CN112812235A - 水性环氧改性树脂及其制备方法、涂料及其制备方法 - Google Patents
水性环氧改性树脂及其制备方法、涂料及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种水性环氧改性树脂及其制备方法、涂料及其制备方法,其中水性环氧改性树脂,包括下列重量份的原料:环氧树脂15~25份、二乙二醇丁醚5~7份、水性聚氨酯分散体10~15份、乙二醇丁醚40~50份、三羟甲基丙烷4~8份、丙烯酸2~10份,丙烯酸丁酯5~10份,丙烯酸羟基乙酯8~15份,甲基丙烯酸甲酯5~15份、聚合引发剂1~2份制成、异丙醇10~15份。采用本发明,只需运用一种涂料便能满足轻中防腐领域对涂料的要求,同时能克服领域传统的多涂层配套的不便,可取代原有多种涂料混用的局面,耐盐雾及防老化等综合性能好。
Description
技术领域
本发明涉及涂料领域,特别是涉及一种水性环氧改性树脂及其制备方法、涂料及其制备方法。
背景技术
目前涂料领域,要同时满足高要求的盐雾与老化性能,尤其是高规格的综合性能,都需要两至三种涂料(底漆、中间漆、面漆或者底漆、面漆的复合防腐涂层体系)搭配使用,各种涂料各司其职,底漆主要负责盐雾,面漆主要负责老化,再根据最终外观的要求,决定是否上中间漆过渡。
采用多种涂料搭配使用,操作工序复杂,施工周期长,造价成本高。因此,无论是对现场的施工便捷度,还是对施工效率和成本来说,都是极为不利,同时,还需要在搭配使用时,综合考虑各层涂层的配套结合问题,如果涂层间的配套性不好,会造成整个涂层体系质量降低。
目前市面也有底面合一的涂料产品,但其盐雾和老化性能不好,并未得到广泛使用。
因此本领域技术人员致力于开发一种高盐雾、高耐候的水性环氧改性树脂及其制备方法及相应涂料及其制备方法。
发明内容
有鉴于现有技术的上述缺陷,本发明所要解决的技术问题是提供一种高盐雾、高耐候的水性环氧改性树脂及其制备方法及相应涂料及其制备方法。
为实现上述目的,本发明提供了一种水性环氧改性树脂,包括下列重量份的原料:环氧树脂15~25份、二乙二醇丁醚5~7份、水性聚氨酯分散体10~15份、乙二醇丁醚40~50份、三羟甲基丙烷4~8份、丙烯酸2~10份,丙烯酸丁酯5~10份,丙烯酸羟基乙酯8~15份,甲基丙烯酸甲酯5~15份、聚合引发剂1~2份制成、异丙醇10~15份。
较佳的,包括下列重量份的原料:环氧树脂20~25份、二乙二醇丁醚6份、水性聚氨酯分散体10~15份、乙二醇丁醚40~45份、三羟甲基丙烷7~8份、丙烯酸2~5份,丙烯酸丁酯8~10份,丙烯酸羟基乙酯12~15份,甲基丙烯酸甲酯10~15份、聚合引发剂1~2份、异丙醇10~15份。
较佳的,所述聚合引发剂为过氧化苯甲酸叔丁酯、甲基丙烯酸甲酯和偶氮二异丁氰中的一种或多种。
本发明还提供一种如上所述的水性环氧改性树脂的制备方法,包括如下步骤:
S1:将环氧树脂溶解到二乙二醇丁醚中,溶解均匀后缓缓加入水性聚氨酯分散体、乙二醇丁醚;
S2:升温至140℃~160℃;
S3:缓慢滴加三羟甲基丙烷,保温搅拌4~6小时;
S4:丙烯酸、丙烯酸丁酯、丙烯酸羟基乙酯、甲基丙烯酸甲酯混合均匀后用3~4hr均匀滴加至反应器中,滴加完后分2~4次加入聚合引发剂,保温反应2~3h,降温到70℃~90℃,加入异丙醇,搅拌均匀。
本发明还提供一种涂料,包括如上所述的水性环氧改性树脂。
较佳的,包括下列重量份的原料:去离子水8~15份,水性环氧改性树脂35~45份,异氰酸酯固化剂10~15份,着色颜料2~18份,绢云母1~2份,硫酸钡10~15份,滑石粉0.2~0.8份,高分子聚合型分散剂0.2~0.8份,含硅消泡剂0.2~0.8份,PUA聚氨酯增稠剂0.5~1份,低表面张力基材润湿剂0.2~0.8份,含硅流平剂0.5~1份,防沉剂0.2~0.5份,助溶剂8~15份。
较佳的,包括下列重量份的原料:去离子水10~12份,水性环氧改性树脂35~40份,异氰酸酯固化剂10~12份,着色颜料2~6份,绢云母1~2份,硫酸钡10~12份,滑石粉0.2~0.6份,高分子聚合型分散剂0.2~0.6份,含硅消泡剂0.6~0.8份,PUA聚氨酯增稠剂0.8~1份,低表面张力基材润湿剂0.4~0.6份,含硅流平剂0.5~0.8份,防沉剂0.2~0.5份,助溶剂8~12份。
较佳的,所述异氰酸酯固化剂包括60%~80%重量的六亚甲基二异氰酯固化剂,其余为溶剂,其中溶剂为丙二醇甲醚醋酸酯或丙二醇二碳酸酯中的一种或两种。
本发明还提供一种如上所述的涂料的制备方法,包括以下步骤:
F1:在第一容器中加入去离子水,以150~300r/min的速度搅拌,搅拌状态下加入水性环氧改性树脂,搅拌5~10分钟后,在搅拌状态下依次加入高分子聚合型分散剂、含硅消泡剂,保持该搅拌速度4~8分钟,搅拌状态下,依次加入防沉剂、及由着色颜料、绢云母、硫酸钡和滑石粉组成的颜填料,将搅拌速度提升至350~500r/min,保持搅拌12~20分钟;
F2:研磨至细度为25~35μm,制得浆料;
F3:搅拌状态下,在制得的第一容器浆料中,依次加入低表面张力基材润湿剂、含硅流平剂、助溶剂,搅拌均匀,并最终用PUA聚氨酯增稠剂进行粘度的调整,得甲组分涂料部分,12~24h后进行封闭包装;
F4:制备异氰酸酯固化剂,设置含有滴加管道的封闭容器,确保容器干净干燥,通入氮气加以除水和排空气保护,3~5分钟后,加入六亚甲基二异氰酯固化剂,以150~300r/min的速度搅拌,加入溶剂将搅拌速度提升至350~500r/min,保持搅拌12~20分钟,得异氰酸酯固化剂,10~20分钟后,撤出氮气保护,即刻进行封闭包装,得到乙组份固化剂
现场使用之前,提前0.3~0.8h,将上述甲乙两个组分进行5~6:1的质量比,进行配比,并加入甲组分涂料部分和乙组份固化剂总质量的0~15%去离子水进行稀释,搅拌均匀,即可。
本发明以三羟甲基丙烷为交联剂,用环氧树脂改性聚氨酯分散体,然后加入甲基丙烯酸甲酯和偶氮二异丁氰作为引发剂,得到环氧改性的水性聚氨酯分散体,然后加入引发剂,乳液聚合得到聚氨酯-环氧-丙烯酸酯杂合分散体。主体树脂首先用环氧接枝改性聚氨酯分散体,然后自由基乳液聚合在主链上同时得到刚性的丙烯酸架构。一个树脂同时具有环氧、聚氨酯和丙烯酸三种结构的杂合,能同时兼顾三种结构所带来的优点。而且这种改性能克服传统的环氧树脂与丙烯酸树脂物料共混的相容性与稳定性差的问题。
另外,本发明以水性环氧改性丙烯酸-聚氨酯树脂为主体成膜物,搭配异氰酸酯固化剂作为交联剂,同时加入一些防锈填料、着色颜料为填充和功能粉料,补充一些助剂和溶剂辅助成膜,进而制备成综合性能优异的底面合一涂料,使得涂料的盐雾、老化满足500小时以上的功能,只需要一种涂料即可达到高要求的盐雾与老化性能,大大提高了涂料涂覆的效率,节约了成本。
本发明的有益效果是:本发明具有如下有益效果:
1、只需运用一种涂料便能满足轻中防腐领域对涂料的应用,同时能克服这些领域传统的多涂层配套的不便,可取代原有多种涂料混用的局面,耐盐雾及防老化等综合性能好;
2、由于主体结构为聚氨酯,它对底材的应用适应性极广,几乎各种类型的金属材质、大部分塑料橡胶和玻璃上都能附着,且性能优异;
3、由于没有太多的主树脂混合,因此,产品的稳定性极佳。
具体实施方式
下面对本发明作进一步说明,本发明中的份数是指每个原材料的质量份占比。
本申请实施例中未特别说明的,均为市售常规产品。
实施例1至4制备水性环氧改性树脂
实施例1至4中各个原料的来源如下:
环氧树脂采用环氧树脂E-12,采购于深圳市吉田化工有限公司;
水性聚氨酯分散体来源于荷兰帝斯曼化学;
乙二醇丁醚和二乙二醇丁醚,均采购于成都欣正通化工有限公司;
三羟甲基丙烷,采购于上海海域化工有限公司;
丙烯酸、丙烯酸丁酯、丙烯酸羟基乙酯和甲基丙烯酸甲酯采购于上海曙灿实业有限公司;
过氧化苯甲酸叔丁酯、偶氮二异丁氰,采购于泰州市广和飞化工有限公司;
异丙醇,采购于成都欣正通化工有限公司。
实施例1至实施例4中各原料成份用量见表1
表1实施例1至4配料表 单位:重量份
实施例1至4制备的水性环氧改性树脂的制备包括如下步骤:
S1:将环氧树脂溶解到二乙二醇丁醚中,溶解均匀后缓缓加入水性聚氨酯分散体、乙二醇丁醚;
S2:升温至140℃~160℃;
S3:缓慢滴加三羟甲基丙烷,保温搅拌4~6小时;
S4:丙烯酸、丙烯酸丁酯、丙烯酸羟基乙酯、甲基丙烯酸甲酯混合均匀后用3~4hr均匀滴加至反应器中,滴加完后分2~4次加入聚合引发剂,保温反应2~3h,降温到70℃~90℃,加入异丙醇,搅拌均匀,即制得水性环氧改性树脂。
实施例5至8,制备本申请中涂料
实施例5至8中各个原料的来源如下:
水性环氧改性树脂为申请人自制,分别采用本发明中实施例1至实施例4所制得的水性环氧改性树脂;
异氰酸酯固化剂为申请人自制,原料及重量份见表2;
去离子水为申请人自制,采用申请人公司的去离子水机;
着色颜料为二氧化钛,炭黑或氧化铁红,着色颜料为常见材料,为常规市售品;
绢云母、硫酸钡、滑石粉,填料为,为常规市售品;
高分子聚合型分散剂为德国毕克化学生产的BYK-190水性分散剂;
PUA聚氨酯增稠剂为OMG 6020
低表面张力基材润湿剂为迪高TEGO WET 280;
含硅流平剂为德国毕克化学BYK-381;
防沉剂为美国德谦海名斯的BENTONE LT;
六亚甲基二异氰酯固化剂为拜耳的2487/1或2655中的一种或两种;
丙二醇甲醚醋酸酯和丙二醇二碳酸酯为常见材料,采用常规市售品;
助溶剂采用二丙二醇丁醚和丙二醇甲醚中的一种或两种,为常见材料,采用常规市售品。
实施例5至实施例8中各原料成份用量见表2
表2实施例5至8配料表 单位:重量份
其中,实施例5至8中异氰酸酯固化剂的组成如表3所示。
表3实施例5至8中异氰酸酯固化剂成分表
其中,实施例5至8中助溶剂的组成如表4所示。
表4实施例5至8中助溶剂成分表
实施例5至8中所有原料备妥后,按下列方法步骤制备:
F1:在第一容器中加入去离子水,以150~300r/min的速度搅拌,搅拌状态下加入水性环氧改性树脂,搅拌5~10分钟后,在搅拌状态下依次加入高分子聚合型分散剂、含硅消泡剂,保持该搅拌速度4~8分钟,搅拌状态下,依次加入防沉剂、及由着色颜料、绢云母、硫酸钡和滑石粉组成的颜填料,将搅拌速度提升至350~500r/min,保持搅拌12~20分钟;
F2:研磨至细度为25~35μm,制得浆料
F3:搅拌状态下,在制得的第一容器浆料中,依次加入低表面张力基材润湿剂、含硅流平剂、助溶剂,搅拌均匀,并最终用PUA聚氨酯增稠剂进行粘度的调整,得甲组分涂料部分,12~24h后进行封闭包装;
F4:制备异氰酸酯固化剂,设置含有滴加管道的封闭容器,确保容器干净干燥,通入氮气加以除水和排空气保护,3-5分钟后,加入六亚甲基二异氰酯固化剂,以150~300r/min的速度搅拌,加入溶剂将搅拌速度提升至350~500r/min,保持搅拌12~20分钟,得异氰酸酯固化剂,10~20分钟后,撤出氮气保护,即刻进行封闭包装,得到乙组份固化剂
现场使用之前,提前0.3~0.8h,将上述甲组分涂料部分和乙组份固化剂两个组分进行5~6:1的质量比,进行配比,并加入甲组分涂料部分和乙组份固化剂总质量0~15%的去离子水进行稀释,搅拌均匀,即可。
将实施例5至8制备所得涂料进行性能测试,测试方法如下:
将实施例5至8所制得涂料分别喷涂在热轧板和铝板上,喷涂厚度为40~60um,表干15分钟后80℃烤40分钟,烘烤后室温养护7天。后将热轧板和铝板拿出后,分别做如下测试,测试结果见表5及表6。
表5:热轧板测试结果
表6:铝板测试结果
通过以上试验可知,采用本申请制备的涂料具有极好的耐盐雾性、耐水性及耐碱性,可适用于各种极端环境。
以上详细描述了本发明的较佳具体实施例。应当理解,本领域的普通技术人员无需创造性劳动就可以根据本发明的构思作出诸多修改和变化。因此,凡本技术领域中技术人员依本发明的构思在现有技术的基础上通过逻辑分析、推理或者有限的实验可以得到的技术方案,皆应在由权利要求书所确定的保护范围内。
Claims (9)
1.一种水性环氧改性树脂,其特征是,包括下列重量份的原料:环氧树脂15~25份、二乙二醇丁醚5~7份、水性聚氨酯分散体10~15份、乙二醇丁醚40~50份、三羟甲基丙烷4~8份、丙烯酸2~10份,丙烯酸丁酯5~10份,丙烯酸羟基乙酯8~15份,甲基丙烯酸甲酯5~15份、聚合引发剂1~2份制成、异丙醇10~15份。
2.如权利要求1所述的水性环氧改性树脂,其特征是,包括下列重量份的原料:环氧树脂20~25份、二乙二醇丁醚6份、水性聚氨酯分散体10~15份、乙二醇丁醚40~45份、三羟甲基丙烷7~8份、丙烯酸2~5份,丙烯酸丁酯8~10份,丙烯酸羟基乙酯12~15份,甲基丙烯酸甲酯10~15份、聚合引发剂1~2份、异丙醇10~15份。
3.如权利要求1所述的水性环氧改性树脂,其特征是:所述聚合引发剂为过氧化苯甲酸叔丁酯、甲基丙烯酸甲酯和偶氮二异丁氰中的一种或多种。
4.一种如权利要求1至3任一所述的水性环氧改性树脂的制备方法,其特征是,包括如下步骤:
S1:将环氧树脂溶解到二乙二醇丁醚中,溶解均匀后缓缓加入水性聚氨酯分散体、乙二醇丁醚;
S2:升温至140℃~160℃;
S3:缓慢滴加三羟甲基丙烷,保温搅拌4~6小时;
S4:丙烯酸、丙烯酸丁酯、丙烯酸羟基乙酯、甲基丙烯酸甲酯混合均匀后用3~4hr均匀滴加至反应器中,滴加完后分2~4次加入聚合引发剂,保温反应2~3h,降温到70℃~90℃,加入异丙醇,搅拌均匀。
5.一种涂料,包括如权利要求1至3任一所述的水性环氧改性树脂。
6.如权利要求5所述的涂料,其特征是,包括下列重量份的原料:去离子水8~15份,水性环氧改性树脂35~45份,异氰酸酯固化剂10~15份,着色颜料2~18份,绢云母1~2份,硫酸钡10~15份,滑石粉0.2~0.8份,高分子聚合型分散剂0.2~0.8份,含硅消泡剂0.2~0.8份,PUA聚氨酯增稠剂0.5~1份,低表面张力基材润湿剂0.2~0.8份,含硅流平剂0.5~1份,防沉剂0.2~0.5份,助溶剂8~15份。
7.如权利要求6所述的涂料,其特征是,包括下列重量份的原料:去离子水10~12份,水性环氧改性树脂35~40份,异氰酸酯固化剂10~12份,着色颜料2~6份,绢云母1~2份,硫酸钡10~12份,滑石粉0.2~0.6份,高分子聚合型分散剂0.2~0.6份,含硅消泡剂0.6~0.8份,PUA聚氨酯增稠剂0.8~1份,低表面张力基材润湿剂0.4~0.6份,含硅流平剂0.5~0.8份,防沉剂0.2~0.5份,助溶剂8~12份。
8.如权利要求6或7所述的涂料,其特征是,所述异氰酸酯固化剂包括60%~80%重量的六亚甲基二异氰酯固化剂,其余为溶剂,其中溶剂为丙二醇甲醚醋酸酯或丙二醇二碳酸酯中的一种或两种。
9.如权利要求5至8任一所述的涂料的制备方法,其特征是,包括以下步骤:
F1:在第一容器中加入去离子水,以150~300r/min的速度搅拌,搅拌状态下加入水性环氧改性树脂,搅拌5~10分钟后,在搅拌状态下依次加入高分子聚合型分散剂、含硅消泡剂,保持该搅拌速度4~8分钟,搅拌状态下,依次加入防沉剂、及由着色颜料、绢云母、硫酸钡和滑石粉组成的颜填料,将搅拌速度提升至350~500r/min,保持搅拌12~20分钟;
F2:研磨至细度为25~35μm,制得浆料;
F3:搅拌状态下,在制得的第一容器浆料中,依次加入低表面张力基材润湿剂、含硅流平剂、助溶剂,搅拌均匀,并最终用PUA聚氨酯增稠剂进行粘度的调整,制得甲组分涂料部分,12~24h后进行封闭包装;
F4:制备异氰酸酯固化剂,设置含有滴加管道的封闭容器,确保容器干净干燥,通入氮气加以除水和排空气保护,3~5分钟后,加入六亚甲基二异氰酯固化剂,以150~300r/min的速度搅拌,加入溶剂将搅拌速度提升至350~500r/min,保持搅拌12~20分钟,得异氰酸酯固化剂,10~20分钟后,撤出氮气保护,即刻进行封闭包装,得到乙组份固化剂;
现场使用之前,提前0.3~0.8h,将上述甲组分涂料部分和乙组份固化剂按照5~6:1的质量比,进行配比,并加入甲组分涂料部分和乙组份固化剂总质量0~15%的去离子水进行稀释,搅拌均匀,即可。
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