聚苯乙烯键合纤维素苯基氨基甲酸酯固定相的制备

Preparation of polystyrene bonded cellulose phenyl carbamate stationary phase

以交联聚苯乙烯树脂为原料,丁二酸酐为酰基化试剂,经Friedel-Crafts酰基化反应,制得脂肪族羧酸型树脂羧酸型聚苯乙烯(PS—COOH).将纤维素苯基氨基甲酸酯通过纤维素糖单元上的羟基与酰氯化的羧酸型功能树脂氯代羧酚型聚苯乙烯(PS—COC l)反应,得到键合型纤维素类手性固定相.通过红外光谱对树脂进行表征,并研究纤维素酯不同的键合方法、纤维素酯之间的"互穿"作用、酰化剂用量、纤维素苯基氨基甲酸酯用量对该反应的影响及衍生化纤维素相对分子质量分级和相对分子质量分布.结果表明:PS—COOH树脂与酰化剂用量为1∶7,PS—COOH树脂与纤维素苯基氨基甲酸酯的投料比为1.0∶1.1为宜;使用纤维素二苯基氨基甲酸酯和纤维素三苯基氨基甲酸酯"互穿"后键合大大提高质量增加率;通过二次沉淀的方法可以得到相对分子质量窄分布的纤维素酯.

A kind of aliphatic carboxyl acid resin（PS—COOH） was prepared with crosslinked polystyrene and succinic anhydride by Friedel-Crafts acetylation functional reaction and the bonded cellulose chiral stationary phase was obtained by the reaction of the chlorided carboxylic acid resin（PS—COCl） and the cellulose phenylcarbamate.The cellulose derivative was attached to the resin through the hydroxyl of the sugar unit.The chirality modified polystyrene was characterized by infrared spectroscopy（IR）.The influences of bonding methods,interpenetration of cellulose esters,the amount of acetylation reagent and cellulose phenylcarbamate on the reaction were investigated.In addition,cellulose derivative was fractionally precipitated and the molecular weight distribution was discussed.The results showed that the better ratio of PS—COOH and acetylation reagent was 1∶7and that of PS—COOH and cellulose phenylcarbamate was 1.0∶1.1.The growth rate was greatly increased while cellulose triphenylcarbamate and cellulose diphenylcarbamate interpenetrated.Narrow molecular-weight distribution was obtained by secondaryprecipitation.