CN106318008A - 聚合物包封的tio2涂料调配物 - Google Patents

聚合物包封的tio2涂料调配物 Download PDF

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CN106318008A
CN106318008A CN201610443504.XA CN201610443504A CN106318008A CN 106318008 A CN106318008 A CN 106318008A CN 201610443504 A CN201610443504 A CN 201610443504A CN 106318008 A CN106318008 A CN 106318008A
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J·C·勃林
D·G·凯利
P·罗
Y·蒂瓦里
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Rohm and Haas Co
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Abstract

本发明为一种组合物，其包含a)用包封包含二丙酮丙烯酰胺结构单元的丙烯酸或苯乙烯‑丙烯酸聚合物包封TiO2颗粒的水分散液；以及b)己二酸二酰肼。所述组合物可用于涂料应用中并且示出了相对于不包括二丙酮丙烯酰胺官能化包封聚合物和己二酸二酰肼的组合物的光泽度的出人意料的改善。

Description

聚合物包封的TIO2涂料调配物
背景技术
本发明涉及一种聚合物包封的TiO2涂料调配物及其制备，更具体地说呈现改善的光泽度的涂料调配物。
乳浊颜料(如TiO2)用于涂料调配物中以提供白度和不透明度(遮盖力)以隐藏在其上应用涂料的衬底。调配者希望最大化遮盖力同时最小化用于调配物中的乳浊颜料的量。为此，通过Allen等人(US 8,283,404)的用于聚合物包封的TiO2颗粒的有效组合物的开发表示在提高在涂料调配物中的TiO2颗粒的间距的效率中的显著进展。随后，Bardman等人(US 2014/0011943)根据Allen等人的发现改善用于制备包封有在环境温度下成膜的聚合物的TiO2的实际上粗粒自由水分散液的方法。
尽管遮盖力效率已被显著改善，但是对于含聚合物包封的TiO2颗粒的调配物的持续关注中的一个是相对于不使用包封技术对调配物的光泽度发展：较大复合颗粒本身产生比其未包封的对应部分低的光泽。因此，期望的是寻找一种改善在含聚合物包封的TiO2颗粒的涂层组合物中的光泽度的方式。
发明内容
本发明通过提供一种组合物解决在本领域中的需要，所述组合物包含a)用包封丙烯酸或苯乙烯-丙烯酸聚合物包封的TiO2颗粒，和以包封聚合物的重量计0.5重量％至5重量％的二丙酮丙烯酰胺结构单元的水分散液；以及b)以包封聚合物的重量计0.2重量％至3重量％的己二酸二酰肼。本发明的组合物提供了相对于不含有在包封聚合物中的二丙酮丙烯酰胺基团和在稳定水性分散液的水相中的己二酸二酰肼的类似组合物的改善的光泽度。
具体实施方式
本发明为一种组合物，其包含a)用包封丙烯酸或苯乙烯-丙烯酸聚合物包封的TiO2颗粒的水分散液，所述聚合物包含以包封聚合物的重量计0.5重量％至5重量％的二丙酮丙烯酰胺结构单元；以及b)以包封聚合物的重量计0.2重量％至3重量％的己二酸二酰肼。
具有用丙烯酸或苯乙烯-丙烯酸包封聚合物的TiO2的包封可以以多种方式(包括描述于US 8,283,404和US 2014/0011943中的那些方法)实现。包封丙烯酸或苯乙烯-丙烯酸聚合物优选在室温下成膜；也就是说，选择单体的性质和相对浓度以产生如通过福克斯(Fox)方程式测定的Tg优选不超过20℃、更优选不超过10℃并且最优选不超过0℃；并且优选不低于-40℃并且更优选不低于-30℃的聚合物。(参见《美国物理学会公报(Bulletin ofthe American Physical Society)》1，3，第123页(1956))。本领域的普通技术人员将能够制备期望Tg的聚合物。
如本文所用，术语“丙烯酸或苯乙烯-丙烯酸包封聚合物”是指包含30重量％至99.5重量％的一种或多种丙烯酸酯或甲基丙烯酸酯单体的结构单元或30重量％至99.5重量％的苯乙烯和一种或多种丙烯酸酯或甲基丙烯酸酯单体的结构单元的聚合物。如本文所用，“结构单元”是指所述单体后聚合的残余物。示出了甲基丙烯酸甲酯的结构单元：
其中虚线表示结构单元附接到聚合物主链的点。
用于制备包封丙烯酸或苯乙烯-丙烯酸聚合物的单体优选包括a)甲基丙烯酸甲酯或苯乙烯或其组合，以及b)丙烯酸乙酯、丙烯酸丁酯或丙烯酸乙基己酯或其组合。适于制备包封聚合物的其它辅助单体包括含羧酸的单体(如丙烯酸、甲基丙烯酸或衣康酸)；磺酸单体或其盐(如2-丙烯酰胺基-2-甲基丙磺酸和苯乙烯磺酸钠)；以及交联单体(如甲基丙烯酸烯丙酯和二乙烯基苯)。
包封聚合物的丙烯酸或苯乙烯-丙烯酸包封聚合物包封聚合物的重要特征为，以包封聚合物的重量计，存在0.5重量％、优选1重量％至5重量％、优选至3重量％的二丙酮丙烯酰胺结构单元。
本发明的组合物还包括以包封聚合物的重量计0.2重量％、优选0.5重量％至3重量％、优选至1.5重量％的己二酸二酰肼。
本发明的组合物可用于涂料调配物中并且可与以下材料中的一种或多种混合：分散剂、消泡剂、表面活性剂、溶剂、附加粘结剂、增稠剂、增充剂、聚结剂、杀生物剂以及着色剂。已出人意料地发现，相比于不含有己二酸二酰肼并且包含用不是用二丙酮丙烯酰胺结构单元官能化的聚合物的丙烯酸或苯乙烯-丙烯酸包封的TiO2颗粒的组合物，包含己二酸二酰肼和用用二丙酮丙烯酰胺结构单元官能化的聚合物的丙烯酸或苯乙烯-丙烯酸包封的TiO2颗粒的水性涂料组合物呈现改善的光泽度。
在以下实例中，基本上如在美国专利公开20100/298483，第7页，第0053段以及第8页，第0059段中所公开的制备TiO2-分散剂浆液。
实例
比较实例1-不用后聚合交联制备聚合物包封的TiO2复合材料
通过将水(60g)、BIO-SOFT S-101表面活性剂(6.5g，用氨中和，25％水溶液)、甲基丙烯酸(0.84g)、苯乙烯磺酸钠(0.84g)、丙烯酸丁酯(150.11)、甲基丙烯酸甲酯(126.21g)、脲基甲基丙烯酯(7g)以及苯甲酮(4.2g，在丙烯酸丁酯中的40％溶液)混合制备单体乳液(ME)。
配备有机械浆式搅拌器、热电偶、N2入口以及回流冷凝器的2L的4颈圆底烧瓶中添加TiO2-分散剂浆液(479.45g)和水(30g)。在N2下将混合物加热至50℃；向烧瓶中依次添加BIO-SOFT S-101表面活性剂在水(20g)中的预混合水溶液(3.36g，用氨中和，25％水溶液)、苯乙烯磺酸钠的预混合水溶液(0.74g，在20g水中)、七水合硫酸铁的水溶液的混合物(6.53g，0.10％铁)以及乙二胺四乙酸水溶液(EDTA，0.28g，1％)。将叔丁基过氧化氢溶液(0.77g，在60g水中)和异抗坏血酸溶液(0.46g，在60g水中)以0.65g/min的速率进料至烧瓶。在3min后，将ME以5g/min的速率进料至反应器，并且允许烧瓶温度放热至65℃并且维持在该温度下。在完成ME添加后，将单体乳液容器用添加到烧瓶的去离子水(5g)冲洗。持续添加共进料催化剂和活化剂直至完成。在所有进料完成之后，烧瓶冷却到室温。当烧瓶温度达到45℃时，将ACRYSOLTM ASE-60增稠剂的水溶液(5.5g，在10g水中，陶氏化学公司(The DowChemical Company)或其附属公司的商标)以1.5g/min的速率添加到烧瓶，接着以0.4g/min的速率添加29％氢氧化铵水溶液(2g)和水(2g)的溶液，并且以0.5g/min的速率添加ROCIMATM BT 2S杀生物剂(2.6g，陶氏化学公司或其附属公司的商标)和水(6g)的溶液。
在烧瓶冷却到室温之后，过滤内含物以移除任何凝胶。发现经过滤的分散液的固体含量为58.3％，其中pH为9.0。
实例1-用后聚合交联制备聚合物包封的TiO2复合材料
通过将水(60g)、Polystep A-16-22表面活性剂(7.22g)、甲基丙烯酸(0.84g)、苯乙烯磺酸钠(0.84g)、二丙酮丙烯酰胺(5.6g)、丙烯酸丁酯(150.11)、甲基丙烯酸甲酯(120.68g)、脲基甲基丙烯酯(7g)以及苯甲酮(4.2g，在丙烯酸丁酯中的40％溶液)混合制备单体乳液(ME)。
向配备有机械浆式搅拌器、热电偶、N2入口以及回流冷凝器的2L的4颈圆底烧瓶中添加TiO2-聚合物浆液(479.45g)和水(30g)。在N2下将混合物加热至50℃；接着向烧瓶中依次添加Polystep A-16-22表面活性剂的预混合水溶液(3.73g，在20g水中)、苯乙烯磺酸钠的预混合水溶液(2.91g，在20g水中)、七水合硫酸铁的水溶液的混合物(6.53g，0.10％铁)以及EDTA水溶液(0.28g，1％)。将叔丁基过氧化氢溶液(3.08g，在60g水中)和异抗坏血酸溶液(1.82g，在61g水中)以0.65g/min的速率进料至烧瓶。在3min后，将ME以5g/min的速率进料至反应器，并且允许烧瓶温度放热至65℃并且控制在该温度下。在完成ME添加后，将单体乳液容器用5g添加到烧瓶的去离子水冲洗。持续添加共进料催化剂和活化剂直至完成。在所有进料完成之后，烧瓶冷却到室温。当烧瓶温度达到45℃时，将己二酸二酰肼的水性悬浮液(2.8g，在10g水中)添加到烧瓶，随后以0.4g/min的速率添加29％氢氧化铵水溶液(1g)和水(2g)的溶液，并且以0.5g/min的速率添加ROCIMATM BT 2S杀生物剂(2.6g)和水(6g)的溶液。
在烧瓶冷却到室温之后，过滤内含物以移除任何凝胶。发现经过滤的分散液的固体含量为58.4％，其中pH为8.0。
根据来自实例1和比较实例1的涂料调配物
表1示出了用于形成18.0％(油漆1和油漆2)以及14.4％(油漆3和油漆4)颜料容积浓度(PVC)涂料调配物的添加剂。
缩略语
缩写 产品名称
丙烯酸粘结剂 RHOPLEXTM HG-706丙烯酸粘结剂
表面活性剂 TERGITOLTM 15-s-40表面活性剂
消泡剂 Foamstar A-34D消泡剂
聚结剂 Texanol聚结剂
RM1 ACRYSOLTM RM-2020NPR流变改性剂
RM2 ACRYSOLTM RM-8W流变改性剂
RHOPLEX、TERGITOL和ACRYSOL都是陶氏化学公司或其附属公司的商标。
表1-含聚合物包封的TiO2复合材料的涂料调配物
光泽度测量
调配的油漆样品用3-密耳Bird涂覆器涂覆到Leneta白色卡片(WB形式)。允许样品干燥24h，并且用来自于毕克加德纳(BYK Gardner)的Micro-TRI-光泽计测量光泽度。
通过如下库贝尔卡-芒克(Kubelka-Munk)测试方法测量遮盖力(S/密耳)：
库贝尔卡-芒克S/密耳测试方法
对于每种油漆，使用1.5密耳Bird刮涂棒在黑色释放卡(Black Release Chart)(Leneta Form RC-BC)上制备两个刮涂物，并且允许所述卡干燥过夜。使用模板，在每个卡上用X-ACTO刀具切出3.25″×4″矩形。在每个划线区域中使用毕克加德纳45度反射计(BYKGardner 45°Reflectomer)测量y反射率(在以矩形顶部开始的对角线上测量五次)并且记录平均y反射率。使用3″25密耳阻塞刮涂棒在黑色乙烯卡(Black Vinyl Charts)(Leneta FormP121-10N)上制备对于每种油漆的厚膜刮涂物，并且允许所述卡干燥过夜。在刮涂物的五个不同区域中测量y-反射率，并且记录平均y-反射率。通过以下公式1给出库贝尔卡-芒克遮盖力值S：
公式1
S = R X × ( 1 - R 2 ) × ln 1 - ( R B × R ) 1 - R B R
其中X是平均膜厚度，R是厚膜的平均反射率，并且RB是对于薄膜的黑色的平均反射率。X可以通过漆膜的重量(Wpf)、干膜的密度(D)以及膜面积(A)计算。3.25″×4″模板的膜面积是13in2。
X ( m i l s ) = W p f ( g ) × 1000 ( m i l / i n ) D ( l b s / g a l ) × 1.964 ( g / in 3 / l b s / g a l ) × A ( i n )
表2示出对于四个油漆样品的遮盖力和光泽度。光泽度是在1天后以20°和60°测量的。
表2-遮盖力和光泽度结果
如表2所示，使用来自实例1的复合粒子制备的油漆(油漆2和油漆4)示出显著改进的20°光泽度以及统计学上显著改进的60°光泽度，而基本上不损耗遮盖力。

Claims (3)

1.一种组合物，其包含a)用包封丙烯酸或苯乙烯-丙烯酸聚合物包封的TiO2颗粒的水分散液，所述聚合物包含以所述包封聚合物的重量计0.5重量％至5重量％的二丙酮丙烯酰胺结构单元；以及b)以所述包封聚合物的重量计0.2重量％至3重量％的己二酸二酰肼。
2.根据权利要求1所述的组合物，其中所述包封丙烯酸或苯乙烯-丙烯酸聚合物的计算的Tg为-30℃至20℃。
3.根据权利要求2所述的组合物，其中以所述包封聚合物的重量计，所述包封丙烯酸或苯乙烯-丙烯酸聚合物包含1重量％至3重量％的二丙酮丙烯酰胺结构单元；并且其中以所述包封聚合物的重量计，所述组合物包含来自b)的0.5重量％至1.5重量％的己二酸二酰肼。
CN201610443504.XA 2015-07-01 2016-06-20 聚合物包封的tio2涂料调配物 Pending CN106318008A (zh)

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