化工学报
化工學報
화공학보
CIESC Jorunal
2015年
10期
4275-4280
,共6页
杜凯迪%唐二军%袁淼%刘少杰%赵地顺
杜凱迪%唐二軍%袁淼%劉少傑%趙地順
두개적%당이군%원묘%류소걸%조지순
离子液体%ATRP%微晶纤维素%界面%均化作用
離子液體%ATRP%微晶纖維素%界麵%均化作用
리자액체%ATRP%미정섬유소%계면%균화작용
ionic liquid%ATRP%microcrystalline cellulose%interface%homogenization
在氯化1-烯丙基-3-甲基咪唑([AMIM]Cl)离子液体中,采用原子转移自由基(ATRP)法接枝改性微晶纤维素,合成了微晶纤维素-g-甲基丙烯酸二乙氨基乙酯(MCC-g-PDEAEMA)聚合物分子刷。通过加入助溶剂形成均相反应体系,解决了功能性单体甲基丙烯酸二乙氨基乙酯(DEAEMA)在[AMIM]Cl离子液体中的溶解问题。分别研究了离子液体中均相与非均相的反应机理,结果表明:在均相体系中,生成的反应副产物PDEAEMA较少,聚合物分子刷的接枝效率较高,分子量分布窄,ATRP 反应可控性好。实验确定了均相体系最佳反应条件:CuBr/PMDETA/ DEAEMA/乙醇的摩尔比为1:15:150:300, MCC-g-PDEAEMA的接枝效率可达78.1%。通过红外、核磁和GPC对聚合物表征发现,侧链PDEAEMA成功地接枝到微晶纤维素骨架上,生成的聚合物分子刷的分子量分布均匀。
在氯化1-烯丙基-3-甲基咪唑([AMIM]Cl)離子液體中,採用原子轉移自由基(ATRP)法接枝改性微晶纖維素,閤成瞭微晶纖維素-g-甲基丙烯痠二乙氨基乙酯(MCC-g-PDEAEMA)聚閤物分子刷。通過加入助溶劑形成均相反應體繫,解決瞭功能性單體甲基丙烯痠二乙氨基乙酯(DEAEMA)在[AMIM]Cl離子液體中的溶解問題。分彆研究瞭離子液體中均相與非均相的反應機理,結果錶明:在均相體繫中,生成的反應副產物PDEAEMA較少,聚閤物分子刷的接枝效率較高,分子量分佈窄,ATRP 反應可控性好。實驗確定瞭均相體繫最佳反應條件:CuBr/PMDETA/ DEAEMA/乙醇的摩爾比為1:15:150:300, MCC-g-PDEAEMA的接枝效率可達78.1%。通過紅外、覈磁和GPC對聚閤物錶徵髮現,側鏈PDEAEMA成功地接枝到微晶纖維素骨架上,生成的聚閤物分子刷的分子量分佈均勻。
재록화1-희병기-3-갑기미서([AMIM]Cl)리자액체중,채용원자전이자유기(ATRP)법접지개성미정섬유소,합성료미정섬유소-g-갑기병희산이을안기을지(MCC-g-PDEAEMA)취합물분자쇄。통과가입조용제형성균상반응체계,해결료공능성단체갑기병희산이을안기을지(DEAEMA)재[AMIM]Cl리자액체중적용해문제。분별연구료리자액체중균상여비균상적반응궤리,결과표명:재균상체계중,생성적반응부산물PDEAEMA교소,취합물분자쇄적접지효솔교고,분자량분포착,ATRP 반응가공성호。실험학정료균상체계최가반응조건:CuBr/PMDETA/ DEAEMA/을순적마이비위1:15:150:300, MCC-g-PDEAEMA적접지효솔가체78.1%。통과홍외、핵자화GPC대취합물표정발현,측련PDEAEMA성공지접지도미정섬유소골가상,생성적취합물분자쇄적분자량분포균균。
The microcrystalline cellulose-g-poly[2-(diethylamino)ethyl methacrylate] (MCC-g-PDEAEMA) polymer brushes were synthesized under control by atom transfer radical polymerization (ATRP) in the ionic liquid 1-allyl-3-methylimidazolium chloride ([AMIM]Cl). Ethyl alcohol was used as the cosolvent to form a homogeneous system and solve the problem that the functional monomerN,N-diethylamino-2-ethyl methacrylate (DEAEMA) hardly dissolved in [AMIM]Cl. The synthetic mechanism of heterogeneous system and homogeneous system in [AMIM]Cl was analyzed. The experiments showed that the byproduct PDEAEMA in the homogeneous system was reduced and the grafting efficiency of the polymer brushes was improved. Meanwhile, the molecular weight distribution was narrow and ATRP was easily controlled. Optimum reaction conditions in the homogeneous system were attained at CuBr/PMDETA/DEAEMA/ethyl alcohol molar ratio of 1:15:150:300. The grafting efficiency could reach to 78.1%. MCC-g-PDEAEMA was characterized through FTIR spectroscopy,1H NMR spectroscopy and GPC. The results proved that the PDEAEMA side chains were covalently bonded to the MCC backbone and the molecular weight distribution of the polymer brushes were even.