丙烯酸十八酯原子转移自由基聚合
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摘要
本文成功地利用原子转移自由基聚合方法进行丙烯酸十八酯的本体、溶液聚合及丙烯酸十八酯和苯乙烯的嵌段共聚合，考察了聚合温度、催化剂用量、引发剂用量、聚合时间、[ODA]_0／[EBP]_0比例等因素对聚合动力学、聚合物分子量和分子量分布的影响，计算了不同条件下的动力学数据。用ATRP法制备的苯乙烯作大分子引发剂引发丙烯酸十八酯的原子转移自由基嵌段共聚合，合成了分子量分布较窄的ABA型嵌段聚合物P(ODA-b-St-b-ODA)。并且用得到的ABA型嵌段聚合物继续进行ATRP聚合以期得到交联的具有形状记忆功能的智能型凝胶材料。用凝胶渗透色谱、核磁共振、差示扫描量热法、X-射线粉末衍射对聚合物进行了一系列的表征。发现丙烯酸十八酯的本体聚合和溶液聚合均具有“活性”／可控聚合特征，且溶液聚合比本体聚合可控性好，聚合物分子量分布较窄，在体系[ODA_0：[EBP]_0：[FeCl_2.4H_2O]_0：[PPh_3]_0配比为100：1：1～1.5：2～3时聚合反应可控性较好。苯乙烯大分子引发的苯乙烯和丙烯酸十八酯的嵌段共聚同样具有“活性”／可控聚合特征，所得嵌段聚合物PODA-b-PSt-b-PODA分子量分布较窄(M_w／M_n在1.34～1.43之间)。用嵌段聚合物继续ATRP反应，没有能够得到预期的完全交联的凝胶材料。
Bulk polymerization and solution polymerization of octadecyl acrylate(ODA) has been conducted successfully by atom transfer radical polymerization (ATRP).We also prepared ABA triblock colopolymer of styrene and octadecyl acrylate (ODA). The effects of polymerization temperature, amount of catalyst and initiator, reaction time and system molar ratios on the rates of ATRP of ODA was investigated. Molecular weight and moleculer weight distribution of polymer was also discussed in this paper. The apparent propagation rate constants (kpapp) under different conditions were calculated. Polystyrene (X-PSt-X) was further used as macroinitiator for the block copolymerization of styrene and octadecyl acrylate. Atom Transfer Radical Polymerization (ATRP) of triblock copolymers was also arranged for the sake of obtaining aptitude gel material with shape memory function. GPC, 'H-NMR, DSCU X-ray powder diffraction were used to characterize the polymer we prepared. We found that bulk polymerization and solution polymerization of octadecyl acrylate both had the characteristics of " living " / controlled radical polymerization. Solution polymerization could be better controlled than bulk polymerization generally. And the polymer had narrow moleculer weight distribution. When the ratio of [ODA]0:[EBP]0:[FeCl2.4H2O]0:[PPh3]0 was during the range of 100: 1 : 1~1.5: 2~3, reaction was controlled preferably. Block polymerization of styrene and octadecyl acrylate also had the characteristics of " living " / controlled radical polymerization. The ABA triblock copolymers are with narrow moleculer weight
distribution (Mw/Mn=1 .34~ 1.43).
Bulk polymerization and solution polymerization of octadecyl acrylate(ODA) has been conducted successfully by atom transfer radical polymerization (ATRP).We also prepared ABA triblock colopolymer of styrene and octadecyl acrylate (ODA). The effects of polymerization temperature, amount of catalyst and initiator, reaction time and system molar ratios on the rates of ATRP of ODA was investigated. Molecular weight and moleculer weight distribution of polymer was also discussed in this paper. The apparent propagation rate constants (kpapp) under different conditions were calculated. Polystyrene (X-PSt-X) was further used as macroinitiator for the block copolymerization of styrene and octadecyl acrylate. Atom Transfer Radical Polymerization (ATRP) of triblock copolymers was also arranged for the sake of obtaining aptitude gel material with shape memory function. GPC, 'H-NMR, DSCU X-ray powder diffraction were used to characterize the polymer we prepared. We found that bulk polymerization and solution polymerization of octadecyl acrylate both had the characteristics of " living " / controlled radical polymerization. Solution polymerization could be better controlled than bulk polymerization generally. And the polymer had narrow moleculer weight distribution. When the ratio of [ODA]0:[EBP]0:[FeCl2.4H2O]0:[PPh3]0 was during the range of 100: 1 : 1~1.5: 2~3, reaction was controlled preferably. Block polymerization of styrene and octadecyl acrylate also had the characteristics of " living " / controlled radical polymerization. The ABA triblock copolymers are with narrow moleculer weight
distribution (Mw/Mn=1 .34~ 1.43).
引文
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