CN115286947B - 一种高固体份、高耐水性抗菌水性聚氨酯涂料及其制备方法 - Google Patents
一种高固体份、高耐水性抗菌水性聚氨酯涂料及其制备方法 Download PDFInfo
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- CN115286947B CN115286947B CN202210997635.8A CN202210997635A CN115286947B CN 115286947 B CN115286947 B CN 115286947B CN 202210997635 A CN202210997635 A CN 202210997635A CN 115286947 B CN115286947 B CN 115286947B
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Abstract
本发明公开了一种高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，包括如下步骤：加入40～80质量份二异氰酸酯、80～160质量份多元醇、6～24质量份组合扩链剂、0.4～1.2质量份催化剂、12～26质量份羟基丙烯酸酯、2～6质量份中和剂发生扩链反应，制得组分1；加入30～60质量份二异氰酸酯、30～50质量份多元醇、8～15质量份甲基丙烯酸异冰片酯、0.2～1.2质量份催化剂、12～20质量份羟基丙烯酸酯发生扩链反应，制得组分2；S3、取组分1和组分2混合，S1中组合扩链剂包括甲基丙烯酸异冰片酯和亲水性扩链剂。本发明采用双羟基化甲基丙烯酸异冰片酯作为扩链剂的组分之一，将其引入聚氨酯分子链，可以增强涂层的疏水性，因此能够改善水性聚氨酯耐水性差的弊病，同时赋予涂层抗菌性。
Description
技术领域
本发明涉及水性聚氨酯涂料领域，特别是一种高固体份、高耐水性抗菌水性聚氨酯涂料及其制备方法。
背景技术
聚氨酯(PU)涂层作为一种高性能涂层材料已经被广泛使用在家具、医疗、电子、船舶等领域。虽然溶剂型PU涂料涂层光泽度、耐腐蚀性都明显优于水性涂料，但是它气味大、毒性高。由于国家现在对环保的要求越来越严格，水性聚氨酯在未来的发展前景巨大。但是，水性聚氨酯在合成过程中常常会引入亲水基团，从而涂层的耐水性低于油性涂料。此外，水性涂料中水的蒸发潜热高，具有较高能耗。因此，开发高固含量、高耐水性的水性聚氨酯涂料具有重要意义。
现有耐水性水性聚氨酯涂料的研究主要是在涂料中引入耐水性组分。如CN108727554B公布了一种蒙脱土改性水性聚氨酯的纳米复合乳液，乳液具有高的耐水性，但是乳液固含量最高只有20％。CN 113292962 A公布了一种蓖麻油基水性聚氨酯/明胶互穿网络结构胶粘剂，通过蓖麻油来增强胶粘剂的耐水性。虽然水性胶粘剂的固含量最高有50％，但是粘度很高，不方便施工。丙烯酸涂料具有较高的耐水性，但是存在耐溶剂性差、热黏冷脆等缺点。因此，丙烯酸改性水性聚氨酯能够起到协同作用，增强涂层的耐水性。CN107286306A公开了一种水性聚氨酯丙烯酸酯共聚乳液及其制备方法。所述水性聚氨酯丙烯酸酯共聚乳液是先以二异氰酸酯、阻燃多元醇、非阻燃多元醇、含酸性基团的扩链剂、羟基丙烯酸酯和封端剂为原料，通过化学接枝的方法制备出含有碳碳双键的含磷水性聚氨酯乳液，再在磷酸酯类表面活性剂的保护下，以丙烯酸酯、含碳碳双键的磷酸酯、乙烯基硅油、乙烯基硅烷偶联剂、丙烯酸类交联剂为原料进行乳液聚合，制备得到。该发明提供的水性聚氨酯丙烯酸酯共聚乳液具有较高的固含量，干燥用时少，其干燥后的制品具有良好的阻燃性能和耐热分解性能。该专利中采用含酸性基团的扩链剂，该专利制备的共聚乳液仅具有阻燃性能，不具有抗菌功能。
发明内容
本发明所要解决的技术问题是，针对现有技术不足，提供一种高固体份、高耐水性抗菌水性聚氨酯涂料及其制备方法，提升所制得涂料的耐水性、抗菌性，提高固含量。
为解决上述技术问题，本发明所采用的技术方案是：一种高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，包括如下步骤：
S1、加入40～80质量份二异氰酸酯、80～160质量份多元醇、6～24质量份组合扩链剂、0.4～1.2质量份催化剂、12～26质量份羟基丙烯酸酯、2～6质量份中和剂发生扩链反应，制得组分1；
S2、加入30～60质量份二异氰酸酯、30～50质量份多元醇、8～15质量份甲基丙烯酸异冰片酯、0.2～1.2质量份催化剂、12～20质量份羟基丙烯酸酯发生扩链反应，制得组分2；
S3、取质量比为3～5:1的组分1和组分2混合，组分1和组分2的总质量份为20-50份，加入30-35质量份去离子水、5～10质量份光引发剂、0.02～0.1质量份消泡剂和0.04～0.2质量份流平剂分散均匀，得到水性聚氨酯涂料；
S1中组合扩链剂包括双羟基化甲基丙烯酸异冰片酯和亲水性扩链剂。
本发明中，高固体份指的是固含量为20～60％，特别是40～60％，高耐水性指的是涂层在浸泡48小时后表面不泛白，浸泡72小时后表面泛白，干燥后恢复透明状态，最大的水接触角为83°～85°。
本发明引入双羟基化甲基丙烯酸异冰片酯作为组合扩链剂的组分之一，甲基丙烯酸异冰片酯因其特定的分子结构，引入聚氨酯分子链时可以增强涂层的疏水性，因此能够提高水性聚氨酯涂料的耐水性，拓展了聚氨酯涂层的适用范围。双羟基化甲基丙烯酸异冰片酯结构相较于外加型抗菌剂具有广谱性、耐久性，不存在抗菌剂释放对环境造成影响。本发明将双羟基化甲基丙烯酸异冰片酯用于阴离子水性聚氨酯的制备。
本发明通过设计核壳结构分散体，降低涂料的亲水基团含量，在提高涂层固含量的同时，提高了涂层的耐水性。乳液粒子是以类似球型结构存在。本方案通过设计核壳结构，可以降低乳液粒子的结合水含量，从而增加粒子之间的流动性，降低涂料粘度。核壳结构的设计使得涂料单位体积内，乳液粒子的占有空间更大，使得固含量增加。
本发明设计核壳结构是通过亲水性的组分1和油性的组分2实现水包油结构的乳液粒子。组分1和组分2的质量比为3～5:1，比例高于3～5:1，乳液粒子亲水性好，乳液颗粒粒径较小，乳液稳定性好。在固含量超过40％的时候，粘度会升高比较快，不适合施工使用。当比例低于3～5:1时，乳液粒子过大，涂料稳定性降低，达不到预期6个月的储存时间。组分1和组分2的质量比优选为4。
进一步优选地，S1中，加入30～40质量份二异氰酸酯、50～80质量份多元醇、3～6质量份组合扩链剂、0.2～0.3质量份催化剂、12～20质量份羟基丙烯酸酯、2～6质量份中和剂；
S2中，加入40～60质量份二异氰酸酯、30～40质量份多元醇、8～10质量份双羟基化甲基丙烯酸异冰片酯、0.2～0.3质量份催化剂、12～20质量份羟基丙烯酸酯。
在本发明的一些优选的实施例中，所述亲水性扩链剂为二羟甲基丙酸，双羟基化甲基丙烯酸异冰片酯和二羟甲基丙酸的质量比为1～5：2～7。
本发明在组分1使用组合扩链剂是为了降低树脂的亲水基团含量，从而获得涂层更加优异的耐水性。采用质量比为1～5：2～7的双羟基化甲基丙烯酸异冰片酯和二羟甲基丙酸的组合扩链剂，不仅可正常制备聚氨酯预聚物，而且可使聚氨酯预聚物所制得涂料具有耐水性、抗菌性。组分2中只选择双羟基化甲基丙烯酸异冰片酯作为扩链剂是为了提高涂层中抗菌剂的含量，使得涂层抗菌效果更好。
在本发明的一些优选的实施例中，扩链反应的温度为60～80℃，反应时间为4～9小时，优选为60℃。
在本发明的一些优选的实施例中，所述二异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、苯二甲撑二异氰酸酯和四甲基苯二甲基二异氰酸酯中的一种或多种。
在本发明的一些优选的实施例中，所述多元醇为聚己内酯二元醇和聚己内酯三元醇中的一种或多种。
在本发明的一些优选的实施例中，所述催化剂为二丁基二月桂酸锡、辛酸亚锡、二醋酸二丁基锡和有机铋类催化剂中的一种或多种，优选为有机铋类催化剂DY-20。
在本发明的一些优选的实施例中，所述羟基丙烯酸酯为丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯和甲基丙烯酸羟丁酯中的一种或多种；
所述中和剂为氨水、氢氧化钠、氢氧化钾、三乙胺和三正丁胺中的一种或多种，优选为三乙胺。
在本发明的一些优选的实施例中，光引发剂为1-羟基环己基苯基甲酮、2-羟基-2-甲基-1-苯基丙酮和2-羟基-4-(2-羟乙氧基)-2-甲基苯丙酮中的一种或者多种。
在本发明的一些优选的实施例中，消泡剂为AFCONA2503、2505、2507、2524和2590中的一种或者多种；
流平剂为AFCONA3030、3522、3585和3588中的一种或者多种。
本发明还公开了一种利用所述的方法制备的高固体份、高耐水性抗菌水性聚氨酯涂料。
在制得的聚氨酯预聚物中按质量份加入去离子水、光引发剂、消泡剂和流平剂，分散的转速为2000～3000r/min，优选为3000r/min。
所述水性聚氨酯涂料粘度为0～5000mPa·s。
与现有技术相比，本发明所具有的有益效果为：
1.本发明采用一种天然的产物异冰片酯的衍生物甲基丙烯酸异冰片酯作为扩链剂，将其引入聚氨酯分子链。甲基丙烯酸异冰片酯因其特定的分子结构，引入聚氨酯分子链时可以增强涂层的疏水性，因此能够改善水性聚氨酯耐水性差的弊病，同时赋予涂层抗菌性。
2.本发明通过制备核壳结构获得高固体份、低粘度的水性聚氨酯涂料。通过核壳结构设计，降低了乳液粒子水化层消耗水的量，使得乳液粒子具有更好的流动性，从而降低涂料粘度。组分2作为核心材料的引入，可以使得涂层亲水基团的含量降低，从而提高涂层的耐水性。同时，双羟基化甲基丙烯酸异冰片酯的含量提高，使得涂层抗菌效果更加优异。双羟基化甲基丙烯酸异冰片酯的含量提高与涂层低亲水基团含量的共同作用下，使得涂层具有优异的耐水性。
附图说明
图1为抗菌剂双羟基化甲基丙烯酸异冰片酯合成表征核磁共振氢谱图和红外光谱图。
图2水性聚氨酯涂料固含量为40％的数字照片。
图3水性聚氨酯涂料在3000r/min中离心15分钟前后对比数字照片。
图4水性聚氨酯热重分析固含量图。
图5水性聚氨酯涂料抗菌效果图。
图中a为大肠杆菌，b为金黄色葡萄球菌。1号样品为空白样品，2号样品为1组分，3号样品为抗菌涂料。
图6水性涂层耐水性图。
图a油性涂料，图b本发明涂料，图c普通水性涂料。涂层水中浸泡8天样品图。水性涂层在浸泡24小时后表面泛白，干燥后恢复透明状态。普通水性聚氨酯在5天时发生起泡和锈蚀。
图7涂层EIS测试图。
图a，b油性涂料，图c，d本发明涂料，图e，f普通水性涂料。涂层在3.5％氯化钠溶液中浸泡不同时间的阻抗和相位角图。从图中可以看出，本发明涂料与油性涂料具有类似的防护性能。
图8涂层水接触角测试图。
图a普通水性涂料，图b本发明涂料，图c油性涂料。普通水性涂料的接触角(72°)，油性涂料(83°)，水性聚氨酯具有最大的水接触角(85°)。
具体实施方式
一种抗菌水性聚氨酯涂料的制备方法，包括如下步骤：
S1、将异佛尔酮二异氰酸酯(IPDI)、聚己内酯二元醇、二羟甲基丙酸(DMPA)、双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、催化剂按比例加入三口烧瓶，60～80℃条件下反应2～4小时，再加入一定量甲基丙烯酸羟乙酯(HEMA)反应2～4小时，再加入一定量三乙胺反应0.5～1小时，得到组分1。
其中，原料按照质量份数制备：
S2、将异佛尔酮二异氰酸酯(IPDI)、聚己内酯三元醇、双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、催化剂按比例加入三口烧瓶，60～80℃条件下反应2～4小时，再加入一定量甲基丙烯酸羟乙酯(HEMA)反应2～4小时，得到组分2。
其中，原料按照质量份数制备：
S3、将组分1和组分2按照比例混合，加入一定量去离子水、光引发剂、消泡剂和流平剂，在高速分散机的条件下分散30分钟，得到水性聚氨酯涂料。
S1和S2中，所述IBA(OH)2合成步骤如下：
将1-硫代甘油、甲基丙烯酸异冰片酯、光引发剂和四氢呋喃加入锥形瓶中，在紫外光照下，20～40℃反应2～6小时；
将上述步骤中产物旋蒸，再加入去离子水洗涤，再用无水乙醚萃取2～3遍，蒸干溶剂得到产品IBA(OH)2。
其中，原料按照质量分数制备：
光引发剂为2,2-二甲氧基-2-苯基苯乙酮、二苯基乙酮、1-羟基环己基苯基甲酮中的一种，优选为2,2-二甲氧基-2-苯基苯乙酮。
IBA(OH)2可自制，也可以外购。
实施例1
首先将8g1-硫代甘油、10g甲基丙烯酸异冰片酯、1g光引发剂和20ml四氢呋喃加入锥形瓶中，在紫外光照下，25℃反应4小时，然后将产物旋蒸，再加入去离子水洗涤，再用无水乙醚萃取2～3遍，蒸干溶剂得到产品IBA(OH)2，合成表征红外光谱图和核磁共振氢谱图如图1。
将50g异佛尔酮二异氰酸酯(IPDI)、100g聚己内酯二元醇(PCL)、6.5g二羟甲基丙酸(DMPA)、2g双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、1g催化剂加入三口烧瓶，60℃条件下反应4小时，再加入13g甲基丙烯酸羟乙酯(HEMA)反应2小时，再加入2份三乙胺反应0.5小时，得到组分1。将35g异佛尔酮二异氰酸酯(IPDI)、30g聚己内酯三元醇(PCL)、8g双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、1g催化剂加入三口烧瓶，60℃条件下反应4小时，再加入13g甲基丙烯酸羟乙酯(HEMA)反应2小时，得到组分2。将组分1和组分2按照4：1的比例，总质量为20g，加入30g去离子水、5g光引发剂、0.1g消泡剂AFCONA3030和0.2g流平剂AFCONA2524，在高速分散机3000r/min条件下分散30分钟，制备出固含量40％的水性聚氨酯涂料(如图2所示)。
将制备的水性聚氨酯涂料(含量40％)放置在高速离心机中，3000r/min离心测试15分钟，没有出现沉淀(如图3所示)，说明涂料至少能够在常温放置6个月。将添加抗菌剂的涂料与没有添加抗菌剂的涂料进行抗菌实验，说明本发明的涂料具有良好的抗菌效果(如图5所示)。
将制备的水性聚氨酯抗菌涂料喷涂在玻璃片和钢板上，40℃下烘烤5分钟，待水分烘干后，采用UV光固化机固化，制备得到无色透明的抗菌涂层。经测试该涂层的耐水性、耐酸碱性比一般水性聚氨酯涂料优异，如图6和表1所示。
表1、涂层性能表
实施例2
将50g异佛尔酮二异氰酸酯(IPDI)、100g聚己内酯二元醇(PCL)、6.5g二羟甲基丙酸(DMPA)、2g双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、1g催化剂加入三口烧瓶，60℃条件下反应4小时，再加入13g甲基丙烯酸羟乙酯(HEMA)反应2小时，再加入2份三乙胺反应0.5小时，得到组分1。将35g异佛尔酮二异氰酸酯(IPDI)、30g聚己内酯三元醇(PCL)、8g双羟基化甲基丙烯酸异冰片酯(IBA(OH)2)、1g催化剂加入三口烧瓶，60℃条件下反应4小时，再加入13g甲基丙烯酸羟乙酯(HEMA)反应2小时，得到组分2。将组分1和组分2按照4：1的比例，总质量为50g，加入约35g去离子水、5g光引发剂、0.1g消泡剂AFCONA3030和0.2g流平剂AFCONA2524，在高速分散机3000r/min条件下分散30分钟，制备出固含量60％的水性聚氨酯涂料。
设计60％固含量水性聚氨酯乳液的热重分析如图4所示。
图4为水性聚氨酯热重分析固含量图。
Claims (9)
1. 一种高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于，步骤如下：
S1、加入40~80质量份二异氰酸酯、80~160质量份多元醇、6~24质量份组合扩链剂、0.4~1.2质量份催化剂、12~26质量份羟基丙烯酸酯、2~6质量份中和剂发生扩链反应，制得组分1；
S2、加入30~60质量份二异氰酸酯、30~50质量份多元醇、8~15质量份双羟基化甲基丙烯酸异冰片酯、0.2~1.2质量份催化剂、12~20质量份羟基丙烯酸酯发生扩链反应，制得组分2；
S3、取质量比为3~5:1的组分1和组分2混合，组分1和组分2的总质量份为20-50份，加入30-35质量份去离子水、5~10质量份光引发剂、0.02~0.1质量份消泡剂和0.04~0.2质量份流平剂分散均匀，得到水性聚氨酯涂料；
S1中组合扩链剂包括双羟基化甲基丙烯酸异冰片酯和亲水性扩链剂；
所述亲水性扩链剂为二羟甲基丙酸，双羟基化甲基丙烯酸异冰片酯和二羟甲基丙酸的质量比为1~5：2~7。
2.根据权利要求1所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于，扩链反应的温度为60~80℃，反应时间为4~9小时。
3.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：所述二异氰酸酯为甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、苯二甲撑二异氰酸酯和四甲基苯二甲基二异氰酸酯中的一种或多种。
4.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：所述多元醇为聚己内酯二元醇和聚己内酯三元醇中的一种或多种。
5.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：所述催化剂为二丁基二月桂酸锡、辛酸亚锡、二醋酸二丁基锡和有机铋类催化剂中的一种或多种。
6.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：所述羟基丙烯酸酯为丙烯酸羟乙酯、丙烯酸羟丙酯、丙烯酸羟丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸羟丙酯和甲基丙烯酸羟丁酯中的一种或多种；
所述中和剂为氨水、氢氧化钠、氢氧化钾、三乙胺和三正丁胺中的一种或多种。
7.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：光引发剂为1-羟基环己基苯基甲酮、2-羟基-2-甲基-1-苯基丙酮和2-羟基-4-(2-羟乙氧基)-2-甲基苯丙酮中的一种或者多种。
8.根据权利要求1-2任意一项所述的高固体份、高耐水性抗菌水性聚氨酯涂料的制备方法，其特征在于：消泡剂为AFCONA2503、2505、2507、2524和2590中的一种或者多种；
流平剂为AFCONA3030、3522、3585和3588中的一种或者多种。
9.一种利用权利要求1-8任意一项所述的方法制备的高固体份、高耐水性抗菌水性聚氨酯涂料。
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