CN105860016B - 一种环保防指纹聚氨酯树脂的制备方法 - Google Patents

一种环保防指纹聚氨酯树脂的制备方法 Download PDF

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CN105860016B
CN105860016B CN201610300315.7A CN201610300315A CN105860016B CN 105860016 B CN105860016 B CN 105860016B CN 201610300315 A CN201610300315 A CN 201610300315A CN 105860016 B CN105860016 B CN 105860016B
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徐海涛
汪超
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Nanchang Hangkong University
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Abstract

本发明涉及一种环保防指纹聚氨酯树脂的制备方法，所述的制备方法包括：1）含氟小分子扩链剂与异氰酸酯反应，制备端基为‑NCO的聚氨酯预聚体。2）使用季戊四醇三丙烯酸酯封端聚氨酯预聚体，获得环保防指纹树脂。本发明制备的环保耐指纹树脂可以直接涂覆于金属基材表面，不需要额外添加任何的有机溶剂或者有机稀释剂，绿色环保，可以实现零有机污染物排放，本发明制备的防指纹聚氨酯树脂可以被电子束固化成膜，固化后形成的固化膜具有优良的耐指纹性。

Description

一种环保防指纹聚氨酯树脂的制备方法
技术领域
本发明涉及一种防指纹聚氨酯树脂的制备方法，特别涉及一种环保防指纹聚氨酯树脂的制备方法，属于金属表面处理技术领域。
背景技术
金属材料，比如冷轧钢板、不锈钢板、铝合金等，在生活中的应用越来越广泛。在一些领域，如家具包边、家电外壳、电子产品外壳等，需要金属材料表面具备防指纹性能。
目前通用的金属表面防指纹处理技术是在其表面涂覆一层六价铬防指纹漆膜，但随着环保要求的提高，尤其是RoHs指令的提出，六价铬酸盐漆膜将逐渐被淘汰，由于六价铬潜在的致癌性。
本发明旨在解决上述问题，而提供一种环保的防指纹树脂，并提供制备方法。由本发明制备得到的防指纹树脂可直接涂覆于金属基材表面，不需要额外添加任何的有机溶剂或者有机稀释剂，绿色环保，并可以通过电子束固化，固化后形成的漆膜具有优良的防指纹性。
发明内容
本发明旨在提供一种金属基材表面用环保防指纹聚安酯树脂的制备方法，该方法的特征是：
1）向干燥的反应釜内，加入1.0摩尔份1-甲基-1H-5-((3, 3, 4, 4, 5, 5, 6, 6,7, 7, 8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑和1.05摩尔份2-溴-2-硝基-1, 3-丙二醇和400毫升乙酸乙酯和100毫升二甲苯，室温搅拌1小时，使原料混合，升高温度至70℃，并恒温在70℃搅拌反应24-36小时，停止反应，降至室温，过滤除去固体，取滤液，静置2小时，分液，除去有机相，粗产物进一步在80 ℃真空干燥24小时，得小分子扩链剂1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9, 9, 10,10, 10-十七氟癸基)甲酯基)-咪唑溴盐；
2）向干燥的反应釜中，加入2.0 摩尔份的异佛尔酮二异氰酸酯和0.04-0.05摩尔份的二丁基二氯化锡和0.02-0.03摩尔份的对苯二酚，25℃机械搅拌1小时，使原料充分混合，将1.0 摩尔份的1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7,7, 8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑溴盐加入上述混合物中，控制加料速度，控制反应釜内温度在45-50℃，加料完毕后，升高温度至60℃，并恒温在60℃机械搅拌反应8-10小时，停止反应，得聚氨酯预聚体；
3）向干燥的反应釜中，加入1.0 摩尔份的聚氨酯预聚体和300毫升丙酮和100毫升的二氯甲烷和0.001-0.002摩尔份的辛酸亚锡和0.01-0.02摩尔份的对苯二酚，升高温度至45-50℃，机械搅拌1小时，用恒压滴液漏斗向反应釜内滴加2.0 摩尔份的季戊四醇三丙烯酸酯，控制滴加速度，控制反应釜内温度在45-55℃，滴加完毕后，升高温度至75℃，并恒温在75℃机械搅拌反应24-36小时，停止反应，减压蒸馏除去丙酮和二氯甲烷，得环保防指纹聚氨酯树脂产物。
进一步，所述的环保防指纹聚氨酯树脂的结构式为：
Figure 334541DEST_PATH_IMAGE001
进一步，所述的环保防指纹聚氨酯树脂可以通过刮涂、淋涂、喷涂等方式涂覆于金属基材表面。
进一步，所述的涂覆在金属基材表面的环保防指纹聚氨酯树脂的干厚，可以是10~100微米，优选20~50微米，更优选30~34微米。
本发明的优点：本发明制备的环保耐指纹树脂可以直接涂覆于金属基材表面，不需要额外添加任何的有机溶剂或者有机稀释剂，绿色环保，可以实现零有机污染物排放，本发明制备的防指纹聚氨酯树脂可以被电子束固化成膜，固化后形成的固化膜具有优良的耐指纹性。
具体实施方式
以下对本发明的原理和特征进行描述，所举实施例只用于解释本发明，并非用于限定本发明的范围。
实施例1：
向干燥的反应釜内，加入1.0摩尔份1-甲基-1H-5-((3, 3, 4, 4, 5, 5, 6, 6,7, 7, 8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑和1.05摩尔份2-溴-2-硝基-1, 3-丙二醇和400毫升乙酸乙酯和100毫升二甲苯，室温搅拌1小时，使原料混合，升高温度至70℃，并恒温在70℃搅拌反应24小时，停止反应，降至室温，过滤除去固体，取滤液，静置2小时，分液，除去有机相，粗产物进一步在80 ℃真空干燥24小时，得小分子扩链剂1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9, 9, 10, 10,10-十七氟癸基)甲酯基)-咪唑溴盐；
向干燥的反应釜中，加入2.0 摩尔份的异佛尔酮二异氰酸酯和0.04摩尔份的二丁基二氯化锡和0.02摩尔份的对苯二酚，25℃机械搅拌1小时，使原料充分混合，将1.0 摩尔份的1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9,9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑溴盐加入上述混合物中，控制加料速度，控制反应釜内温度在45℃，加料完毕后，升高温度至60℃，并恒温在60℃机械搅拌反应8小时，停止反应，得聚氨酯预聚体；
向干燥的反应釜中，加入1.0 摩尔份的聚氨酯预聚体和300毫升丙酮和100毫升的二氯甲烷和0.001摩尔份的辛酸亚锡和0.01摩尔份的对苯二酚，升高温度至45℃，机械搅拌1小时，用恒压滴液漏斗向反应釜内滴加2.0 摩尔份的季戊四醇三丙烯酸酯，控制滴加速度，控制反应釜内温度在45℃，滴加完毕后，升高温度至75℃，并恒温在75℃机械搅拌反应24小时，停止反应，减压蒸馏除去丙酮和二氯甲烷，得环保防指纹聚氨酯树脂产物。
实施例2：
向干燥的反应釜内，加入1.0摩尔份1-甲基-1H-5-((3, 3, 4, 4, 5, 5, 6, 6,7, 7, 8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑和1.05摩尔份2-溴-2-硝基-1, 3-丙二醇和400毫升乙酸乙酯和100毫升二甲苯，室温搅拌1小时，使原料混合，升高温度至70℃，并恒温在70℃搅拌反应36小时，停止反应，降至室温，过滤除去固体，取滤液，静置2小时，分液，除去有机相，粗产物进一步在80 ℃真空干燥24小时，得小分子扩链剂1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9, 9, 10, 10,10-十七氟癸基)甲酯基)-咪唑溴盐；
向干燥的反应釜中，加入2.0 摩尔份的异佛尔酮二异氰酸酯和0.05摩尔份的二丁基二氯化锡和0.03摩尔份的对苯二酚，25℃机械搅拌1小时，使原料充分混合，将1.0 摩尔份的1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9,9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑溴盐加入上述混合物中，控制加料速度，控制反应釜内温度在50℃，加料完毕后，升高温度至60℃，并恒温在60℃机械搅拌反应10小时，停止反应，得聚氨酯预聚体；
向干燥的反应釜中，加入1.0 摩尔份的聚氨酯预聚体和300毫升丙酮和100毫升的二氯甲烷和0.002摩尔份的辛酸亚锡和0.02摩尔份的对苯二酚，升高温度至50℃，机械搅拌1小时，用恒压滴液漏斗向反应釜内滴加2.0 摩尔份的季戊四醇三丙烯酸酯，控制滴加速度，控制反应釜内温度在55℃，滴加完毕后，升高温度至75℃，并恒温在75℃机械搅拌反应36小时，停止反应，减压蒸馏除去丙酮和二氯甲烷，得环保防指纹聚氨酯树脂产物。
通过下面的试验测试本发明的环保防指纹聚氨酯树脂的性能。
试验实施例1：
将实施例1制备的环保防指纹树脂通过线棒涂布器刮涂于不锈钢板上，涂布厚度35微米，使用电子束固化仪在空气气氛进行固化，电子束辐射剂量为200-220千戈瑞，漆膜固化后，在电热鼓风干燥箱内25℃静置2小时后，测试其性能，性能测试结果如表1。
试验实施例2：
将实施例2制备的环保防指纹树脂通过线棒涂布器刮涂于不锈钢板上，涂布厚度35微米，使用电子束固化仪在空气气氛进行固化，电子束辐射剂量为200-220千戈瑞，漆膜固化后，在电热鼓风干燥箱内25℃静置2小时后，测试其性能，性能测试结果如表1。
接触角的测试方法：使用日本岛津PCL-2接触角仪测试十六烷在防指纹漆膜表面的接触角，即滴即测。
铅笔硬度的测试方法：按照《GB1720-89》测试。
附着力的测试方法：按照《GB/T1720-79(89)》测试。
表1 电子束固化后防指纹漆膜的性能
测试项目 实施例1 实施例2
接触角 72.6<sup>o</sup> 72.3<sup> o</sup>
铅笔硬度 4H 4H
附着力(级) 2 2
以上所述仅为本发明的部分实施例，并不用以限制本发明。

Claims (1)

1.一种环保防指纹聚氨酯树脂的制备方法，其特征在于，所述的制备方法包括：
1）向干燥的反应釜内，加入1.0摩尔份1-甲基-1H-5-((3, 3, 4, 4, 5, 5, 6, 6, 7,7, 8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑和1.05摩尔份2-溴-2-硝基-1,3-丙二醇和400毫升乙酸乙酯和100毫升二甲苯，室温搅拌1小时，使原料混合，升高温度至70℃，并恒温在70℃搅拌反应24-36小时，停止反应，降至室温，过滤除去固体，取滤液，静置2小时，分液，除去有机相，粗产物进一步在80 ℃真空干燥24小时，得小分子扩链剂1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7, 8, 8, 9, 9, 10, 10,10-十七氟癸基)甲酯基)-咪唑溴盐；
2）向干燥的反应釜中，加入2.0 摩尔份的异佛尔酮二异氰酸酯和0.04-0.05摩尔份的二丁基二氯化锡和0.02-0.03摩尔份的对苯二酚，25℃机械搅拌1小时，使原料充分混合，将1.0 摩尔份的1-甲基-3-(2-硝基-1, 3-丙二醇)-5-((3, 3, 4, 4, 5, 5, 6, 6, 7, 7,8, 8, 9, 9, 10, 10, 10-十七氟癸基)甲酯基)-咪唑溴盐加入上述混合物中，控制加料速度，控制反应釜内温度在45-50℃，加料完毕后，升高温度至60℃，并恒温在60℃机械搅拌反应8-10小时，停止反应，得聚氨酯预聚体；
3）向干燥的反应釜中，加入1.0 摩尔份的聚氨酯预聚体和300毫升丙酮和100毫升的二氯甲烷和0.001-0.002摩尔份的辛酸亚锡和0.01-0.02摩尔份的对苯二酚，升高温度至45-50℃，机械搅拌1小时，用恒压滴液漏斗向反应釜内滴加2.0 摩尔份的季戊四醇三丙烯酸酯，控制滴加速度，控制反应釜内温度在45-55℃，滴加完毕后，升高温度至75℃，并恒温在75℃机械搅拌反应24-36小时，停止反应，减压蒸馏除去丙酮和二氯甲烷，得环保防指纹聚氨酯树脂产物。
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