CN112321792A - 一种用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法 - Google Patents
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Abstract
本发明公开了一种用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法,包括:在反应釜中加入聚酯二元醇、二异氰酸酯、2,2‑二羟甲基丙酸及辛酸亚锡,搅拌均匀并升温至80~90℃反应2小时,降温至70℃以下,加入1,4‑丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体;将该聚氨酯预聚体降温至40℃以下,并倒入分散机分散,加入三乙胺,中和反应0.5小时,然后在高速分散条件下,加入去离子水进行乳化分散;向乳化分散后的产物中滴加胺类扩链剂,继续反应30分钟,即制得水性聚氨酯树脂。本发明不含VOCs、硬度高、抗黏连性好,对塑料基材具有良好的附着力,可用于制备环保型塑料薄膜底涂,能提高油墨在塑料薄膜上的附着力。
Description
技术领域
本发明涉及塑料薄膜印刷涂层领域,尤其涉及一种用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法。
背景技术
在塑料包装印刷领域,塑料薄膜与油墨层之间的附着牢度至关重要。不同包装产品对油墨附着力的要求也不同。如图1所示,油墨印刷前在PET等塑料薄膜上涂布一层底涂,能够有效提高油墨对基材的附着牢度。底涂作为连接塑料薄膜和油墨层的桥梁,不仅要对塑料薄膜具有优异的粘接力,还需要对油墨层具有同样优异的牢度,从而才能提高整体涂层牢度。
塑料薄膜用底涂主要由树脂粘结剂、助剂及溶剂组成;其中,树脂粘结剂对底涂的性能起决定作用。聚氨酯树脂的分子结构中含有酯基、氨酯基以及脲基等极性基团,这使其对PET等塑料薄膜具有优异的附着力,因此聚氨酯树脂被广泛用于制塑料薄膜底涂。
目前,市场上塑料薄膜印刷用底涂多为溶剂型底涂。由于底涂本身涂布量少,涂层薄,在印刷过程中需要添加大量溶剂进行稀释,而溶剂的使用不仅增加了企业成本,而且会产生大量VOCs,这会对环境造成污染,因此开发环保型的塑料薄膜用底涂及树脂已成为人们的共识。水性底涂是以水为溶剂的环保型底涂剂,具有气味低、安全性高、无VOC排放等优点,符合当前环保型产品的发展趋势。但水性底涂由于在实际应用中往往会出现流平性差、质量稳定性不好等缺点,因此其商业化应用受到了很大限制。
发明内容
针对现有技术中的上述不足之处,本发明提供了一种用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法。该水性聚氨酯树脂以水为稀释溶剂,不含有机溶剂,不仅能减少VOCs排放,而且能大大降低材料成本。同时,使用该水性聚氨酯树脂制备的塑料薄膜用水性底涂印刷适性好、附着力高,能有效解决现有塑料薄膜用底涂存在的问题。
本发明的目的是通过以下技术方案实现的:
一种用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,包括以下步骤:
步骤A、在反应釜中加入15~30重量份的聚酯二元醇、8~15重量份的二异氰酸酯、1~4重量份的2,2-二羟甲基丙酸(DMPA)以及0.01重量份的辛酸亚锡,搅拌均匀,并升温至80℃~90℃反应2小时,降温至70℃以下,加入0.5~1重量份的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体;
步骤B、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以不低于500r/min的转速进行分散,加入1~3重量份的三乙胺,中和反应0.5小时,然后在以不低于1000r/min转速的分散条件下,加入50~70重量份温度在15℃以下的去离子水进行乳化分散;
步骤C、向上述乳化分散后的产物中滴加0.5~3重量份的胺类扩链剂,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
优选地,所述的聚酯二元醇采用分子量为2000的聚己二酸1,2-丙二醇酯二醇、分子量为2000的聚己二酸2-甲基-1,3-丙二醇酯二醇、分子量为2000的聚己二酸新戊二醇酯二醇中的至少一种。
优选地,所述的异氰酸酯采用异佛尔酮二异氰酸酯和4,4′-二环己基甲烷二异氰酸酯中的至少一种。
优选地,所述的胺类扩链剂采用乙二胺、羟乙基乙二胺、1,6-己二胺中的至少一种。
一种用于塑料薄膜底涂的水性聚氨酯树脂,采用上述的用于塑料薄膜底涂的水性聚氨酯树脂的制备方法制备而成。
由上述本发明提供的技术方案可以看出,本发明提供的用于塑料薄膜底涂的水性聚氨酯树脂在制备过程中以水为分散剂,不使用任何有机溶剂,不仅安全环保无污染,而且减少了普通水性聚氨酯制备中的溶剂脱除步骤,制备工艺简单。同时,本发明在水性聚氨酯树脂合成过程中,添加了适量亲水单体DMPA,这有效提高了聚氨酯在水中的分散性。此外,本发明所提供的水性聚氨酯在后期扩链过程中仅使用少量双官能度的直链型扩链剂,既能防止树脂乳液粒径过大造成的树脂不稳定,也有利于树脂成膜后的柔软度,从而提高了该水性聚氨酯制备的塑料薄膜底涂的成膜性和稳定性。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域的普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他附图。
图1为现有技术中PET印刷薄膜涂层结构示意图。
具体实施方式
下面结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明的保护范围。
下面对本发明所提供的用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法进行详细描述。本发明实施例中未作详细描述的内容属于本领域专业技术人员公知的现有技术。
一种用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,包括以下步骤:
步骤A、在反应釜中加入15~30重量份的聚酯二元醇、8~15重量份的二异氰酸酯、1~4重量份的2,2-二羟甲基丙酸(DMPA)以及0.01重量份的辛酸亚锡,搅拌均匀,并升温至80℃~90℃反应2小时,降温至70℃以下,加入0.5~1重量份的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体;
步骤B、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以不低于500r/min的转速进行分散,然后加入1~3重量份的三乙胺,中和反应0.5小时,然后在以不低于1000r/min转速的分散条件下,加入50~70重量份温度在15℃以下的去离子水进行乳化分散;
步骤C、向上述乳化分散后的产物中滴加0.5~3重量份的胺类扩链剂,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
具体地,该用于塑料薄膜底涂的水性聚氨酯树脂的制备方法包括以下实施方案:
(1)所述的聚酯二元醇采用分子量为2000的聚己二酸1,2-丙二醇酯二醇、分子量为2000的聚己二酸2-甲基-1,3-丙二醇酯二醇、分子量为2000的聚己二酸新戊二醇酯二醇中的至少一种。
(2)所述的异氰酸酯采用异佛尔酮二异氰酸酯和4,4′-二环己基甲烷二异氰酸酯中的至少一种。
(3)所述的胺类扩链剂采用乙二胺、羟乙基乙二胺、1,6-己二胺中的至少一种。
进一步地,本发明以15~30重量份的聚酯二元醇、8~15重量份的二异氰酸酯、1~4重量份的2,2-二羟甲基丙酸(DMPA)、0.01重量份的辛酸亚锡、0.5~1重量份的1,4-丁二醇、1~3重量份的三乙胺、0.5~3重量份的胺类扩链剂以及50~70重量份的去离子水为原料制成用于塑料薄膜底涂的水性聚氨酯树脂。本发明制得的用于塑料薄膜底涂的水性聚氨酯树脂不含VOCs,硬度高,抗黏连性好,对多种塑料基材具有良好的附着力;本发明可用于制备环保型塑料薄膜印刷油墨用底涂,提高油墨在塑料薄膜上的附着力。
为了更加清晰地展现出本发明所提供的技术方案及所产生的技术效果,下面以具体实施例对本发明实施例所提供的用于塑料薄膜底涂的水性聚氨酯树脂及其制备方法进行详细描述。
实施例1
一种用于塑料薄膜底涂的水性聚氨酯树脂,其制备方法包括以下步骤:
步骤a1、在反应釜中投入220g分子量为2000的聚己二酸1,2-丙二醇酯二醇、146g异佛尔酮二异氰酸酯、20g的2,2-二羟甲基丙酸(DMPA)以及0.1g的催化剂辛酸亚锡,搅拌均匀,并缓慢升温至85℃反应2小时,降温至70℃以下,加入8g的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体。
步骤b1、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以600r/min的速度低速分散,缓慢加入15.1g的三乙胺,中和反应0.5小时,然后在1000r/min的高速分散条件下,加入630g温度在15℃以下的去离子水进行乳化分散。
步骤c1、向上述乳化分散后的产物中缓慢滴加10g乙二胺,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
实施例2
一种用于塑料薄膜底涂的水性聚氨酯树脂,其制备方法包括以下步骤:
步骤a2、在反应釜中投入200kg分子量为2000的聚己二酸2-甲基-1,3-丙二醇酯二醇、120kg异佛尔酮二异氰酸酯、18kg的2,2-二羟甲基丙酸(DMPA)以及0.1g的辛酸亚锡,搅拌均匀,并缓慢升温至80℃反应2小时,降温至70℃以下,加入7kg的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体。
步骤b2、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以500r/min的速度低速分散,缓慢加入13.6kg的三乙胺,中和反应0.5小时,然后在1200r/min的高速分散条件下,加入550kg温度在15℃以下的去离子水进行乳化分散。
步骤c2、向上述乳化分散后的产物中缓慢滴加12.8kg的羟乙基乙二胺,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
实施例3
一种用于塑料薄膜底涂的水性聚氨酯树脂,其制备方法包括以下步骤:
步骤a3、在反应釜中投入44kg分子量为2000的聚己二酸新戊二醇酯二醇、30kg的4,4′-二环己基甲烷二异氰酸酯、4kg的2,2-二羟甲基丙酸(DMPA)以及0.02kg的辛酸亚锡,搅拌均匀,并缓慢升温至90℃反应2小时,降温至70℃以下,加入0.5~1重量份的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体。
步骤b3、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以500r/min的速度低速分散,缓慢加入3.02kg的三乙胺,中和反应0.5小时,然后在1000r/min的高速分散条件下,加入132kg温度在15℃以下的去离子水进行乳化分散。
步骤c3、向上述乳化分散后的产物中缓慢滴加2.1kg的1,6-己二胺,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
综上可见,本发明实施例不含有机溶剂成分,整个过程无VOCs排放,更加安全环保。同时由该水性聚氨酯树脂制备的塑料薄膜用底涂对PET塑料薄膜的附着力高,印刷适性好,是一种新型环保水性底涂。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (5)
1.一种用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,其特征在于,包括以下步骤:
步骤A、在反应釜中加入15~30重量份的聚酯二元醇、8~15重量份的二异氰酸酯、1~4重量份的2,2-二羟甲基丙酸以及0.01重量份的辛酸亚锡,搅拌均匀,并升温至80℃~90℃反应2小时,降温至70℃以下,加入0.5~1重量份的1,4-丁二醇,再升温至85℃继续反应1小时,得到聚氨酯预聚体;
步骤B、将所述聚氨酯预聚体降温至40℃以下,并倒入分散机中以不低于500r/min的转速进行分散,加入1~3重量份的三乙胺,中和反应0.5小时,然后在以不低于1000r/min转速的分散条件下,加入50~70重量份温度在15℃以下的去离子水进行乳化分散;
步骤C、向上述乳化分散后的产物中滴加0.5~3重量份的胺类扩链剂,继续反应30分钟,从而制得固含量为40%的用于塑料薄膜底涂的水性聚氨酯树脂。
2.根据权利要求1所述的用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,其特征在于,所述的聚酯二元醇采用分子量为2000的聚己二酸1,2-丙二醇酯二醇、分子量为2000的聚己二酸2-甲基-1,3-丙二醇酯二醇、分子量为2000的聚己二酸新戊二醇酯二醇中的至少一种。
3.根据权利要求1或2所述的用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,其特征在于,所述的异氰酸酯采用异佛尔酮二异氰酸酯和4,4′-二环己基甲烷二异氰酸酯中的至少一种。
4.根据权利要求1或2所述的用于塑料薄膜底涂的水性聚氨酯树脂的制备方法,其特征在于,所述的胺类扩链剂采用乙二胺、羟乙基乙二胺、1,6-己二胺中的至少一种。
5.一种用于塑料薄膜底涂的水性聚氨酯树脂,其特征在于,采用上述权利要求1至4中任一项所述的用于塑料薄膜底涂的水性聚氨酯树脂的制备方法制备而成。
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