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

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

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。

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 terpenebased 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.