CN116855221A - 一种uv延迟固化聚氨酯胶黏剂及其制备方法 - Google Patents
一种uv延迟固化聚氨酯胶黏剂及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种UV延迟固化聚氨酯胶黏剂,按重量份计,包括以下组分:聚氨酯预聚体34‑56份、硅烷偶联剂2‑7份、填料1‑5份,催化剂0.5‑2份,抗氧剂0.1‑0.5份。本发明提供了一种UV延迟固化聚氨酯胶黏剂,所述胶黏剂为湿气固化,并且无腐蚀性、稳定性高。本发明提供了一种新型聚氨酯预聚体,未反应游离的聚丙烯酸丁酯单体和芳香族异氰酸酯含量少,有利于提高胶黏剂的稳定性,并且安全性更高。通过将多种组分进行复配,得到胶黏剂性能优异,稳定性高,对种UV延迟固化聚氨酯胶黏剂的发展具有重要意义。本发明胶黏剂的制备方法简单易于操作,便于推广和使用,节约生产成本。
Description
技术领域
本发明属于胶黏剂技术领域,具体涉及一种UV延迟固化聚氨酯胶黏剂及其制备方法。
背景技术
近年来国家对于环保的要求越来越高,环保的湿气固化聚氨酯胶黏剂越来越受欢迎,逐渐已被广泛使用。其作用机理是聚氨酯预聚体与空气中的水分子发生化学反应,固化交联而形成稳定的化学结构。CN 103232829A公开了一种光-湿气双固化胶黏剂的研制及产业化,该方法选择丙烯酸酯树脂、可光-湿气双重固化的聚硅氧烷丙烯酸酯树脂、丙烯酸活性稀释剂、光引发剂和阻聚剂,按适合的配方比例,制备出光-湿气双固化胶黏剂。CN112920762 A公开了一种快速粘接的UV/湿气双重固化胶黏剂及其制备方法。所述胶黏剂的各组分按质量份数计分别为:聚氨酯丙烯酸树脂10.0-50.0份、UV/湿气双重固化聚氨酯丙烯酸树脂10.0-50.0份、活性稀释剂5-30.0份、光引发剂0.1-8.0份、湿气固化催化剂0.01-2.0份、增粘树脂0-15份、触变剂0.5-10份。市面上现有的单纯湿气固化的胶黏剂,通常因游离的丙烯酸单体或异氰酸酯降低胶黏剂的性能,胶黏剂存在腐蚀性、稳定性差等问题。
发明内容
本发明的目的是提供一种UV延迟固化聚氨酯胶黏剂及其制备方法,本发明制备的胶黏剂可以实现湿气固化,并且具有无腐蚀性、稳定性高的优点。
为了实现上述目的,本发明提供了以下技术方案:
本发明第一方面提供了一种UV延迟固化聚氨酯胶黏剂,按重量份计,包括以下组分:聚氨酯预聚体34-56份、硅烷偶联剂2-7份、填料1-5份,催化剂0.5-2份,抗氧剂0.1-0.5份。
优选的,按重量份计,包括以下组分:聚氨酯预聚体48份、硅烷偶联剂5份、填料3份,催化剂1份,抗氧剂0.3份。
在一种优选的实施方式中,所述聚氨酯预聚体由摩尔比为(1.3-1.6):1:(0.3-0.5)的芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯制得。优选的,所述聚氨酯预聚体由摩尔比为1.5:1:0.4的芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯制得。
在一种优选的实施方式中,所述聚氨酯预聚体的制备方法为:将芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,温度80-110℃,反应2-4h。
优选的,所述聚氨酯预聚体的制备方法为:将芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,温度95℃,反应3h。
本发明提供了聚氨酯预聚体,聚氨酯预聚体未反应游离的聚丙烯酸丁酯单体和芳香族异氰酸酯含量少,预聚体的双官能团主链一端NCO,另一端为丙烯酸双键,可以保证胶黏剂的稳定性,同时低游离预聚体显著改进了胶黏剂的性能。发明人发现当聚氨酯预聚体由摩尔比为1.5:1:0.4的芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯在特定反应条件下制得,胶黏剂的稳定性更高,发明人猜测是因为该条件下制备的聚氨酯预聚体的游离组分含量低、相对分子质量分布较窄、分子结构更为规整,聚氨酯预聚体的稳定性更高。与其余组分复配得到的胶黏剂稳定性高。
优选的,所述芳香族异氰酸酯为二苯基甲烷二异氰酸酯。
CAS101-68-8。
优选的,所述聚丙烯酸丁酯的数均分子量为10000。购自阿拉丁,P404923。
为了提高聚氨酯预聚体的稳定性,优选的,所述脂肪族聚酯多元醇为聚己二酸乙二醇酯和聚己二酸新戊二醇酯,摩尔比为1~3:1。优选的,所述脂肪族聚酯多元醇为聚己二酸乙二醇酯和聚己二酸新戊二醇酯,摩尔比为2:1。
优选的,所述聚己二酸乙二醇酯的分子量为1000,官能度为2,羟值为106~118mgKOH/g,酸值为0.5mg KOH/g;购自上海汇得科技股份有限公司,品名HDPOL-2210。所述聚己二酸新戊二醇酯的分子量为2000,官能度为2,羟值为53~59mg KOH/g,酸值为0.5mg KOH/g。购自上海汇得科技股份有限公司,品名HDPOL-3320。
本发明选用聚酯二元醇参与反应,本发明选用特定种类和性能的聚酯二元醇,从而获得相对分子质量较小、相对分子质量分布较窄的聚酯预聚体,可以提高胶黏剂的粘接性。
在一种优选的实施方式中,所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,重量比为1:1~5;优选的,所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,重量比为1:4,购自阿拉丁。所述抗氧剂为2,6-二叔丁基对甲酚;购自阿拉丁。
在一种优选的实施方式中,所述填料选自钛白粉、炭黑、滑石粉、碳酸钙、气相二氧化硅中的一种或多种。
优选的,所述填料选自炭黑和气相二氧化硅,重量比为1:1。购自默克。
本发明通过将多种组分进行复配,得到胶黏剂具有很高的稳定性。发明人发现将本发明的聚氨酯预聚体与三乙烯二胺和N,N-二甲基环己胺、2,6-二叔丁基对甲酚、三乙烯二胺和N,N-二甲基环己胺、炭黑和气相二氧化硅进行复配得到胶黏剂性能更加。发明人猜测是炭黑和气相二氧化硅表面能极大地提高2,6-二叔丁基对甲酚的耐迁移,减少抗氧剂损失,并且2,6-二叔丁基对甲酚可改善炭黑和气相二氧化硅与聚氨酯预聚体的相容性。本发明的催化剂可以促进聚氨酯胶黏剂反应速度,得到的胶黏剂的性能更佳。
本发明第二方面提供了所述的一种UV延迟固化聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)制备聚氨酯预聚体;
(2)将聚氨酯预聚体、硅烷偶联剂、填料、催化剂、抗氧剂混合,95~110℃搅拌10~20min,制得胶黏剂。
与现有技术相比,本发明的优点和有益效果为:
1.本发明提供了一种UV延迟固化聚氨酯胶黏剂,所述胶黏剂为湿气固化,并且无腐蚀性、稳定性高。
2.本发明提供了一种新型聚氨酯预聚体,未反应游离的聚丙烯酸丁酯单体和芳香族异氰酸酯含量少,有利于提高胶黏剂的稳定性,并且安全性更高。
3.本发明通过将多种组分进行复配,得到胶黏剂性能优异,稳定性高,对种UV延迟固化聚氨酯胶黏剂的发展具有重要意义。
4.本发明胶黏剂的制备方法简单易于操作,便于推广和使用,节约生产成本。
具体实施方式
下面将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。基于本发明中的实施例,本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例,都属于本发明保护的范围。
实施例1
本实施例提供了一种UV延迟固化聚氨酯胶黏剂,按重量份计,包括以下组分:聚氨酯预聚体48份、硅烷偶联剂5份、填料3份,催化剂1份,抗氧剂0.3份。
所述聚氨酯预聚体的制备方法为:将摩尔比为1.5:1:0.4芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,温度95℃,反应3h。
所述芳香族异氰酸酯为二苯基甲烷二异氰酸酯。所述聚丙烯酸丁酯的数均分子量为10000。
所述脂肪族聚酯多元醇为聚己二酸乙二醇酯和聚己二酸新戊二醇酯,摩尔比为2:1。所述聚己二酸乙二醇酯的分子量为1000,官能度为2,羟值为106~118mg KOH/g,酸值为0.5mg KOH/g;所述聚己二酸新戊二醇酯的分子量为2000,官能度为2,羟值为53~59mgKOH/g,酸值为0.5mg KOH/g。
所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,重量比为1:4。所述抗氧剂为2,6-二叔丁基对甲酚。所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,三乙烯二胺和N,N-二甲基环己胺的重量比为1:4,所述填料选自炭黑和气相二氧化硅,重量比为1:1。
所述的一种UV延迟固化聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)制备聚氨酯预聚体;
(2)将聚氨酯预聚体、硅烷偶联剂、填料、催化剂、抗氧剂混合,105℃搅拌15min,制得胶黏剂。
实施例2
本实施例与实施例1的区别为:聚氨酯预聚体50份、硅烷偶联剂3份、填料5份,催化剂0.5份,抗氧剂0.5份。
实施例3
本实施例与实施例1的区别为:所述聚氨酯预聚体的制备方法为:将摩尔比为1.3:1:0.5芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,温度80℃,反应4h。
对比例1
本对比例与实施例1的区别为:聚氨酯预聚体60份、硅烷偶联剂5份、填料6份,催化剂4份,抗氧剂2份。
对比例2
本对比例与实施例1的区别为:所述聚氨酯预聚体的制备方法为:将摩尔比为0.9:1:0.8芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,温度115℃,反应3h。
对比例3
本对比例与实施例1的区别为:所述脂肪族聚酯多元醇为聚己二酸乙二醇酯和聚己二酸新戊二醇酯,聚己二酸乙二醇酯和聚己二酸新戊二醇酯摩尔比为1:3。所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,三乙烯二胺和N,N-二甲基环己胺重量比为5:1。
对比例4
所述脂肪族聚酯多元醇为聚己二酸乙二醇酯,所述聚己二酸乙二醇酯的分子量为700,官能度为2,羟值为150~170mg KOH/g,酸值为0.5mg KOH/g;购自上海汇得科技股份有限公司,品名HDPOL-3305。
对比例5
本对比例与实施例1的区别为:所述聚己二酸新戊二醇酯的分子量为2000,官能度为2,羟值为53~59mg KOH/g,酸值为0.5mg KOH/g。购自上海汇得科技股份有限公司,品名HDPOL-3320。
对比例6
本对比例与实施例1的区别为:不包含填料和催化剂。
性能测试
将实施例和对比例制备的胶黏剂涂在铝合金基板上,用365nm的UV-LED光源对胶黏剂照射10000mJ/cm2的能量,然后在铝合金基板上贴合另一块铝合金基板,分别固化1h、24h、72h以及72h后老化,用万能材料试验机沿着剪切方向以100mm/min的速度运行至样件粘接失效,通过最大力值结合粘接面积(25.4mm*12.7mm,胶厚0.15mm,)计算胶黏剂对铝合金基板的粘接强度。结果见表1。
表1胶黏剂的稳定性测试结果
通过实施例可知,本发明制备的胶黏剂的粘接性强且稳定性高,通过对比例可知,聚氨酯预聚体制备方法的改变以及其余组分的变化,均会降低胶黏剂的粘接性和稳定性。
以上所述是本发明的优选实施方式,应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明所述原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种UV延迟固化聚氨酯胶黏剂,其特征在于,按重量份计,包括以下组分:聚氨酯预聚体34-56份、硅烷偶联剂2-7份、填料1-5份,催化剂0.5-2份,抗氧剂0.1-0.5份。
2.根据权利要求1所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述聚氨酯预聚体由摩尔比为(1.3-1.6):1:(0.3-0.5)的芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯制得。
3.根据权利要求2所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述聚氨酯预聚体的制备方法为:将芳香族异氰酸酯、脂肪族聚酯多元醇和聚丙烯酸丁酯混合,在氮气保护下,80-110℃下反应2-4h。
4.根据权利要求2所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述芳香族异氰酸酯为二苯基甲烷二异氰酸酯。
5.根据权利要求2所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述脂肪族聚酯多元醇为聚己二酸乙二醇酯和聚己二酸新戊二醇酯,摩尔比为1~3:1。
6.根据权利要求5所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述聚己二酸乙二醇酯的分子量为1000,官能度为2,羟值为106~118mg KOH/g,酸值为0.5mg KOH/g;所述聚己二酸新戊二醇酯的分子量为2000,官能度为2,羟值为53~59mg KOH/g,酸值为0.5mgKOH/g。
7.根据权利要求2所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述聚丙烯酸丁酯的数均分子量为10000。
8.根据权利要求1所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述催化剂选自三乙烯二胺和N,N-二甲基环己胺,重量比为1:1~5;所述抗氧剂为2,6-二叔丁基对甲酚。
9.根据权利要求1所述的一种UV延迟固化聚氨酯胶黏剂,其特征在于,所述填料选自钛白粉、炭黑、滑石粉、碳酸钙、气相二氧化硅中的一种或多种。
10.权利要求1~9任一项所述的一种UV延迟固化聚氨酯胶黏剂的制备方法,其特征在于,包括以下步骤:
(1)制备聚氨酯预聚体;
(2)将聚氨酯预聚体、硅烷偶联剂、填料、催化剂、抗氧剂混合,95~110℃搅拌10~20min,制得胶黏剂。
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