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答辩人： 茹 捷 指导教师： 曾汉民 教授

半互穿网络膜耐溶剂性能研究. 答辩人： 茹 捷 指导教师： 曾汉民 教授. 一、前言. 互穿网络聚合物（ IPN ） 半互穿网络聚合物（ semi-IPN ）. 1.1 研究背景和意义. 手机外壳表面涂料 —— 光油，主要成分为聚丙烯酸酯类（ PA ）线型高聚物 市售工业品一般具有良好透明度和光泽度，但耐溶剂性和耐磨性差 研制和开发一种既保持良好外观又耐溶剂耐磨的手机光油具有重要现实意义. 1.2 实验思路和方案. 互穿网络聚合物在溶剂中溶胀但不溶解

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答辩人： 茹 捷 指导教师： 曾汉民 教授

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  1. 半互穿网络膜耐溶剂性能研究 答辩人： 茹 捷 指导教师： 曾汉民 教授

  2. 一、前言 • 互穿网络聚合物（IPN） • 半互穿网络聚合物（semi-IPN）

  3. 1.1研究背景和意义 • 手机外壳表面涂料——光油，主要成分为聚丙烯酸酯类（PA）线型高聚物 市售工业品一般具有良好透明度和光泽度，但耐溶剂性和耐磨性差 • 研制和开发一种既保持良好外观又耐溶剂耐磨的手机光油具有重要现实意义

  4. 1.2实验思路和方案 • 互穿网络聚合物在溶剂中溶胀但不溶解 • 以手机光油（PA）为基，加入交联单体二丙烯酸正己酯（HDDA）和热引发剂BPO进行热引发聚合形成PA/PHDDA半-IPN——提高耐溶剂性 • 在PA/PHDDA半-IPN基础上添加改性纳米粒子CaCO3/SiO2/KH-570形成PA/PHDDA/纳米粒子 半-IPN——提高耐磨性 • KH-570——甲基丙烯酰氧基丙基三甲氧基硅烷

  5. 二、实验部分 • 膜的制备 纯PA膜 1. 非IPN膜 PA/纳米粒子膜 PA/PHDDA半-IPN膜 2.半-IPN膜 PA/PHDDA/纳米粒子 半-IPN膜

  6. 简单工艺流程 原位聚合法制备PA/PHDDA/纳米粒子 半-IPN膜 搅拌15min纳米粒子 光油＋HDDA＋635溶剂 超声 BPO N2 75℃搅拌 60℃ 30min 成膜 涂膜 原位聚合

  7. 性能测试 失重法 耐溶剂性 扫描电镜 透光率 光学性能 光泽度 耐热性能 热重分析

  8. 三、结果与讨论 性能分析 • 纯PA膜 • PA/纳米粒子膜 • PA/PHDDA半-IPN膜 • PA/PHDDA/纳米粒子 半-IPN膜

  9. 3.1纯PA膜 • 耐溶剂性能 Figure 1. Ethanol resistance of Figure 2. Acetone resistance of pure PA films pure PA films

  10. SEM (a) pure PA film (b) after being washed by ethanol (c) after being washed by acetone (c) Figure 3. SEM images of pure PA film before and after being washed by ethanol and acetone (a)

  11. 3.2 PA/纳米粒子膜 • 耐溶剂性能 Figure 4. Ethanol resistance of Figure 5. Acetone resistance of PA/nanoparticle films PA/nanoparticle films

  12. SEM (a) (b) (a) PA/nanoparticle film (b) after being washed by ethanol Figure 6-1. SEM images of PA/nanoparticle film before and after being washed by ethanol

  13. (c)×3,300 (d)×10,000 Figure 6-2. SEM images of PA/nanoparticle film after being washed by acetone

  14. 光学性能 Table 1. Optical properties of pure PA films and PA/nanoparticle films 考虑涂膜工艺的影响，我们认为：透光率>75％，光泽度>70％即基本符合应用要求标准。

  15. 3.3 PA/PHDDA 半-IPN膜 • 耐溶剂性 Figure 7. Ethanol resistance of Figure 8. Ethanol resistance of PA/PHDDA semi-IPN films PA/PHDDA semi-IPN films Note: BPO/HDDA=0.1% (mass%) Note: BPO/HDDA=1% (mass%)

  16. Figure 9. Acetone resistance of PA/PHDDA semi-IPN films Note: BPO/HDDA=0.1%(mass%)

  17. SEM (b) (a) (a) PA/PHDDA semi-IPN film (c) (b) after being washed by ethanol (c) after being washed by acetone Figure 10. SEM images of PA/PHDDA semi-IPN film before and after being washed by ethanol and acetone

  18. Table 2. Optical properties of pure PA films and PA/PHDDA semi-IPN films • 光学性能

  19. 3.4 PA/PHDDA/纳米粒子 半-IPN膜 • 耐溶剂性 Figure 11. Ethanol resistance of PA/PHDDA/nanoparticle semi-IPN films Note：BPO/HDDA=1.0%(mass%)

  20. SEM (a)×3,300 (b)×50,000 Figure 12-1. SEM images of PA/PHDDA/nanoparticle semi-IPN film before being washed

  21. (c) (d) ×3,300 (c) PA/PHDDA/nanoparticle semi-IPN film after being washed by ethanol (d) after being washed by acetone (e) after being washed by acetone (e) ×10,000 Figure 12-2. SEM images of PA/PHDDA/ nanoparticle semi-IPN film after being washed by ethanol and acetone

  22. Table 3. Optical properties of pure PA films and PA/PHDDA/nanoparticle semi-IPN films • 光学性能

  23. 3.5 耐热性能 • 热重分析 1.pure PA film 2.PA/PHDDA semi-IPN film 3.PA/PHDDA/nanoparticle semi-IPN film Figure 15. DTG curves of different types of films Figure 14. TG curves of different types of films

  24. 四、结论 • 耐溶剂性 半-IPN膜提高了光油的耐溶剂性。 同等条件下增加交联单体含量即增加了单位体积的有效网络数目或者同等条件下增加引发剂含量即增加了网络交联密度，膜的耐溶剂性提高。 • 光学性能 与纯PA膜相比，PA/PHDDA半-IPN膜和PA/PHDDA/纳米粒子 半-IPN膜无论透光率或是光泽度都有所下降。 但完全可以做到符合我们认为的应用要求标准（透光率>75％，光泽度>70％），因此可认为半-IPN膜基本能保持膜的光泽度和透明度。 • 耐热性能 通过热重分析可以看出：纯PA膜与PA/PHDDA 半-IPN膜相比耐热性能相差不大；而PA/PHDDA/纳米粒子 半-IPN膜相比前两者，耐热性能明显改善，表明无机纳米粒子的引入可提高膜的耐热性能。

  25. 致谢 本工作是在曾汉民教授的悉心指导下完成的。在此谨向曾老师致以崇高的敬意和衷心的感谢。 刘国军博士在整个论文研究和写作中给予了具体指导和诸多帮助，在此深表感谢！ 衷心感谢材料所全体老师和同学的帮助和鼓励。 衷心感谢化工学院综合化学实验创新基金的资助。

  26. 敬 请 批 评 指 正 谢 谢！

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