CN110591547A - 一种阻燃隔热水性聚酰亚胺涂料及其应用 - Google Patents
一种阻燃隔热水性聚酰亚胺涂料及其应用 Download PDFInfo
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- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
本发明提供了一种阻燃隔热水性聚酰亚胺涂料及其制备和应用方法，由按照质量份数计的如下组分制备而成：阻燃剂6‑25重量份，改性剂6‑30重量份，二酸20‑80重量份，二胺25‑85重量份，中和剂5‑15重量份，溶剂10‑100重量份，助剂2‑16重量份，颜料1‑17重量份，具备优良的耐热、耐有机溶剂、耐酸、耐碱，而且具备阻燃性能的同时，还具备较高的剥离强度和断裂伸长率。具有较好的使用价值，且不含有机溶剂，符合当今社会绿色环保的理念。
Description
本发明涉及一种阻燃隔热水性聚酰亚胺涂料及其制备方法，属于涂料技术领域。
背景技术
随着人们安全和环保意识的加强，水性涂料的研究得以迅速发展，水性涂料是指将树脂溶于水或分散于水中而形成的涂料，与溶剂型相比具有无溶剂、无污染、成膜性好、和其他聚合物尤其是乳液型聚合物易掺混有利于改性等优点。90年代后已逐渐在外墙外墙、建筑内墙、地面建筑、顶棚、屋面防水、器件保护、作画颜料和服装染色等方面得以应用，但是还存在许多缺点，需要通过各种改性，完善其功能。现代的涂料正在逐步成为一类多功能性的工程材料，是化学工业中的一个重要行业，但是还存在许多缺点，需要通过各种改性，完善其功能。
发明内容
发明目的：针对现有技术在的缺陷、本发明的目的是提供一种阻燃隔热水性聚酰亚胺涂料及制备方法，所述涂料具有较好的化学耐心、力学性能、阻燃性能和隔热性能，具有较好的使用价值。
技术方案：为实现上述目的，本发明通过下述技术方案实现：阻燃剂6-23重量份，改性剂8-25重量份，二酸32-70重量份，二胺35-75重量份，有机胺中和剂6-13重量份，溶剂15-90重量份，助剂3-14重量份，颜料3-14重量份。
上述阻燃隔热水性聚酰亚胺涂料的制备方法，包括以下步骤：
在干燥氮气的保护下,将改性剂和阻燃填料按计量加入四口瓶烧瓶中,混合均匀后常温反应3h,得到组分A。
以二胺和二酐在搅拌下加热，当温度达到100℃左右，开始析出水，同时反应系统逐渐变为深褐色的均匀溶液。继续加热，反应系统温度逐步上升，粘度亦同时增加。约经一小时后温度达到130℃，水继续析出，至反应物残余酸值比为22％即为反应终点。冷却至80-110℃时加入中和剂，便形成聚酰胺酸的铵盐。待形成铵盐后，将剩余的氨蒸出，便可获得几乎没有氨味的水性聚酰亚胺。最后，加入组分A、助剂、颜料，并充分搅拌混合。
所述涂料的各方面性能：
| 性能 | 数值 | 单位 |
| 氧指数 | 30 | ％ |
| 粘度 | 5608 | mPa·s |
| 剥离强度 | 0.780 | N/mm |
| 拉伸剪切强度 | 21.1 | MPa |
| 软化点 | 98±3 | ℃ |
| 拉伸模量 | 4.0 | GPa |
本发明所述的阻燃隔热水性聚酰亚胺涂料具有较好的强度、阻燃性能和优异的隔热性能，可以广泛应用在工业领域。
具体实施方法
以下通过具体实施方式的描述对本发明作进一步说明，但这并非是对本发明的限制，本领域技术人员根据本发明的基本思想，可以做出各种修改或改进，但是只要不脱离本发明的基本思想，均在本发明的范围之内。
实施案例一：
在干燥氮气的保护下,将分散剂和卤素阻燃剂填料按计量加入四口瓶烧瓶中,混合均匀后常温反应3h,得到组分A。
1克分子的双核偏苯三甲酸二酐和1克分子4、4’-二氨基二苯甲烷在400克乙二醇中于120℃下加热45分钟，然后加入100克二乙醇胺、280克水，搅拌后得到聚合物溶液。此溶液涂于铜线上烘烤后便可得到具有优良柔曲性能的聚酰亚胺绝缘涂层。最后，加入流平剂、铬黄粉，并充分搅拌混合。
所述涂料的各方面性能：
| 性能 | 数值 | 单位 |
| 氧指数 | 29 | ％ |
| 粘度 | 5608 | mPa·s |
| 剥离强度 | 0.780 | N/mm |
| 拉伸剪切强度 | 21.1 | MPa |
| 软化点 | 98±3 | ℃ |
| 拉伸模量 | 4.0 | GPa |
实施案例二：在干燥氮气的保护下,将偶联剂和磷系阻燃剂填料按计量加入四口瓶烧瓶中,混合均匀后常温反应3h,得到组分A。
将均苯四甲酸二酐(PMDA，22.6g，0.10mol)通过在脱气蒸馏水(250cm3)中回流1小时，完全水解为四羧酸。4、4’-二氨基二苯醚(4、4’-ODA，21.13g，0.105mol)加入溶液中，在回流温度下剧烈搅拌超过五分钟，然后边搅拌边冷却至室温。一种细白色固体从溶液中析出，在进过数个循环的抽空和冲洗后，将正压约为20psi的氮气充入容器中。合成的混合物被定量地转移到帕尔压力容器的玻璃衬里。反应混合物加热到135℃，并搅拌1小时。温度升高到180℃，并保持2小时，之后边搅拌边冷却到室温。淡橙色的固体被从反应容器中移出来，经过过滤和用水冲洗之后，再研磨成粉末。继续使用热水(100cm3)，甲醇(100cm3)，丙酮(100cm3)，清洗，最后用二氯甲烷(100cm3)清洗。将产品在约50℃的真空烘箱中干燥过夜并收集到浅橙色粉末(35.0g，87.5％)。最后，加入消泡剂、钛白粉，并充分搅拌混合。
所述涂料的各方面性能：
实施案例三：
在干燥氮气的保护下,将偶联剂和氮系阻燃剂填料按计量加入四口瓶烧瓶中,混合均匀后常温反应3h,得到组分A。
以ODA和PMDA在搅拌下加热，当温度达到100℃左右，开始析出水，同时反应系统逐渐变为深褐色的均匀溶液。继续加热，反应系统温度逐步上升，粘度亦同时增加。约经一小时后温度达到130℃，水继续析出，至反应物残余酸值比为22％即为反应终点。冷却至80-110℃时加入氨水溶液，便形成聚酰胺酸的铵盐。待形成铵盐后，将剩余的氨蒸出，便可获得几乎没有氨味的水性聚酰亚胺。最后，加入消泡剂、钛白粉，并充分搅拌混合。
所述涂料的各方面性能：
| 性能 | 数值 | 单位 |
| 氧指数 | 29 | ％ |
| 粘度 | 5608 | mPa·s |
| 剥离强度 | 0.780 | N/mm |
| 拉伸剪切强度 | 21.1 | MPa |
| 软化点 | 98±3 | ℃ |
| 拉伸模量 | 4.0 | GPa |
Claims (9)
1.一种阻燃隔热水性聚酰亚胺涂料，其特征在于，其原料组分包括：
阻燃剂6-25重量份，改性剂6-30重量份，二酸20-80重量份，二胺25-85重量份，中和剂5-15重量份，溶剂10-100重量份，助剂2-16重量份，颜料1-17重量份。
2.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，其原料组分包括：
阻燃剂6-23重量份，改性剂8-25重量份，二酸32-70重量份，二胺35-75重量份，有机胺中和剂6-13重量份，溶剂15-90重量份，助剂3-14重量份，颜料3-14重量份。
3.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述阻燃剂为卤素阻燃剂、磷系阻燃剂、氮系阻燃剂、无机阻燃剂中的一种或者多种混合。
4.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述颜料为着色颜料或者体质颜料中的一种或者多种混合；
优选的，所述着色颜料选自钛白粉、铬黄中的一种或者多种混合；
优选的，所述体质颜料选自碳酸钙、滑石粉中的一种或者多种混合。
5.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述二胺为ODA、MPD、BAPP、HDA、DDS、间苯二胺、邻苯二胺、中的一种或者多种混合，且不局限于这几种二胺。
6.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述二酐为PMDA、BPDA、BTDA、ODPA、TDPA、HQDPA中的一种或者多种混合，且不局限于这几种二酐。
7.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述中和剂为三乙醇胺、二乙醇胺、乙二胺、三乙胺、二乙胺、乙醇胺、氨水、二甲基乙醇胺、吡啶中的一种或者多种混合，且不局限于这几种中和剂。
8.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述助剂为优化助剂或者加工助剂中的一种或者多种混合；
优选的，所述优化助剂选自偶联剂、分散剂、抗氧化剂、紫外线吸收剂中的一种或者多种混合；
优选的，所述加工助剂选自消泡剂、流平剂、底材润湿剂中的一种或者多种混合。
9.如权利要求1所述的一种阻燃隔热水性聚酰亚胺涂料，其特征在于，所述改性剂为偶联剂、分散剂、抗氧化剂、紫外线吸收剂中的一种或者多种混合。
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