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作 者:史鸿鑫[1] 何杰[1] 赵琴琴[1] 武宏科[1] 项菊萍[1] 沈海民[1]
机构地区:[1]浙江工业大学绿色化学合成技术国家重点实验室培育基地,杭州310032
出 处:《化工生产与技术》2013年第1期1-5,69,共5页Chemical Production and Technology
基 金:浙江省科技厅资助项目(2011R09002-10)
摘 要:以全氟壬烯(PFN)、甘油和二聚甘油(DG)为原料,在吡啶(C5H5N)存在下经醚化反应,分别制备了全氟壬烯甘油醚(I)和全氟壬烯二聚甘油醚(II)。用傅立叶变换红外光谱仪、质谱方法对其结构进行了表征,并测试了表面张力。合成全氟壬烯甘油醚的较佳工艺条件为n(PFN):n(甘油):n(C5H5N)=1:4:1,以N,N-二甲基甲酰胺(DMF)为溶剂,在75℃反应7 h,收率82.4%。合成全氟壬烯二聚甘油醚的较佳工艺条件为n(DG):n(PFN):n(C5H5N)=1:1.25:1.5,DMF为溶剂,60℃反应5 h。0.5 g/L全氟壬烯甘油醚和全氟壬烯二聚甘油醚水溶液的表面张力分别为29.23 mN/m和25.10 mN/m。Perfluorononene glycerol ether(Ⅰ) and perfluorononenyl diglycerol ether(Ⅱ) were prepared respectively by etherification from perfluorononene(PFN),glycerol and diglycerol(DG) in pyridine(C 5 H 5 N),and were characterized by IR and MS.The surface tensions of aqueous solutions of the ethers were investigated.The optimal process conditions of Ⅰ were: molar ratio of PFN,glycerol and pyridine was 1:4:1,the reactants agitated at 75 ℃ for 7 h in DMF to give I the yield of 82.4%.The optimal process conditions of Ⅱ were: molar ratio of DG,PFN and pyridine was 1:1.25:1.5,the reactants agitated at 60 ℃ for 5 h in DMF.The surface tensions of 0.5 g/L aqueous solution of Ⅰ and Ⅱ were 29.23 mN/m and 25.10 mN/m respectively.
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