CN108610942A - 一种丙烯酸酯改性聚氨酯防水涂料及其制备方法 - Google Patents

一种丙烯酸酯改性聚氨酯防水涂料及其制备方法 Download PDF

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CN108610942A
CN108610942A CN201810479481.7A CN201810479481A CN108610942A CN 108610942 A CN108610942 A CN 108610942A CN 201810479481 A CN201810479481 A CN 201810479481A CN 108610942 A CN108610942 A CN 108610942A
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乔启信
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ANHUI LANGKAIQI BUILDING MATERIALS Co Ltd
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Abstract

本发明公开一种丙烯酸酯改性聚氨酯防水涂料，包括以下重量份组分：丙烯酸酯15‑45份、聚醚多元醇50‑80份、甲苯二异氰酸酯12‑30份、果糖3‑7份、二羟甲基丙酸2‑6份、N‑甲基吡咯烷酮10‑30份、三乙胺4‑10份、催化剂0.02‑0.5份、偶氮二异丁腈1‑3份、去离子水10‑20份、无机填料30‑60份。其制备方法如下：聚醚多元醇、甲苯二异氰酸酯在催化剂的作用下，进行亲核加成反应，再与果糖、二羟甲基丙酸、丙烯酸酯进一步交联，中和、分散后，得上述防水涂料。本发明集中果糖、丙烯酸酯、聚氨酯三者优势，克服传统丙烯酸酯改性聚氨酯交联程度低的缺陷，可与不同极性的界面形成作用力，且耐高低温冲击、机械强度高、自净能力强。

Description

一种丙烯酸酯改性聚氨酯防水涂料及其制备方法
技术领域
本发明涉及聚氨酯防水涂料技术领域，具体涉及一种丙烯酸酯改性聚氨酯防水涂料及其制备方法。
背景技术
聚氨酯防水涂料是由异氰酸酯、聚醚等经加成聚合反应而成的含异氰酸酯基的预聚体，配以催化剂、无水助剂、无水填充剂、溶剂等，经混合等工序加工制成的单组分聚氨酯防水涂料。单一的水性聚氨酯涂料对非极性基材的粘结力低、抗老化性能差、耐水性较差，丙烯酸酯具有优良的抗老化性、耐候性、耐水性，与聚氨酯具有良好的互补性，因此，采用丙烯酸酯单体与聚氨酯进行加成是一种改良聚氨酯的常用方法，但是交联化程度不高，致使其力学性能和热稳定性仍未得到有效改善。
申请号为CN201510212511.4的专利，公开一种丙烯酸酯改性聚氨酯乳液型防水涂料及其制备方法，先合成聚氨酯预聚体和聚丙烯酸酯预聚体，再进行混合反应，制得上述涂料，克服了单一水性聚氨酯的不足，即粘结力低、抗老化性能差、耐水性较差，但是改性后的聚氨酯聚合度和交联度仍较低，其力学性质和热稳定性欠佳。
发明内容
针对现有技术的不足之处，本发明的目的在于提供一种丙烯酸酯改性聚氨酯防水涂料及其制备方法。
本发明的技术方案概述如下：
一种丙烯酸酯改性聚氨酯防水涂料，包括以下重量份组分：
优选的是，所述丙烯酸酯包括丙烯酸甲酯、丙烯酸乙酯、丙烯酸羟乙酯的一种或多种。
优选的是，所述聚醚多元醇包括聚丙二醇、聚乙内酯二元醇、聚四氢呋喃二醇的一种或多种。
优选的是，所述催化剂包括二月桂酸二丁基锡、辛酸亚锡、异辛酸铋的一种或多种。
优选的是，所述无机填料包括以下重量比组分：电气石粉20-30％、钛白粉15-25％、二氧化硅空心微球35-60％、滑石粉5-10％。
优选的是，所述无机填料平均粒径≤50μm。
本发明还提供上述一种丙烯酸酯改性聚氨酯防水涂料的制备方法，包括以下步骤：
S1：将聚醚多元醇、甲苯二异氰酸酯、催化剂置于反应釜中，抽真空后，充入80-120KPa氮气，并加热至80-100℃，进行亲核加成反应，得聚氨酯预聚体；
S2：待聚氨酯预聚体自然冷却至70℃，加入果糖和二羟甲基丙酸，搅拌反应1-2h，期间，持续性滴加甲基吡咯烷酮，降低粘度，反应至-NCO含量低于4％，得果糖改性聚氨酯预聚体；
S3：向果糖改性聚氨酯预聚体分散于去离子水中，并滴加丙烯酸酯，待丙烯酸酯充分溶胀后，升温至80℃，加入偶氮二异丁腈，反应3h，得丙烯酸酯改性聚氨酯壳-核复合乳液；
S4：40℃下，向丙烯酸酯改性聚氨酯壳-核复合乳液中加入三乙胺，进行中和反应，再加入无机填料，以4000-5000rpm的转速搅拌1h，并同时进行超声辅助分散，制得所述丙烯酸酯改性聚氨酯防水涂料。
本发明的有益效果：
(1)不同于传统丙烯酸酯改良聚氨酯的方法，本发明先通过多羟基果糖对聚氨酯预聚体进行预处理，生成高交联度的网状结构，再采用丙烯酸酯单体对聚氨酯进一步改性，集中了果糖的高聚合性和环保性、丙烯酸酯的耐户外老化性和耐候性、聚氨酯的柔韧性和抗寒性等优点，使三者优势有机结合起来，将聚氨酯热分解温度提高至374℃，拉伸强度提高至2.6MPa，断裂伸长率提高至548％，明显加强了聚氨酯的综合性能。
(2)本发明引入含电气石粉、钛白粉、二氧化硅空心微球及滑石粉的填料，在提高防水涂料机械强度的同时，提高了涂料的防污清洁能力，绿色环保。
具体实施方式
下面结合实施例对本发明做进一步的详细说明，以令本领域技术人员参照说明书文字能够据以实施。
实施例1
S1：将50份聚丙二醇、12份甲苯二异氰酸酯、0.02份二月桂酸二丁基锡置于反应釜中，抽真空后，充入80KPa氮气，并加热至80℃，进行亲核加成反应，得聚氨酯预聚体；
S2：待聚氨酯预聚体自然冷却至70℃，加入3份果糖和2份二羟甲基丙酸，搅拌反应1h，期间，持续性滴加10份甲基吡咯烷酮，降低粘度，反应至-NCO含量低于4％，得果糖改性聚氨酯预聚体；
S3：向果糖改性聚氨酯预聚体分散于10份去离子水中，并滴加15份丙烯酸甲酯，待丙烯酸甲酯充分溶胀后，升温至80℃，加入1份偶氮二异丁腈，反应3h，得丙烯酸酯改性聚氨酯壳-核复合乳液；
S4：40℃下，向丙烯酸酯改性聚氨酯壳-核复合乳液中加入4份三乙胺，进行中和反应，再加入30份无机填料，该无机填料平均粒径≤50μm，由30％电气石粉、25％钛白粉、35％二氧化硅空心微球、10％滑石粉组成，并以4000rpm的转速搅拌1h，同时进行超声辅助分散，制得所述丙烯酸酯改性聚氨酯防水涂料。
实施例2
丙烯酸乙酯30份、聚乙内酯二元醇65份、甲苯二异氰酸酯21份、果糖5份、二羟甲基丙酸4份、N-甲基吡咯烷酮20份、三乙胺7份、辛酸亚锡0.26份、偶氮二异丁腈2份、去离子水15份、无机填料45份。
电气石粉15％、钛白粉20％、二氧化硅空心微球47.5％、滑石粉7.5％。
步骤同实施例1，区别在于：
S1：总氮压力为100KPa，加热温度为90℃；
S2：搅拌反应时间为1.5h；
S4：搅拌转速为4500rpm。
实施例3
丙烯酸羟乙酯45份、聚四氢呋喃二醇80份、甲苯二异氰酸酯30份、果糖7份、二羟甲基丙酸6份、N-甲基吡咯烷酮10-30份、三乙胺10份、异辛酸铋0.5份、偶氮二异丁腈3份、去离子水20份、无机填料60份。
电气石粉20％、钛白粉15％、二氧化硅空心微球60％、滑石粉5％。
步骤同实施例1，区别在于：
S1：总氮压力为120KPa，加热温度为100℃；
S2：搅拌反应时间为2h；
S4：搅拌转速为5000rpm。
按照GB/T16777-2008《聚氨酯防水涂料》对实施例1-3进行性能测定，性能分析如下表所示。
由上表可知，本发明生产的改性聚氨酯防水涂料满足I型聚氨酯防水涂料基本标准要求，具有优异的热稳定性、耐水性、耐受性及力学性能。
尽管本发明的实施方案已公开如上，但其并不仅仅限于说明书和实施方式中所列运用，它完全可以被适用于各种适合本发明的领域，对于熟悉本领域的人员而言，可容易地实现另外的修改，因此在不背离权利要求及等同范围所限定的一般概念下，本发明并不限于特定的细节。

Claims (7)

1.一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，包括以下重量份组分：
2.根据权利要求1所述一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，所述丙烯酸酯包括丙烯酸甲酯、丙烯酸乙酯、丙烯酸羟乙酯的一种或多种。
3.根据权利要求1所述一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，所述聚醚多元醇包括聚丙二醇、聚乙内酯二元醇、聚四氢呋喃二醇的一种或多种。
4.根据权利要求1所述一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，所述催化剂包括二月桂酸二丁基锡、辛酸亚锡、异辛酸铋的一种或多种。
5.根据权利要求1所述一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，所述无机填料包括以下重量比组分：电气石粉20-30％、钛白粉15-25％、二氧化硅空心微球35-60％、滑石粉5-10％。
6.根据权利要求1或5任一项所述一种丙烯酸酯改性聚氨酯防水涂料，其特征在于，所述无机填料平均粒径≤50μm。
7.如权利要求1-6任一项所述一种丙烯酸酯改性聚氨酯防水涂料的制备方法，其特征在于，包括以下步骤：
S1：将聚醚多元醇、甲苯二异氰酸酯、催化剂置于反应釜中，抽真空后，充入80-120KPa氮气，并加热至80-100℃，进行亲核加成反应，得聚氨酯预聚体；
S2：待聚氨酯预聚体自然冷却至70℃，加入果糖和二羟甲基丙酸，搅拌反应1-2h，期间，持续性滴加甲基吡咯烷酮，降低粘度，反应至-NCO含量低于4％，得果糖改性聚氨酯预聚体；
S3：向果糖改性聚氨酯预聚体分散于去离子水中，并滴加丙烯酸酯，待丙烯酸酯充分溶胀后，升温至80℃，加入偶氮二异丁腈，反应3h，得丙烯酸酯改性聚氨酯壳-核复合乳液；
S4：40℃下，向丙烯酸酯改性聚氨酯壳-核复合乳液中加入三乙胺，进行中和反应，再加入无机填料，以4000-5000rpm的转速搅拌1h，并同时进行超声辅助分散，制得所述丙烯酸酯改性聚氨酯防水涂料。
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Application publication date: 20181002