CN107880235A - 一种高耐候性氟改性uv固化多臂型水性聚氨酯树脂的制备方法 - Google Patents
一种高耐候性氟改性uv固化多臂型水性聚氨酯树脂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种高耐候性氟改性UV固化多臂型水性聚氨酯树脂的制备方法。本发明利用有机氟的耐水、耐候、耐溶剂、耐低温性能对耐水、耐候性较差的聚酯型水性聚氨酯树脂进行改性。本发明的聚酯型水性聚氨酯经有机氟进行链段改性得到含有氟元素的聚酯型多臂型水性聚氨酯,该聚合物成膜后,聚合物中的有机氟链段更倾向于表面聚集取向,而聚氨酯链段朝向内层。这样既能在保证聚酯型聚氨酯树脂优良的附着力、硬度、固化速率等的同时又赋予改性聚氨酯涂膜优良的耐水性、耐溶剂性和耐候性。
Description
技术领域
本发明属于高分子材料技术领域,具体涉及一种高耐候性氟改性UV固化多臂型水性聚氨酯树脂的制备方法。
背景介绍
紫外光固化水性树脂继承和发展了传统UV固化技术和水性涂料技术的许多优点,如低成本、低粘度、良好的涂布适应性、设备简单、无毒性、无刺激性、不燃性等。由于UV固化水性树脂的优点突出,近年来得到较快的发展,其产品已被众多领域应用。
但水性聚氨酯的有些性能还不能满足实际需要,如硬度、耐水性、热稳定性、表面性能和拉伸强度等,因而,限制了涂膜的应用范围。所以,对水性聚氨酯的改性就成为必然趋势。
含氟材料由于具有优异的疏水、疏油、耐酸碱及耐溶剂性,已成为自清洁外墙涂料及大型机器保护涂层的首要选择,被越来越多地用在建筑业、机械行业、工业设备、大型钢结构、体育设施等领域。用含氟聚合物对水性聚氨酯的改性研究已有许多报道,HyejinLim等合成大分子含氟二醇,以其作扩链剂引入聚氨酯链中,合成侧链含氟水性聚氨酯;HongTan等以含氟侧链引入聚氨酯中,研究了氟链段在表面的迁移。通过在水性聚氨酯中引入含氟基团可得到氟改性聚氨酯,含氟链段对主链及内部分子形成“屏蔽保护”,不仅可提高碳碳键的稳定性,使含氟水性聚合物物理性能稳定,还提高涂层的耐水性、耐侯性、耐油性、抗污性。
发明内容
本发明的目的在于提供一种利用高分子有机氟进行改性制备耐水、耐候、耐溶剂性多臂型水性聚氨酯乳液及其制备方法。本发明的多臂型水性聚氨酯经有机氟进行聚氨酯末端改性得到主链含有有机氟聚酯型水性聚氨酯,该聚合物成膜后,聚合物末端有机氟链段更倾向于表面聚集取向,而聚氨酯链段朝向内层。这样既能在保证聚酯型聚氨酯树脂优良的附着力、硬度、固化速率等的同时又赋予改性聚氨酯涂膜优良的耐水性、耐溶剂性和耐候性。
本发明的技术方案是:
一种高耐候性氟改性UV固化多臂型水性聚氨酯树脂的制备方法,包括如下步骤:
(1)含氟二元醇的合成:将一定量的异佛尔酮二异氰酸酯(IPDI)、有机氟醇、混合加入250ml单口烧瓶中,在氮气保护下,升温至80℃恒温反应2~3小时,再加入一定量的三羟甲基丙烷(TMP)继续反应,NCO含量达到理论值后停止反应,得到含氟二元醇;
(2)含氟聚氨酯预聚体的合成:将一定量的催化剂和二异氰酸酯加入250ml三口烧瓶中将温度升至40~45℃滴加一定量的聚酯二元醇和含氟二元醇,反应3-4小时当NCO达到理论值时结束,得到含氟聚氨酯预聚体。
(3)NCO半封端含活性封端剂预聚物的合成:将上述预聚体放入250ml三口烧瓶中,在N2保护下将温度升高至70℃,加入扩链剂反应3-4小时当NCO达到理论值后加入活性封端剂、阻聚剂、溶剂A保温反应3-4小时,NCO达到理论值,反应停止,得到异氰酸酯封端含活性封端剂预聚物;
(4)多臂型水性聚氨酯乳液的制备:将一定量的催化剂、活性多元醇加入250ml三口烧瓶中将温度升至70~75℃,在氮气氛围下加入不同含量的异氰酸酯封端含氟预聚物和异氰酸酯封端含活性封端剂预聚物;反应3-4小时,当-NCO红外吸收峰完全消失时终止反应;将反应温度降至40~45℃,加入一定量的中和剂,高速剪切30min,再加入去离子水,剪切乳化30min,减压旋蒸除去溶剂A,即得超支化水性聚氨酯乳液。
步骤(1)和(3)中所述扩链剂为二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)中的至少一种;
步骤(3)中所述催化剂为二月桂酸二丁基锡、辛酸亚锡中的至少一种;
步骤(3)中所述二异氰酸酯为甲苯二异氰酸酯(TDI)、4,4'-二苯基甲烷二异氰酸酯(MDI)、异佛尔酮二异氰酸酯(IPDI)、1,6-己二异氰酸酯(HDI)二环己基甲烷二异氰酸酷(HMDI)中的至少一种;
步骤(3)中所述活性封端剂为丙烯酸羟乙酯(HEA)、甲基丙烯酸羟乙酯(HEMA)、丙烯酸羟丙酯(HPA)、甲基丙烯酸羟丙酯(HPMA)、季戊四醇三丙烯酸酯(PETA)中的至少一种;
步骤(3)中所述阻聚剂为对苯二酚、对甲氧基苯酚中的至少一种;
步骤(3)中所述聚酯二元醇为聚碳酸酯二元醇、聚己内酯二元醇、己二酸聚酯二元醇中的至少一种;
步骤(3)中所述有机氟醇为3,3,4,4,5,5,6,6,7,7,8,8,8-十三氟-1-辛醇、全氟-1-辛醇、3,3,4,4,5,5,6,6,6-九氟-1-己醇、1H,1H,2H,2H-全氟癸醇、2,2,3,3,4,4,4-七氟代-1-丁醇中的至少一种;
步骤(3)和(4)中所述溶剂A为丙酮、丁酮中的至少一种;
步骤(4)中的活性多元醇为丙三醇、季戊四醇、双季戊四醇中的至少一种;
步骤(4)中的中和剂为三乙胺。
本发明的有益效果是:通过以上反应,合成得到耐水、耐候可UV固化多臂型水性聚氨酯树脂涂料用树脂。该树脂可用于提高涂料的耐水性、耐候性、防污性、耐热性,可广泛用于塑料、薄膜、门窗等具有耐水、耐候、防污要求的表面。
具体实施方式
实施例1
含氟二元醇的合成:将23.21g 1H,1H,2H,2H-全氟癸醇,11.10g IPDI以及0.05g催化剂DBTDL加入到有N2保护装置的250ml三口烧瓶中,升温至80℃反应3h,再加入6.71gTMP继续反应。NCO全部反应完成后,停止反应,得到含氟二元醇。
含氟聚氨酯预聚物的合成:将0.03g二月桂酸二丁基锡(DTBDL)和13.34g异佛尔酮二异氰酸酯(IPDI)加入100ml三口烧瓶中将温度升至40℃,氮气氛围下滴加20g聚碳酸酯二醇和4.1g含氟二元醇,反应4小时当NCO达到理论值时结束,得到含氟聚氨酯预聚体。
NCO半封端含活性封端剂预聚物的合成:将上述预聚体放入250ml三口烧瓶中,在N2保护下将温度升高至70℃,加入3.02g二羟甲基丙酸(DMPA)反应3小时当NCO达到理论值后加入2.24g季戊四醇三丙烯酸酯(PETA)、0.01g对甲氧基苯酚、5.0g丙酮保温反应3小时,NCO达到理论值,反应停止,NCO半封端含氟预聚物;
多臂型水性聚氨酯乳液的制备:将0.09g二月桂酸二丁基锡(DTBDL)、0.23g甘油和15g丙酮加入250ml三口烧瓶中温度升至70℃,加入以上NCO半封端含活性封端剂预聚物。反应4小时,当-NCO红外吸收峰完全消失时终止反应。将反应温度降至0℃,加入2.60g三乙胺中和剂,高速剪切30min,再加入50.0g离子水,剪切乳化40min,减压旋蒸除去丙酮,即得多臂型水性聚氨酯乳液。
Claims (2)
1.一种高耐候性氟改性UV固化多臂型水性聚氨酯树脂的制备方法,其特征步骤为:
(1)含氟二元醇的合成:将一定量的异佛尔酮二异氰酸酯(IPDI)、有机氟醇、混合加入250ml单口烧瓶中,在氮气保护下,升温至80℃恒温反应2~3小时,再加入一定量的三羟甲基丙烷(TMP)继续反应,NCO含量达到理论值后停止反应,得到含氟二元醇;
(2)含氟聚氨酯预聚体的合成:将一定量的催化剂和二异氰酸酯加入250ml三口烧瓶中将温度升至40~45℃滴加一定量的聚酯二元醇和含氟二元醇,反应3-4小时当NCO达到理论值时结束,得到含氟聚氨酯预聚体。
(3)NCO半封端含活性封端剂预聚物的合成:将上述预聚体放入250ml三口烧瓶中,在N2保护下将温度升高至70℃,加入扩链剂反应3-4小时当NCO达到理论值后加入活性封端剂、阻聚剂、溶剂A保温反应3-4小时,NCO达到理论值,反应停止,得到异氰酸酯封端含活性封端剂预聚物;
(4)多臂型水性聚氨酯乳液的制备:将一定量的催化剂、活性多元醇加入250ml三口烧瓶中将温度升至70~75℃,在氮气氛围下加入异氰酸酯封端含活性封端剂预聚物;反应3-4小时,当-NCO红外吸收峰完全消失时终止反应;将反应温度降至40~45℃,加入一定量的中和剂,高速剪切30min,再加入去离子水,剪切乳化30min,减压旋蒸除去溶剂A,即得多臂型水性聚氨酯乳液。
2.如权利要求1所述的一种高耐候性氟改性UV固化多臂型水性聚氨酯树脂的制备方法,其特征在于:
步骤(1)和(3)中所述扩链剂为二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)中的至少一种;
步骤(3)中所述催化剂为二月桂酸二丁基锡、辛酸亚锡中的至少一种;
步骤(3)中所述二异氰酸酯为甲苯二异氰酸酯(TDI)、4,4'-二苯基甲烷二异氰酸酯(MDI)、异佛尔酮二异氰酸酯(IPDI)、1,6-己二异氰酸酯(HDI)二环己基甲烷二异氰酸酷(HMDI)中的至少一种;
步骤(3)中所述活性封端剂为丙烯酸羟乙酯(HEA)、甲基丙烯酸羟乙酯(HEMA)、丙烯酸羟丙酯(HPA)、甲基丙烯酸羟丙酯(HPMA)、季戊四醇三丙烯酸酯(PETA)中的至少一种;
步骤(3)中所述阻聚剂为对苯二酚、对甲氧基苯酚中的至少一种;
步骤(3)中所述聚酯二元醇为聚碳酸酯二元醇、聚己内酯二元醇、己二酸聚酯二元醇中的至少一种;
步骤(3)中所述有机氟醇为3,3,4,4,5,5,6,6,7,7,8,8,8-十三氟-1-辛醇、全氟-1-辛醇、3,3,4,4,5,5,6,6,6-九氟-1-己醇、1H,1H,2H,2H-全氟癸醇、2,2,3,3,4,4,4-七氟代-1-丁醇中的至少一种;
步骤(3)和(4)中所述溶剂A为丙酮、丁酮中的至少一种;
步骤(4)中的活性多元醇为丙三醇、季戊四醇、双季戊四醇中的至少一种;
步骤(4)中的中和剂为三乙胺。
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