polymers" J.Macromol.Sci.-Pure Appl.Chem.A33. 1531-1540 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Takafumi Nishiura, Tatsuki Kitayama, Shuji Hirotani: "Preparation of a Uniform Poly (methyl methacrylate) Macromonomer and Its Polymerization" Macromol.Rapid Commun.18. 37-43 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Uniform Poly (methyl methacrylate) s with Controlled Architecture" Trends in Polym.Sci.5. 223-229 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Takafumi Nishiura, Tatsuki, Kitayama, Koichi Ute: "Toward Uniform Polymer Architecture Through Stereospecific Living Polymerization and Chromatographic Separation Technique" Macromol.Symp.118. 135-141 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Ute: "Fractionation of Polymer Homologs with Packed Column Supercritical Fluid Chromatography" "Packed-Column Supercritical Fluid Chromatography Marcel Dekker, New York". 349-368 (1997)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Tatsuki Kitayama, Koichi Ute, Takufumi Nishiura: "Uniform Polyolefin and Polymethacrylate" Macromol.Symp.in press).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada, Tatsuki Kitayama, Koichi Ute, Takufumi Nishiura: "Preparation of Uniform Stereoregular Polymer, stereoblock Polymer and Copolymer of Methacrylate, and Their Stereocomplex Formation" Macromol.Symp.in press).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1997 Final Research Report Summary
  • [Publications] Koichi Hatada: "Uniform poly(methyl methacrylate)s with Controlled Architecture" Trends in Polymer Science. 5. 223-229 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Koichi Hatada: "Toward Uniform Polymer Architecture Through Stereospecific Living Polymerization and Chromatographic Separation Technique" Macromolecular Symposia. 118. 135-141 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Takafumi Nishiura: "Intra-and Intermolecular Stereocomplex Formation of Uniform Stereoblock Poly(methyl methacrylate)" Polymer Journal. 28. 1021-1023 (1996)

    • Related Report
      1997 Annual Research Report
  • [Publications] Koichi Hatada: "Uniform Polyolefin and Polymethacrylate" Macromolecular Symposia,in press.

    • Related Report
      1997 Annual Research Report
  • [Publications] Koichi Hatada: "Preparation of Uniform Stereoregular Polymer,Stereoblock Polymer and Copolymer of Methacrylate,and Their Stereocomplex Formation" Macromolecular Symposia,in press.

    • Related Report
      1997 Annual Research Report
  • [Publications] 畑田耕一: "立体規則性均一構造高分子の構築" 高分子論文集. 54. 661-673 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Koichi Ute: "Supercritical Fluid Chromatography with Packed Columus" Marcel Dekker, 472 (1997)

    • Related Report
      1997 Annual Research Report
  • [Publications] Koichi Hatada: "Preparation and Solution Properties of Uniform Three-arm Star Poly(methyl methacrylate)" Polymer Bulletin. 36-4. 399-405 (1996)

    • Related Report
      1996 Annual Research Report
  • [Publications] Takafumi Nishiura: "Intra-and Intermolecular Stereocomplex Formation of Uniform Stereoblock Poly(methyl methacrylate)" Polymer Journal. 28-11. 1021-1023 (1996)

    • Related Report
      1996 Annual Research Report
  • [Publications] Koichi Hatada: "Preparation of Uniform Poly(methyl methacrylate)Macromonomer and Its Polymerization" Macromolecular Rapid Communications. 18-1. 37-43 (1997)

    • Related Report
      1996 Annual Research Report
  • [Publications] Koichi Hatada: "Toward Uniform Polymer Architecture Through Stereospecific Living Polymerization and Chromatographic Separation Technique" Macromolecular Chemistry and Physics in press.

    • Related Report
      1996 Annual Research Report
  • [Publications] 右手浩一: "「均一ポリマー」の調製とその構造・物性研究への展開" 海外高分子研究. 41. 128-133 (1995)

    • Related Report
      1996 Annual Research Report
  • [Publications] 畑田耕一: "均一ポリマーの化学" 高分子加工. 46-1. 2-10 (1997)

    • Related Report
      1996 Annual Research Report
  • [Publications] Koichi Hatada: "Preparation of Uniform Stereoblock poly(methyl methacrylate)" Polymer Journal. 28. 185-188 (1996)

    • Related Report
      1995 Annual Research Report
  • [Publications] Koichi Ute: "Controlled Synthesis of Isotactic and Symmetrical Poly(methylmethacrylate)Directed toward Uniform Polymers with High Crystallinity" Polymer Journal. 27. 951-958 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Koichi Ute: "Glass Transition Temperature and Melting Temperature of Uniform Isotactic and syndiotactic Poly(methyl methacrylate)s from 13mer to 50mer" Polymer. 36. 1415-1419 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Koichi Hatada: "polymers of α-and β-Substituted Acrylates with controlled Structures" Macromolecular Symposia. 89. 465-478 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] Koichi Ute: "Stabilization of Oligo(butyl isocyanate)by Acetyl End-Capping" Polymer Journal. 27. 445-448 (1995)

    • Related Report
      1995 Annual Research Report
  • [Publications] 右手浩一: "分子量の最も大きい単分散高分子は?" 高分子. 45. 104-105 (1996)

    • Related Report
      1995 Annual Research Report

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Published: 1995-04-01   Modified: 2016-04-21  

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