阴离子型聚硅氧烷改性萜烯基环氧树脂多元醇水分散体的制备、表征及微观结构

以萜烯基环氧树脂(TME)与新戊二醇(NPG)反应,合成了萜烯基环氧树脂基多元醇(T-N),再以端羟丙基聚硅氧烷(HTP)、2,4-甲苯二异氰酸酯(TDI)及2,2-二(羟甲基)丙酸(DMPA)改性T-N,制备了阴离子型聚硅氧烷改性萜烯基环氧树脂多元醇(T-N-S)水分散体,并以红外光谱(FT-IR)、核磁共振光谱(NMR)表征了多元醇的化学结构。研究了反应条件、改性剂HTP用量等对多元醇水分散体稳定性及微观结构的影响。结果表明:DMPA与TDI物质的量比为1∶2,丙酮为溶剂(用量为反应物总质量的1.5~2倍),丙酮回流温度(56℃)下反应3 h,再加入T-N及HTP,继续反应4 h,所合成的T-N-S能够较好地在水中分散。透射电子显微镜分析表明,当HTP用量为T-N质量的3%~12%时,制备的T-N-S水分散体粒子均为球形粒子,粒径范围100~300 nm。

Preparation,Characterization and Micro-structure of Anionic Polysiloxane Modified Terpene-based Epoxy Resin Polyol Dispersion

Terpene-based epoxy resin polyol (T-N) was prepared via the reaction of terpene-based epoxy resin(TME) and neopentyl glycol(NPG).Then the T-N was modified with hydroxypropyl terminated polysiloxane(HTP), 2,4 tolylene diisocyanate(TDI) and 2,2-bis (hydroxymethyl) propionic acid(DMPA) to obtain the anionic polysiloxane-modified terpene-based epoxy resin polyol (T-N-S) dispersion.The chemical structure of the T-N-S was characterized by FT-IR and NMR.The micro-morphology of T-N-S was determined by transmission electron microscopy (TEM) and particles size measurement.And the effects of reaction condition and siloxane content on the stability and micro-structure of the polyol dispersion were studied.T-N-S dispersion was obtained at the conditions of DMPA and TDI were mixed with the molar ratio 1∶2 in the presence of solvent acetone (the amount of solvent was 1.5-2 times based on the reactants mass) and refluxed at 56 ℃ for 3 h.Then HTP and T-N were added in to the reaction and continued to feflux for 4 h.The obtained T-N-S dispersion showed good stability and the particle size of the dispersion ranged from 100 to 300 nm when the dosage of HTP was 3%-12% of T-N by weight.