CN105732943A - 一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法 - Google Patents
一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法 Download PDFInfo
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Abstract
本发明涉及一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，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，获得高透明防指纹树脂。本发明制备的防指纹树脂可以直接涂覆于聚甲基丙烯酸甲酯材料表面，并可以被电子束固化，固化后形成的固化膜具有优良的防指纹性和高透明性。
Description
技术领域
本发明涉及一种高透明防指纹树脂的制备方法，特别涉及一种电子束固化聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，属于材料表面处理技术领域。
背景技术
聚甲基丙烯酯甲酯，俗称有机玻璃，有极好的透光性，可透过92%以上的太阳光，并且机械强度较高，有优良的耐热耐寒性，耐腐蚀，绝缘性能良好，尺寸稳定，易于成型，在车灯、仪表零件，光学镜片，装饰礼品、广告灯箱等领域具有广泛应用。但是聚甲基丙烯酸甲酯表面硬度不够，容易擦毛，另外，聚甲基丙烯酸甲酯表面容易沾染指纹、油污，影响视觉效果。
目前常用的聚甲基丙烯酯甲酯表面耐指纹处理技术是在聚甲基丙烯酯甲酯表面涂覆一层紫外光固化透明涂层，涂层内添加有含氟聚醚防污剂，具有一定的耐指纹效果，但这种外添加类型的含氟聚醚防污剂不耐磨损，随着磨损次数的增多，涂层表面的含氟聚醚防污剂会越来越少直至消失，最终失去耐指纹效果。另外，目前的紫外光固化涂层硬度不高，容易被硬物损坏。
本发明旨在解决上述问题，而提供一种高透明防指纹树脂，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聚甲基丙烯酯甲酯表面，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与透光性。
发明内容
本发明旨在提供一种高透明防指纹树脂的制备方法，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-酸-1H,1H,2H,2H-全氟-1-癸酯和1.1摩尔份的3-氯-1,2-丙二醇，以鼓泡的方式每分钟0.5升的流速通入氮气1小时，在氮气保护下，升高温度至60-70℃，并恒温在60-70℃机械搅拌反应24-36小时，停止反应，减压蒸馏除去过量的3-氯-1,2-丙二醇，进一步在80℃真空干燥24小时，得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯。
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和0.03-0.05摩尔份的辛酸亚锡和0.04-0.05摩尔份的苯醌，室温机械搅拌1小时，使原料充分混合，将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯加入上述混合物中，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55℃，并恒温在55℃机械搅拌反应24-30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500毫升丙酮和500毫升二氯甲烷和0.006-0.007摩尔份的辛酸亚锡和0.04-0.05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70℃，并恒温在70℃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，得高透明防指纹树脂产物。
进一步，所述的高透明防纹树脂的结构式为：
。
进一步，所述的高透明防指纹透明树脂可以通过刮涂、淋涂、喷涂等方式涂覆于聚甲基丙烯酸甲酯表面。
进一步，所述的涂覆在聚甲基丙烯酸甲酯表面的防指纹树脂的干厚，可以是10~100微米，优选20~50微米，更优选25~35微米。
本发明的优点是：本发明制备的防指纹树脂可以直接涂覆于聚甲基丙烯酸甲酯材料表面，并可以被电子束固化，固化后形成的固化膜具有优良的防指纹性和高透明性。
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-酸-1H,1H,2H,2H-全氟-1-癸酯和1.1摩尔份的3-氯-1,2-丙二醇，以鼓泡的方式每分钟0.5升的流速通入氮气1小时，在氮气保护下，升高温度至60-70℃，并恒温在60-70℃机械搅拌反应24小时，停止反应，减压蒸馏除去过量的3-氯-1,2-丙二醇，进一步在80℃真空干燥24小时，得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯。
向干燥的反应釜中，加入2.0摩尔份的异佛尔酮二异氰酸和0.03摩尔份的辛酸亚锡和0.04摩尔份的苯醌，室温机械搅拌1小时，使原料充分混合，将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯加入上述混合物中，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55℃，并恒温在55℃机械搅拌反应24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500毫升丙酮和500毫升二氯甲烷和0.006摩尔份的辛酸亚锡和0.04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70℃，并恒温在70℃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，得高透明防指纹树脂产物。
实施例2：
向干燥的反应釜内，加入1.0摩尔份1-甲基-1H-5-酸-1H,1H,2H,2H-全氟-1-癸酯和1.1摩尔份的3-氯-1,2-丙二醇，以鼓泡的方式每分钟0.5升的流速通入氮气1小时，在氮气保护下，升高温度至60-70℃，并恒温在60-70℃机械搅拌反应36小时，停止反应，减压蒸馏除去过量的3-氯-1,2-丙二醇，进一步在80℃真空干燥24小时，得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯。
向干燥的反应釜中，加入2.0摩尔份的异佛尔酮二异氰酸和0.05摩尔份的辛酸亚锡和0.05摩尔份的苯醌，室温机械搅拌1小时，使原料充分混合，将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯加入上述混合物中，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55℃，并恒温在55℃机械搅拌反应30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500毫升丙酮和500毫升二氯甲烷和0.007摩尔份的辛酸亚锡和0.05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70℃，并恒温在70℃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，得高透明防指纹树脂产物。
通过下面的试验测试本发明的防指纹树脂的性能。
试验实施例1：
将实施例1制备的防指纹树脂通过线棒涂布器刮涂于聚甲基丙烯酸甲酯板上，涂布厚度40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210-220千戈瑞，漆膜固化后，在电热鼓风干燥箱内25℃静置24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制备的防指纹树脂通过线棒涂布器刮涂于聚甲基丙烯酸甲酯板上，涂布厚度40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210-220千戈瑞，漆膜固化后，在电热鼓风干燥箱内25℃静置24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耐指纹膜表面的接触角，即滴即测。
附着力的测试方法：按照《GB/T1720-79(89)》测试。
铅笔硬度的测试方法：按照《GB1720-89》测试。
反射率的测试方法：采用LCD-5200光电特性测试仪，扫描380-780纳米波段，按照GBT2680-1994公开的太阳光各波段分布特性，计算样品对可见光的反射率。
透光率的测试方法：使用日本岛津公司UV3100型分光光度计测试从聚甲基丙烯酸甲酯上剥离的透明膜的透光率。
雾度的测试方法：使用日本电色NDH2000N雾度计测试。
表1电子束固化后耐指纹膜的性能
| 测试项目 | 实施例1 | 实施例2 |
| 接触角 | 73.1o | 73.5o |
| 铅笔硬度 | 5H | 5H |
| 附着力(级) | 1 | 1 |
| 反射率 | 2.2 | 2.1 |
| 雾度(%) | 0.9 | 1.0 |
| 透光率(%) | 92.3 | 92.5 |
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 (4)
1.一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，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-酸-1H,1H,2H,2H-全氟-1-癸酯和1.1摩尔份的3-氯-1,2-丙二醇，以鼓泡的方式每分钟0.5升的流速通入氮气1小时，在氮气保护下，升高温度至60-70℃，并恒温在60-70℃机械搅拌反应24-36小时，停止反应，减压蒸馏除去过量的3-氯-1,2-丙二醇，进一步在80℃真空干燥24小时，得含氟小分子扩链剂1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯；
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和0.03-0.05摩尔份的辛酸亚锡和0.04-0.05摩尔份的苯醌，室温机械搅拌1小时，使原料充分混合，将1.0摩尔份的1-甲基-3-(1,2-丙二醇)-5-酸-1H,1H,2H,2H-全氟-1-癸酯加入上述混合物中，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55℃，并恒温在55℃机械搅拌反应24-30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500毫升丙酮和500毫升二氯甲烷和0.006-0.007摩尔份的辛酸亚锡和0.04-0.05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70℃，并恒温在70℃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，得高透明防指纹树脂产物。
2.根据权利要求1所述的一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，其特征在于：所述的高透明防纹树脂的结构式为：
。
3.根据权利要求1所述的一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，其特征在于：所述的高透明防指纹透明树脂可以通过刮涂、淋涂、喷涂方式涂覆于聚甲基丙烯酸甲酯表面。
4.根据权利要求1所述的一种聚甲基丙烯酸甲酯用高透明防指纹树脂的制备方法，其特征在于：所述的涂覆在聚甲基丙烯酸甲酯表面的防指纹树脂的干厚或是10~100微米，优选20~50微米，更优选25~35微米。
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