CN112266687A - 一种季铵盐型研磨树脂的制备方法及免研磨阳离子型彩色电泳色浆 - Google Patents

一种季铵盐型研磨树脂的制备方法及免研磨阳离子型彩色电泳色浆 Download PDF

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CN112266687A
CN112266687A CN202011179699.4A CN202011179699A CN112266687A CN 112266687 A CN112266687 A CN 112266687A CN 202011179699 A CN202011179699 A CN 202011179699A CN 112266687 A CN112266687 A CN 112266687A
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贾龙娟
刘薇薇
赵颖
胡浩东
刘铭
倪锦程
黄磊
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Abstract

本发明涉及季铵盐型研磨树脂制备方法及免研磨阳离子型彩色电泳色浆，本发明通过将基础环氧树脂、双酚A、三苯基膦、酮类溶剂进行升温扩链反应得到环氧树脂中间产物；将TDI滴加醇醚类封闭剂，升温后保温反应，得到半封闭异氰酸酯；在环氧树脂中间产物中加入半封闭异氰酸酯进行接枝反应，加入聚乙烯蜡及醇醚类溶剂搅拌获得非水溶研磨树脂；将半封闭异氰酸酯滴加叔胺进行胺化反应后加有机酸得到季铵盐型异氰酸酯；稀释后非水溶研磨树脂加入季铵盐型异氰酸酯，保温反应加入去离子水稀释，获得季铵盐型研磨树脂。通过以上季铵盐型研磨树脂制得阳离子型彩色电泳色浆产品涂膜耐磨性佳、耐候性提升，并有免研磨、高生产效率，耐热环境存储稳定等特点。

Description

一种季铵盐型研磨树脂的制备方法及免研磨阳离子型彩色电 泳色浆
技术领域
本发明属于水性电泳色浆技术领域，具体涉及一种季铵盐型研磨树脂的制备方法及免研磨阳离子型彩色电泳色浆。
背景技术
电泳涂料具有低VOC、绿色环保、利用率高、自动化程度高、性能优异等优点，在工业涂装方面占据重要地位。电泳涂料高生产效率、高装饰性优势日趋明显。现如今，彩色电泳色浆依然存在生产、供货周期长，制备设备成本较高，耐磨性、耐候性较差的问题。
发明内容
本发明的主要目的在于提供一种免研磨的阳离子彩色电泳色浆，所述电泳色浆采用季铵盐研磨树脂，在树脂体系中引入聚乙烯蜡，使用醇醚溶剂溶解后胺化前加入，提供改性有机颜料。
所述季铵盐型研磨树脂由以下方法制备：
S1.将50重量份的YD-128环氧树脂、20重量份的双酚A树脂、占总重量0.2‰的三苯基膦、20重量份的酮类溶剂在140-150℃进行扩链反应，得到环氧当量650-730的环氧树脂中间产物；
S2.将10-12重量份的TDI升温至45-55℃，滴加8-10重量份的醇醚类封闭剂，滴加结束，升温至70-80℃保温2-3h，得到封闭率55％半封闭异氰酸酯；
S3.环氧当量为650-730的环氧树脂中间产物控制温度在140-150℃，滴加以上半封闭异氰酸酯，达到接枝率20％的环氧树脂；降温控制温度110℃以下，加入总量4％聚乙烯蜡及1.5倍量的醇醚类溶剂溶解得到搅拌均匀的非水溶研磨树脂；
S4.将10-12重量份的叔胺升温至70-90℃，滴加以上封闭率55％半封闭异氰酸酯，反应2-3h；加入5-7重量份的有机酸后保温2-3h，季铵盐型水溶性异氰酸酯。
S5.在非水溶性研磨树脂中加入以上季铵盐型水溶性异氰酸酯，控制胺化率90％，反应8-10h；加入去离子水稀释，得到固体份为30％的季铵盐型研磨树脂。
进一步的，所述的季胺盐型研磨树脂的制备方法中，所述酮类溶剂为丙酮、丁酮、甲基异丁基酮中的至少一种。
进一步的，所述的季胺盐型研磨树脂的制备方法，经过所述扩链、接枝反应后树脂计入醇醚类溶剂溶解的聚乙烯蜡，即提高漆膜耐候性，提供彩色漆膜耐磨性。
进一步的，本发明还包括一种免研磨阳离子彩色电泳色浆，其特征在于包括上述的季铵盐型研磨树脂、有机颜料和去离子水，其中，有机颜料为颜谷科技黑彩色水性色粉；
本发明的电泳涂料具有以下优点：①彩色电泳色浆生产过程免研磨、提高生产、缩短供货周期；②彩色电泳色浆生产设备投资少；③；聚乙烯蜡提高彩色漆膜耐磨性，小五金类外观件上使用周期更长；④漆膜表层聚乙烯蜡组分起到部分阻隔作用，使漆膜整体耐候性提升；
具体实施方式
以下，结合实施例对于本发明作进一步说明，实施例仅用于解释说明而不用于限定本发明的保护范围。
首先，对制备所述季铵盐型研磨树脂的过程进行说明。
S1.将50重量份的YD-128环氧树脂、20重量份的双酚A树脂、占总重量0.2‰的三苯基膦、20重量份的酮类溶剂在140-150℃进行扩链反应，得到环氧当量650-730的环氧树脂中间产物；
S2.将10-12重量份的TDI升温至45-55℃，滴加8-10重量份的醇醚类封闭剂，滴加结束，升温至70-80℃保温2-3h，得到封闭率55％半封闭异氰酸酯；
S3.环氧当量为650-730的环氧树脂中间产物控制温度在140-150℃，滴加以上半封闭异氰酸酯，达到接枝率20％的环氧树脂；降温控制温度110℃以下，加入总量4％聚乙烯蜡及1.5倍量的醇醚类溶剂溶解得到搅拌均匀的非水溶研磨树脂；
S4.将10-12重量份的叔胺升温至70-90℃，滴加以上封闭率55％半封闭异氰酸酯，反应2-3h；加入5-7重量份的有机酸后保温2-3h，季铵盐型水溶性异氰酸酯。
S5.在非水溶性研磨树脂中加入以上季铵盐型水溶性异氰酸酯，控制胺化率90％，反应8-10h；加入去离子水稀释，得到固体份为30％的季铵盐型研磨树脂。
所述酮类溶剂为丙酮、丁酮、甲基异丁基酮中的至少一种。
经过所述扩链、接枝反应后树脂计入醇醚类溶剂溶解的聚乙烯蜡，即提高漆膜耐候性，提供彩色漆膜耐磨性。
接着对所述免研磨阳离子彩色电泳色浆的制备方式作进一步的说明。
Figure BDA0002749740720000041
表一
按照上述表一中的配方分别进行制备色浆，制备工艺为：按顺序将上述方式制备的季铵盐型研磨树脂及水性色粉加入敞口塑料圆柱形容器中，用分散机开1500±50rpp/min转速分散5-10min后，搅拌状态下加入去离子水调粘度，控制色浆粘度为30-50″；继续分散5-10min后，周转至1L容量研磨缸中，研磨缸通冷却水情况下，开启转速4500-5000rpp/min分散30分钟，得到细度≤15μm的色浆。
原漆热储稳定性测试：
将上述色浆进行50℃条件下耐高温测试144h，状态轻微分层、细度15μm、无沉淀。
漆膜外观测试：
按照色浆：HLS阳离子型乳液：去离子水＝100:400:1200比例，将上述两个测试方案中的槽液使用机械搅拌熟化24小时，在槽液温度30-32℃，电泳制板对比镀锡铁板、磷化板，控制膜厚18μm-20μm；烘烤条件180℃/20-30分钟；测试QUVA(GB/T14522-2008)；镀锡铁板对应测试QUVA288h，满足失光等级2级(失光率＜15％)、变色等级2级(△E≤3.0)；磷化板对应测试QUVA408h，满足失光等级2级(失光率＜15％)、变色等级2级(△E≤3.0)。

Claims (4)

1.一种季铵盐型研磨树脂的制备方法，其特征在于，包括以下步骤：
S1.将50重量份的YD-128环氧树脂、20重量份的双酚A树脂、占总重量0.2‰的三苯基膦、20重量份的酮类溶剂在140-150℃进行扩链反应，得到环氧当量650-730的环氧树脂中间产物；
S2.将10-12重量份的TDI升温至45-55℃，滴加8-10重量份的醇醚类封闭剂，滴加结束，升温至70-80℃保温2-3h，得到封闭率55％半封闭异氰酸酯；
S3.将环氧当量为650-730的环氧树脂中间产物控制温度在140-150℃，滴加以上半封闭异氰酸酯，达到接枝率20％的环氧树脂；降温控制温度110℃以下，加入总量4％聚乙烯蜡及1.5倍量的醇醚类溶剂溶解得到搅拌均匀的非水溶研磨树脂；
S4.将10-12重量份的叔胺升温至70-90℃，滴加以上封闭率55％半封闭异氰酸酯，反应2-3h；加入5-7重量份的有机酸后保温2-3h，得到季铵盐型水溶性异氰酸酯；
S5.在非水溶性研磨树脂中加入以上季铵盐型水溶性异氰酸酯，控制胺化率90％，反应8-10h；加入去离子水稀释，得到固体份为30％的季铵盐型研磨树脂。
2.如权利要求1所述的一种季胺盐型研磨树脂的制备方法，其特征在于酮类溶剂为丙酮、丁酮、甲基异丁基酮中的至少一种。
3.如权利要求1所述的一种季胺盐型研磨树脂的制备方法，其特征在于，扩链、接枝反应后树脂计入醇醚类溶剂溶解的聚乙烯蜡。
4.一种免研磨阳离子彩色电泳色浆，包括权利要求1～3任一所述的季铵盐型研磨树脂，其特征在于，还包括水性色粉和去离子水。
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