Electronic Supplementary Information Pvdf-hfp/ether-modified Polysiloxane Membranes Obtained via Airbrush Spraying as Active Separators for Application in Lithium Ion Batteries
Electronic Supplementary Information Pvdf-hfp/ether-modified Polysiloxane Membranes Obtained via Airbrush Spraying as Active Separators for Application in Lithium Ion Batteries
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通讯作者：
S. M. Seidel;S. Jeschke;P. Vettikuzha;H. Wiemhöfer
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作者：
S. M. Seidel;S. Jeschke;P. Vettikuzha;H. Wiemhöfer
侧链三甘醇烯丙基甲基醚2（PEO 3）的实验合成图S1：合成三甘醇烯丙基甲基醚2（PEO 3）的反应方案。采用BRESLOW和LIGHT的文献方法合成了乙二醇烯丙基甲基醚2。1将醇1（263.0 mL，275.6 g，1.6 mol，1.0 eq.）存在于具有机械搅拌器和滴液漏斗的IL三颈圆底烧瓶中，并用水/冰浴冷却至0 °C。将KOH（102.1 g，1.8 mol，1.1 eq.）添加到酒精中。搅拌1小时后，将烯丙基溴（140.5 mL，196.7 g，1.6 mol，1.0 eq.）在冷却下，在滴液漏斗上缓慢加入。搅拌3天后，用Büchner漏斗滤出沉淀的KBr，用正己烷洗涤滤饼。滤液经MgSO 4干燥，随后减压浓缩。蒸馏后，得到相应的乙二醇烯丙基甲基醚2，为透明无色液体（265.5g，1.3mol，产率：80%; bp.：66-68 ℃，2.1 × 10-1毫巴）。GC-MS（Cl）：m/z = 205 [M+H] +。图S2：合成聚硅氧烷-梳形-丙基（三环氧乙烷）4（PSx-PEO 3）的反应方案。聚硅氧烷PSx-PEO 3 4根据卡拉塔斯等人通过氢化硅烷化反应合成。2在加入KARSTEDT-催化剂Pt（dvs）下，将三甘醇烯丙基甲基醚2加入到聚甲基氢硅氧烷（PMHS）3中。获得呈澄清无色粘性液体的产物。
Experimental Synthesis of side chain triethylene glycol allyl methyl ether 2 (PEO3) Fig. S1: Reaction scheme of the synthesis of triethylene glycol allyl methyl ether 2 (PEO3). The synthesis of ethylene glycol allyl methyl ether 2 was done by a modified procedure of a literature instruction of BRESLOW and LIGHT. 1 Alcohol 1 (263.0 mL, 275.6 g, 1.6 mol, 1.0 eq.) was presented in a 1 L triple-neck round-bottom flask with a mechanic stirrer and a dropping funnel and cooled down to 0 °C with an water/ice bath. KOH (102.1 g, 1.8 mol, 1.1 eq.) was added to the alcohol. After stirring for 1 h, allyl bromide (140.5 mL, 196.7 g, 1.6 mol, 1.0 eq.) was slowly added over the dropping funnel under cooling. After 3 d of stirring, the precipitated KBr was filtered off by a Büchner funnel and the filter cake was washed with n-hexane. The filtrate was dried over MgSO 4 and subsequently concentrated under diminished pressure. After distillation, the corresponding ethylene glycol allyl methyl ether 2 was obtained as a clear and colorless liquid (265.5 g, 1.3 mol, yield: 80%; bp.: 66-68 °C, 2.1 x 10-1 mbar). GC-MS (CI): m/z = 205 [M+H] +. Synthesis of polysiloxane-comb-propyl(triethylene oxide) 4 (PSx-PEO3) Fig. S2: Reaction scheme of the synthesis of the polysiloxane-comb-propyl(triethylene oxide) 4 (PSx-PEO3). The polysiloxane PSx-PEO3 4 was synthesized via a hydrosilylation reaction according to KARATAS et al.. 2 Triethylene glycol allyl methyl ether 2 was added to polymethylhydrosiloxane (PMHS) 3 under addition of the KARSTEDT-catalyst Pt(dvs). The product was obtained as clear and colorless viscous liquid.