CN105542111A - 一种耐高温转移镀铝水性聚氨酯乳液及其制备方法 - Google Patents

一种耐高温转移镀铝水性聚氨酯乳液及其制备方法 Download PDF

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CN105542111A
CN105542111A CN201610061847.XA CN201610061847A CN105542111A CN 105542111 A CN105542111 A CN 105542111A CN 201610061847 A CN201610061847 A CN 201610061847A CN 105542111 A CN105542111 A CN 105542111A
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张丹年
朱天寿
唐克卫
王志剑
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XI'AN GREAT SKY NEW MATERIAL CO Ltd
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Abstract

本发明涉及一种耐高温转移镀铝水性聚氨酯乳液及其制备方法，属于涂料领域。所述的水性聚氨酯乳液包括以下重量份的原料：聚酯多元醇20-60，二异氰酸酯10-30，亲水扩链剂1-5，小分子醇类扩链剂1-3，中和剂0.2-2，胺类扩链剂0.5-5，水性硅溶胶30-55，润湿剂2-5，流平剂2-4，去离子水80-240。其制备方法为将聚酯多元醇与二异氰酸酯反应得到预聚体后加入扩链剂进行扩链反应，经中和反应、乳化后加入胺类扩链剂，再与水性硅溶胶、润湿剂、流平剂混合即可。本发明提供的水性聚氨酯乳液耐温高达180℃，膜不失光、不黄变，具有良好的剥离效果，无疑似苯存在，可广泛应用于食品、烟草行业的包装涂料领域。

Description

一种耐高温转移镀铝水性聚氨酯乳液及其制备方法
技术领域
本发明属于涂料领域，具体涉及一种耐高温转移镀铝水性聚氨酯乳液及其制备方法。
背景技术
转移镀铝涂料是镀铝膜和镀铝纸的重要组成部分，但是，传统的溶剂型转移涂料中挥发性有机物（VOCs）含量高、气味大、严重污染环境，残留的溶剂导致镀铝纸产生不良的气味，不能完全满足烟草包装行业的VOCs要求。
然而，水性聚氨酯乳液是环境友好性涂料，其以水代替有机溶剂作为分散介质，合成工艺稳定。其涂膜具有不燃、无毒、不污染环境等优点，但目前市场上供应的水性聚氨酯乳液达不到烟草包装行业的VOCs要求，耐温效果不好，不能满足市场要求。因此，开发耐高温，转移效果好的水性转移镀铝涂料，迫在眉睫，随着高速剥离机械的推广，这一要求更为突出。
发明内容
本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种耐高温转移镀铝水性聚氨酯乳液及其制备方法。
为实现上述发明目的，本发明采用如下技术方案：
一种耐高温转移镀铝水性聚氨酯乳液，包括以下重量份数的原料：
聚酯多元醇20-60份；
二异氰酸酯10-30份；
亲水扩链剂1-5份；
小分子醇类扩链剂1-3份；
中和剂0.2-2份；
胺类扩链剂0.5-5份；
水性硅溶胶30-55份；
润湿剂2-5份；
流平剂2-4份；
去离子水80-240份。
优选地，所述的聚酯多元醇为聚己二酸丁二醇酯多元醇、聚己内酯多元醇、聚碳酸酯多元醇、聚己二酸新戊二醇多元醇、聚丙烯酸酯多元醇中的一种或几种。
优选地，所述的二异氰酸酯为二环已基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二环已基甲烷二异氰酸酯、1,4-环己烷二异氰酸酯、三甲基-1,6-六亚甲基二异氰酸酯或环己烷二亚甲基二异氰酸酯。
优选地，所述的亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸、乙二氨基磺酸钠、1,4-丁二醇-2-磺酸钠中的一种或几种；所述的小分子醇类扩链剂为乙二醇、1,4-丁二醇、丙二醇、新戊二醇或1,6-己二醇；所述的胺类扩链剂为乙二胺、异佛尔酮二胺或丙二胺。
优选地，所述水性硅溶胶的pH值为7.0-9.0。
优选地，所述的润湿剂为聚氧乙烯烷基醚；所述的流平剂为聚醚硅氧烷共聚物。
优选地，所述中和剂为三乙胺、N,N二甲基乙醇胺、三乙醇胺。
一种耐高温转移镀铝水性聚氨酯乳液的制备方法，包括以下步骤：
A．将聚酯多元醇在120℃下真空脱水1-2小时，降温至40℃，加入二异氰酸酯，搅拌，升温，控制反应温度为70-80℃，反应2-3小时；
B．加入亲水扩链剂，小分子醇类扩链剂，在70-80℃下继续反应1-2小时；
C．将步骤B得到的生成物降温至40℃，加入中和剂，中和反应1小时；
D．向上述步骤C得到的生成物中加入去离子水，在40℃下高速分散转相，乳化；
E．向步骤D得到的初乳液中加入胺类扩链剂，控制反应温度在40℃-50℃，进行扩链反应，反应0.5小时，得水性聚氨酯乳液；
F．向步骤E得到的乳液中加入水性硅溶胶、润湿剂、流平剂，即得耐高温转移镀铝水性聚氨酯乳液。
与现有技术相比，本发明具有如下优点：
本发明工艺稳定，制备出的耐高温转移镀铝水性聚氨酯乳液无疑似苯存在，VOCs满足食品、烟草行业包装要求，耐温高达180度，具有良好的剥离效果，膜不失光，不黄变，对铝层有极好的保护能力，是目前用于取代溶剂型转移涂料生产高光真空镀铝金银卡纸的水性环保材料，在食品、烟草包装领域有广泛的应用。
具体实施方式
下面结合具体实施例对本发明进行详细说明。
实施例1
(1)将20份聚己内酯二元醇（Mn=2000）在120℃下真空脱水1小时，然后将其置于装有搅拌器，回流冷凝管，温度计的三口烧瓶中，降温至40℃，加入12份的异佛尔酮二异氰酸酯，控制反应温度70℃，反应3小时；
(2)加入1.5份的二羟甲基丙酸，1.5份1,4-丁二醇，在70℃下继续反应2小时；
(3)加入2份1,4-丁二醇-2-磺酸钠，在70℃下继续反应2小时；
(4)将步骤(3)的生成物降温至40℃，加入1份三乙胺，中和反应1小时；
(5)向步骤(4)的生成物中加入85份去离子水，在40℃下高速分散转相，乳化30分钟，得到初乳液；
(6)向所述初乳液中加入0.5份二乙胺，控制温度40℃，反应0.5小时，得到水性聚氨酯乳液；
(7)向所述水性聚氨酯乳液中加入30份水性硅溶胶、2份聚氧乙烯烷基醚、4份聚醚硅氧烷共聚物，混合均匀，得到耐高温转移镀铝水性聚氨酯乳液。
实施例2
(1)将30份聚碳酸酯二元醇（Mn=1000）在120℃下真空脱水2小时，然后将其置于装有搅拌器，回流冷凝管，温度计的三口烧瓶中，降温至40℃，加入20份的二环已基甲烷二异氰酸酯，控制反应温度80℃，反应2小时；
(2)加入1份的二羟甲基丁酸，0.8份乙二醇，在80℃下继续反应2小时；
(3)将步骤(2)的生成物降温至40℃，加入1份三乙胺中和反应1小时，中和反应后加入120份去离子水，在40℃下高速分散转相，乳化30分钟，得到初乳液；
(4)向所述初乳液中加入2份丙二胺，控制温度50℃，反应0.5小时，得到水性聚氨酯乳液；
(5)向上述水性聚氨酯乳液中加入40份水性硅溶胶、5份聚氧乙烯烷基醚、3份聚醚硅氧烷共聚物，混合均匀，得到耐高温转移镀铝水性聚氨酯乳液。
实施例3
(1)将60份聚己二酸丁二醇酯二元醇（Mn=2000）在120℃下真空脱水2小时，然后将其置于装有搅拌器，回流冷凝管，温度计的三口烧瓶中，降温至40℃，加入12份的六亚甲基二异氰酸酯，控制反应温度75℃，反应2小时；
(2)加入1.5份的二羟甲基丁酸，1份丙二醇，在75℃下继续反应2小时；
(3)加入2份的乙二氨基乙磺酸钠，在75℃下反应2小时；
(4)将步骤(3)的生成物降温至40℃，加入0.9份N,N二甲基乙醇胺，中和反应1小时；
(5)加入180份去离子水，在40℃下高速分散转相，乳化30分钟，得到初乳液；
(6)向所述初乳液中加入3份异佛尔酮二胺，控制温度50℃，反应0.5小时，得到水性聚氨酯乳液；
(7)向上述水性聚氨酯乳液中加入50份水性硅溶胶、4份聚氧乙烯烷基醚、2份聚醚硅氧烷共聚物，混合均匀，得到耐高温转移镀铝水性聚氨酯乳液。
实施例4
(1)将40份聚己二酸新戊二醇酯二元醇(Mn=2000)在120℃下真空脱水２小时，然后将其置于装有搅拌器，回流冷凝管，温度计的三口烧瓶中，降温至40℃，加入12份的1，4-环己烷二异氰酸酯，控制反应温度70℃，反应3小时；
(2)加入0.3份的二羟甲基丙酸，2.5份1.6-己二醇，在70℃下继续反应2小时；
(3)将步骤(2)的生成物降温至40℃，加入0.4份三乙醇胺中和反应1小时，加入130份去离子水，在40℃下高速分散转相，乳化30分钟，得到初乳液；
(4)向所述初乳液中加入1.5份乙二胺，控制温度50℃，反应0.5小时，得到水性聚氨酯乳液；
(5)向上述聚氨酯乳液中加入55份水性硅溶胶、5份聚氧乙烯烷基醚、2份聚醚硅氧烷共聚物，混合均匀，得到耐高温转移镀铝水性聚氨酯乳液。
实施例5
(1)30份将聚丙烯酸酯二元醇（Mn=1000）在120℃下真空脱水1小时，然后将其置于装有搅拌器，回流冷凝管，温度计的三口烧瓶中，降温至40℃，加入18份的环己烷二亚甲基二异氰酸酯，控制反应温度80℃，反应2小时；
(2)加入3份二羟甲基丙酸，２份新戊二醇，在80℃下继续反应2小时；
(3)加入1份1,4-丁二醇-2-磺酸钠，在80℃下反应2小时；
(4)将步骤(3)的生成物降温至40℃，加入0.2份三乙胺，中和反应1小时；
(5)加入130份去离子水，在40℃下高速分散转相，乳化30分钟，得到初乳液；
(6)向所述初乳液中加入2.5份异佛尔酮二胺，控制温度40℃，反应0.5小时，得到水性聚氨酯乳液；
(7)向上述水性聚氨酯乳液中加入50份水性硅溶胶、5份聚氧乙烯烷基醚、4份聚醚硅氧烷共聚物，混合均匀，得到耐高温转移镀铝水性聚氨酯乳液。
上述实施例1-5制备出的耐高温转移镀铝水性聚氨酯乳液，通过气相色谱法检测无疑似苯存在，使用安全、环保。将所述耐高温转移镀铝水性聚氨酯乳液对PET膜进行涂布，固化成膜后镀铝，与卡纸复合后PET膜剥离干净，镀铝层转移非常充分，当温度到达180℃时，铝层仍持久光亮、不氧化、不起皱，制备的耐高温转移镀铝水性聚氨酯乳液对铝层有极好的保护能力，而目前市面上现售的聚氨酯乳液，耐温一般在120℃以下。
本发明的内容不限于具体实施例所列举，本领域技术人员通过阅读本说明书而对本发明技术方案采取的任何等效的变换，均为本发明的权利要求所涵盖。

Claims (8)

1.一种耐高温转移镀铝水性聚氨酯乳液，其特征在于：包括以下重量份数的原料：
聚酯多元醇20-60份；
二异氰酸酯10-30份；
亲水扩链剂1-5份；
小分子醇类扩链剂1-3份；
中和剂0.2-2份；
胺类扩链剂0.5-5份；
水性硅溶胶30-55份；
润湿剂2-5份；
流平剂2-4份；
去离子水80-240份。
2.根据权利要求1所述的耐高温转移镀铝水性聚氨酯乳液，其特征在于：所述的聚酯多元醇为聚己二酸丁二醇酯多元醇、聚己内酯多元醇、聚碳酸酯多元醇、聚己二酸新戊二醇多元醇、聚丙烯酸酯多元醇中的一种或几种。
3.根据权利要求1所述的耐高温转移镀铝水性聚氨酯乳液，其特征在于：所述的二异氰酸酯为二环已基甲烷二异氰酸酯、异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、二环已基甲烷二异氰酸酯、1,4-环己烷二异氰酸酯、三甲基-1,6-六亚甲基二异氰酸酯或环己烷二亚甲基二异氰酸酯。
4.根据权利要求1所述的耐高温转移镀铝水性聚氨酯乳液，其特征在于：所述的亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸、乙二氨基磺酸钠、1,4-丁二醇-2-磺酸钠中的一种或几种；所述的小分子醇类扩链剂为乙二醇、1,4-丁二醇、丙二醇、新戊二醇或1,6-己二醇；所述的胺类扩链剂为乙二胺、异佛尔酮二胺或丙二胺。
5.根据权利要求1所述的耐高温转移镀铝水性聚氨酯乳液，其特征在于：所述水性硅溶胶的pH值为7.0-9.0。
6.根据权利要求1所述的耐高温转移水性聚氨酯乳液，其特征在于：所述的润湿剂为聚氧乙烯烷基醚；所述的流平剂为聚醚硅氧烷共聚物。
7.根据权利要求1所述的耐高温转移镀铝水性聚氨酯乳液，其特征在于：所述中和剂为三乙胺、N,N二甲基乙醇胺或三乙醇胺。
8.一种如权利要求1-7所述的耐高温转移镀铝水性聚氨酯乳液的制备方法，其特征在于：该方法包括以下步骤：
A．将聚酯多元醇在120℃下真空脱水1-2小时，降温至40℃，加入二异氰酸酯，搅拌，升温，控制反应温度为70-80℃，反应2-3小时；
B．加入亲水扩链剂，小分子醇类扩链剂，在70-80℃下继续反应1-2小时；
C．将步骤B得到的生成物降温至40℃，加入中和剂，中和反应1小时；
D．向上述步骤C得到的生成物中加入去离子水，在40℃下高速分散转相，乳化；
E．向步骤D得到的初乳液中加入胺类扩链剂，控制反应温度在40℃-50℃，进行扩链反应，反应0.5小时，得水性聚氨酯乳液；
F．向步骤E得到的乳液中加入水性硅溶胶、润湿剂、流平剂，即得耐高温转移镀铝水性聚氨酯乳液。
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