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Citation: DING Wei, SUN Ying, LV Chongfu, JING Hui, YU Tao, QU Guangmiao. Synthesis of Star Polyacrylamide by Single Electron Transfer Living Radical Polymerization in Ionic Liquid System[J]. Chinese Journal of Applied Chemistry, ;2011, 28(10): 1148-1154. doi: 10.3724/SP.J.1095.2011.00620 shu

Synthesis of Star Polyacrylamide by Single Electron Transfer Living Radical Polymerization in Ionic Liquid System

DING Wei ^a,, ,
SUN Ying ^a,b ,
LV Chongfu ^a,b ,
JING Hui ^a ,
YU Tao ^a ,
QU Guangmiao ^a

1.
a Chemistry and Chemical Engineering College of Northeast Petroleum University, Provincial Key Laboratory of Oil & Gas Chemical Technology, Daqing 163318;
2.
b Guangfa Chemical Industry of Datong Coal Mine Group Co., Ltd, Datong

Corresponding author: DING Wei,
Received Date: 19 October 2010
Available Online: 30 December 2010
Fund Project: 国家科技重大专项(2008ZX05011) (2008ZX05011)黑龙江省自然科学基金重点项目(ZJG0507) (ZJG0507)黑龙江省自然科学基金青年基金(QC08C33)资助项目 (QC08C33)黑龙江省研究生创新科研基金(YJSCX2008-044HLJ)资助项目 (YJSCX2008-044HLJ)

A single electron transfer living radical polymerization(SET-LRP) is able to rapidly achieve high molecular mass,with excellent control of molecular mass distribution,represents a robust and versatile method for the rapid synthesis of macromolecules with defined architecture.The SET-LRP of acryl amide(AM) was investigated at 40℃ in 1-butyl,3-methyl tetrafluoroborate([Bmim]BF₄) ionic liquid,using Cu⁰ power/tris(2-dimethylamin ethyl) amine(Me₆-TREN) as catalyst,2,2-dibromomethyl-1,3-dibromopropane(PEBr₄) as initiator.The polymerization showed some "living" features:the conversion and ln([M]₀/[M]) increased linearly with time as well as the number-average molecular mass increased linearly with conversion.The star polyacrylamide(sPAM) prepared via SET-LRP was characterized by GPC and ¹H NMR to identify its polymerization mechanism,and the results showed that the polymer had the perfect functional chain ends and relatively low molecular mass distribution M_w/M_n≈1.26(M_n^GPC=14.1×10³,conversion rate is 43.4%),indicating a controlled polymerization.The effects of water,catalyst and initiator on polymerization were studied,and the dynamic experiments were carried out.A small amount of water added could accerlerate the polymerization,the apparent rate constants of propagation(k_p^app) were 0.04248 h^-1 and 0.14869 h^-1 for adding free water and 0.5 mL H₂O respectively;the control of polymerization could be improved with the presence of catalyst and increasing the concentration of initiator.The polymerization rate of SET-LRP increased with the amount of catalyst and initiator.In addition,M_n increased with the amount of catalyst or decreasing the amount of initiator and was closed to the theoretical molecular mass.The molecular mass distribution showed a decreasing trend,the minimum was about 1.26.The[Bmim]BF₄ ionic liquid was a good solvent to PEBr₄ and acryl amide,and the polymers were easily separated from the catalyst.
- single electron transfer living radical polymerization,
- ionic liquid,
- star polymer,
- acrylamide
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