A new way to prepare cellulose-type chiral stationary phases （CSPs） has been established in the present work.Cellulose microspheres with a volume-average diameter of 11.5 m were prepared by an emulsion-solidificatio...A new way to prepare cellulose-type chiral stationary phases （CSPs） has been established in the present work.Cellulose microspheres with a volume-average diameter of 11.5 m were prepared by an emulsion-solidification method.Three new CSPs were obtained by crosslinking the cellulose microspheres with terephthaloyl chloride （TPC）,and then modifying the crosslinked microspheres with 4-methylbenzoyl chloride,3,5-dimethylbenzoyl chloride and 3,5-dichlorobenzoyl chloride,respectively.The microspheres and the CSPs were characterized by FT-IR,element analysis and scanning electronic microscopy （SEM）.The chiral recognition ability of the CSPs was evaluated with high-performance liquid chromatography （HPLC）.The chromatographic results demonstrate that the CSP prepared from 3,5-dichlorobenzoyl chloride possesses better chiral recognition ability compared with two other CSPs.展开更多
[ Objective ] This study aimed to provide basic data for studying the relationship between structure and property of cellulose microspheres by measuring molecular weight of cellulose and cellulose microspheres with vi...[ Objective ] This study aimed to provide basic data for studying the relationship between structure and property of cellulose microspheres by measuring molecular weight of cellulose and cellulose microspheres with viscosity method and gel permeation chromatography （GPC） method. [ Method] In viscosity method, cadmium ethylenediamine was used as the solvent, intrinsic viscosity η of the solution was determined at 25 ℃ by using a Ubbelohde viscometer, to calculate the molecular weight of cellulose; in GPC method, 8% LiC1 / N, N-dimethylacetamide （LiC1/DMAc） was used as the solvent and 0.5% LiC1/DMAc was used as the mobile phase to determine the relative molecular weight and distribution of cellulose and cellulose microspheres. In addition, the determination results were analyzed to compare these two methods. [ Result ] Viscosity-average molecular weight Mr/ of cellulose and cellulose microspheres determined with viscosity method were 224,532 and 16,686, respectively; weight-average molecular weight Mw of cellulose and cellulose microspheres determined with GPC method were 284,196 and 22,345, respectively. [ Conclusion] The determination results of （;PC method are relatively close to the actual value and could truly reflect the characteristics of molecular weialat distribution of eellulose and cellulose mierosr, heres.展开更多
基金Supported by the National Natural Science Foundation of China (50973086)the Research Project of Department of Education of Hubei Province (Z20081501)
文摘A new way to prepare cellulose-type chiral stationary phases （CSPs） has been established in the present work.Cellulose microspheres with a volume-average diameter of 11.5 m were prepared by an emulsion-solidification method.Three new CSPs were obtained by crosslinking the cellulose microspheres with terephthaloyl chloride （TPC）,and then modifying the crosslinked microspheres with 4-methylbenzoyl chloride,3,5-dimethylbenzoyl chloride and 3,5-dichlorobenzoyl chloride,respectively.The microspheres and the CSPs were characterized by FT-IR,element analysis and scanning electronic microscopy （SEM）.The chiral recognition ability of the CSPs was evaluated with high-performance liquid chromatography （HPLC）.The chromatographic results demonstrate that the CSP prepared from 3,5-dichlorobenzoyl chloride possesses better chiral recognition ability compared with two other CSPs.
基金Supported by Natural Science Foundation of Guangxi(0991024Z)
文摘[ Objective ] This study aimed to provide basic data for studying the relationship between structure and property of cellulose microspheres by measuring molecular weight of cellulose and cellulose microspheres with viscosity method and gel permeation chromatography （GPC） method. [ Method] In viscosity method, cadmium ethylenediamine was used as the solvent, intrinsic viscosity η of the solution was determined at 25 ℃ by using a Ubbelohde viscometer, to calculate the molecular weight of cellulose; in GPC method, 8% LiC1 / N, N-dimethylacetamide （LiC1/DMAc） was used as the solvent and 0.5% LiC1/DMAc was used as the mobile phase to determine the relative molecular weight and distribution of cellulose and cellulose microspheres. In addition, the determination results were analyzed to compare these two methods. [ Result ] Viscosity-average molecular weight Mr/ of cellulose and cellulose microspheres determined with viscosity method were 224,532 and 16,686, respectively; weight-average molecular weight Mw of cellulose and cellulose microspheres determined with GPC method were 284,196 and 22,345, respectively. [ Conclusion] The determination results of （;PC method are relatively close to the actual value and could truly reflect the characteristics of molecular weialat distribution of eellulose and cellulose mierosr, heres.
