CN105778041B - 一种耐磨耐指纹树脂的制备方法 - Google Patents
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Abstract
本发明涉及一种耐磨耐指纹树脂的制备方法,所述的制备方法包括:1)含氟小分子扩链剂与异氰酸酯反应,制备端基为‑NCO的聚氨酯预聚体。2)使用季戊四醇三丙烯酸酯封端聚氨酯预聚体,获得耐磨耐指纹树脂。本发明制备的耐指纹树脂可以直接涂覆于纤维素材料表面,并可以被电子束固化,固化后形成的固化膜具有优良的耐指纹性和高耐磨性。
Description
技术领域
本发明涉及一种耐磨耐指纹树脂的制备方法,特别涉及一种电子束冷固化耐磨耐指纹树脂的制备方法,属于材料表面处理技术领域。
背景技术
纤维素材料在生活中的应用越来越广泛,如卡纸、纸板、硬木、软木、木饰面板、木肩板、刨花板等。在某些领域,如纤维素门窗、纤维素桌椅、纤维素扶手等,要求纤维素材料表面具有耐指纹性能以及较高的耐磨性。
目前常用的纤维素材料表面耐指纹处理技术是在纤维素材料表面涂覆一层紫外光固化透明涂层,涂层内添加有含氟聚醚防污剂,具有一定的耐指纹效果,但这种外添加类型的含氟聚醚防污剂不耐磨损,随着磨损次数的增多,涂层表面的含氟聚醚防污剂会越来越少直至消失,最终失去耐指纹效果。另外,目前的紫外光固化涂层内包含有机稀释剂,如己二醇二丙烯酸酯、1,3-丁二醇二丙烯酸酯、二丙二醇二丙烯酸酯、二乙二醇二丙烯酸酯等,这些有机稀释剂是致敏源,对人体存在潜在的危害。
本发明旨在解决上述问题,而提供一种绿色环保的耐磨耐指纹树脂,并提供制备方法。由本发明制备得到的耐磨耐指纹树脂可直接涂覆于纤维素材料表面,不需要额外添加任何的有机溶剂或者有机稀释剂,绿色环保,并可以通过电子束冷固化,特别适合纤维素材料类热敏基材,固化后形成的漆膜具有优良的防指纹性与耐磨性。
发明内容
本发明旨在提供一种耐磨耐指纹树脂的制备方法,该方法的特征是:
1)向干燥的反应釜内,加入1.0摩尔份1-甲基-1H-5-酸-1H,1H,2H,2H-全氟-1-十二酯和1.1摩尔份的3-氯-1,2-丙二醇,以鼓泡的方式每分钟1升的流速通入氮气1小时,在氮气保护下,升高温度至55-60 ℃,并恒温在55-60 ℃机械搅拌反应24-36小时,停止反应,减压蒸馏除去过量的3-氯-1,2-丙二醇,进一步在80 ℃真空干燥24小时,得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯。
2)向干燥的反应釜中,加入2.0摩尔份的异佛尔酮二异氰酸和0.03-0.05摩尔份的二丁基二氯化锡和0.04-0.05摩尔份的苯醌,室温机械搅拌1小时,使原料充分混合,将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯加入上述混合物中,控制加料速度,控制反应釜内温度在45-50 ℃,加料完毕后,升高温度至55 ℃,并恒温在55℃机械搅拌反应12-15小时,停止反应,得聚氨酯预聚体。
3)向干燥的反应釜中,加入1.0摩尔份的聚氨酯预聚体和1000毫升丙酮和200毫升二氯甲烷和0.002-0.004摩尔份的辛酸亚锡和0.04-0.05摩尔份的对苯二酚,升高温度至45-50 ℃,机械搅拌1小时,用恒压滴液漏斗向反应釜内滴加2.0摩尔份的季戊四醇三丙烯酸酯,控制滴加速度,控制反应釜内温度在45-55 ℃,滴加完毕后,升高温度至75 ℃,并恒温在75 ℃机械搅拌反应36-40小时,停止反应,减压蒸馏除去丙酮和二氯甲烷,得耐磨耐指纹树脂产物。
进一步,所述的耐磨耐指纹树脂的结构式为:
进一步,所述的耐磨耐指纹透明树脂可以通过刮涂、淋涂、喷涂等方式涂覆于纤维素材料表面。
进一步,所述的涂覆在纤维素材料表面的耐磨耐指纹树脂的干厚,可以是10~100微米,优选20~60微米,更优选30~50微米。
本发明的优点是:本发明制备的耐指纹树脂可以直接涂覆于纤维素材料表面,并可以被电子束固化,固化后形成的固化膜具有优良的耐指纹性和高耐磨性。
具体实施方式
以下对本发明的原理和特征进行描述,所举实施例只用于解释本发明,并非用于限定本发明的范围。
实施例1:
向干燥的反应釜内,加入1.0摩尔份1-甲基-1H-5-酸-1H,1H,2H,2H-全氟-1-十二酯和1.1摩尔份的3-氯-1,2-丙二醇,以鼓泡的方式每分钟1升的流速通入氮气1小时,在氮气保护下,升高温度至55-60 ℃,并恒温在55-60 ℃机械搅拌反应24小时,停止反应,减压蒸馏除去过量的3-氯-1,2-丙二醇,进一步在80 ℃真空干燥24小时,得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯。
向干燥的反应釜中,加入2.0摩尔份的异佛尔酮二异氰酸和0.03摩尔份的二丁基二氯化锡和0.04摩尔份的苯醌,室温机械搅拌1小时,使原料充分混合,将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯加入上述混合物中,控制加料速度,控制反应釜内温度在45-50 ℃,加料完毕后,升高温度至55 ℃,并恒温在55 ℃机械搅拌反应12小时,停止反应,得聚氨酯预聚体。
向干燥的反应釜中,加入1.0摩尔份的聚氨酯预聚体和1000毫升丙酮和200毫升二氯甲烷和0.002摩尔份的辛酸亚锡和0.04摩尔份的对苯二酚,升高温度至45-50 ℃,机械搅拌1小时,用恒压滴液漏斗向反应釜内滴加2.0摩尔份的季戊四醇三丙烯酸酯,控制滴加速度,控制反应釜内温度在45-55 ℃,滴加完毕后,升高温度至75 ℃,并恒温在75 ℃机械搅拌反应36小时,停止反应,减压蒸馏除去丙酮和二氯甲烷,得耐磨耐指纹树脂产物。
实施例2:
向干燥的反应釜内,加入1.0摩尔份1-甲基-1H-5-酸-1H,1H,2H,2H-全氟-1-十二酯和1.1摩尔份的3-氯-1,2-丙二醇,以鼓泡的方式每分钟1升的流速通入氮气1小时,在氮气保护下,升高温度至55-60 ℃,并恒温在55-60 ℃机械搅拌反应36小时,停止反应,减压蒸馏除去过量的3-氯-1,2-丙二醇,进一步在80 ℃真空干燥24小时,得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯。
向干燥的反应釜中,加入2.0摩尔份的异佛尔酮二异氰酸和0.05摩尔份的二丁基二氯化锡和0.05摩尔份的苯醌,室温机械搅拌1小时,使原料充分混合,将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-十二酯加入上述混合物中,控制加料速度,控制反应釜内温度在45-50 ℃,加料完毕后,升高温度至55 ℃,并恒温在55 ℃机械搅拌反应15小时,停止反应,得聚氨酯预聚体。
向干燥的反应釜中,加入1.0摩尔份的聚氨酯预聚体和1000毫升丙酮和200毫升二氯甲烷和0.004摩尔份的辛酸亚锡和0.05摩尔份的对苯二酚,升高温度至45-50 ℃,机械搅拌1小时,用恒压滴液漏斗向反应釜内滴加2.0摩尔份的季戊四醇三丙烯酸酯,控制滴加速度,控制反应釜内温度在45-55℃,滴加完毕后,升高温度至75 ℃,并恒温在75 ℃机械搅拌反应40小时,停止反应,减压蒸馏除去丙酮和二氯甲烷,得耐磨耐指纹树脂产物。
通过下面的试验测试本发明的耐磨耐指纹树脂的性能。
试验实施例1:
将实施例1制备的耐指纹树脂通过线棒涂布器刮涂于刨花板上,涂布厚度40微米,使用电子束固化仪在空气气氛进行固化,电子束辐射剂量为210-220千戈瑞,漆膜固化后,在电热鼓风干燥箱内25 ℃静置24小时后,测试其性能,性能测试结果如表1。
试验实施例2:
将实施例2制备的耐指纹树脂通过线棒涂布器刮涂于刨花板上,涂布厚度40微米,使用电子束固化仪在空气气氛进行固化,电子束辐射剂量为210-220千戈瑞,漆膜固化后,在电热鼓风干燥箱内25 ℃静置24小时后,测试其性能,性能测试结果如表1。
耐磨性的测试方法:按照《GB/T1768-1979》测试。
接触角的测试方法:使用日本岛津PCL-2接触角仪测试十六烷在耐指纹膜表面的接触角,即滴即测。
附着力的测试方法:按照《GB/T1720-79(89)》测试。
表1电子束固化后耐指纹膜的性能
以上所述仅为本发明的部分实施例,并不限制本发明。
Claims (1)
1.一种耐磨耐指纹树脂的制备方法,其特征在于,所述的制备方法包括:
1)向干燥的反应釜内,加入1.0摩尔份3-甲基-1H-4-(1H, 1H, 2H, 2H-全氟十二烷基氧基羰基)咪唑和1.1摩尔份的3-氯-1, 2-丙二醇,以鼓泡的方式每分钟1升的流速通入氮气1小时,在氮气保护下,升高温度至55-60 ℃,并恒温在55-60 ℃机械搅拌反应24-36小时,停止反应,减压蒸馏除去过量的3-氯-1, 2-丙二醇,进一步在80 ℃真空干燥24小时,得含氟小分子扩链剂;
2)向干燥的反应釜内,加入2.0摩尔份的异佛尔酮二异氰酸酯和0.03-0.05摩尔份的二丁基二氯化锡和0.04-0.05摩尔份的苯醌,室温机械搅拌1小时,使原料充分混合,将1.0摩尔份的步骤1)制备的含氟小分子扩链剂加入上述混合物中,控制加料速度,控制反应釜内温度在45-50 ℃,加料完毕后,升高温度至55 ℃,并恒温在55℃机械搅拌反应12-15小时,停止反应,得聚氨酯预聚体;
3)向干燥的反应釜内,加入1.0摩尔份的聚氨酯预聚体和1000毫升丙酮和200毫升二氯甲烷和0.002-0.004摩尔份的辛酸亚锡和0.04-0.05摩尔份的对苯二酚,升高温度至45-50℃,机械搅拌1小时,用恒压滴液漏斗向反应釜内滴加2.0摩尔份季戊四醇三丙烯酸酯,控制滴加速度,控制反应釜内温度在45-55 ℃,滴加完毕后,升高温度至75 ℃,并恒温在75 ℃机械搅拌反应36-40小时,停止反应,减压蒸馏除去丙酮和二氯甲烷,得耐磨耐指纹树脂产物;产物结构式如下:
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