CN105647330A - 一种功能水性聚氨酯涂料的制备方法 - Google Patents
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Abstract
本发明涉及一种功能水性聚氨酯涂料的制备方法，包括以下步骤：在四口烧瓶中加入聚四氢呋喃二醇，再加入异佛尔酮二异氰酸酯，得到预聚体；向预聚体加入1，4-丁二醇，加入含有二羟甲基丙酸的N-甲基毗咯烷酮溶液，得到扩链体系；滴加甲基丙烯酸β-羟乙酯，加入三乙胺，高速搅拌分散至上述乳液分散完全，得到水性聚氨酯乳液；以水性聚氨酯乳液为原料，以全氟辛酸铵和十二烷基硫酸钠为乳化剂，滴加甲基丙烯酸甲酯和甲基丙烯酸十二氟庚酯，并以过硫酸钾和亚硫酸氢钠的氧化还原体系作为引发剂进行乳液聚合，得到氟化聚氨酯-丙烯酸酯乳液，即为功能水性聚氨酯涂料，该功能水性聚氨酯涂料具有防水、防渗漏、强附着、耐腐蚀、耐压等优异性能。
Description
技术领域
本发明涉及一种功能水性聚氨酯涂料的制备方法，用于涂料的制备。
背景技术
由于人们对材料性能的要求不断提高，作为具有多种优良性能的含氟聚氨酯材料受到了各界的广泛关注。
目前，聚氨酯己经在涂料、黏合剂、航空航天材料、医用制品等领域得到了应用，尤其是绿色环保的水性含氟聚氨酯材料成为了近年来的研究热点。含氟水性聚氨酯一丙烯酸酯涂料作为水性涂料中综合性能最好的一类，含氟高聚物作为一类特种高分子材料，由于氟原子具有半径小，电负性强、碳氟键的键能高等特点，因此含氟链段的引入，使材料具有较低的表面能、良好的疏水疏油性、耐高低温以及抗沾污等性能。
在聚氨酯大分子结构中引入含氟基团，既能够保留聚氨酯材料优异的机械性能和两相微结构特征，又有希望消除因对聚氨酯进行亲水改性而导致涂膜耐水性下降的弊病，同时赋予涂膜优异的表面性能，目前采用氟改性聚氨酯己成为水性聚氨酯材料的一个新兴发展方向。
现有的水性聚氨酯涂料的制备较为困难，制备出来的涂料达不到较好的防渗透、耐腐蚀、耐压等性能，使得实际应用中不能体现出最佳的效果。
因此有必要设计一种功能水性聚氨酯涂料的制备方法，以克服上述问题。
发明内容
本发明的目的在于克服现有技术之缺陷，提供了一种功能水性聚氨酯涂料的制备方法，其制备出来的功能水性聚氨酯涂料，具有防水、防渗漏、强附着、耐腐蚀、耐压等优异性能。
本发明是这样实现的：
本发明提供一种功能水性聚氨酯涂料的制备方法，包括以下步骤：步骤一：在四口烧瓶中加入聚四氢呋喃二醇，于110-120℃进行真空脱水1-1.5小时，将温度降至75-80℃，再加入异佛尔酮二异氰酸酯，进行预聚合反应，反应1-2小时，得到预聚体；步骤二：在75-80℃的条件下，向上述预聚体加入1，4-丁二醇，反应1-2小时后，加入含有二羟甲基丙酸的N-甲基毗咯烷酮溶液，并在75-80℃的条件下，反应3-4小时，得到扩链体系；步骤三：将上述扩链体系降温至35-40℃，滴加甲基丙烯酸β-羟乙酯，反应1-2小时，待体系降至室温后，加入三乙胺得到乳液，并加入去离子水，高速搅拌分散至上述乳液分散完全，得到水性聚氨酯乳液；步骤四：以上述水性聚氨酯乳液为原料，在55-60℃氮气保护下，以全氟辛酸铵和十二烷基硫酸钠为乳化剂，向水性聚氨酯乳液中滴加甲基丙烯酸甲酯和甲基丙烯酸十二氟庚酯单体，并以过硫酸钾和亚硫酸氢钠的氧化还原体系作为引发剂进行乳液聚合，最后得到氟化聚氨酯-丙烯酸酯乳液，即为功能水性聚氨酯涂料。
进一步地，在步骤一中加入二丁基二月桂酸锡作为反应催化剂。
进一步地，步骤四中，全氟辛酸铵和十二烷基硫酸钠的质量比为1:1。
本发明具有以下有益效果：
本发明提供了一种功能水性聚氨酯涂料的制备方法，通过上述制备方法制备出来的功能水性聚氨酯涂料具有防水、防渗漏、强附着、耐腐蚀、耐压等优异性能。
具体实施方式
下面将对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其它实施例，都属于本发明保护的范围。
本发明实施例提供一种功能水性聚氨酯涂料的制备方法，用于制备功能水性聚氨酯涂料。
本发明采用异佛尔酮二异氰酸酯和聚四氢呋喃二醇作为原料，其中聚四氢呋喃二醇的相对分子量为1000，以1，4一丁二醇和二羟甲基丙酸作为扩链剂，含有双键并且含有羟基的甲基丙烯酸β-羟乙酯作为封端剂，制备出聚氨酯大分子单体，并将其进行水分散后得到聚氨酯乳液；用甲基丙烯酸甲酯和甲基丙烯酸十二氟庚酯与双键封端的聚氨酯大分子单体通过乳液共聚合的方法制备出含氟水性聚氨酯一丙烯酸酯乳液。
本发明的制备包括以下步骤：
步骤一，进行预聚合反应：在四口烧瓶中加入聚四氢呋喃二醇，于110-120℃进行真空脱水1-1.5小时，将温度降至75-80℃，再加入异佛尔酮二异氰酸酯，进行预聚合反应，反应1-2小时，得到预聚体；在预聚合反应中加入2-3滴二丁基二月桂酸锡作为反应催化剂。
步骤二，进行扩链：在75-80℃的条件下，向上述预聚体中缓慢加入1，4-丁二醇，反应1-2小时后，加入含有二羟甲基丙酸的N-甲基毗咯烷酮溶液，并在75-80℃的条件下，反应3-4小时，得到扩链体系。
步骤三，进行水分散：将上述扩链体系降温至35-40℃，滴加甲基丙烯酸β-羟乙酯，反应1-2小时，待体系降至室温后，加入三乙胺，中和上述液体中90%的醋酸根离子，得到乳液，一段时间后，加入去离子水，高速搅拌分散至上述乳液分散完全，得到水性聚氨酯乳液。
步骤四，制备氟化聚氨酯-丙烯酸酯乳液：以上述水性聚氨酯乳液为原料，在55-60℃氮气保护下，以全氟辛酸铵和十二烷基硫酸钠为乳化剂，其中，全氟辛酸铵和十二烷基硫酸钠的质量比为1:1。向水性聚氨酯乳液中滴加甲基丙烯酸甲酯和甲基丙烯酸十二氟庚酯单体，并以过硫酸钾和亚硫酸氢钠的氧化还原体系作为引发剂进行乳液聚合，最后得到氟化聚氨酯-丙烯酸酯乳液，即为功能水性聚氨酯涂料。通过上述制备方法制备出来的功能水性聚氨酯涂料具有防水、防渗漏、强附着、耐腐蚀、耐压等优异性能。
本发明将含氟丙烯酸酯、甲基丙烯酸甲酯和双键封端的聚氨酯预聚体通过乳液共聚合,成功制备了氟化聚氨酯-丙烯酸酯乳液，所得乳液均一稳定，成膜后材料具有优异的表面性能和力学性能。所制备的氟化聚氨酯-丙烯酸酯乳液均一稳定，薄膜力学性能优良、耐水性良好、而且对环境污染很小，因此作为一种新型的功能水性涂料，完全能够满足使用的需求。
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、改进等，均应包含在本发明的保护范围之内。
Claims (3)
1.一种功能水性聚氨酯涂料的制备方法，其特征在于，包括以下步骤：
步骤一：在四口烧瓶中加入聚四氢呋喃二醇，于110-120℃进行真空脱水1-1.5小时，将温度降至75-80℃，再加入异佛尔酮二异氰酸酯，进行预聚合反应，反应1-2小时，得到预聚体；
步骤二：在75-80℃的条件下，向上述预聚体加入1，4-丁二醇，反应1-2小时后，加入含有二羟甲基丙酸的N-甲基毗咯烷酮溶液，并在75-80℃的条件下，反应3-4小时，得到扩链体系；
步骤三：将上述扩链体系降温至35-40℃，滴加甲基丙烯酸β-羟乙酯，反应1-2小时，待体系降至室温后，加入三乙胺得到乳液，并加入去离子水，高速搅拌分散至上述乳液分散完全，得到水性聚氨酯乳液；
步骤四：以上述水性聚氨酯乳液为原料，在55-60℃氮气保护下，以全氟辛酸铵和十二烷基硫酸钠为乳化剂，向水性聚氨酯乳液中滴加甲基丙烯酸甲酯和甲基丙烯酸十二氟庚酯单体，并以过硫酸钾和亚硫酸氢钠的氧化还原体系作为引发剂进行乳液聚合，最后得到氟化聚氨酯-丙烯酸酯乳液，即为功能水性聚氨酯涂料。
2.如权利要求1所述的一种功能水性聚氨酯涂料的制备方法，其特征在于：在步骤一中加入二丁基二月桂酸锡作为反应催化剂。
3.如权利要求1或2所述的一种功能水性聚氨酯涂料的制备方法，其特征在于：步骤四中，全氟辛酸铵和十二烷基硫酸钠的质量比为1:1。
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