CN111393613B - 一种易分散自消光水性聚氨酯固化剂及制备方法 - Google Patents

一种易分散自消光水性聚氨酯固化剂及制备方法 Download PDF

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CN111393613B
CN111393613B CN202010357939.9A CN202010357939A CN111393613B CN 111393613 B CN111393613 B CN 111393613B CN 202010357939 A CN202010357939 A CN 202010357939A CN 111393613 B CN111393613 B CN 111393613B
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李同军
蔡锡松
万李
岑婉莹
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Guangdong Badfu New Material Co ltd
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Abstract

本发明公开一种易分散自消光水性聚氨酯固化剂及制备方法，按重量份计，由以下原料制成：多异氰酸酯预聚物600‑750份，多异氰酸酯单体5‑15份，磺酸盐或其衍生物1‑15份，亲水扩链剂5‑15份，聚醚多元醇15‑25份，催化剂1‑10份，助分散剂和稳定剂共10‑35份。本发明采用分步制备，先加入磺酸盐，改善固化剂的水分散性，再加入亲水扩链剂和亲水聚醚进一步提高分子量，同时提供接枝点，继续升温接枝NCO，进而得到可自乳化且同时形成稳定粒径相对较大的水性多异氰酸酯固化剂。本发明可与水性羟丙乳液或羟丙分散体配套制成双组份羟丙涂料。复配粒径相对较小(粒径小于250nm)的羟丙乳液，尤其使涂膜的哑光效果更佳。

Description

一种易分散自消光水性聚氨酯固化剂及制备方法
技术领域
本发明涉及一种易分散自消光水性聚氨酯固化剂及制备方法，属于聚氨酯涂料领域。
背景技术
随着低碳经济、绿色化学、低VOC及节能减排等相关法律法规的出现，环保已成为当今涂料树脂行业发展的趋势。双组份水性聚氨酯技术正符合这一原则，它可解决水性单组份聚氨酯涂膜物理性能差的问题，性能可媲美溶剂型双组份聚氨酯涂膜且具有水性涂料树脂低VOC的特点。其中，水分散型多异氰酸酯作为双组份水性聚氨酯的重要组分，对涂膜的性能起到了至关重要的作用，具有广阔的应用前景。
目前，国内的水性多异氰酸酯固化剂为了有较好的自乳化分散性能，多采用非离子如聚醚类物质改性，往往出现涂膜干燥时间长，涂膜耐水性差的缺点。此外，随着当前涂膜审美观念的转变，消光涂层因具有自然的外观而被广泛应用于各类面漆中，目前消光涂料主要通过在树脂中添加消光剂而成，但采用该方法通常出现消光剂与树脂不相容，导致出现树脂贮存稳定性差、涂膜表面光泽不均及涂膜物理强度不足等缺点，受到摩擦容易变亮，涂膜表面消光保持度较差。
发明内容
针对上述现有技术存在的问题，本发明提供一种易分散自消光水性聚氨酯固化剂及制备方法。
为了实现上述目的，本发明采用的一种易分散自消光水性聚氨酯固化剂，按重量份计，由以下原料制成：多异氰酸酯预聚物600-750份，多异氰酸酯单体5-15份，磺酸盐或其衍生物1-15份，亲水扩链剂5-15份，聚醚多元醇15-25份，催化剂1-10份，助分散剂和稳定剂共10-35份。
作为改进，所述多异氰酸酯单体采用六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯中的一种或两种。
作为改进，所述多异氰酸酯预聚物采用脂肪二异氰酸酯的缩二脲，二异氰酸酯的二聚体或多聚体中的一种或两种。
作为改进，所述磺酸盐采用对苯羟基磺酸钠、1,4-丁二醇磺酸钠、二氨基苯磺酸钠、氨基磺酸钠中的至少一种。
作为改进，所述助分散剂和稳定剂采用丙二醇甲醚醋酸酯、二丙二醇二甲醚、丙二醇丁醚醋酸酯中的一种或两种。
作为改进，所述亲水扩链剂采用2,2-二羟甲基丁酸、2,2-二羟甲基丙酸、乳酸中的一种或两种。
作为改进，所述聚醚多元醇采用分子量为350，450，500或1000的聚乙二醇单甲醚中的一种或两种。
作为改进，所述催化剂采用二月桂酸二丁基锡、辛酸亚锡、三乙胺、有机铋、N-甲基吡咯烷酮、二甲基环己胺，三亚乙基二胺，三甲基羟乙基亚乙基二胺中的两种或两种以上。
另外，本发明还公开了一种易分散自消光水性聚氨酯固化剂的制备方法，包括以下步骤：
1)将配方量的多异氰酸酯预聚物、配方量磺酸盐或其衍生物、及催化剂中的组合叔胺类催化剂、配方量助分散剂和稳定剂，放入反应釜中，打开搅拌器进行搅拌，反应温度控制在60-90℃，保温2～3.5h；
2)加入配方量亲水扩链剂及聚醚多元醇、催化剂中的金属类催化剂，在1h内滴加完毕，保温0.5-1.5h；
3)再次升温至110-140℃，直至体系变澄清后，加入催化剂中的胺类催化剂，滴加配方量的多异氰酸酯单体，控制滴加0.5-1.5h，保温1.5-2.5h。
4)降温冷却至40℃，出料。
其中，所述步骤1)中，在催化磺酸盐或其衍生物反应时，采用的催化剂为两种叔铵类催化剂的混合，且催化剂的摩尔质量与磺酸盐或其衍生物的摩尔质量比为(0.1-0.8):1。
与现有技术相比，本发明的优点在于采用分步制备的方法，先加入磺酸盐，改善了固化剂的水分散性，再加入亲水扩链剂和亲水聚醚多元醇，进一步提高分子量，同时提供接枝点，继续升温接枝NCO，使得-NCO继续与生成的氨基甲酸酯键继续反应形成交联结点，达到增大多异氰酸酯预聚物粒径的效果，进而得到可自乳化且同时形成稳定粒径相对较大(粒径在1000-1500nm)的水性多异氰酸酯固化剂，合成出的样品配漆具有储存稳定性高，耐性优异，透气性好，光泽度波动小的特点。
本发明可与水性羟丙乳液或羟丙分散体配套制成双组份羟丙涂料。复配粒径相对较小(粒径小于250nm)的羟丙乳液，尤其使涂膜的哑光效果更佳。
本发明优点在于催化剂组合搭配使用具有协同作用，可以起到用量少、催化效率高的效果，进而有效缩短反应时间。
本发明优点在于过程中无需有机溶剂加入再抽提，而大多公开文献则是先将磺酸盐溶于有机溶剂中，与多异氰酸酯预聚物反应，然后再蒸馏出有机溶剂，在蒸馏过程中存在蒸馏时间长、效率低，部分蒸汽挥发至环境中造成污染，本发明则是通过加入少量助分散剂、组合催化剂，通过在反应温度下改变溶解度平衡的方法使磺酸盐合成进去。而助分散剂又可作为稳定剂，同时也是环境友好性溶剂，无需抽提。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明了，下面对本发明进行进一步详细说明。但是应该理解，此处所描述的具体实施例仅仅用以解释本发明，并不用于限制本发明的范围。
除非另有定义，本文所使用的所有的技术术语和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同，本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的，不是旨在于限制本发明。
实施例1
一种易分散自消光水性聚氨酯固化剂的制备方法，包括以下步骤：
1)将六亚甲基二异氰酸酯的三聚体630g、对羟基苯磺酸钠9.6g、丙二醇丁醚醋酸酯12g、二甲基环己胺3g、三甲基羟乙基亚乙基二胺2g加入反应釜中，加热并搅拌，当加热至80℃时保温2h；
2)加入有机铋0.15g，滴加分子量为350的聚乙二醇单甲醚17.5g、2,2-二羟甲基丙酸6.7g，在1h内滴加完毕，保温1h；
3)再次升温至130℃，直至体系变澄清后，加入二甲基环己胺0.25g，滴加六亚甲基二异氰酸酯8g，滴加1.5h，保温2h；
4)降温至40℃出料。
实施例2
一种易分散自消光水性聚氨酯固化剂的制备方法，包括以下步骤：
1)将六亚甲基二异氰酸酯的三聚体720g、对羟基苯磺酸钠10.3g、丙二醇丁醚醋酸酯30g、二甲基环己胺1.8g，三甲基羟乙基亚乙基二胺1.2g加入反应釜中，加热并搅拌，当加热至80℃时保温2h；
2)加入辛酸亚锡0.12g，滴加分子量为500的聚乙二醇单甲醚15g，2,2-二羟甲基丙酸10.2g在1h内滴加完毕，保温1h；
3)再次升温至130℃，直至体系变澄清后，加入二甲基环己胺0.3g，滴加六亚甲基二异氰酸酯11.3g，滴加2h，保温1h；
4)降温冷却至35℃，出料。
实施例3
一种易分散自消光水性聚氨酯固化剂的制备方法，包括以下步骤：
1)将异佛尔酮二异氰酸酯三聚体(70％，NCO％＝12.2％.)630g、氨基磺酸钠2.2g、丙二醇丁醚醋酸酯16.3g、三亚乙基二胺0.5g、NMP 0.5g加入反应釜中，加热并搅拌，当加热至75℃时保温计时2h；
2)升温至85℃，加入二月桂酸二丁基锡0.15g，滴加分子量为500的聚乙二醇单甲醚20g，2,2-二羟甲基丙酸10.2g，在1h内滴加完毕，保温1h；
3)再次升温至130℃，直至体系变澄清后，加入N-甲基吡咯烷酮0.2g，滴加13.6g异佛尔酮二异氰酸酯，滴加2h，保温1h；
4)降温冷却至40℃，出料。
实施例1-3制得的固化剂NCO值分别为20.3％，20.8％，11.8％，对应的羟丙乳的羟值为2.4％。分别采用HG\T 5065-2016《建筑涂料用罩面清漆》，GB\22374-2008《地坪涂装材料标准》对试样进行检测，本实验所选用的聚氨酯固化剂与羟丙组分有效交联官能团比NCO:OH值＝1.3:1，结果见下表1。
表1双组分水性聚氨酯面漆性能测试结果
Figure BDA0002474100320000051
本发明所采用的A组分参照表2所示配方制得。
表2羟基丙烯酸乳液配方
Figure BDA0002474100320000052
Figure BDA0002474100320000061
*注：RS-3915固含为41％。
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内所作的任何修改、等同替换或改进等，均应包含在本发明的保护范围之内。

Claims (2)

1.一种易分散自消光水性聚氨酯固化剂，其特征在于，按重量份计，由以下原料制成：多异氰酸酯预聚物600-750份，多异氰酸酯单体5-15份，磺酸盐1-15份，亲水扩链剂5-15份，分子量为350、450、500或1000的聚乙二醇单甲醚中的一种或两种15-25份，催化剂1-10份，助分散剂和稳定剂共10-35份；所述磺酸盐采用对苯羟基磺酸钠、二氨基苯磺酸钠、氨基磺酸钠中的至少一种；所述助分散剂和稳定剂采用丙二醇甲醚醋酸酯、二丙二醇二甲醚、丙二醇丁醚醋酸酯中的一种或两种；所述催化剂采用二月桂酸二丁基锡、辛酸亚锡、三乙胺、有机铋、二甲基环己胺、三亚乙基二胺、三甲基羟乙基亚乙基二胺中的两种或两种以上；
所述多异氰酸酯预聚物采用二异氰酸酯的二聚体、六亚甲基二异氰酸酯的三聚体、异佛尔酮二异氰酸酯的三聚体中的一种或两种；所述亲水扩链剂采用2,2-二羟甲基丁酸、2,2-二羟甲基丙酸中的一种或两种；
所述易分散自消光水性聚氨酯固化剂的制备方法，包括以下步骤：
1）将配方量的多异氰酸酯预聚物、配方量磺酸盐、及催化剂中的组合叔胺类催化剂、配方量助分散剂和稳定剂，放入反应釜中，打开搅拌器进行搅拌，反应温度控制在60-90 ℃，保温2~3.5 h；在催化磺酸盐反应时，采用的催化剂为两种叔胺类催化剂的混合，且催化剂的摩尔量与磺酸盐的摩尔量比为（0.1-0.8）:1；
2）加入配方量亲水扩链剂及分子量为350、450、500或1000的聚乙二醇单甲醚中的一种或两种，催化剂中的金属类催化剂，在1 h内滴加完毕，保温0.5-1.5 h；
3）再次升温至110-140 ℃，直至体系变澄清后，加入催化剂中的胺类催化剂，滴加配方量的多异氰酸酯单体，控制滴加0.5-1.5 h，保温1.5-2.5 h；
4）降温冷却至40 ℃，出料。
2.根据权利要求1所述的一种易分散自消光水性聚氨酯固化剂，其特征在于，所述多异氰酸酯单体采用六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、异佛尔酮二异氰酸酯中的一种或两种。
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