CAJ | 학술논문

将2-溴代异丁酰溴和蓖麻油的羟基按物质的量比1∶1进行酯化反应,一步法合成蓖麻油基的活性聚合用原子转移自由基聚合( ATRP)引发剂,采用FT-IR、1H NMR和13C NMR对其结构进行表征。红外谱图中3500 cm-1处的羟基的伸缩振动峰减弱,1740 cm-1处的酯基峰增强,表明蓖麻油中的羟基官能团基转变为酯基,溴代异丁酰基官能团成功接枝到蓖麻油分子上,1H NMR和13 C NMR谱图的分析结果进一步证明蓖麻油基ATRP引发剂的合成和结构的正确性。采用单体/引发剂/溴化亚铜/配体物质的量之比100∶1∶0.5∶1,反应温度60℃(苯乙烯80℃)的聚合反应体系,GPC、1H NMR和13C NMR谱图结果显示,蓖麻油基ATRP引发剂可以高效的引发甲基丙烯酸甲酯,以及苯乙烯的ATRP聚合反应,整个过程高效和可控制。
장2-추대이정선추화비마유적간기안물질적량비1∶1진행지화반응,일보법합성비마유기적활성취합용원자전이자유기취합( ATRP)인발제,채용FT-IR、1H NMR화13C NMR대기결구진행표정。홍외보도중3500 cm-1처적간기적신축진동봉감약,1740 cm-1처적지기봉증강,표명비마유중적간기관능단기전변위지기,추대이정선기관능단성공접지도비마유분자상,1H NMR화13 C NMR보도적분석결과진일보증명비마유기ATRP인발제적합성화결구적정학성。채용단체/인발제/추화아동/배체물질적량지비100∶1∶0.5∶1,반응온도60℃(분을희80℃)적취합반응체계,GPC、1H NMR화13C NMR보도결과현시,비마유기ATRP인발제가이고효적인발갑기병희산갑지,이급분을희적ATRP취합반응,정개과정고효화가공제。
Castor oil based atom transfer radical polymerization ( ATRP ) initiator was synthesized by one-pot reaction of 2-bromoisobutyryl bromide with hydroxyl group in castor oil under hydroxyl-to-bromide molar ratio of 1∶1 and characterized by means of FT-IR, 1H NMR and 13C NMR . The results showed that the esterification for the synthesis of castor oil based ATRP initiator is prompt and highly efficient. In FT-IR spectrum, the conversion of hydroxyl group to ester group resulted in the decrease in the intensity of peak at 3500 cm-1 corresponding to hydroxyl group and increase of peak at 1740 cm-1 corresponding to ester group. This indicated that 2-bromoisobutyryl group was grafted on castor oil successfully. Subsequently, the castor oil based ATRP initiator was used to trigger the ATRP of methyl methacrylate ( MMA) and styrene ( St) under the condition of feeding molar ratio (monomer/initiator/CuBr/ligand) of 100∶1∶0. 5∶1 and reaction temperature 60 ℃ for MMA and 80 ℃ for St, respectively. GPC curves and spectra of 1H NMR and 13C NMR showed that polymerization process of MMA, as well as St, was highly efficient and well controlled.