赵文朋,张阳倩,赵雪钦,张毅民.化学通报,2020,83(12):1149-1154.
响应面法优化磺丁基醚-β-环糊精合成工艺
Optimization of Synthesis Process of Sulfobutyl Ether-β-Cyclodextrin by Response Surface Methodology
投稿时间:2020-05-05  修订日期:2020-08-28
DOI:
中文关键词:  磺丁基醚-β-环糊精  β-环糊精  1,4-丁磺内酯  碱性电解水  响应曲面法
英文关键词:Sulfobutyl ether-β-cyclodextrin  β-cyclodextrin  1,4-butane sultone  Alkaline electrolyzed water  Response surface methodology
基金项目:天津大学校企合作项目(2018GKF-0730)资助
作者单位E-mail
赵文朋 天津大学绿色合成与转化教育部重点实验室 天津大学化工学院 天津 300350  
张阳倩 天津大学绿色合成与转化教育部重点实验室 天津大学化工学院 天津 300350  
赵雪钦 天津大学绿色合成与转化教育部重点实验室 天津大学化工学院 天津 300350  
张毅民 天津大学绿色合成与转化教育部重点实验室 天津大学化工学院 天津 300350 zhangym@tju.edu.cn 
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中文摘要:
      以碱性电解水为介质、β-环糊精(β-CD)和1,4-丁磺内酯为原料,分别采用水浴法和微波法合成了取代度为3的SBE-β-CD。考察了两种不同工艺条件下反应温度、反应时间和碱性电解水pH对产物收率的影响。以产物收率为响应值,采用Box-Behnken响应曲面设计探究了微波法中各变量及其交互作用对产物收率的影响,并建立回归方程预测模型。结果表明,相较于水浴法,微波法反应时间缩短了十几个小时,产物收率提高约10%~20%。优化合成工艺参数为:反应温度77℃,反应时间2.75h,碱性电解水pH=12.7,该条件下产物收率达到70.4%,与模型的理论预测值较为接近。
英文摘要:
      Using alkaline electrolyzed water as medium, SBE-β-CD with degree of substitution 3 was synthesized by water bath method and microwave method respectively with β-CD and 1,4-butane sultone as raw materials. The effects of react temperature, react time and pH of alkaline electrolyzed water on the yield of product were investigated under two different conditions. Using product yield as response value, Box-Behnken response surface design was used to explore the influences of various variables and their interaction on product yield in microwave method, and the prediction model of regression equation was established. The results showed that the reaction time of microwave method was shortened by more than ten hours compared with the water bath method, and the product yield was increased by about 10%~20%. The optimum reaction conditions were obtained as follows:the react temperature was 77℃, the react time was 2.75 h, and pH of alkaline electrolyzed water was 12.7. Under the optimum reaction conditions, the product yield of 70.4% was obtained, which was close to the theoretical prediction value of the model.
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