CN106317374A - 一种封闭型聚氨酯－环氧树脂复合乳液的制备方法 - Google Patents

一种封闭型聚氨酯－环氧树脂复合乳液的制备方法 Download PDF

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CN106317374A
CN106317374A CN201610681137.7A CN201610681137A CN106317374A CN 106317374 A CN106317374 A CN 106317374A CN 201610681137 A CN201610681137 A CN 201610681137A CN 106317374 A CN106317374 A CN 106317374A
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夏学云
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Abstract

本发明公开了一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，包括环氧树脂的开环和封闭型聚氨酯－环氧树脂复合乳液的合成。本发明通过提高环氧树脂的用量，较大辐度地提高乳液的耐腐蚀性能，从而制备出具有良好的稳定性和优异的防腐性能的复合乳液。

Description

一种封闭型聚氨酯－环氧树脂复合乳液的制备方法
技术领域
本发明涉及涂料科学技术领域，具体涉及一种封闭型聚氨酯-环氧树脂复合乳液的制备方法。
背景技术
众所周知，金属材料是一种应用非常广泛的工程材料。但这些金属材料与周围环境中的腐蚀介质接触会发生腐蚀反应，导致金属腐蚀每时每刻都在发生，给国民经济带来巨大损失因此，通过研宄金属材料的腐烛防护方法来减少金属腐蚀造成的经济损失对于国民经济的发展具有十分重要的意义。
防腐涂料的涂装防护不仅能保护金属制品免受腐蚀，而且还能赋予金属制品色彩和光泽等装饰性能，是目前应用最为广泛的金属材料保护方法之一。随着国内外相关法律法规对溶剂型涂料中的挥发性有机物（及有害空气污染物限制越来越严格环境友好、使用安全的水性金属防腐涂料成为了防腐涂料研究的热点。
环氧树脂改性聚氨酯成膜体系兼顾了聚氨酯和环氧树脂的优异性能，已成为水性金属防腐涂料领域重要的研究方向。常见的用于单组份涂料的聚氨酯环氧树脂复合乳液中环氧树脂用量有限，且乳液中残留的环氧基降低乳液稳定性，不能满足高要求的防腐需求。
发明内容
为解决现有技术存在的问题，本发明提供一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，通过提高环氧树脂的用量，较大辐度地提高乳液的耐腐蚀性能，从而制备出具有良好的稳定性和优异的防腐性能的复合乳液。
为实现上述目的，本发明采用的技术方案为：
一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，包括以下步骤：
1）环氧树脂的开环
称取50g双酚A 型环氧树脂溶解在N-甲基吡咯烷酮与丙酮的混合溶剂中，完全溶解后加入11.04g二乙醇胺，在75～80℃下开环反应8h左右冷却出料；
2）封闭型聚氨酯－环氧树脂复合乳液的合成
称取12g的甲苯二异氰酸酯和5.30g聚醚二元醇，于75℃下反应至—NCO值接近理论值，再根据实验配方设计量，于70℃下逐步加入1，4－丁二醇、二羟甲基丙酸反应至—NCO值接近理论值，制得端—NCO聚氨酯预聚体，然后加入封闭剂甲乙酮肟，70℃下反应30min，将预聚体的部分—NCO基封闭，后加入上述制备的开环的双酚A型环氧树脂，于60～70℃下与剩余的—NCO完全反应。视体系粘度加入适量的N—甲基吡咯烷酮与丙酮混合溶剂调节粘度，降温至40℃以下，经三乙胺中和后，在7000 rpm强剪切下加水分散制得封闭型聚氨酯－环氧树脂复合乳液。
所述N-甲基吡咯烷酮与丙酮的混合溶剂中，N-甲基吡咯烷酮与丙酮的质量比为1:1。
所述的—NCO基为异氰酸酯基。
涂膜的制备：对50 mm×120 mm×0.3 mm的马口铁片进行打磨、醇洗和烘干等预处理后，采用人工刷涂法将乳液均勻涂刷在马口铁板上，表干后放入120~130 ℃恒温烘箱中烘烤约40 min，再于25℃下放置24 h。
本发明的有益效果：
1）本发明采用小分子胺类化合物对环氧树脂开环，消除环氧基对乳液存稳定性的负面影响。
2）为实现树脂的水性化，本发明采用的二羟甲基丙酸，在聚合物分子设计中，主要起亲水扩链的作用，在分子链中引入亲水的，使其能水分散成稳定的乳液。
3）为解决常规环氧树脂改性聚氨酷方法中环氧树脂改性用量不足的问题，进一步提高涂膜的防腐烛性能，本发明利用封闭型聚氨醋合成方法对基团的“保护”与“释放”的灵活性，采用封闭剂对聚氨酯预聚体上的端基进行部分封闭后再将环氧树脂接枝到聚氨酯分子链中，形成“潜伏”的交联点，减小乳液合成阶段体系的交联密度，从而可以大幅提高环氧树脂的改性用量而不影响乳液性能。
4）本发明采用的甲乙酮肟对异氰酸酯具有较高的封闭速率和合适的解封温度，是合适的封闭剂选择。
具体实施方式
下面结合实施例对本发明的具体实施技术方案做进一步详细说明。
一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，包括以下步骤：
1）环氧树脂的开环
称取50g双酚A 型环氧树脂溶解在N-甲基吡咯烷酮与丙酮的混合溶剂中，完全溶解后加入11.04g二乙醇胺，在75～80℃下开环反应8h左右冷却出料；
2）封闭型聚氨酯—环氧树脂复合乳液的合成
称取12g的甲苯二异氰酸酯和5.30g聚醚二元醇，于75℃下反应至—NCO值接近理论值，再根据实验配方设计量，于70℃下逐步加入1，4－丁二醇、二羟甲基丙酸反应至—NCO值接近理论值，制得端—NCO聚氨酯预聚体，然后加入封闭剂甲乙酮肟，70℃下反应30min，将预聚体的部分—NCO基封闭，后加入上述制备的开环的双酚A型环氧树脂，于60～70℃下与剩余的—NCO完全反应。视体系粘度加入适量的N—甲基吡咯烷酮与丙酮混合溶剂调节粘度，降温至40℃以下，经三乙胺中和后，在7000 rpm强剪切下加水分散制得封闭型聚氨酯－环氧树脂复合乳液。
所述N-甲基吡咯烷酮与丙酮的混合溶剂中，N-甲基吡咯烷酮与丙酮的质量比为1:1。
所述的—NCO基为异氰酸酯基。
涂膜的制备：对50 mm×120 mm×0.3 mm的马口铁片进行打磨、醇洗和烘干等预处理后，采用人工刷涂法将乳液均勻涂刷在马口铁板上，表干后放入120~130 ℃恒温烘箱中烘烤约40 min，再于25℃下放置24 h。
对不同种类涂膜进行浸泡腐蚀实验，得到的结果如下：
表格中的非封闭型是指非封闭型聚氨酯-环氧树脂涂膜乳液，环氧树脂用量为8%。
涂膜防腐蚀性能研究表明：封闭型聚氨酯环氧树脂成膜体系的耐腐蚀性能远远强于非封闭型聚氨酯环氧树脂成膜体系。环氧树脂用量为24%的封闭型聚氨酯—环氧树脂涂膜，耐3.5%盐水15天以上，耐0.1mol/L NaOH溶液12天以上，耐0.1mol/L H2SO4溶液10天以上。
以上显示和描述了本发明的材料组成、制备方法和技术特点。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (3)

1. 一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，其特征在于，包括以下步骤：
1）环氧树脂的开环
称取50g双酚A 型环氧树脂溶解在N-甲基吡咯烷酮与丙酮的混合溶剂中，完全溶解后加入11.04g二乙醇胺，在75～80℃下开环反应8h左右冷却出料；
2）封闭型聚氨酯－环氧树脂复合乳液的合成
称取12g的甲苯二异氰酸酯和5.30g聚醚二元醇，于75℃下反应至—NCO值接近理论值，再根据实验配方设计量，于70℃下逐步加入1，4－丁二醇、二羟甲基丙酸反应至—NCO值接近理论值，制得端—NCO聚氨酯预聚体，然后加入封闭剂甲乙酮肟，70℃下反应30min，将预聚体的部分—NCO基封闭，后加入上述制备的开环的双酚A型环氧树脂，于60～70℃下与剩余的—NCO完全反应。视体系粘度加入适量的N—甲基吡咯烷酮与丙酮混合溶剂调节粘度，降温至40℃以下，经三乙胺中和后，在7000 rpm强剪切下加水分散制得封闭型聚氨酯－环氧树脂复合乳液。
2.根据权利要求1所述的一种封闭型聚氨酯－环氧树脂复合乳液的制备方法，其特征在于，所述N-甲基吡咯烷酮与丙酮的混合溶剂中，N-甲基吡咯烷酮与丙酮的质量比为1:1。
3.根据权利要求1所述的一种封闭型聚氨酯-环氧树脂复合溶液的制备方法，其特征在于，所述的—NCO基为异氰酸酯基。
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CN108409932A (zh) * 2018-02-12 2018-08-17 常州光辉化工有限公司 一种改性环氧树脂的制备方法及其在重防腐涂料中的应用
CN110272674A (zh) * 2019-05-16 2019-09-24 Ppg涂料(天津)有限公司 单组份底漆组合物
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CN114197212A (zh) * 2022-01-30 2022-03-18 苏州大学 一种水性聚氨酯乳化改性环氧树脂硬挺剂及其制备方法
CN114197212B (zh) * 2022-01-30 2023-11-10 苏州大学 一种水性聚氨酯乳化改性环氧树脂硬挺剂及其制备方法

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Application publication date: 20170111