CN107216800A - 一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法 - Google Patents

一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法 Download PDF

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CN107216800A
CN107216800A CN201710506736.XA CN201710506736A CN107216800A CN 107216800 A CN107216800 A CN 107216800A CN 201710506736 A CN201710506736 A CN 201710506736A CN 107216800 A CN107216800 A CN 107216800A
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Abstract

本发明公开了一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法,将纳米硫酸钡粉末，用聚氨基葡糖溶胶进行包裹后得聚氨基葡糖分子膜包覆改性纳米硫酸钡，与聚醚三元醇N330混合后进行插层得聚醚三元醇N330插层改性纳米硫酸钡复合物，与二苯基甲烷二异氰酸酯一起为主要合成原料，合成出水性聚氨酯预聚体，加入交联剂在红外干燥箱中进行交联后，进行乳化分散形成涂料,本发明的涂料具有较好的实际应用价值，也具有良好的疏水性能，适用于建筑、装饰、工业制造等用途且制备方法，其工艺条件简单，操作方便，易实现。

Description

一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法
技术领域
本发明涉及聚氨酯涂料，更具体地，涉及一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法。
背景技术
纳米硫酸钡是一种新型的无机材料，它既具有普通硫酸钡的特点，又具有新的特殊功能，纳米硫酸钡颗粒，由于具有表面效应、量子隧道效应、尺寸效应等重要的纳米结构特性，使得它的各种物理化学特性与普通材料的性能大有不同，作为一种新颖的高功能性的无机填充材料，它在聚合物复合材料、医学、陶瓷、油墨、涂料、造纸等诸多领域的应用前景都较为广阔。
聚氨酯树脂是一种具有高强度、抗撕裂性和高耐磨性的高分子材料，广泛应用于日常生活、农业生产和医疗等领域中。聚氨酯树脂在涂料工业中也有广泛应用，由其制成的聚氨酯涂料可分为双组分聚氨酯涂料和单组分聚氨酯涂料两大类。
张晗在《聚乙烯-硫酸钡纳米复合材料的制备和表征》一文中利用乙二胺四乙酸二钠（EDTA）络合法一步沉淀制备纳米硫酸钡溶液，制备出纳米硫酸钡，并用硬脂酸对硫酸钡表面进行表面有机修饰后，采用熔融共混填充的方法填充到PE基体中，使用的设备为双螺杆挤出造粒机，从而改善了硫酸钡颗粒的稳定性，但纳米硫酸钡仍有一定的团聚现象颗粒很小。
发明内容
本发明目的为了弥补已有技术的缺陷，提高稳定性与疏水性，提供一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法。
本发明是通过以下技术方案实现的：
一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，包括以下步骤：
（1）将2-5重量份的聚氨基葡糖加入适量醋酸中配置成0.1-1mol/L聚氨基葡糖的稀冰醋酸溶液，控制溶液pH值为4.5-5.5，加入20-30重量份硫酸钡，搅拌30-50分钟，调节溶液pH值为10-12，搅拌反应30-50分钟，过滤干燥6-12小时后，通过研磨机研磨成粉状，得改性纳米硫酸钡，待用；
（2）将改性纳米硫酸钡与25-30重量份聚醚三元醇N330，混合，用三辊机研磨，制得聚醚三元醇N330插层改性纳米硫酸钡复合物；
（3）将步骤（2）所得聚醚三元醇N330插层改性纳米硫酸钡复合物干燥脱水12-24小时后缓慢加入20-25二苯基甲烷二异氰酸酯,与0.02-1重量份催化剂，在惰性气体氛围中80-85℃反应15-20分钟后，加入适量丙酮稀释后反应3-4小时后降温至60-70℃,加入5-10重量份二羟甲基丙酸、0.1-0.3重量份戊二醛在红外干燥箱中反应1-12小时，待用；
（4）将步骤（3）所得产物加入适量三乙胺进行反应20-30分钟，中和至pH值为6-7，室温下反应20-30分钟，加入去离子水高速搅拌进行乳化分散后，既得所述疏水改性纳米硫酸钡填充水性聚氨酯涂料。
所述调节pH是使用0.5mol/L氢氧化钠溶液。
所述催化剂为稀土复合催化剂。
所述惰性气体为氮气。
所述的红外干燥箱中反应温度为40-50℃。
本发明的优点是：
本发明将纳米硫酸钡粉末，用聚氨基葡糖溶胶进行包裹后得聚氨基葡糖分子膜包覆改性纳米硫酸钡，与聚醚三元醇N330混合后进行插层得聚醚三元醇N330插层改性纳米硫酸钡复合物，以聚醚三元醇N330插层改性纳米硫酸钡复合物、二苯基甲烷二异氰酸酯为主要合成原料，加入稀土复合催化剂，合成出水性聚氨酯预聚体，加入交联剂在红外干燥箱中进行交联后，进行乳化分散形成涂料；聚氨基葡糖采用电荷作用与纳米硫酸钡结合，使得硫酸钡的亲水性降低，改性纳米硫酸钡表面的羟基与聚氨酯分子链的极性基团相互作用，使聚氨酯分子链能较好地插入到硫酸钡之间，加入交联剂后聚氨基葡糖自身进行交联，聚氨酯预聚体进行交联，聚氨基葡糖与聚氨酯预聚体之间进行交联，三者的协同效应，使体系形成稳定的体系，本发明的涂料具有较好的实际应用价值，也具有良好的疏水性能，适用于建筑、装饰、工业制造等用途且制备方法，其工艺条件简单，操作方便，易实现。
具体实施方式
一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，包括以下步骤：
（1）将4重量份的聚氨基葡糖加入适量醋酸中配置成0.5mol/L聚氨基葡糖的稀冰醋酸溶液，控制溶液pH值为4.5-5.5，加入25重量份硫酸钡，搅拌40分钟，调节溶液pH值为10-12，搅拌反应40分钟，过滤干燥9小时后，得改性纳米硫酸钡，待用；
（2）将改性纳米硫酸钡与28重量份聚醚三元醇N330，混合，用三辊机研磨，制得聚醚三元醇N330插层改性纳米硫酸钡复合物；
（3）将步骤（2）所得聚醚三元醇N330插层改性纳米硫酸钡复合物干燥脱水18小时后缓慢加入23二苯基甲烷二异氰酸酯,与0.1重量份催化剂，在惰性气体氛围中85℃反应15分钟后，加入适量丙酮稀释后反应3.5小时后降温至65℃,加入8重量份二羟甲基丙酸、0.2重量份戊二醛在红外干燥箱中反应10小时，待用；
（4）将步骤（3）所得产物加入适量三乙胺进行反应25分钟，中和至pH值为6-7，室温下反应25分钟，加入去离子水高速搅拌进行乳化分散后，既得所述疏水改性纳米硫酸钡填充水性聚氨酯涂料。
所述调节pH是使用0.5mol/L氢氧化钠溶液。
所述催化剂为稀土复合催化剂。
所述惰性气体为氮气。
所述的红外干燥箱中反应温度为40-50℃。

Claims (5)

1.一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，其特征在于，包括以下步骤：
（1）将2-5重量份的聚氨基葡糖加入适量醋酸中配置成0.1-1mol/L聚氨基葡糖的稀冰醋酸溶液，控制溶液pH值为4.5-5.5，加入20-30重量份硫酸钡，搅拌30-50分钟，调节溶液pH值为10-12，搅拌反应30-50分钟，过滤干燥6-12小时后，通过研磨机研磨成粉状，得改性纳米硫酸钡，待用；
（2）将改性纳米硫酸钡与25-30重量份聚醚三元醇N330，混合，用三辊机研磨，制得聚醚三元醇N330插层改性纳米硫酸钡复合物；
（3）将步骤（2）所得聚醚三元醇N330插层改性纳米硫酸钡复合物干燥脱水12-24小时后缓慢加入20-25二苯基甲烷二异氰酸酯,与0.02-1重量份催化剂，在惰性气体氛围中80-85℃反应15-20分钟后，加入适量丙酮稀释后反应3-4小时后降温至60-70℃,加入5-10重量份二羟甲基丙酸、0.1-0.3重量份戊二醛在红外干燥箱中反应1-12小时，待用；
（4）将步骤（3）所得产物加入适量三乙胺进行反应20-30分钟，中和至pH值为6-7，室温下反应20-30分钟，加入去离子水高速搅拌进行乳化分散后，既得所述疏水改性纳米硫酸钡填充水性聚氨酯涂料。
2.根据权利要求1一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，其特征在于，所述调节pH是使用0.5mol/L氢氧化钠溶液。
3.根据权利要求1一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，其特征在于，所述催化剂为稀土复合催化剂。
4.根据权利要求1一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，其特征在于，所述惰性气体为氮气。
5.根据权利要求1一种疏水改性纳米硫酸钡填充水性聚氨酯涂料的制备方法，其特征在于，所述的红外干燥箱中反应温度为40-50℃。
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Cited By (1)

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CN111684020A (zh) * 2018-02-08 2020-09-18 毕克化学有限公司 层状硅酸盐的分层方法

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