CN106366863A - 一种阴极电泳涂料的制备方法 - Google Patents
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Abstract
本发明涉及一种阴极电泳涂料的制备方法,属于涂料制备技术领域。本发明首先以三羟甲基丙烷、N‑甲基二乙醇胺和异佛尔酮二异氰酸酯等物质为原料,制备得到水基端羟基阳离子聚氨酯乳液,再利用其改性钠基蒙脱石,得到有机改性蒙脱土,接着将环氧树脂E‑44溶解于乙二醇丁醚后,与三乙醇胺进行加热搅拌混合,再与水基端羟基阳离子聚氨酯乳液等物质混合,得到基料树脂,最后将其与去离子水进行混合剪切分散,得到基料树脂乳液后,与钛白粉、有机改性蒙脱土等物质混合球磨,即可。本发明制备的阴极电泳涂料光泽度高,涂膜光泽为78~80;在质量分数5%硫酸溶液中浸泡浸泡2~3天,不会出现起泡、涂膜剥离现象,具有较高的耐酸性,提高防腐蚀性能。
Description
技术领域
本发明涉及一种阴极电泳涂料的制备方法,属于涂料制备技术领域。
背景技术
阴极电泳涂料为双组分,其一组份为白色均匀乳状液体,另一组分为灰色(或黑色)颜料浆状物。其原料主要有环氧树脂、醚醇化合物、异氰酸酯等。阴极电泳涂料有紫外光固化电泳涂料、自分层阴极电泳涂料和边角防锈型阴极电泳涂料等。紫外光固化涂料是利用紫外光照射涂料树脂发生聚合架桥反应的固化方式,在低温的条件下短时间内就能完成涂料的固化过程。自分层涂料指涂料一次施工在底材上后,能自发的直接产生相分离,在成膜过程中分成两个连续的不同功能涂层,形成不同组成的复合涂层系统,每层显示出不同的特性。边角防锈型阴极电泳涂料在涂膜熔融时,由于高相对分子质量树脂添加剂的作用而抑制了涂膜的热流动性,达到固化温度后,由于该树脂自身的熔融和交联反应而形成均匀的涂膜。
阴极电泳涂料应用比较广泛,其配比主要以环氧树脂作为主要成膜物质,具有较好的防腐蚀能力。但是由于对颜料的润湿性较差,普通阴极电泳涂料涂膜光泽低,装饰性较差,仅作为底漆使用。由于环氧树脂在水性化过程中一般都采用胺改性,导致涂膜的耐酸性能不足,我国目前阴极电泳涂料标准中对耐酸性的规定仅为质量分数5%硫酸溶液中浸泡24h无异常,若浸泡2~3天即出现起泡、涂膜剥离现象,这远远不能满足石油管道等行业对防腐性能的要求。
发明内容
本发明所要解决的技术问题:针对目前阴极电泳涂料涂膜光泽度低,装饰性差,且其耐酸性能差,不能满足石油管道等行业对防腐性能的要求的问题,本发明首先以三羟甲基丙烷、N-甲基二乙醇胺和异佛尔酮二异氰酸酯等物质为原料,制备得到水基端羟基阳离子聚氨酯乳液,再利用其改性钠基蒙脱石,得到有机改性蒙脱土,接着将环氧树脂E-44溶解于乙二醇丁醚后,与三乙醇胺进行加热搅拌混合,再与水基端羟基阳离子聚氨酯乳液等物质混合,得到基料树脂,最后将其与去离子水进行混合剪切分散,得到基料树脂乳液后,与钛白粉、有机改性蒙脱土等物质混合球磨,即可得到阴极电泳涂料。本发明制备的阴极电泳涂料涂膜光泽度高,耐酸性能好,具有较强的防腐蚀性能。
为解决上述技术问题,本发明采用的技术方案是:
(1)称取1.2~1.5g三羟甲基丙烷,装入三口烧瓶中,加入16~18mL N-甲基二乙醇胺,并加热至100~105℃,保持温度1~2h,降温至40~50℃,以1mL/min滴加18~20mL异佛尔酮二异氰酸酯,加入0.1~0.2mL二月桂酸二丁基锡,以300~400r/min搅拌1~2h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至100~120mL去离子水中,以500~600r/min搅拌混合20~30min,得水基端羟基阳离子聚氨酯乳液,备用;
(2)称取10~12g钠基蒙脱土,加入250~300mL去离子水中,在70~80℃恒温水浴下,保持温度1~2h,加入50~60mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡3~4h,随后抽滤,并用去离子水洗涤滤饼3~5次,再将洗涤后的滤饼装入真空干燥箱中,在105~110℃下干燥至恒重,得有机改性蒙脱土,备用;
(3)称取200~300g环氧树脂E-44装入三口烧瓶中,加入80~100mL乙二醇丁醚,在70~80℃恒温水浴下,以300~400r/min搅拌至环氧树脂E-44完全溶解,加入30~32mL三乙醇胺,加热至98~100℃,以200~300r/min搅拌反应2~3h,随后降温至50~60℃,加入160~180g聚酰胺树脂HY-508,50~60mL步骤(1)制备的水基端羟基阳离子聚氨酯乳液,加热至90~100℃,再以500~600r/min搅拌反应2~3h,并用冰醋酸调节pH呈中性,得基料树脂;
(4)分别量取20~30mL上述基料树脂、20~30mL去离子水,加入高速剪切机中,以8000~12000r/min剪切分散10~15min,得基料树脂乳液,向基料树脂乳液中加入5~6g钛白粉,5~6g步骤(2)制备的有机改性蒙脱土,3~5mL异丙醇,混合均匀后倒入球磨机中,以300~400r/min球磨20~30min,随后出料得阴极电泳涂料。
本发明的应用方法:按质量比3:1,将去离子水与上述制备的阴极电泳涂料进行搅拌混合均匀后,置于清理干净后的电泳槽中作为槽液后,采用不锈钢作为阳极,马口铁作为阴极进行电泳涂装,在槽液温度25~30℃、电压为70~80V下电泳2~3min后,再闪蒸4~5min,最后固化2~3min即可。经检测,漆件外观平整光滑无缩孔,光泽度高,涂膜光泽为78~80,且在质量分数5%硫酸溶液中浸泡浸泡2~3天,不会出现起泡、涂膜剥离现象。
本发明与其他方法相比,有益技术效果是:
(1)本发明制备的阴极电泳涂料光泽度高,涂膜光泽为78~80;
(2)本发明制备的阴极电泳涂料在5%硫酸溶液中浸泡浸泡2~3天,不会出现起泡、涂膜剥离现象,具有较高的耐酸性,提高了其防腐蚀性能。
具体实施方式
首先称取1.2~1.5g三羟甲基丙烷,装入三口烧瓶中,加入16~18mL N-甲基二乙醇胺,并加热至100~105℃,保持温度1~2h,降温至40~50℃,以1mL/min滴加18~20mL异佛尔酮二异氰酸酯,加入0.1~0.2mL二月桂酸二丁基锡,以300~400r/min搅拌1~2h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至100~120mL去离子水中,以500~600r/min搅拌混合20~30min,得水基端羟基阳离子聚氨酯乳液,备用;再称取10~12g钠基蒙脱土,加入250~300mL去离子水中,在70~80℃恒温水浴下,保持温度1~2h,加入50~60mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡3~4h,随后抽滤,并用去离子水洗涤滤饼3~5次,再将洗涤后的滤饼装入真空干燥箱中,在105~110℃下干燥至恒重,得有机改性蒙脱土,备用;
接着称取200~300g环氧树脂E-44装入三口烧瓶中,加入80~100mL乙二醇丁醚,在70~80℃恒温水浴下,以300~400r/min搅拌至环氧树脂E-44完全溶解,加入30~32mL三乙醇胺,加热至98~100℃,以200~300r/min搅拌反应2~3h,随后降温至50~60℃,加入160~180g聚酰胺树脂HY-508,50~60mL制备的水基端羟基阳离子聚氨酯乳液,加热至90~100℃,再以500~600r/min搅拌反应2~3h,并用冰醋酸调节pH呈中性,得基料树脂;最后分别量取20~30mL上述基料树脂、20~30mL去离子水,加入高速剪切机中,以8000~12000r/min剪切分散10~15min,得基料树脂乳液,向基料树脂乳液中加入5~6g钛白粉,5~6g制备的有机改性蒙脱土,3~5mL异丙醇,混合均匀后倒入球磨机中,以300~400r/min球磨20~30min,随后出料得阴极电泳涂料。
实例1
首先称取1.5g三羟甲基丙烷,装入三口烧瓶中,加入18mL N-甲基二乙醇胺,并加热至105℃,保持温度2h,降温至50℃,以1mL/min滴加20mL异佛尔酮二异氰酸酯,加入0.2mL二月桂酸二丁基锡,以400r/min搅拌2h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至120mL去离子水中,以600r/min搅拌混合30min,得水基端羟基阳离子聚氨酯乳液,备用;再称取12g钠基蒙脱土,加入300mL去离子水中,在80℃恒温水浴下,保持温度2h,加入60mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡4h,随后抽滤,并用去离子水洗涤滤饼5次,再将洗涤后的滤饼装入真空干燥箱中,在110℃下干燥至恒重,得有机改性蒙脱土,备用;接着称取300g环氧树脂E-44装入三口烧瓶中,加入100mL乙二醇丁醚,在80℃恒温水浴下,以400r/min搅拌至环氧树脂E-44完全溶解,加入32mL三乙醇胺,加热至100℃,以300r/min搅拌反应3h,随后降温至60℃,加入180g聚酰胺树脂HY-508,60mL制备的水基端羟基阳离子聚氨酯乳液,加热至100℃,再以600r/min搅拌反应3h,并用冰醋酸调节pH呈中性,得基料树脂;最后分别量取30mL上述基料树脂、30mL去离子水,加入高速剪切机中,以12000r/min剪切分散15min,得基料树脂乳液,向基料树脂乳液中加入6g钛白粉,6g制备的有机改性蒙脱土,5mL异丙醇,混合均匀后倒入球磨机中,以400r/min球磨30min,随后出料得阴极电泳涂料。
按质量比3:1,将去离子水与上述制备的阴极电泳涂料进行搅拌混合均匀后,置于清理干净后的电泳槽中作为槽液后,采用不锈钢作为阳极,马口铁作为阴极进行电泳涂装,在槽液温度30℃、电压为80V下电泳3min后,再闪蒸5min,最后固化3min即可。经检测,漆件外观平整光滑无缩孔,光泽度高,涂膜光泽为80,且在质量分数5%硫酸溶液中浸泡浸泡3天,不会出现起泡、涂膜剥离现象。
实例2
首先称取1.2g三羟甲基丙烷,装入三口烧瓶中,加入16mL N-甲基二乙醇胺,并加热至100℃,保持温度1h,降温至40℃,以1mL/min滴加18mL异佛尔酮二异氰酸酯,加入0.1mL二月桂酸二丁基锡,以300r/min搅拌1h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至100mL去离子水中,以500r/min搅拌混合20min,得水基端羟基阳离子聚氨酯乳液,备用;再称取10g钠基蒙脱土,加入250mL去离子水中,在70℃恒温水浴下,保持温度1h,加入50mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡3h,随后抽滤,并用去离子水洗涤滤饼3次,再将洗涤后的滤饼装入真空干燥箱中,在105℃下干燥至恒重,得有机改性蒙脱土,备用;接着称取200g环氧树脂E-44装入三口烧瓶中,加入80mL乙二醇丁醚,在70℃恒温水浴下,以300r/min搅拌至环氧树脂E-44完全溶解,加入30mL三乙醇胺,加热至98℃,以200r/min搅拌反应2h,随后降温至50℃,加入160g聚酰胺树脂HY-508,50mL制备的水基端羟基阳离子聚氨酯乳液,加热至90℃,再以500r/min搅拌反应2h,并用冰醋酸调节pH呈中性,得基料树脂;最后分别量取20mL上述基料树脂、20mL去离子水,加入高速剪切机中,以8000r/min剪切分散10min,得基料树脂乳液,向基料树脂乳液中加入5g钛白粉,5g制备的有机改性蒙脱土,3mL异丙醇,混合均匀后倒入球磨机中,以300r/min球磨20min,随后出料得阴极电泳涂料。
按质量比3:1,将去离子水与上述制备的阴极电泳涂料进行搅拌混合均匀后,置于清理干净后的电泳槽中作为槽液后,采用不锈钢作为阳极,马口铁作为阴极进行电泳涂装,在槽液温度25℃、电压为70V下电泳2min后,再闪蒸4min,最后固化2min即可。经检测,漆件外观平整光滑无缩孔,光泽度高,涂膜光泽为78,且在质量分数5%硫酸溶液中浸泡浸泡2天,不会出现起泡、涂膜剥离现象。
实例3
首先称取1.3g三羟甲基丙烷,装入三口烧瓶中,加入17mL N-甲基二乙醇胺,并加热至102℃,保持温度1h,降温至45℃,以1mL/min滴加19mL异佛尔酮二异氰酸酯,加入0.1mL二月桂酸二丁基锡,以350r/min搅拌2h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至110mL去离子水中,以550r/min搅拌混合25min,得水基端羟基阳离子聚氨酯乳液,备用;再称取11g钠基蒙脱土,加入270mL去离子水中,在75℃恒温水浴下,保持温度1h,加入55mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡4h,随后抽滤,并用去离子水洗涤滤饼4次,再将洗涤后的滤饼装入真空干燥箱中,在107℃下干燥至恒重,得有机改性蒙脱土,备用;接着称取250g环氧树脂E-44装入三口烧瓶中,加入90mL乙二醇丁醚,在70℃恒温水浴下,以350r/min搅拌至环氧树脂E-44完全溶解,加入31mL三乙醇胺,加热至99℃,以220r/min搅拌反应2h,随后降温至55℃,加入170g聚酰胺树脂HY-508,55mL制备的水基端羟基阳离子聚氨酯乳液,加热至95℃,再以550r/min搅拌反应2h,并用冰醋酸调节pH呈中性,得基料树脂;最后分别量取25mL上述基料树脂、25mL去离子水,加入高速剪切机中,以9000r/min剪切分散15min,得基料树脂乳液,向基料树脂乳液中加入6g钛白粉,5g制备的有机改性蒙脱土,4mL异丙醇,混合均匀后倒入球磨机中,以350r/min球磨25min,随后出料得阴极电泳涂料。
按质量比3:1,将去离子水与上述制备的阴极电泳涂料进行搅拌混合均匀后,置于清理干净后的电泳槽中作为槽液后,采用不锈钢作为阳极,马口铁作为阴极进行电泳涂装,在槽液温度27℃、电压为75V下电泳2min后,再闪蒸4min,最后固化2min即可。经检测,漆件外观平整光滑无缩孔,光泽度高,涂膜光泽为79,且在质量分数5%硫酸溶液中浸泡浸泡3天,不会出现起泡、涂膜剥离现象。
Claims (1)
1.一种阴极电泳涂料的制备方法,其特征在于具体制备步骤为:
(1)称取1.2~1.5g三羟甲基丙烷,装入三口烧瓶中,加入16~18mL N-甲基二乙醇胺,并加热至100~105℃,保持温度1~2h,降温至40~50℃,以1mL/min滴加18~20mL异佛尔酮二异氰酸酯,加入0.1~0.2mL二月桂酸二丁基锡,以300~400r/min搅拌1~2h,并用冰醋酸调节pH呈中性,得水基端羟基阳离子聚氨酯,将水基端羟基阳离子聚氨酯加入至100~120mL去离子水中,以500~600r/min搅拌混合20~30min,得水基端羟基阳离子聚氨酯乳液,备用;
(2)称取10~12g钠基蒙脱土,加入250~300mL去离子水中,在70~80℃恒温水浴下,保持温度1~2h,加入50~60mL上述水基端羟基阳离子聚氨酯乳液,以300W超声振荡3~4h,随后抽滤,并用去离子水洗涤滤饼3~5次,再将洗涤后的滤饼装入真空干燥箱中,在105~110℃下干燥至恒重,得有机改性蒙脱土,备用;
(3)称取200~300g环氧树脂E-44装入三口烧瓶中,加入80~100mL乙二醇丁醚,在70~80℃恒温水浴下,以300~400r/min搅拌至环氧树脂E-44完全溶解,加入30~32mL三乙醇胺,加热至98~100℃,以200~300r/min搅拌反应2~3h,随后降温至50~60℃,加入160~180g聚酰胺树脂HY-508,50~60mL步骤(1)制备的水基端羟基阳离子聚氨酯乳液,加热至90~100℃,再以500~600r/min搅拌反应2~3h,并用冰醋酸调节pH呈中性,得基料树脂;
(4)分别量取20~30mL上述基料树脂、20~30mL去离子水,加入高速剪切机中,以8000~12000r/min剪切分散10~15min,得基料树脂乳液,向基料树脂乳液中加入5~6g钛白粉,5~6g步骤(2)制备的有机改性蒙脱土,3~5mL异丙醇,混合均匀后倒入球磨机中,以300~400r/min球磨20~30min,随后出料得阴极电泳涂料。
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