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蒎烷基端羟基聚醚的合成与表征

Synthesis and Characterization of Pinane-Base End Hydroxy Polyethers

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【作者】 杜莉娟杨晓琴曾韬陈朱辉

【Author】 Lijuan Du;Xiaoqin Yang;Tao Zeng;Zhuhui Chen;College of Chemical Engineering, Nanjing Forestry University, Jiangsu Key Laboratory of Biomass-Based Green Fuels and Chemicals;

【机构】 南京林业大学化学工程学院,江苏省生物质绿色燃料与化学品重点实验室

【摘要】 以三氟化硼乙醚作催化剂,乙二醇(EG)为起始剂,进行了2,3-环氧蒎烷的均聚和与环氧氯丙烷(ECH)的共聚反应。红外光谱(FT-IR)、元素分析(EA)和核磁共振(1H-NMR)分析结果表明,单体发生了低相对分子质量的均聚和共聚反应,分别得到了具有端羟基的新型蒎烷基均聚醚和蒎烷基-ECH共聚醚。分别探讨了合成2种聚醚的适宜工艺条件,蒎烷基均聚醚:BF3·OEt2用量为原料质量的1.0%,EG用量为原料质量的1.2%,CH2Cl2用量与原料等质量,0℃反应5h。蒎烷基-ECH共聚醚中n(2,3-环氧蒎烷)∶n(ECH)为0.5∶1,BF3·OEt2用量为原料质量的1.0%,EG用量为原料质量的1.5%,CH2Cl2用量为原料等质量,0℃反应6h。在上述工艺条件下,制得的蒎烷基均聚醚重均相对分子质量(Mw)为500 g/mol,蒎烷基-ECH共聚醚的重均相对分子质量(Mw)约为700 g/mol。

【Abstract】 Using boron trifluoride diethyl ether as catalyst, ethylene glycol(EG)as the starting agent, the homopolymerization reaction of 2,3-epoxy pinane and the copolymerization reaction of 2,3-epoxy pinane and epichlorohydrin(ECH)were carried out. The results of FT-IR, EA and 1H-NMR analysis show that the low molecular weight homopolymerization and copolymerization reaction happened and the end hydroxy pinane-base polyether and pinane-base-ECHcopolyetherwere obtained, respectively. The optimal technical conditions for synthesisof two kinds of polyether were discussed. Pinane-base polyether for: the mass of catalyst BF3 ·OEt2 is 1.0% of the raw materials mass, initiator dosage of EG is 1.2% of the raw material mass, mass of CH2 Cl2 equals the mass of raw material, reaction time of 5 h, temperature of 0℃. n(2,3-epoxy pinane)∶ n(ECH)of Pinane-base-ECH polyether is 0.5∶1, catalyst dosage of BF3 ·OEt2 is 1.0% of the raw material mass,initiator dosages of EG are 1.5% of the raw material mass, dosages of CH2 Cl2 equals the mass of raw material, reaction time of 6 h, temperature of 0℃. Under the optimum polymerization conditions, the results demonstrate that the weight-average molecular weight( Mw)of pinanebase polyether and pinane-base-ECH copolyether is 500 g/mol and 700 g/mol, respectivley.

【基金】 国家自然科学基金资助项目(30771686);江苏省高校优势学科建设工程项目资助(164020639);江苏省普通高校研究生科研创新计划项目基金资助(CXZZ11_0528);南京林业大学优秀博士学位论文创新基金项目资助(2011YB016)
  • 【文献出处】 高分子材料科学与工程 ,Polymer Materials Science & Engineering , 编辑部邮箱 ,2013年11期
  • 【分类号】TQ326.5
  • 【下载频次】59
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