常温酮肼自交联纳米环氧树脂乳液的制备与表征  

Preparation and characterization of ambient self cross-linkable epoxy nano emulsion modified by ketone and hydrazine

作　　者：袁腾[1] 周显宏[2] 王锋[1] 胡剑青[1] 涂伟萍[1] 

机构地区：[1]华南理工大学化学与化工学院广东省绿色化学产品技术重点实验室,广东广州510640 [2]东莞理工学院化学与环境工程学院,广东东莞523808

出　　处：《化工学报》2015年第6期2321-2328,共8页CIESC Journal

基　　金：中央高校基本科研业务费专项资金(2013ZM0072);广东省重大科技专项计划资金项目(2010A080406002);广东省科技计划项目(2013B090600004);广东省绿色化学产品技术重点实验室开放基金(GC201201);广州市国际科技交流与合作专项资金(2012J5100043)~~

摘　　要：以环氧树脂E-20合成了环氧月桂酸酯,以丙烯酸单体与双丙酮丙烯酰胺（DAAM）对其进行接枝改性,添加己二酸二酰肼（ADH）制备了常温酮肼自交联纳米环氧树脂乳液。以红外光谱仪表征了合成过程中各步产物及乳液固化后的结构,结果表明得到了设计结构的树脂,干燥后涂膜的FTIR谱图表明酮羰基与酰肼基发生交联反应生成了腙;DSC分析表明合成的树脂具有两个玻璃化温度（Tg）,分别为丙烯酸接枝环氧树脂和纯丙烯酸树脂的Tg,前者低于常温,表明可以实现常温自交联。在改性环氧树脂乳液的合成过程中,以粒径分析和综合性能分析对功能性单体配比进行了研究,结果发现当MAA与E-20质量比为11.0%~14.7%、DAAM的用量为2%~3%、m（ADH）/m（DAAM）为0.8~1.0时,制得的乳液具有良好的储存稳定性和涂膜性能。透射电镜及粒径测试表明乳液粒径为纳米级,约88 nm,且粒径分布均匀,基本呈稳定的球形结构。将所制备的纳米乳液配制成防腐涂料,性能测试表明该涂料具有良好的综合性能。Epoxy laurate was synthesized from epoxy resin E-20, and then modified by grafting with acrylic acid monomer and diacetone acrylamide（DAAM）, while by adding adipic acid dihydrazide（ADH）, to prepare a ketone and hydrazine self-cross-linking at room temperature nano epoxy resin emulsion. The structure of the products synthesized in each step and the emulsion after curing were characterized with infrared spectroscopy, which proved that the design resin structure was obtained. FTIR spectrum of the film of the emulsion showed that hydrazone was produced by ketone reaction with hydrazide. The glass transition temperature（Tg） of the resin was studied with DSC analysis. The synthetic resin had two Tg, the Tg of acrylic acid graft epoxy resin and the Tg of pure acrylic resin, respectively, and the Tg of acrylic acid graft epoxy resin was lower than room temperature, indicating that self-cross-linking reaction could occur at room temperature. The ratio of functional monomer was investigated with particle size analysis and integrated performance analysis during the synthesis process of the modified epoxy resin emulsion. When mass ratio of E-20 and MAA was 11.0%~14.7%, the amount of DAAM was 2%~3%, and m（ADH）/m（DAAM） was 0.8~1.0, good emulsion storage stability and film properties were obtained. The morphology and particle size of the emulsion were studied with transmission electron microscopy and particle size analysis, showing that particle size of emulsion was about 88 nm, and particle size distribution was uniform, existing substantially as stable spherical structure. Test results proved that the anti-corrosion coatings prepared from the nano epoxy emulsion showed good comprehensive performance.

关 键 词：酮肼自交联 丙烯酸改性 纳米粒子 乳液 粒度分布 

分 类 号：TQ631[化学工程—精细化工]