CN109593174A - 一种高光泽抗刮伤水性聚氨酯及其制备方法 - Google Patents

一种高光泽抗刮伤水性聚氨酯及其制备方法 Download PDF

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CN109593174A
CN109593174A CN201811496683.9A CN201811496683A CN109593174A CN 109593174 A CN109593174 A CN 109593174A CN 201811496683 A CN201811496683 A CN 201811496683A CN 109593174 A CN109593174 A CN 109593174A
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王辉
杜芳琪
黄芳芳
汤德芳
李海锋
戚奇杰
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China Tobacco Zhejiang Industrial Co Ltd
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Abstract

本发明提供一种高光泽抗刮伤水性聚氨酯，该聚氨酯具有高光泽度，耐高温、不发白以及容易剥离性能；该聚氨酯按重量百分比计算由以下组份组成：6.9～7.1％的聚醚二元醇、6.5～7％的聚酯二元醇、0.1～0.3％的三羟甲基丙烷、8.4～8.6％的氢化苯基甲烷二异氰酸酯、1.4～1.6％的二羟甲基丙酸、0.3～0.5％的1，4‑环己烷二甲醇、1.2～1.7％的N‑甲基吡咯烷酮、14.5～14.8％的丙酮、1.1～1.3％的三乙胺、54.9～58.4％的水以及0.1～0.3％的异佛尔酮二胺。

Description

一种高光泽抗刮伤水性聚氨酯及其制备方法
技术领域
本发明属于水性涂料领域，涉及一种高光泽抗刮伤水性聚氨酯及其制备方法，尤其是涉及一种可制造高光泽、易剥离、耐高温，适合凹印和胶印的水性聚氨酯镭射转移涂料的水性聚氨酯及其制备方法。
背景技术
水性聚氨酯以水为分散介质，具有无毒、不易燃烧、不污染环境、节能、安全可靠等优点，符合绿色工业的发展要求，因此近年来水性聚氨酯涂料获得了广泛的关注和国内外的重视。
但因水性聚氨酯镭射转移涂料的研究尚不完善，水性聚氨酯镭射转移涂料的性能还存在许多不理想的情况，比如水性聚氨酯镭射转移涂料成膜后的剥离性、光泽度、耐高温性能等还不能满足要求，这些性能与生产涂料的树脂本身的性能有密切的关系。
发明内容
为了解决以上技术问题，本发明的发明人针对用于水性镭射转移涂料的水性聚氨酯树脂的高光泽、耐高温、剥离性等方面进行了研究。
第一方面，本发明提供一种高光泽抗刮伤水性聚氨酯，该聚氨酯具有高光泽度，耐高温、不发白以及容易剥离性能；该聚氨酯按重量百分比计算由以下组份组成：6.9～7.1％的聚醚二元醇、6.5～7％的聚酯二元醇、0.1～0.3％的三羟甲基丙烷、8.4～8.6％的氢化苯基甲烷二异氰酸酯、1.4～1.6％的二羟甲基丙酸、0.3～0.5％的1，4-环己烷二甲醇、1.2～1.7％的N-甲基吡咯烷酮、14.5～14.8％的丙酮、1.1～1.3％的三乙胺、54.9～58.4％的水以及0.1～0.3％的异佛尔酮二胺。
作为优选，所述的聚醚二元醇分子量为3000。
作为优选，所述的聚酯二元醇分子量为1000。
第二方面，本发明提供上述所述高光泽抗刮伤水性聚氨酯的制备方法，该方法包括如下步骤：
(1)备料：按上述所述高光泽抗刮伤水性聚氨酯的组分及比例备料；
(2)原料混合、加热、脱水：量取聚醚二元醇、聚酯二元醇，加入三羟甲基丙烷，将三者搅拌均匀加热至120℃，真空-0.06mpa下脱水1-2h，然后降温至80-95℃，得混合物1；
(3)预聚物合成：把氢化苯基甲烷二异氰酸酯加入步骤(2)所得混合物1中，在80-95℃的温度下，搅拌反应1-2h，然后加入亲水剂二羟甲基丙酸、1，4-环己烷二甲醇和N-甲基吡咯烷酮，维持80℃温度继续反应1-2h，再降温至55-65℃，加入丙酮，维持温度继续反应1-2h，得到预聚物；
(4)预聚物中和、分散、后扩链：将预聚物的温度降至30～40℃，加入中和剂三乙胺，加水强力搅拌，滴加后扩链剂异佛尔酮二胺，保持搅拌1-1.5h，得分散液；
(5)脱溶、过滤：将(4)得到的分散液在搅拌状态下升温至60℃，保持-0.06MPa真空，搅拌1h-2h，脱出丙酮，得到水性聚氨酯树脂。
作为优选，所述步骤(3)中的预聚物合成步骤为：把氢化苯基甲烷二异氰酸酯加入步骤(2)所得混合物1中，在80-95℃的温度下，搅拌反应1-2h，然后加入二羟甲基丙酸、1，4-环己烷二甲醇和N-甲基吡咯烷酮，维持80℃温度继续反应1-2h，再降温至60℃，加入丙酮，维持温度继续反应2h，得到预聚物。
作为优选，所述步骤(4)的预聚物中和、分散、后扩链步骤为：将预聚物的温度降至30～40℃，加入中和剂三乙胺，加水强力搅拌，滴加后扩链剂异佛尔酮二胺，保持搅拌1h，得分散液。
在本发明其他一些实施方式中，步骤3)中的亲水剂选自二羟基半酯，乙二胺基乙磺酸钠，1,4-丁二醇-2-磺酸钠，N-甲基二乙醇胺(HO-CH2CH2-N(-CH3)-CH2CH2-OH)或水溶性聚氧化乙烯二醇，然而其与亲水剂二羟甲基丙酸相比，其获得预聚物的时间以及最终获得聚氨酯的性能均存在劣势，因此本发明优选采取亲水剂二羟甲基丙酸。
本发明提供的抗刮伤水性聚氨酯的制备方法中，将三羟甲基丙烷与聚酯聚醚二元醇混合均匀后同时与氢化苯基甲烷二异氰酸酯聚合可以明显增加光泽度，最终达到高光泽和抗刮伤的效果。
与现有技术相比，本发明具有如下优点：
1.本发明提供的聚氨酯具有镀铝剥离后有极高的光泽度，成膜后在180℃高温下不变软、不发白，更适应包装领域的生产工艺。
2.本发明提供的聚氨酯剥离性能好，该聚氨酯涂布到PET或者OPP膜上成膜后，用3M胶粘带标准检测方法检测，其膜很容易完全剥离，不会出现断裂遗留现象，与现有技术对比，其剥离强度低，剥离性能好。
3.现有技术一般成膜后光泽度低，耐高温130℃-150℃，剥离强度高。
具体实施方式
下面结合具体实施例对本发明予以详细说明，但不用来限制本发明的范围。
实施例1
(1)按照以下组分和比例进行备料
分子量为3000的聚醚二元醇6.9KG，分子量为1000的聚酯二元醇7KG，三羟甲基丙烷0.3KG，氢化苯基甲烷二异氰酸酯8.4KG，二羟甲基丙酸1.4KG；1，4-环己烷二甲醇0.5KG，N甲基吡咯烷酮1.2kg，丙酮14.5kg，三乙胺1.1kg，水58.4kg，异佛尔酮二胺0.3kg；
(2)原料混合、加热、脱水
量取聚醚二元醇、聚酯二元醇，加入扩链剂三羟甲基丙烷，将三者搅拌均匀加热至120℃，真空-0.06mpa下脱水1h，然后降温至80℃，得混合物1；
(3)预聚物合成
把氢化苯基甲烷二异氰酸酯加入上述步骤(2)所得混合物中，控制温度为90℃，搅拌反应2h，然后加入亲水剂二羟甲基丙酸、扩链剂1,4-环己烷二甲醇，N-甲基吡咯烷酮，维持温度80℃继续反应1h，再降温至60℃加入丙酮，维持温度60℃继续搅拌2h，得到预聚物。
(4)预聚物中和、分散、扩链、脱溶
将预聚物的温度降至40℃，加入三乙胺中和搅拌1分钟，加水强力搅拌5分钟，滴加扩链剂异佛尔酮二胺，保持搅拌1h，升温至60℃，真空-0.06MPa，保持搅拌1小时，脱出丙酮，得到水性聚氨酯乳液。
实施例2
(1)按照以下组分和比例进行备料
分子量为3000的聚醚二元醇7KG，分子量为1000的聚酯二元醇6.8KG，三羟甲基丙烷0.2KG，氢化苯基甲烷二异氰酸酯8.5KG，二羟甲基丙酸1.5KG；1，4-环己烷二甲醇0.4KG，N甲基吡咯烷酮1.5kg，丙酮14.6kg，三乙胺1.2kg，水58.1kg，异佛尔酮二胺0.2kg；
(2)原料混合、加热、脱水
量取聚醚二元醇、聚酯二元醇，加入扩链剂三羟甲基丙烷，将三者搅拌均匀加热至120℃，真空-0.06mpa下脱水1h，然后降温至80℃，得混合物1；
(3)预聚物合成
把氢化苯基甲烷二异氰酸酯加入上述步骤(2)所得混合物中，控制温度为90℃，搅拌反应2h，然后加入亲水剂二羟甲基丙酸、扩链剂1,4-环己烷二甲醇，N-甲基吡咯烷酮，维持温度80℃继续反应1h，再降温至60℃加入丙酮，维持温度60℃继续搅拌2h，得到预聚物。
(4)预聚物中和、分散、扩链、脱溶
将预聚物的温度降至40℃，加入三乙胺中和搅拌1分钟，加水强力搅拌5分钟，滴加扩链剂异佛尔酮二胺，保持搅拌1h，升温至60℃，真空-0.06MPa，保持搅拌1小时，脱出丙酮，得到水性聚氨酯乳液。
实施例3
(1)按照以下组分和比例进行备料
分子量为3000的聚醚二元醇7.1KG，分子量为1000的聚酯二元醇6.5KG，三羟甲基丙烷0.1KG，氢化苯基甲烷二异氰酸酯8.6KG，二羟甲基丙酸1.6KG；1，4-环己烷二甲醇0.3KG，N甲基吡咯烷酮1.7kg，丙酮14.8kg，三乙胺1.3kg，水57.9kg，异佛尔酮二胺0.1kg；
(2)原料混合、加热、脱水
量取聚醚二元醇、聚酯二元醇，加入扩链剂三羟甲基丙烷，将三者搅拌均匀加热至120℃，真空-0.06mpa下脱水1h，然后降温至80℃，得混合物1；
(3)预聚物合成
把氢化苯基甲烷二异氰酸酯加入上述步骤(2)所得混合物中，控制温度为90℃，搅拌反应2h，然后加入亲水剂二羟甲基丙酸、扩链剂1,4-环己烷二甲醇，N-甲基吡咯烷酮，维持温度80℃继续反应1h，再降温至60℃加入丙酮，维持温度60℃继续搅拌2h，得到预聚物。
(4)预聚物中和、分散、扩链、脱溶
将预聚物的温度降至40℃，加入三乙胺中和搅拌1分钟，加水强力搅拌5分钟，滴加扩链剂异佛尔酮二胺，保持搅拌1h，升温至60℃，真空-0.06MPa，保持搅拌1小时，脱出丙酮，得到水性聚氨酯乳液。
试验例
将按照实施例1～3方法制备的水性聚氨酯树脂涂布到PET或者OPP膜上成膜后，模压后镀铝测光泽度，耐温性、剥离性，并以目前市场上树脂作为对照例，具体结果见表1。
经测试：本发明制备的水性聚氨酯树脂光泽度高，暗区光泽度可达到90度以上；用塑封仪测试耐温性，耐温高，可达到160℃以上；用3M胶粘带标准检测方法检测，其膜很容易完全剥离，不会出现断裂遗留现象，与现有技术对比，其剥离强度低，易剥离性良好。
表1水性聚氨酯树脂性能测试结果
由表1可知，实施例1-3的水性聚氨酯树脂涂层耐温性、光泽度、剥离性符合使用要求。由此可见，本发明效果符合转移涂料用树脂的技术指标，适合做水性镭射转移涂料。
以上所述的仅是本发明的一些实施方式。对于本领域的普通技术人员来说，在不脱离本发明创造构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。

Claims (6)

1.一种高光泽抗刮伤水性聚氨酯，其特征在于：该聚氨酯按重量百分比计算由以下组份组成：6.9～7.1％的聚醚二元醇、6.5～7％的聚酯二元醇、0.1～0.3％的三羟甲基丙烷、8.4～8.6％的氢化苯基甲烷二异氰酸酯、1.4～1.6％的二羟甲基丙酸、0.3～0.5％的1，4-环己烷二甲醇、1.2～1.7％的N-甲基吡咯烷酮、14.5～14.8％的丙酮、1.1～1.3％的三乙胺、54.9～58.4％的水以及0.1～0.3％的异佛尔酮二胺。
2.根据权利要求1所述的高光泽抗刮伤水性聚氨酯，其特征在于：所述的聚醚二元醇分子量为3000。
3.根据权利要求1所述的高光泽抗刮伤水性聚氨酯，其特征在于：所述的聚酯二元醇分子量为1000。
4.如权利要求1～3任意一项所述高光泽抗刮伤水性聚氨酯的制备方法，其特征在于：该方法包括如下步骤：
(1)备料：按权利要求1～3任意一项所述高光泽抗刮伤水性聚氨酯的组分及比例备料；
(2)原料混合、加热、脱水：量取聚醚二元醇、聚酯二元醇，加入三羟甲基丙烷，将三者搅拌均匀加热至120℃，真空-0.06mpa下脱水1-2h，然后降温至80-95℃，得混合物1；
(3)预聚物合成：把氢化苯基甲烷二异氰酸酯加入步骤(2)所得混合物1中，在80-95℃的温度下，搅拌反应1-2h，然后加入二羟甲基丙酸、1，4-环己烷二甲醇和N-甲基吡咯烷酮，维持80℃温度继续反应1-2h，再降温至55-65℃，加入丙酮，维持温度继续反应1-2h，得到预聚物；
(4)预聚物中和、分散、后扩链：将预聚物的温度降至30～40℃，加入中和剂三乙胺，加水强力搅拌，滴加后扩链剂异佛尔酮二胺，保持搅拌1-1.5h，得分散液；
(5)脱溶、过滤：将(4)得到的分散液在搅拌状态下升温至60℃，保持-0.06MPa真空，搅拌1h-2h，脱出丙酮，得到水性聚氨酯树脂。
5.如权利要求4所述的高光泽抗刮伤水性聚氨酯的制备方法，其特征在于：所述步骤(3)中的预聚物合成步骤为：把氢化苯基甲烷二异氰酸酯加入步骤(2)所得混合物1中，在80-95℃的温度下，搅拌反应1-2h，然后加入二羟甲基丙酸、1，4-环己烷二甲醇和N-甲基吡咯烷酮，维持80℃温度继续反应1-2h，再降温至60℃，加入丙酮，维持温度继续反应2h，得到预聚物。
6.如权利要求4所述的高光泽抗刮伤水性聚氨酯的制备方法，其特征在于：所述步骤(4)的预聚物中和、分散、后扩链步骤为：将预聚物的温度降至30～40℃，加入中和剂三乙胺，加水强力搅拌，滴加后扩链剂异佛尔酮二胺，保持搅拌1h，得分散液。
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