季铵盐型聚醚改性三硅氧烷的合成与性能测试
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摘要
以1,1,1,3,5,5,5-七甲基三硅氧烷(HTSO)和烯丙基环氧基聚醚(APEE)为原料,在氯铂酸催化下,经硅氢加成反应先制得环氧基聚醚改性三硅氧烷(ETS),ETS再与N,N-二甲基十二烷基叔胺(DMA12)进行开环反应合成一类新型表面活性剂——季铵盐型聚醚改性三硅氧烷(QATS)。通过IR和1HNMR对QATS的结构进行了表征,并对QATS的表面张力、发泡性、乳化力进行了测试。同时对QATS的合成条件进行了优化,最佳合成条件为:n(ETS)∶n(DMA12)=1∶1.05,反应时间6 h,反应温度80℃。性能测试结果表明:QATS溶液的临界胶束浓度(cmc)为1.0 g/L,临界胶束浓度时的表面张力(γcmc)为21.08 m N/m;质量分数为0.1%的QATS发泡力为1.93,5 min时的稳泡力为0.857;质量分数为0.5%的QATS对汽油、乙酸乙酯、异戊醇和苯的乳化力良好。
Using 1,1,1,3,5,5,5-heptamethyltrisioxane(HTSO) and allyl polyoxyalkylene glycidolether(APEE) as raw materials and chloroplatinic acid as catalyst, the epoxy group trisiloxane(ETS) was synthesized through hydrosilylation reaction. Then a new kind of quaternary ammonium salt type polyether modified trisiloxane surfactant(QATS) was prepared through the ring-opening reaction of ETS with N,N-dimethyl dodecyl tertiary amine DMA12. The structure of QATS was characterized by IR and1 HNMR, and the surface tension,foaming properties and emulsifying power of QATS were measured. The QATS synthesis conditions were optimized as follows: n(ETS)∶n(DMA12) =1∶1.05, the reaction time was 6 h and the reaction temperature was80 ℃. The experimental results showed that the surface tension(γcmc) of QATS solution was 21.08 m N/m at the critical micelle concentration(cmc) of 1.0 g/L. The foaming power of 0.1%(mass fraction) QATS solution was 1.93 and foam stability after 5 min was 0.857. The 0.5%(mass fraction) of QATS had good emulsifying power to gasoline, ethyl acetate, isoamyl alcohol and benzene.
Using 1,1,1,3,5,5,5-heptamethyltrisioxane(HTSO) and allyl polyoxyalkylene glycidolether(APEE) as raw materials and chloroplatinic acid as catalyst, the epoxy group trisiloxane(ETS) was synthesized through hydrosilylation reaction. Then a new kind of quaternary ammonium salt type polyether modified trisiloxane surfactant(QATS) was prepared through the ring-opening reaction of ETS with N,N-dimethyl dodecyl tertiary amine DMA12. The structure of QATS was characterized by IR and1 HNMR, and the surface tension,foaming properties and emulsifying power of QATS were measured. The QATS synthesis conditions were optimized as follows: n(ETS)∶n(DMA12) =1∶1.05, the reaction time was 6 h and the reaction temperature was80 ℃. The experimental results showed that the surface tension(γcmc) of QATS solution was 21.08 m N/m at the critical micelle concentration(cmc) of 1.0 g/L. The foaming power of 0.1%(mass fraction) QATS solution was 1.93 and foam stability after 5 min was 0.857. The 0.5%(mass fraction) of QATS had good emulsifying power to gasoline, ethyl acetate, isoamyl alcohol and benzene.
引文
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[2]TAN Jing-lin,FENG Sheng-yu.Effect of counterions on micellizationof pyrrolidinium based silicone ionic liquids in aqueous solutions[J].Journal of Chemical&Engineering Data,2014,59(6):1 830-1 834.
[3]ZHANG Y,ZHANG G Y,HAN F.The spreading and superspreadingbehavior of new glucosamide-based trisiloxane surfactants on hydro-phobic foliag[J].Colloids Surf.A,2006,276:100-106.
[4]HALVERSON J D,MALDARELLI C,COUZIS A.Wetting of hydropho-bic substrates by nanodroplets of aqueous trisiloxane and alkyl polye-thoxylate surfactant solutions[J].Chemical Engineering Science,2009,64:4 657-4 667.
[5]KICKELBICK G,BAUER J,HUESING N.Aggregation behavior ofshort-chain PDMS-b-PEO diblock copolymers in aqueous solutions[J].Langmuir,2003,19:10 073-10 076.
[6]ZHANG Yue,HAN Fu.The spreading behaviour and spreading mech-anism of new glucosamide-based trisiloxane on polystyrene surfaces[J].Journal of Colloid and Interface Science,2009,337:211-217.
[7]POLICELLO G A.Terminally modified,amino,polyether siloxanes:US,6235681B1[P].2011-05-22.
[8]温福山,孔祥双,王维,等.一种新型阳离子三硅氧烷表面活性剂的合成及其表面性能[J].应用化学,2014,31(10):1 216-1 221.
[9]LEATHERMAN M D,POLICELLO G A,PENG W N,et al.Hydrolysisresistant organomodified trisiloxane ionic surfactants:US,20090176893A1[P].2009-07-09.
[10]黄良仙,李顺琴,李婷,等.聚醚氨基改性三硅氧烷的制备及性能[J].印染助剂,2014,31(6):21-26.
[11]黄良仙,李婷,李顺琴,等.新型氟硅表面活性剂的制备及其表面活性[J].陕西科技大学学报,2014,32(2):69-73.
[12]佟哲.端环氧基硅油环氧值测定方法的探讨[J].有机硅材料,2012,26(4):258-261.