响应面法优化单氮杂苯并15-冠-5接枝聚砜

Experimental optimization of polysulfone-graft-mono azabenzo-15-crown-5 ether polymers by response surface methodology

为得到高固载量的接枝聚合物以用于锂同位素分离,以单氮杂苯并15-冠-5(BN15C5)和氯甲基聚砜(CMPSf)为原料,通过亲核取代反应制备单氮杂苯并15-冠-5接枝聚砜(PSf-g-BN15C5),采用单因素实验考察反应温度、反应时间、聚合物质量分数、冠醚和氯甲基化聚砜中氯甲基的物质量之比等因素对冠醚固载量的影响,利用响应面分析法对合成条件进行优化.结果表明,在冠醚与氯甲基的物质量比1.25、聚合物质量分数19.8%±0.5%、反应温度(71.6±0.4)℃、反应时间(7.1±0.1)h条件下,理论预测最大冠醚固载量为0.667 mmol/g,实验所得实际值为0.654 mmol/g,二者吻合性较好.

To obtain a high immobilization amount of grafted polymer for separating lithium isotope a novel polymer of poly - sulfone-graft-mono azabenzo-15-crown-5-ether （PSf-g-BN15C5） polymers were prepared by nucleophilic substitution reaction using mono azabenzo-15-crown-5-ethers（BN15C5） andchloromethylpolysulfone （CMPSf）. The effects of reaction temperature, reaction time, mass fraction of polymer and molar ratio of BN15C5 to CMPSf on the immobilization amount of crown ether were analyzed by single factor tests. Based on i t, the synthesis con-dition was optimized by the response surface methodology in detail. The results showed that the maximum immo-bilization amount obtained was 0.654 mmol/g at reaction temperature of （71 .6±0.4）℃,reactiontimeof （7 .1土 0.1） h, massfractionofpolymerof19.8% ±0.5% , andBN15C5andCMPSfmolarratioof1.25,whichwasclose to the theoretical immobilization amount, 0.667 mmol/g predicted by the response surface methodology.