CN112341599A - 一种紫外光固化哑光树脂及其制备方法 - Google Patents
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Abstract
本发明提供了一种紫外光固化哑光树脂,按重量份数,包括以下组分:聚酯多元醇60~80份,二异氰酸酯10~20份,阻聚剂0~0.1份,抗氧剂0~0.1份,催化剂0~0.1份,羟基丙烯酸酯10~30份。这种紫外光固化哑光树脂,其使用聚酯多元醇、二异氰酸酯和羟基丙烯酸酯作为主体反应物,合成可紫外光固化的哑光树脂,通过使用大分子量聚酯多元醇降低合成树脂的双键密度,使用单体将哑粉悬浮到涂层表面,两个方面同时降低光泽,使合成的树脂具有优异的哑光性能。本发明还提供了上述紫外光固化哑光树脂的制备方法。
Description
技术领域
本发明涉及涂料生产的技术领域,尤其是涉及一种紫外光固化哑光树脂及其制备方法。
背景技术
紫外光固化是在紫外光的中、短波辐照下,液态UV材料中的光引发剂转变为自由基或阳离子,从而引发含活性官能团的树脂聚合交联成不溶不熔的固体涂膜的过程。因具有高效、经济、节能、适用性广和环境友好的优点,紫外光固化技术广泛应用于涂料、油墨、胶粘剂等领域。
近年来,出于使用目的和环境的需求,采用哑光涂层装饰的家具,由于可以减少光污染,而且符合现代美学的要求,受到了广大消费者的欢迎。具有哑光性能的涂料,一般是在紫外光固化涂料的基础上,加入哑光粉后得到。这种涂料是一种低光泽涂料,由其固化得到的漆膜外观光泽柔和,不强烈,因此也称柔光。
公开号为CN107936818A的中国专利,公开了一种紫外光固化无溶剂喷涂哑光面漆,包括如下重量百分比组分:九官能团超支化聚氨酯丙烯酸酯树脂5%-25%,改性环氧丙烯酸酯树脂5%-20%,助剂10.8%-26%,光引发剂3%-6%,UV活性稀释剂30%-60%。该专利的哑光面漆通过引入了九官能团超支化聚氨酯提供高反应速率,并搭配改性环氧丙烯酸酯树脂,来提高耐候性。显然,其使用的九官能团超支化聚氨酯需要额外的制备工序,而且其固化后光泽突出,因此其哑光性能仍有待验证。
因此,如何提供一种可紫外光固化且具有哑光性能的树脂,是本领域的技术人员需要解决的技术问题。
发明内容
为了解决现有技术存在的上述问题,本发明提供了一种紫外光固化哑光树脂,其使用聚酯多元醇、二异氰酸酯和羟基丙烯酸酯作为主体反应物,合成可紫外光固化的哑光树脂,通过使用大分子量聚酯多元醇降低合成树脂的双键密度,使用单体将哑粉悬浮到涂层表面,两个方面同时降低光泽,使合成的树脂具有优异的哑光性能。本发明还提供了上述紫外光固化哑光树脂的制备方法。
为了实现上述目的,本发明提供了如下技术方案:
一种紫外光固化哑光树脂,按重量份数,包括以下组分:
根据作为本发明的技术方案的进一步描述,所述聚酯多元醇树脂分子量在2000~5000。
根据作为本发明的技术方案的进一步描述,所述二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯或二苯基甲烷二异氰酸酯中的至少一种。
根据作为本发明的技术方案的进一步描述,所述抗氧化剂为2,6-二叔丁基苯酚、对苯二酚或亚磷酸酯三苯酯中的至少一种。
根据作为本发明的技术方案的进一步描述,所述催化剂为二月桂酸二丁基锡。
根据作为本发明的技术方案的进一步描述,所述羟基丙烯酸酯为丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯或季戊四醇三丙烯酸酯中的至少一种。
本发明还提供了上述紫外光固化哑光树脂的制备方法,按以下步骤进行制备:
S1.按重量份数,在反应釜中依次投入二异氰酸酯、催化剂、阻聚剂、抗氧剂,升温至40~50℃;
S2.将聚酯多元醇滴入反应釜中并搅拌,接着缓慢升温至55~65℃;
S3.在将聚酯多元醇全部滴入后,反应釜温度保持在60~65℃,1h后检测确定NCO%是否降到起始值的一半,如NCO%过高则继续保温;
S4.滴加部分已经混合均匀的羟基丙烯酸酯,控制反应釜温度缓慢升高,但不超过90℃;
S5.于85-88℃保温,0.5h后测NCO%,在NCO%≤0.5%时,加入剩余的羟基丙烯酸酯,继续于85-88℃保温1h,在确认NCO%≤0.1%,降温;
S6.转釜,按比例加入单体以及哑粉,使用高速分散机以2500rpm分散30min。
进一步地,在S4中,羟基丙烯酸酯的滴加操作在30min内完成滴加。
基于上述的技术方案,本发明取得的技术效果为:
(1)本发明提供的紫外光固化哑光树脂,其使用聚酯多元醇、二异氰酸酯和羟基丙烯酸酯作为主体反应物,合成可紫外光固化的哑光树脂,通过使用大分子量聚酯多元醇降低合成树脂的双键密度,使用单体将哑粉悬浮到涂层表面,两个方面同时降低光泽,使合成的树脂具有优异的哑光性能。
(2)本发明提供的紫外光固化哑光树脂的制备方法,操作简单,通过优选组分和采用程序升温的工艺,可制备得到综合性能较好的可紫外光固化哑光树脂,可以使用到喷涂、辊涂、淋涂等领域,价格便宜的同时还能达到很好的哑光效果,只需要添加3~5个点的哑粉就能将光泽降低到5度左右。
具体实施方式
为了便于理解本发明,下面将结合具体的实施例对本发明进行更全面的描述。本发明给出了的较佳实施方式。但是,本发明可以以许多不同的形式来实现,并不限于本文所描述的实施方式。相反地,提供这些实施方式的目的是使对本发明的公开内容理解的更加透彻全面。
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施方式的目的,不是旨在于限制本发明。
实施例1
一种紫外光固化哑光树脂,按重量份数,包括以下组分:
上述聚酯多元醇树脂分子量在2000~5000。
上述二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯或二苯基甲烷二异氰酸酯中的至少一种。
上述抗氧化剂为2,6-二叔丁基苯酚、对苯二酚或亚磷酸酯三苯酯中的至少一种。
上述催化剂为二月桂酸二丁基锡。
上述羟基丙烯酸酯为丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯或季戊四醇三丙烯酸酯中的至少一种。
上述紫外光固化哑光树脂的制备方法,按以下步骤进行制备:
S1.按重量份数,在反应釜中依次投入二异氰酸酯、催化剂、阻聚剂、抗氧剂,升温至40~50℃;
S2.将聚酯多元醇滴入反应釜中并搅拌,接着缓慢升温至55~65℃;
S3.在将聚酯多元醇全部滴入后,反应釜温度保持在60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
S4.滴加部分已经混合均匀的羟基丙烯酸酯,控制反应釜温度缓慢升高,但不超过90℃;
S5.于85-88℃保温,0.5h后测NCO%,在NCO%≤0.5%时,加入剩余的羟基丙烯酸酯,继续于85-88℃保温1h,在确认NCO%≤0.1%,降温;
S6.转釜,按比例加入单体以及哑粉,使用高速分散机以2500rpm分散30min。
在S4中,羟基丙烯酸酯的滴加操作在30min内完成滴加。
实施例2
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入222.3g异佛尔酮二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将1000g分子量为2000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,用高速分散机以2500rpm分散30min。
实施例3
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入250.24g二苯基甲烷二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将1000g分子量为2000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
实施例4
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入174.16g甲苯二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将1000g分子量为2000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
实施例5
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入222.3g异佛尔酮二异氰酸酯、0.2g二月桂酸二丁基锡、0.25g对羟基苯甲醚和0.13g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将2000g分子量为4000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
实施例6
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入250.24g二苯基甲烷二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将2000g分子量为4000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
实施例7
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入174.16g甲苯二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将2000g分子量为4000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
实施例8
一种紫外光固化哑光树脂,依照以下步骤制备得到:
步骤1):在反应釜中依次投入222.3g异佛尔酮二异氰酸酯、0.15g二月桂酸二丁基锡、0.3g对羟基苯甲醚和0.1g 2,6-二叔丁基-4-甲基苯酚,升温至40~50℃;
步骤2):将1000g分子量2000的聚酯二元醇滴入反应釜中并搅拌,接着缓慢升温至65℃;
步骤3):聚酯多元醇滴入后,反应釜温度保持于60~65℃,1h后检测确NCO%是否降到起始值的一半,如NCO%过高则继续保温;
步骤4):滴加混合均匀的117g季戊四醇三丙烯酸酯与87g丙烯酸羟乙酯,在30min内完成滴加,控制反应釜温度缓慢升高,但不超过90℃;
步骤5):于85-88℃保温,0.5h后,测NCO%,NCO%≤0.5%时,加入剩余的20g丙烯酸羟乙酯,继续于85-88℃保温1h,确认NCO%≤0.1%,降温;
步骤6):转釜,按单体10-30%、哑粉3-10%、分散剂0.1-2%的比例使用单体以及哑粉、分散剂BYK2008,使用高速分散机以2500rpm分散30min。
对比例1
传统的可紫外光固化哑光树脂。
将实施例2~实施例8的紫外光固化哑光树脂,以及对比例1的传统的可紫外光固化哑光树脂,进行检测。测试结果见表1。
表1实施例2-实施例8的紫外光固化哑光树脂,以及对比例1的传统的可紫外光固化哑光树脂的性能测试表
由表1的测试结果可知,实施例2-实施例8提供的紫外光固化哑光树脂,其使用聚酯多元醇、二异氰酸酯和羟基丙烯酸酯作为主体反应物,合成可紫外光固化的哑光树脂,通过使用大分子量聚酯多元醇降低合成树脂的双键密度,使用单体将哑粉悬浮到涂层表面,两个方面同时降低光泽,使合成的树脂具有优异的哑光性能。该可紫外光固化哑光树脂,可以使用到喷涂、辊涂、淋涂等领域,价格便宜的同时还能达到很好的哑光效果,只需要添加3~5个点的哑粉就能将光泽降低到5度左右。另外该树脂还具有良好的附着力和性能表现。
以上内容仅仅为本发明的结构所作的举例和说明,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些显而易见的替换形式均属于本发明的保护范围。
Claims (8)
2.根据权利要求1所述的紫外光固化哑光树脂,其特征在于,所述聚酯多元醇树脂分子量在2000~5000。
3.根据权利要求1所述的紫外光固化哑光树脂,其特征在于,所述二异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯或二苯基甲烷二异氰酸酯中的至少一种。
4.根据权利要求1所述的紫外光固化哑光树脂,其特征在于,所述抗氧化剂为2,6-二叔丁基苯酚、对苯二酚或亚磷酸酯三苯酯中的至少一种。
5.根据权利要求1所述的紫外光固化哑光树脂,其特征在于,所述催化剂为二月桂酸二丁基锡。
6.根据权利要求1所述的紫外光固化哑光树脂,其特征在于,所述羟基丙烯酸酯为丙烯酸羟乙酯、甲基丙烯酸羟乙酯、丙烯酸羟丙酯或季戊四醇三丙烯酸酯中的至少一种。
7.一种如权利要求1-6任一所述的紫外光固化哑光树脂的制备方法,其特征在于,按以下步骤进行制备:
S1.按重量份数,在反应釜中依次投入二异氰酸酯、催化剂、阻聚剂、抗氧剂,升温至40~50℃;
S2.将聚酯多元醇滴入反应釜中并搅拌,接着缓慢升温至55~65℃;
S3.在将聚酯多元醇全部滴入后,反应釜温度保持在60~65℃,1h后检测确定NCO%是否降到起始值的一半,如NCO%过高则继续保温;
S4.滴加部分已经混合均匀的羟基丙烯酸酯,控制反应釜温度缓慢升高,但不超过90℃;
S5.于85-88℃保温,0.5h后测NCO%,在NCO%≤0.5%时,加入剩余的羟基丙烯酸酯,继续于85-88℃保温1h,在确认NCO%≤0.1%,降温;
S6.转釜,按比例加入单体以及哑粉,使用高速分散机以2500rpm分散30min。
8.根据权利要求1所述的制备方法,其特征在于,在S4中,羟基丙烯酸酯的滴加操作在30min内完成滴加。
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