CN114174445B - 聚丙烯酸和聚乙酸乙烯酯胶乳的共混物 - Google Patents
聚丙烯酸和聚乙酸乙烯酯胶乳的共混物 Download PDFInfo
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Abstract
本发明是一种组合物，其包含基于PVA的胶乳和基于EA/MMA的聚丙烯酸胶乳的共混物。本发明的组合物可用于涂料配制品中，以用于提供具有与包含基于PVA的胶乳和基于BA/MMA的聚丙烯酸胶乳的共混物的配制品相比更优异的耐擦洗性的涂层。
Description
背景技术
本发明涉及一种基于聚丙烯酸的胶乳和基于聚(乙酸乙烯酯)的胶乳的共混物。
与含有组成均匀的胶乳的配制品相比，将组成不同的胶乳共混的目的是在水性建筑涂料配制品中实现更好的特性平衡。遗憾的是，将化学不相容的胶乳混合降低混溶性，从而导致一种或多种所需特性的不可接受的退化。
与基于聚丙烯酸胶乳的涂料相比，基于聚(乙酸乙烯酯)(PVA)胶乳的涂料通常赋予涂层优异的擦洗性能。虽然PVA胶乳与聚丙烯酸胶乳相比也具有成本优势，但是由基于PVA胶乳的涂料制成的涂层具有许多由基于聚丙烯酸的涂料提供的劣质特性，包括后续涂层的粘合和耐污染性。试图通过将PVA和聚丙烯酸胶乳组合到单一涂料配制品中来实现两类胶乳的特性益处和成本优势，结果导致耐擦洗性的不可接受的降低。因此，更经济地设计具有基于PVA和聚丙烯酸两者的胶乳的特性优势的胶乳将是有利的。
发明内容
本发明通过提供一种包含第一聚合物颗粒和第二聚合物颗粒的水性分散体的组合物解决了本领域的需求，其中所述第一聚合物颗粒包含基于所述第一聚合物颗粒的重量60至99.8重量百分比的乙酸乙烯酯结构单元，并且所述第二聚合物颗粒包含基于所述第二聚合物颗粒的重量至少80重量百分比的丙烯酸乙酯和甲基丙烯酸甲酯的结构单元，其中所述第二聚合物颗粒中丙烯酸乙酯与甲基丙烯酸甲酯的结构单元的重量比的范围是50:50至95:5；并且其中所述第一聚合物颗粒与所述第二聚合物颗粒的重量比的范围是30:70至90:10。本发明的组合物提供了一种可用于涂料组合物的胶乳混合物，用于提供具有改善的耐擦洗性的涂层。
具体实施方式
本发明是一种包含第一聚合物颗粒和第二聚合物颗粒的水性分散体的组合物，其中所述第一聚合物颗粒包含基于所述第一聚合物颗粒的重量60至99.8重量百分比的乙酸乙烯酯结构单元，并且所述第二聚合物颗粒包含基于所述第二聚合物颗粒的重量至少80重量百分比的丙烯酸乙酯和甲基丙烯酸甲酯的结构单元，其中所述第二聚合物颗粒中丙烯酸乙酯与甲基丙烯酸甲酯的结构单元的重量比的范围是50:50至95:5；并且其中所述第一聚合物颗粒与所述第二聚合物颗粒的重量比的范围是30:70至90:10。
第一聚合物颗粒优选具有如通过动态光散射测量的在150nm、优选250nm至400nm范围内的体积平均粒径。第一聚合物颗粒优选包含60至95重量百分比的乙酸乙烯酯(VA)结构单元，并且优选还包含基于第一聚合物颗粒的重量5、更优选10、更优选15、最优选25至优选40、更优选至38重量百分比的丙烯酸烷基酯的结构单元，诸如丙烯酸乙酯(EA，Tg＝-22℃)、丙烯酸丁酯(BA，Tg＝-54℃)、丙烯酸2-乙基己酯(2-EHA，Tg＝-85℃)，或乙烯或叔碳酸乙烯酯的结构单元。
如本文所用，指定单体的术语“结构单元”是指单体在聚合之后的残余物。例如，甲基丙烯酸甲酯(MMA)的结构单元如下说明：
甲基丙烯酸甲酯的结构单元
其中虚线表示结构单元与聚合物主链的连接点。
第一聚合物颗粒还优选包含0.2至5、更优选至2重量百分比的酸单体的结构单元，诸如羧酸单体、磷酸单体或硫酸单体。合适的羧酸单体包括丙烯酸(AA)、甲基丙烯酸(MAA)和衣康酸(IA)及其盐。
合适的磷酸单体包括醇的膦酸酯和磷酸二氢酯，其中醇含有可聚合的乙烯基或烯基或被可聚合的乙烯基或烯基取代。优选的磷酸二氢酯是丙烯酸羟烷基酯或甲基丙烯酸羟烷基酯的磷酸酯，包括甲基丙烯酸磷酸乙酯(PEM)和甲基丙烯酸磷酸丙酯。其他合适的磷酸单体包括由以下结构表示的可聚合乙氧基化磷酸酯：
及其盐，其中R是H或CH3，其中R1和R2各自独立地是H或CH3，其条件是没有两个相邻的CR2CR1基团各自被甲基取代；每个R3独立地是直链或支链C2-C6亚烷基；m为1至10；n为0至5，其条件是当m为1时，n为1至5；x为1或2；并且y为1或2；并且x+y＝3。当n为0，x为1且y为2时，可聚合的有机磷酸酯或其盐由式II的结构表示：
Sipomer PAM-100、Sipomer PAM-200和Sipomer PAM-600磷酸酯为在式II化合物的范围内可商购的化合物的实例。
合适的硫酸单体的实例包括甲基丙烯酸乙磺酸酯、甲基丙烯酸丙磺酸酯、苯乙烯磺酸、乙烯基磺酸和2-丙烯酰胺基-2-甲基丙磺酸(AMPS)及其盐。
第二聚合物颗粒优选具有如通过动态光散射测量的在70nm、更优选80nm至300nm、更优选至250nm、更优选至200nm并且最优选至150nm范围内的体积平均粒径。优选调节EA与MMA的比率以产生具有如通过福克斯方程计算的在-10℃、优选0℃至30℃、更优选至25℃并且最优选至20℃范围内的Tg的聚合物颗粒。优选地，第二聚合物颗粒中EA与MMA的重量比的范围是60:40、更优选65:45至90:10、更优选至85:15并且最优选至80:20。
第二聚合物颗粒优选包含0.1至3重量百分比的酸单体结构单元，包括羧酸单体、磷酸单体和硫酸单体及其盐，如上文所述。第二聚合物颗粒有利地包括MAA和/或PEM及其盐的结构单元。第二聚合物颗粒中的一种或多种酸单体的结构单元的总浓度优选在基于第二聚合物颗粒的重量0.2至2重量百分比的范围内。
第二聚合物颗粒优选包含基于第二聚合物颗粒的重量至少90、更优选至少95并且最优选至少98.1重量百分比的EA和MMA的结构单元。第二聚合物颗粒包含小于20重量百分比的其他辅助单体的结构单元，诸如BA和丙烯腈(AN)。优选地，第二聚合物颗粒包含基于第二聚合物颗粒的重量小于1.9重量百分比、更优选小于1重量百分比并且最优选0重量百分比的AN结构单元；以及基于第二聚合物颗粒的重量优选小于10、更优选小于5重量百分比的BA结构单元。
本发明的组合物可用作涂料配制品、尤其是用于建筑涂层应用的涂料配制品的粘合剂，其具有优选在20％、更优选40％至70％、更优选至60％范围内的颜料体积浓度。因此，在另一方面，本发明包括一种胶乳涂料组合物，其包含本发明组合物的聚丙烯酸和PVA胶乳以及分散剂、表面活性剂、消泡剂、中和剂、颜料、增链剂、聚结剂和流变改性剂。涂料组合物还可以包含不透明聚合物和杀生物剂。已经意外地发现，在第二聚合物颗粒(对应于基于聚丙烯酸的胶乳)中用EA代替BA始终赋予涂层改善的耐擦洗性，而不会减弱由基于聚丙烯酸的胶乳赋予的其他特性。
实施例
在以下实施例中，使用Brookhaven BI-90粒径分析仪测量胶乳粒径(PS)
中间体实施例1–用EA、MMA和MAA官能化的丙烯酸胶乳的制备
使用去离子水(800g)、Polystep B-5-N乳化剂(16.6g)、EA(1142g)、冰MAA(19.5g)和MMA(774g)制备单体乳液。将去离子水(676g)添加到配备有机械搅拌器、热电偶、回流冷凝器、N2入口以及单体乳液(ME)和引发剂溶液入口的5-L4颈烧瓶中。将水搅拌并加热至87℃，在所述温度下将由去离子水(12g)和Polystep B-5-N乳化剂(19.7g)组成的溶液添加到烧瓶中，接着添加Na2CO3(6.8g)在去离子水(67.1g)中的溶液。然后将一部分ME(58.8g)添加到烧瓶中，接着添加去离子水(17g)和过硫酸铵(APS，6.8g)的引发剂溶液。
约5min之后，将ME的剩余部分连同去离子水(91.5g)和APS(1.0g)的溶液一起在80min内进料到反应器中，反应器温度控制在88℃下。将ME和APS溶液分别以23.9g/min和0.81g/min的速率进料，持续10min，之后在剩余的70min内将ME进料速率增加至35.9g/min，并且将APS溶液进料速率增加至1.22g/min。在ME进料开始43min之后，将N-(2-甲基丙烯酰氧基乙基)亚乙基脲(19.6g)在去离子水(19.6g)中的溶液添加到ME中，接着进行冲洗。
在完成进料之后，将反应器冷却至75℃，然后将七水合硫酸亚铁(0.02g)和VERSENETM 220螯合剂(Dow,Inc.或其附属公司的商标，0.02g)在去离子水(15.4g)中的溶液添加到烧瓶中。将叔丁基过氧化氢(t-BHP，1.4g，70％活性)在去离子水(17.7g)中的溶液和异抗坏血酸(IAA，0.74g)在去离子水(18.3g)中的单独溶液在75℃下在20min进料到反应器中。在完成进料添加之后，将反应混合物冷却至30℃并用氢氧化铵溶液(12.5g，28％水溶液)中和至pH 8.5。
将Kathon；LX 1400防腐剂(1.36g)和VERSENETM 220螯合剂(0.46g)在去离子水(24.4g)中的溶液添加到烧瓶中。过滤所得的胶乳以除去凝结物。所得胶乳的测量的固体含量为50.4％；PS为120nm。
中间体实施例2–用EA、MMA和MAA官能化的丙烯酸胶乳的制备
基本上如中间体实施例1所述进行程序，不同之处在于将叔戊基过氧化氢(t-AHP，1.45g，85％活性)和Polystep B-5-N乳化剂(0.2g)在去离子水(18.1g)中的额外溶液和IAA(1.1g)在去离子水(26.6g)中的单独溶液在75℃下在20min内添加到烧瓶中。所得胶乳的测量的固体为50.0％，并且PS为122nm。
中间体实施例3–用EA、MMA和MAA官能化的丙烯酸胶乳的制备
使用去离子水(800g)、Polystep B-5-N乳化剂(33.2g)、EA(1347g)、冰MAA(19.5g)和MMA(569g)制备ME。将去离子水(1000g)添加到配备有机械搅拌器、热电偶、回流冷凝器、N2入口以及单体乳液(ME)和引发剂溶液入口的5-L 4颈烧瓶中。将水搅拌并加热至87℃，在所述温度下将由去离子水(12g)和Polystep B-5-N乳化剂(39.5g)组成的溶液添加到烧瓶中，接着添加Na2CO3(6.8g)在去离子水(67.1g)中的溶液。然后将一部分ME(58.8g)添加到烧瓶中，接着添加去离子水(17g)和过硫酸铵(APS，6.8g)的引发剂溶液。
约5min之后，将ME的剩余部分连同去离子水(91.5g)和APS(1.0g)的溶液一起在120min内进料到反应器中，反应器温度控制在88℃。将ME和APS溶液分别以12.0g/min和0.41g/min的速率进料，持续10min，之后将ME进料速率增加至18.0g/min，并且将APS溶液进料速率增加至0.61g/min。再过10min之后，对于剩余的100min聚合，将ME进料速率增加至25.2g/min，并且将引发剂溶液增加至0.81g/min。在ME进料开始74min之后，将N-(2-甲基丙烯酰氧基乙基)亚乙基脲(19.6g)在去离子水(19.6g)中的溶液添加到ME中，接着进行冲洗。
在完成进料之后，将反应器冷却至75℃，然后将七水合硫酸亚铁(0.02g)和VERSENETM 220螯合剂(0.02g)在去离子水(15.4g)中的溶液添加到烧瓶中。将t-BHP(1.4g，70％活性)在去离子水(17.7g)中的溶液和IAA(0.74g)在去离子水(18.3g)中的单独溶液在75℃下在20min内添加到反应器中。
在完成进料添加之后，将t-AHP(1.45g)和Polystep B-5-N乳化剂(0.02g)在去离子水(18.1g)中的溶液和IAA(1.1g)在去离子水(26.6g)中的单独溶液在75℃下在20min内进料到反应器中，并且将反应混合物冷却至30℃并用氢氧化铵溶液(12.0g，28％水溶液)中和至pH 8.5。
将Kathon LX 1400防腐剂(1.36g)和VERSENETM 220螯合剂(0.46g)在去离子水(24.4g)中的溶液添加到烧瓶中。过滤所得的胶乳以除去凝结物。所得胶乳的测量的固体含量为46.4％；PS为84nm。
中间体实施例4–用EA、MMA、PEM和MAA官能化的低粒径丙烯酸胶乳的制备
基本上如中间体实施例3所述进行程序，不同之处在于使用去离子水(800g)、Polystep B-5-N乳化剂(33.2g)、EA(1325.5g)、冰MAA(9.8g)、PEM(18.8g，60％活性)和MMA(568.9.1g)制备ME。所得胶乳的测量的固体为46.0％；PS为83nm。
商业丙烯酸胶乳RHOPLEXTM SG-10AF丙烯酸粘合剂(其是w/w/w比率为46/52/1并且固体含量为50％的BA/MMA/MAA胶乳)用于对比中间体实施例1。用此中间体制备对比实施例涂料1、2和3。
对比中间体实施例2–用BA、MMA和MAA官能化的小粒径丙烯酸胶乳的制备
基本上如中间体实施例3所述进行程序，不同之处在于使用去离子水(800g)、Polystep B-5-N乳化剂(30.0g)、BA(1051.8g)、冰MAA(19.5g)和MMA(864.1g)制备ME；并且表面活性剂溶液由去离子水(12g)和Polystep B-5-N乳化剂(42.6g)组成。所得胶乳的测量的固体为46.4％；PS为84nm。
对比中间体实施例3–用BA、MMA、PEM和MAA官能化的低粒径丙烯酸胶乳的制备
基本上如中间体实施例3所述进行程序，不同之处在于使用去离子水(800g)、Polystep B-5-N乳化剂(30.0g)、BA(1030.3g)、冰MAA(18.8g)、PEM(18.8g，60％活性)和MMA(864.1.1g)制备ME；并且表面活性剂溶液由去离子水(12g)和Polystep B-5-N乳化剂(42.6g)组成。所得胶乳的测量的固体为46.4％。所得胶乳的测量的固体为46.1％；PS为85nm。
涂料的制备
将聚合物配制成27.5PVC和50PVC的白色基础涂料。PVC由下式定义：
其中粘合剂固体是指聚合物的来自将颜料和增链剂颗粒粘合在一起的聚合物颗粒的水性分散体的贡献。
表1概述了配制品对比实施例1和对比实施例2中的成分及其水平，这两个配制品均使用如对比中间体实施例1中所述制备的丙烯酸胶乳和商业VA胶乳ROVACETM 9900VA粘合剂(65VA/33.7BA，其中计算的Tg＝6℃，PS＝250nm)来配制。基于胶乳上的固体重量，胶乳以50:50比率组合。(VA胶乳的固体百分比为55％，并且丙烯酸胶乳的固体百分比为50％。
使用高速分散器制备研磨物。使用顶置式搅拌器通过向研磨物中添加成分来进行搅拌过度阶段(letdown stage)。在表1中，165A分散剂是指TAMOLTM 165A分散剂；15-S-9表面活性剂是指TERGITOLTM 15-S-9表面活性剂；SG-10AF是指RHOPLEXTM SG-10AF粘合剂；9900胶乳是指ROVACETM 9900胶乳，其用作所有实施例和对比实施例涂料中的基于VA的胶乳；RM-2020是指ACRYSOLTM RM-2020NPR流变改性剂；RM-75是指ACRYSOLTM RM-75流变改性剂。(TAMOL、TERGITOL、ROVACE、RHOPLEX和ACRYSOL全部是Dow,Inc.或其附属公司的商标。)
耐擦洗性
使用7密耳Dow涂抹棒将涂料涂在Black Leneta乙烯基图表上，一式两份，并且在25℃、50％相对湿度下干燥7天。干燥之后，将每个图表纵向切成两半，为每个涂层产生四个测试条。通过完全混合Leneta标准化磨料型擦洗介质SC-2(636g)、水(318g)和Airex 901W消泡剂(1.5g)来制备擦洗介质。擦洗测试在配备有Masterflex L/S油管泵、具有0.5”x 10密耳黄铜薄片的金属托盘和尼龙硬毛刷的机器上进行。将每个条带放置在薄片上方的金属托盘上，涂覆侧朝上并用夹子固定。将擦洗介质(10g)分布在涂层上，并且在计数器设置为零的情况下开始测试。在每400个循环之后(失效之前)，分布额外量的擦洗介质(10g)，之后继续进行测试。耐擦洗性报告为在0.5”宽度的薄片上在一条连续线中完全去除涂层所需的循环次数。涂层的擦洗循环的平均值和标准偏差基于每个涂层的八次测量来报告。
表2示出了在制备丙烯酸胶乳时用EA代替BA产生的对耐擦洗性的影响。
表2–各种VA/丙烯酸胶乳涂料配制品的擦洗循环数据
数据表明，在制备丙烯酸胶乳时，用EA代替BA显著增强了耐擦洗性。观察到这种改善与VA和丙烯酸粘合剂颗粒(涂料实施例2和3)以及PVC(涂料实施例1和2)的相对量无关，并且在丙烯酸胶乳颗粒进一步用PEM官能化(涂料实施例5)的情况下也看到，这改善了遮盖力。因此，与含有基于VA和MMA/BA的粘合剂的涂料相比，含有基于VA和MMA/EA的粘合剂的涂料的特性总体上得到改善。
Claims (9)
1.一种组合物，其包含第一聚合物颗粒和第二聚合物颗粒的水性分散体，其中所述第一聚合物颗粒包含基于所述第一聚合物颗粒的重量60至99.8重量百分比的乙酸乙烯酯结构单元和5至40重量百分比的丙烯酸烷基酯结构单元，并且所述第二聚合物颗粒包含基于所述第二聚合物颗粒的重量至少80重量百分比的丙烯酸乙酯和甲基丙烯酸甲酯的结构单元，其中所述第二聚合物颗粒中丙烯酸乙酯与甲基丙烯酸甲酯的结构单元的重量比的范围是50:50至95:5；并且其中所述第一聚合物颗粒与所述第二聚合物颗粒的重量比的范围是30:70至90:10。
2.根据权利要求1所述的组合物，其中所述第一聚合物颗粒还包含基于所述第一聚合物颗粒的重量10至38重量百分比的丙烯酸酯结构单元，所述丙烯酸酯是丙烯酸丁酯、丙烯酸乙酯或丙烯酸2-乙基己酯；以及0.2至5重量百分比的酸单体，所述酸单体是羧酸单体、或磷酸单体、或硫酸单体、或其盐。
3.根据权利要求2所述的组合物，其中所述第二聚合物颗粒具有在-10℃至30℃范围内的计算的Tg，并且其中所述第二聚合物颗粒包含0.1至3重量百分比的酸单体结构单元，所述酸单体是羧酸单体、或磷酸单体、或硫酸单体、或其盐。
4.根据权利要求3所述的组合物，其中基于所述第二聚合物颗粒的重量，所述第二聚合物颗粒中的丙烯酸乙酯与甲基丙烯酸甲酯的结构单元的比率在60:40至85:15的范围内，并且其中所述第二聚合物颗粒包含基于所述第二聚合物颗粒的重量至少90重量百分比的丙烯酸乙酯和甲基丙烯酸甲酯的结构单元。
5.根据权利要求4所述的组合物，其中所述第二聚合物颗粒包含基于所述第二聚合物颗粒的重量小于1.9重量百分比的丙烯腈结构单元。
6.根据权利要求3所述的组合物，其中如通过动态光散射测量的所述第一聚合物颗粒的体积平均粒径在200nm至400nm的范围内；并且其中如通过动态光散射测量的所述第二聚合物颗粒的体积平均粒径在70nm至150nm的范围内。
7.根据权利要求3所述的组合物，其中所述酸单体是甲基丙烯酸磷酸乙酯或甲基丙烯酸或其盐，或甲基丙烯酸磷酸乙酯和甲基丙烯酸或其盐。
8.根据权利要求1所述的组合物，其还包含分散剂、表面活性剂、消泡剂、中和剂、颜料、增链剂、聚结剂和流变改性剂。
9.根据权利要求8所述的组合物，其具有在40％至70％范围内的颜料体积浓度。
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| PCT/US2020/044818 WO2021030095A1 (en) | 2019-08-09 | 2020-08-04 | Blend of polyacrylic and polyvinyl acetate latexes |
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| WO2024064581A1 (en) * | 2022-09-20 | 2024-03-28 | Rohm And Haas Company | Microbe resistant acrylic latex composition |
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| WO2021030095A1 (en) | 2021-02-18 |
| US12024638B2 (en) | 2024-07-02 |
| BR112022001545A2 (pt) | 2022-03-22 |
| CA3146864A1 (en) | 2021-02-18 |
| US20220275238A1 (en) | 2022-09-01 |
| AU2020329845A1 (en) | 2022-03-03 |
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| CN114174445A (zh) | 2022-03-11 |
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