含双硫酯结构纳米二氧化硅的合成
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摘要
双硫酯类化合物是RAFT聚合反应中常用的链转移催化剂。合成了2种含羧基官能团的双硫酯(1,2),并通过核磁氢谱、碳谱、质谱、红外光谱等对其结构进行了表征。在此基础上,通过酰胺化反应将双硫酯接枝到纳米二氧化硅表面,所制得的纳米粒子(4)和(5),通过元素分析,XRD,FT-IR,SEM(EDX),TEM和TGA等方法进行了表征。热重分析实验数据计算表明,纳米粒子(4)和(5)中双硫酯的接枝率分别为0. 28 mmol/g和0. 46 mmol/g。
Disulfide compounds are important chain transfer catalysts for RAFT polymerization. Two disulfide compounds( 1,2) containing carboxyl groups were synthesized and grafted onto the surface of Nano silica by amidation reaction. The disulfide compounds( 1,2) were characterized by1 H NMR,13 C NMR,MS,IR etc. All nanoparticles were fully characterized by elemental analysis,XRD,FT-IR,SEM( EDX),TEM and TGA. The TGA experimental data show that the grafting rate of disulfide in nano particles was 0. 28 mmol/g( 4) and 0. 46 mmol/g( 5) respectively.
Disulfide compounds are important chain transfer catalysts for RAFT polymerization. Two disulfide compounds( 1,2) containing carboxyl groups were synthesized and grafted onto the surface of Nano silica by amidation reaction. The disulfide compounds( 1,2) were characterized by1 H NMR,13 C NMR,MS,IR etc. All nanoparticles were fully characterized by elemental analysis,XRD,FT-IR,SEM( EDX),TEM and TGA. The TGA experimental data show that the grafting rate of disulfide in nano particles was 0. 28 mmol/g( 4) and 0. 46 mmol/g( 5) respectively.
引文
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[3]Moad G,Chiefari J,Bill Y K Chong,et al.Living free radical polymerization with reversible addition-fragmentation chain transfer(the life of RAFT)[C]//Macromolecules 99:Polymers in the New Millennium Conference.1999.
[4]Favier A.Experimental Requirements for an Efficient Control of Free-Radical Polymerizations via the Reversible Addition-Fragmentation Chain Transfer(RAFT)Process[J].Macromolecular Rapid Communications,2010,27(9):653-692.
[5]Moad G,Rizzardo E,Thang S H.Radical addition-fragmentation chemistry in polymer synthesis[J].Polymer,2008,49(5):1079-1131.
[6]Christopher J F,Robert J H,Duc N,et al.Ab Initio Emulsion Polymerization by RAFT-Controlled Self-Assembly§[J].Macromolecular Symposia,2005,231(1):84-93.
[7]侯月平,陈志明,余文丰.二硫代苯甲酸合成新工艺研究[J].应用化工,2007,36(2):114-116.
[8]刘春华,潘才元.通过RAFT聚合制备Si O2/接枝共聚物纳米杂化粒子[J].高等学校化学学报,2008,29(2):404-408.
[9]Alonso F,Beletskaya I P,Yus M.Non-conventional methodologies for transition-metal catalysed carbon-carbon coupling:a critical overview.Part 1:The Heck reaction[J].Tetrahedron,2005,61(50):11771-11835.