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双核水杨醛亚胺中性镍催化MMA本体聚合
Bulk polymerization of methyl methacrylate with dinuclear neutral nickel(Ⅱ) catalyst.
【摘要】 经烷基化、甲酰化、Schiff碱缩合反应,制得水杨醛亚胺配体(3),其Na盐与trans-[NiCl(Ph)(PPh3)2]反应合成了中性镍配合物(4){[[O-(3-Cyclohexanyl)(5-CH3)C6H2-ortho-C(H)=N-2,6-C6H3(i-Pr)2]Ni(Ph3P)(Ph)]2-CH2},以GC-MS,1H NMR对中间产物及配合物进行了表征.在Al(i-Bu)3的助催化作用下,配合物(4)能有效催化MMA聚合.考察了温度、时间、Al/Cat(4)和MMA/Cat(4)等对聚合反应的影响.在Al/Cat(4)为10,聚合温度为60℃,聚合时间为15 h,MMA/Cat(4)为1 000的条件下,催化MMA聚合的单体转化率为69.9%,所得PMMA的相对分子质量分布为2.02.
【Abstract】 Substituted salicyladimine ligand(3) was prepared by alkylation,formulation and condensation,it’s sodiumsalt reacted with trans- giving the neutral nickel(Ⅱ) complex(4) {[[O-(3-Cy-clohexanyl)(5-CH3)C6H2-ortho-C(H)=N-2,6-C6H3-(i-Pr)2]Ni(Ph3P)(Ph)]2CH2}.All intermediates and neutral complex(4) were characterized by GC-MS,1H NMR.The complex(4) activated by Al(i-Bu)3 can catalyze MMA polymerization effectively.The effect of polymerization parameters,such as temperature,time,molar ratios of Al/Cat(4),and MMA/Cat(4) were studied in detail.At the polymerization conditions: Al/Cat(4)=10;MMA/Cat(4)=1000;60 ℃;15 h,the conversion of MMA reached 69.9%,and the polydispersity of PMMA was 2.02.
【Key words】 ortho cyclohexyl salicyladimine ligand; late transition metal; dinuclear neutral nickel catalyst; bulk polymerization; methyl methacrylate;
- 【文献出处】 浙江大学学报(理学版) ,Journal of Zhejiang University(Science Edition) , 编辑部邮箱 ,2006年01期
- 【分类号】O643.32
- 【被引频次】8
- 【下载频次】189