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Separation and purification of optically active substancc by crystallization

Research Project

Project/Area Number 07555552
Research Category

Grant-in-Aid for Scientific Research (A)

Allocation TypeSingle-year Grants
Section試験
Research Field 反応・分離工学
Research InstitutionWaseda University

Principal Investigator

TOYOKURA Ken  Waseda Univ.School of Sci.and Eng.prof., 理工学部, 教授 (40063557)

Co-Investigator(Kenkyū-buntansha) HIRASAWA Izumi  Waseda Univ.School of Sci.and Eng.Prof., 理工学部, 教授 (10228778)
Project Period (FY) 1995 – 1996
Project Status Completed (Fiscal Year 1996)
Budget Amount *help
¥2,300,000 (Direct Cost: ¥2,300,000)
Fiscal Year 1996: ¥2,300,000 (Direct Cost: ¥2,300,000)
Keywordsoptical resolution / preferential crystallization / induction time / suspension density / supersaturation / S-Carboxymethyl-DL-Cysteine / Mandelic acid / 光学分割法 / 成長速度 / D・L-SCMC / D・Lマンデル酸 / 相平衡関係 / L体結晶の純度
Research Abstract

Experimental study of aqueous solution of DL-Mandelic acid was carried out to observe solubility data less than 30 percent of L-Mandelic acid against DL-acid by the cooling method under atmospheric pressure. And the solubility curve for the range was more than 30 percent of L-Mandelic acid also observed by high pressure crystallization. From this observed data, a new effective optical resolution process was proposed as a combination between evaporation and high pressure crystallization. And optical resolution of L-SCMC (S-Carboxymethyl-L-Cysteine) from DL-SCMC solution was studied at isoelectric point and supersaturated solution in which L-SCMC seed grew without nucleation of D-SCMC nuclei, was discussed. Crystal growth rate of a single crystal of L-SCMC was observed in aqueous solution of DL-SCMC with 5 and 10 wt% of NaCl for the range of supersaturation of 0.1-0.25 [g/100ml]. From these test's results, crystal growth rate of L-SCMC was affected by concentration D-SCMC "S_D" factor in the solution and disturb factor alpha which was defined by the ratio of supersaturation of L-SCMC to S_D, was proposed. On the other hand, concentration of only L-SCMC in the solution decreased by growth of L-SCMC seed which was added into supersaturated solution, for an initial period of operation just after L-SCMC seed was added, but when the operation continued for a long while, concentration of D-SCMC also started to decrease. This phenomenon was confirmed to come from nucleation of D-SCMC nuclei on the surface of L-SCMC aeed. Then, this nucleation was studied, and waiting time for two-dimensional nucleation of D-SCMC turned out to be affected by supersaturation of the solution and suspension density of crystal in the solution. Operational condition on which only L-SCMC crystal grows, was found out from this data. And crystal growth rate of L-SCMC seed was also observed by evaporatting crystallization and the data was compared with data obtained by cooling crystallization.

Report

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

    (8 results)

All Other

All Publications (8 results)

  • [Publications] K. Toyokura et al.: "Optical Resolution of DL-SCMC in a Cooled type Batch Operation" Crystal Growth of Organic Materials 1996. 105-109 (1996)

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] K. Toyokura et al.: "Concentration change of L-SCMC (S-Carboxymethyl-L-cysteine) in a supersaturated solution of DL-SCMC with suspended L-SCMC seeds in a batch operation" ACS Symposium Series. (to be printed).

    • Description
      「研究成果報告書概要(和文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] K.Toyokura et al: "Optical Resolution of DL-SCMC in a Cooled type Batch Operation" Crystal Growth of Organic Materials. 105-109 (1996)

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] K.Toyokura et al: "Concentration change of L-SCMC (S-Carboxymethyl-L-cysteine) in a supersaturated solution of DL-SCMC with suspended L-SCMC seeds in a batch operation" ACS Symposium Serics. (to be printed).

    • Description
      「研究成果報告書概要(欧文)」より
    • Related Report
      1996 Final Research Report Summary
  • [Publications] K.Toyokura et al: "Optical Resolution of DL-SCMC in a Cooled type Batch Operation" Crystal Growth of Organic Materials 1996. 105-109 (1996)

    • Related Report
      1996 Annual Research Report
  • [Publications] K.Toyokura et al: "Concentration change of L-SCMC(S-Carboxymethyl-L-cysteine)in a supersaturated solution of DL-SCMC with suspended L-SCMC seeds in a batch operation" ACS Symposium Series. (to be printed).

    • Related Report
      1996 Annual Research Report
  • [Publications] 豊倉賢: "Optical Resolution of DL-SCMC in a Cooled type Bach Operation" Crystal Growth of Organic Materials 3. (1996)

    • Related Report
      1995 Annual Research Report
  • [Publications] 豊倉賢: "Crystal Growth of L-SCMC seeds in a DL-SCMC Solution of pH0.5" Crystal Growth of Organic Materials 3. (1996)

    • Related Report
      1995 Annual Research Report

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Published: 1996-04-01   Modified: 2016-04-21  

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