减压辅助法制备PPDO

发布时间：2018-03-10 14:11

本文选题：聚对二氧环己酮　切入点：辛酸亚锡　出处：《材料科学与工程学报》2016年01期 　论文类型：期刊论文

【摘要】：本文以辛酸亚锡(Sn(OCt)_2)为催化剂,乙二醇为引发剂,首次采用减压辅助法合成聚对二氧环己酮(Poly(p-dioxanone),PPDO),并系统研究了引发剂、减压时间及引发时间对聚合反应的影响。利用红外光谱(IR)、核磁光谱(~1H NMR)、特性粘度(η)、X射线广角衍射(WAXD)及差示扫描量热法(DSC)对聚合产物的结构及热力学性能进行初步探讨。IR、~1H NMR及WAXD测试结果表明:减压法能够得到高纯度且晶型相同的PPDO产物。且在减压12h时,单体转化率达到最大值(86.5%)。引发6h时,单体转化率达到84.5%。而未加引发剂时,单体转化率仅为81.1%。DSC测试结果表明:产物的熔融温度(T_m)与结晶温度(T_c)均随减压时间及引发时间的延长呈现先上升后降低的趋势。相比传统方法,减压辅助法能够获得更高的产率。同时有效地避免了溶解-沉淀提纯而引入的杂质。
[Abstract]:In this paper, Poly (p-Dioxanone) PPDOO _ (2) was synthesized by decompression assisted method with Sn-Sn-OCtO _ (2) octanoate as catalyst and ethylene glycol as initiator, and the initiator was studied systematically. The effect of decompression time and initiation time on the polymerization reaction. The structure and thermodynamic properties of the polymerization products were studied by IR, 1H NMR, WAXD and DSCS. The results of 1H NMR and WAXD test showed that the PPDO products with high purity and the same crystal form could be obtained by decompression method, and at 12 h of decompression, The monomer conversion reached the maximum value of 86.5% and reached 84.5% when the monomer was initiated for 6 h. When the initiator was not added, the monomer conversion reached 84.5%. The results of DSC test showed that both the melting temperature and crystallization temperature of the product increased first and then decreased with the prolongation of the decompression time and initiation time, compared with the traditional method, the monomer conversion was only 81.1% and the DSC test showed that the melt temperature and crystallization temperature of the product increased first and then decreased with the prolongation of the decompression time and initiation time. The vacuum assisted method can obtain higher yield and effectively avoid the impurities introduced by solution-precipitation purification.
【作者单位】：四川大学物理科学与技术学院;
【基金】：国家国际科技合作专项资助项目(2013DFB50280)
【分类号】：TQ317

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