Separation and purification of optically active substancc by crystallization

光学活性物质的结晶分离纯化

基本信息

批准号：
07555552
负责人：
TOYOKURA Ken
金额：
$ 1.47万
依托单位：
Waseda University
依托单位国家：
日本
项目类别：
Grant-in-Aid for Scientific Research (A)
财政年份：
1995
资助国家：
日本
起止时间：
1995 至 1996
项目状态：
已结题

项目摘要

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.

在大气压下，通过冷却方法对DL-丙酸水溶液的水溶液进行了溶解度数据，而溶解度数据少于30％。并且该范围的溶解度曲线也超过30％的L-丙酸，也通过高压结晶观察到。从该观察到的数据中，提出了一种新的有效的光学分辨率过程，作为蒸发和高压结晶之间的组合。在等异电点研究了从DL-SCMC溶液中L-SCMC（S-羧甲基-L-半胱氨酸）的光学分辨率，并讨论了L-SCMC种子在没有D-SCMC Nuclei核的情况下生长的L-SCMC种子的过饱和溶液。在DL-SCMC的水溶液中观察到L-SCMC的单个晶体的晶体生长速率，NaCl的5和10 wt％的过饱和范围为0.1-0.25 [g/100ml]。从这些测试的结果中，提出了L-SCMC的晶体生长速率受溶液中的浓度D-SCMC“ S_D”因子的影响，而干扰因子alpha则根据L-SCMC与S_D的过饱和比率定义，这是定义的。另一方面，溶液中仅L-SCMC的浓度通过L-SCMC种子的生长降低，而L-SCMC种子被添加到过饱和溶液中，因为加入L-SCMC种子后的初始运行期，但是当操作持续很长时间后，D-SCMC的浓度也开始降低。该现象被证实来自L-SCMC AEED表面上D-SCMC核的成核。然后，研究了这种成核，并等待D-SCMC的二维成核的时间受到溶液中溶液的过度和溶液中晶体悬浮密度的影响。从这些数据中发现了仅L-SCMC晶体生长的操作条件。还通过蒸发结晶观察到L-SCMC种子的晶体生长速率，并将数据与通过冷却结晶获得的数据进行比较。