CN105037686B - 一种环氧阴极电泳涂料防缩孔树脂的制备 - Google Patents

一种环氧阴极电泳涂料防缩孔树脂的制备 Download PDF

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CN105037686B
CN105037686B CN201510499004.3A CN201510499004A CN105037686B CN 105037686 B CN105037686 B CN 105037686B CN 201510499004 A CN201510499004 A CN 201510499004A CN 105037686 B CN105037686 B CN 105037686B
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谢悦红
渠美丽
袁兴
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Foshan Kefoo Technology Co ltd
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Abstract

本发明提供一种环氧阴极电泳涂料防缩孔树脂的制备，其主要步骤为：（1）制得半封闭异氰酸酯；（2）称取10~12重量份步骤（1）制备的产物，放入四口烧瓶中，加入70~80重量份聚丙二醇醚，7~9重量份甲基异丁基酮，搅拌升温至120℃±5℃，并恒温反应2h，降温至90℃±5℃，加入5~7重量份甲苯二异氰酸酯，升温至120℃±5℃，保温反应1h，得到带聚醚结构和活泼NCO基团的预聚产物；本发明降低了涂料的表面张力而提高对底材的润湿性及抗缩孔能力，并克服现有防缩孔剂与环氧树脂相容性不好的技术难题。

Description

一种环氧阴极电泳涂料防缩孔树脂的制备
技术领域
本发明涉及一种环氧体系阴极电泳涂料中使用的水性防缩孔树脂的制备方法，具体是涉及一种异氰酸酯聚醚改性的半胺化环氧树脂的制备方法，通过此方法制备生产的具有环氧和聚醚结构的多羟基树脂，可以降低涂料的表面张力，提高涂料对底材的润湿性，防止产生缩孔，与环氧体系的阴极电泳涂料相溶性好。
背景技术
阴极电泳涂料具有高效、优质、安全、经济、环保等优势，在汽车、工程机械、电器、五金、军工等行业已得到了广泛应用。电泳涂装中，漆膜缩孔弊病时有发生，造成缩孔的因素也较多，主要分为工艺控制和配方设计两大因素。工艺控制的因素有：（1）前处理除油不干净产生缩孔；（2）电泳漆膜固化前受到污染；（3）槽液参数控制不在要求范围内：比如灰分太低、溶剂含量过高等都可以产生缩孔。配方设计的因素是体系使用的助剂与体系相容性不好产生缩孔。工艺控制的因素通过加强工艺控制和环境条件可以有效的控制缩孔的产生，配方设计的因素则需要通过大量实验选择合适的助剂，或者自己设计合成满足体系要求的助剂。
在设计阴极电泳涂料配方时，需要加入防缩孔剂提高电泳涂料的流平和防缩孔性能。目前，市场销售的环氧体系阴极电泳涂料使用的防缩孔剂主要是水溶性丙烯酸酯类高分子型防缩孔剂。此类防缩孔剂与环氧体系阴极电泳涂料都以水为分散介质，两者表面张力值差别不大。但在烘烤固化的时候，水分蒸发完全，丙烯酸酯类树脂和改性环氧树脂的表面张力差异较大，形成了明显的张力梯度，在烘烤过程中容易出现以表面张力低的树脂为核心形成缩孔或者流平不好。国内有公司设计合成的阴极电泳涂料防缩孔剂为叔碳酸缩水甘油酯改性端氨基聚醚，通过有端氨基聚氧化丙烯醚和端氨基聚氧化乙烯醚与单边环氧官能团的叔碳酸缩水甘油酯反应，合成具有聚醚结构的防缩孔助剂。但此类防缩孔剂的水溶性差，在使用时需要在主体树脂合成时高温加入。
发明内容
本发明的目的在于采用一种多羟基聚醚改性的环氧树脂，降低涂料的表面张力而提高对底材的润湿性及抗缩孔能力，并克服现有防缩孔剂与环氧树脂相容性不好的技术难题，提供一种制备与环氧体系阴极电泳涂料相容性好的防缩孔树脂的方法。
为实现上述发明目的，本发明采用的技术方案步骤如下：
（1）首先称取50~60重量份的甲苯二异氰酸酯加入四口烧瓶，通入氮气，搅拌升温至50℃±5℃，开始滴加40~50重量份乙二醇乙醚，保持温度50~55℃，2h滴加完毕，恒温50℃±5℃， 时间2h，得到半封闭异氰酸酯；
（2）称取10~12重量份步骤（1）制备的产物，放入四口烧瓶中，加入70~80重量份聚丙二醇醚，7~9重量份甲基异丁基酮，搅拌升温至120℃±5℃，并恒温反应2h，降温至90℃±5℃，加入5~7重量份甲苯二异氰酸酯，升温至120℃±5℃，保温反应1h，得到带聚醚结构和活泼NCO基团的预聚产物；
（3）将20~30重量份环氧树脂、6~7重量份的丁酮和10-12重量份丙二醇甲醚加入到四口烧瓶中，升温至80℃±5℃，搅拌溶解，保温3h，加入5~10重量份二乙醇胺和8~9重量份的异丙醇，恒温80℃±5℃，反应2h，后降温至75℃±5℃，开始滴加步骤（2）制备的产物21~23重量份, 滴加时间为30min，再滴加步骤（1）制备的产物14~15重量份，滴加时间为30min，滴加完，升温至80℃±5℃，保温1.5h，冷却，所得产物就是聚醚改性环氧树脂的防缩孔树脂。
进一步地，步骤（2）中所使用的聚丙二醇醚为分子量为2000~3000的2、3官能团聚醚，如N220、N330。
进一步地，步骤（3）中使用的环氧树脂为环氧当量为450-1000的环氧树脂，如E-20、E-14环氧树脂。
本发明还提供一种利用上述聚醚改性环氧树脂的防缩孔树脂制备水性环保型阴极电泳涂料的方法，包括以下步骤：
（1）按质量百分比，将制得的聚醚改性环氧树脂防缩孔树脂：胺改性环氧树脂：固化剂：助剂：有机酸=2~3%：86～90%：5～6%：2~3%：3~4%在中速搅拌条件下混合均匀，备用；
（2）在分散罐中加入质量百分比为纯水49~51%，有机酸1~2%，分散助剂1~2%，高速搅拌，慢慢加入步骤（1）的混合树脂46~48%，约1h加完，加完后继续高速分散1h，过滤，得到乳白色的电泳涂料乳液产品。
使用以上制备乳液与灰色浆按3:1配槽，加入适量纯水，配槽，电泳漆膜外观流平好，平整度高，光泽高，抗缩孔性能好。
本发明针对环氧体系的阴极电泳涂料，制备独特的异氰酸酯聚醚改性半胺化环氧结构，利用聚醚的长链柔韧性和较低的玻璃化温度，增加烘烤时的漆膜流平性，防止缩孔的出现。同时本发明在结构引入长链环氧结构，使得产品的表面张力与胺化环氧树脂表面张力差异缩小，减小了低表面张力核心的形成，有效的防止缩孔的产生，而且可以在较低温度下使用。
具体实施方式：
下面结合具体实施方式对本发明作进一步详细的说明，但本发明绝不限于此实施例。
实施例
1.半封闭物的制备：
称取55g甲苯二异氰酸酯加入四口烧瓶，通入氮气，搅拌升温至50℃，开始滴加乙二醇乙醚44g，保持温度50-55℃，2h滴加完毕，保温50℃2h，得到半封闭异氰酸酯。
2.聚醚改性预聚物的制备：
称取11g步骤（1）产物，置于四口烧瓶中，加入73g聚丙二醇醚， 9g甲基异丁基酮，升温搅拌升温至120℃，保温2h，降温至90℃，加入6g甲苯二异氰酸酯，升温至120℃，保温1h，得到带聚醚结构和活泼NCO基团的产物。
3.聚醚改性环氧树脂防缩孔树脂的制备：
将30g固体环氧树脂、7g的丁酮和10g丙二醇甲醚加入到四口烧瓶中，升温至到80℃，搅拌溶解，保温3h，加入7g二乙醇胺和9g异丙醇，保温80℃2h，保温完毕后降温至75℃，开始滴加步骤（2）聚醚改性预聚物22g，滴加时间为30min，温度80℃，滴完后滴加步骤（1）半封闭异氰酸酯15g，滴加时间为30min，温度80℃，滴加完，保温80℃， 1.5h。保温完毕冷却，所得产物就是聚醚改性环氧树脂的防缩孔树脂。
4.制备水性环保型阴极电泳涂料，包括以下步骤：
（1）中和树脂的制备：
将聚醚改性环氧树脂防缩孔树脂2.7g，胺改性环氧树脂86g，自制固化剂5.8g，助剂2.2g，有机酸3.2g，置于搅拌罐中，60转/分钟的速度搅拌混合均匀，备用。
（2）乳液的制备：
在分散罐中加入纯水49g，有机酸1.3g，分散助剂1.4g，高速搅拌，线速度为20-21m/s，温度控制18~20℃，慢慢加入（1）中和树脂，约0.5h加完，加完后继续高速分散0.5h，过滤，得到乳白色的电泳涂料乳液。
使用以上制备乳液与灰色浆按3:1配槽，控制槽液指标为：
通过上述技术方案的实施，制得水性环氧阴极电泳涂料，配槽电泳漆膜外观流平好，平整度高，光泽高。漆膜性能：

Claims (4)

1.一种环氧阴极电泳涂料防缩孔树脂的制备，其特征在于：
（1）首先称取50~60重量份的甲苯二异氰酸酯加入四口烧瓶，通入氮气，搅拌升温至50℃±5℃，开始滴加40~50重量份乙二醇乙醚，保持温度50~55℃，2h滴加完毕，恒温50℃±5℃，时间2h，得到半封闭异氰酸酯；
（2）称取10~12重量份步骤（1）制备的产物，放入四口烧瓶中，加入70~80重量份聚丙二醇醚，7~9重量份甲基异丁基酮，搅拌升温至120℃±5℃，并恒温反应2h，降温至90℃±5℃，加入5~7重量份甲苯二异氰酸酯，升温至120℃±5℃，保温反应1h，得到带聚醚结构和活泼NCO基团的预聚产物；
（3）将20~30重量份环氧树脂、6~7重量份的丁酮和10-12重量份丙二醇甲醚加入到四口烧瓶中，升温至80℃±5℃，搅拌溶解，保温 3h，加入5~10重量份二乙醇胺和8~9重量份的异丙醇，恒温80℃±5℃，反应2h，后降温至75℃±5℃，开始滴加步骤（2）制备的产物21~23重量份, 滴加时间为30min，再滴加步骤（1）制备的产物14~15 重量份，滴加时间30min，滴加完，升温至80℃±5℃，保温1.5h，冷却，所得产物就是环氧阴极电泳涂料防缩孔树脂。
2.根据权利要求1所述的一种环氧阴极电泳涂料防缩孔树脂的制备， 其特征在于：步骤（2）中所使用的聚丙二醇醚为分子量为2000~3000 的2、3官能团聚醚。
3.根据权利要求1所述的一种环氧阴极电泳涂料防缩孔树脂的制备， 其特征在于：步骤（3）中使用的环氧树脂为环氧当量为450-1000的环氧树脂。
4.一种利用环氧阴极电泳涂料防缩孔树脂制备水性环保型阴极电泳涂料的方法，其特征在于：包括以下步骤：
（1）按质量百分比，将权利要求1制得的环氧阴极电泳涂料防缩孔树脂：胺改性环氧树脂：固化剂：助剂：有机酸 =2~3%：86～90%：5～6%：2~3%： 3~4%在中速搅拌条件下混合均匀，备用，各组分总和等于100%；
（2）在分散罐中加入质量百分比为纯水49~51%，有机酸1~2%，分散助剂1~2%，高速搅拌，慢慢加入步骤（1）的混合树脂46~48%， 1h加完，加完后继续高速分散1h，过滤，得到乳白色的电泳涂料乳液产品。
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