CN112940630A - 一种自修复温敏变色窗贴及其制备方法 - Google Patents

一种自修复温敏变色窗贴及其制备方法 Download PDF

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CN112940630A
CN112940630A CN202110140033.6A CN202110140033A CN112940630A CN 112940630 A CN112940630 A CN 112940630A CN 202110140033 A CN202110140033 A CN 202110140033A CN 112940630 A CN112940630 A CN 112940630A
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吴文璐
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Abstract

本发明公开了一种自修复温敏变色窗贴，所述温敏变色窗贴原料包括聚己二酸丁二醇酯、异佛尔酮二异氰酸酯、二月桂酸二丁基锡、4,4'二氨基二苯二硫醚、硼酸、热致变色材料。本发明还公开了上述自修复温敏变色窗贴的制备方法，该方法制备得到的窗贴具有很好的自修复能力，在窗贴制作过程中加入的热致变色材料能降低室温下红外光的透过率，降低了室内和室外的热交换，从而达到了减小能耗的目的。

Description

一种自修复温敏变色窗贴及其制备方法
技术领域
本发明涉及窗贴技术领域，具体涉及一种自修复温敏变色窗贴。
背景技术
近年来，我国的城市化进程和城镇建设不断加快，从而使得建筑能耗增长迅速，随之而来的能源需求问题开始逐渐给我们带来困扰。据统计，中国的建筑能耗占全社会能源消耗的40％，在全世界都面临能源紧缺的大环境下，建筑节能具有重大意义。因此，我们需要提出更加合理且有效的设计方案，达到减少建筑能耗的目的。
住宅的室内和室外作为发生大量热交换的场景，玻璃是最常见的热交换介质，为了兼顾住宅节能和舒适性，热致变色材料受到关注。热致变色材料是指可通过温度控制例如光透射性这样的光学特性的材料。在建筑物的窗玻璃中应用热致变色材料时，在夏天可反射红外线而将热阻断，在冬天可使红外线透射而利用热。
发明内容
为了减少建筑能耗，减少室内和室外的热交换，本发明提供了一种自修复温敏变色窗贴。
具体是通过以下技术方案实现：
一种自修复温敏变色窗贴，原料以重量份为：20-30份聚己二酸丁二醇酯、5-10份异佛尔酮二异氰酸酯、0.5-1份二月桂酸二丁基锡、0.5-1.5份4,4'二氨基二苯二硫醚、0.2-1份硼酸、2-5份热致变色材料。
所述热致变色材料为W-Eu双掺杂VO2纳米粉体。
所述热致变色材料的制备过程为：将钨酸(H2WO4)和硝酸铕(Eu(NO3)3)加入到稍过量的双氧水中超声分散10min作为A液待用。取V2O5和CH3COOH超声分散于70ml去离子水，再加入3ml浓盐酸作为B液。将B液快速倒入A液中并于80℃水浴下搅拌60min，随后将混合溶液移入聚四氟乙烯反应釜中水热反应4h，反应温度为200℃。待反应完成冷却至室温后将产物取出，经过去离子水和无水乙醇数次洗涤、离心后收集后，在80℃烘箱中干燥8h。最后将干燥好的产物在氩气保护下进行高温退火处理，得到W-Eu双掺杂VO2纳米粉体。
进一步的，钨酸和硝酸铕的配料比为0.5-2.5mmol:0.5-2.5mmol。
进一步的，V2O5和CH3COOH的配料比为0.4-0.6g:0.5-0.7g。
进一步的，高温退火处理条件为：退火温度450℃-550℃，升温速率5℃/min，退火时间4h。
本发明还提供了一种自修复温敏变色窗贴的制备方法，包括以下步骤：
(1)取聚己二酸丁二醇酯置于密炼机中，在真空环境下110℃熔融搅拌2h，搅拌完成后保持真空停止加热并将温度降至80℃，通入干燥的N2，依次加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡和热致变色材料，继续搅拌反应3h，制得聚氨酯预聚物。
(2)恒定温度80℃在N2保护下向聚氨酯预聚物中加入扩链剂4,4'二氨基二苯二硫醚搅拌至混合均匀搅拌扩链2h，停止加热加入扩链剂硼酸溶搅拌10min，混合均匀后，将反应液倒入聚四氟乙烯模具中真空排气泡约30min，于80℃固化10h，得到聚氨酯弹性体。
(3)将所得聚氨酯弹性体用于压延机，制得自修复温敏变色膜。再将温敏变色膜、PET离型膜、聚丙烯酸压敏胶用于涂布机制得自修复温敏变色窗贴。
本发明的有益效果为：
1.本发明选择聚氨酯为窗贴基体材料，通过在主链中引入芳香族二硫键提高链段运动能力，同时利用硼酸构建的硼酸酯键形成可逆交联网络，最终制备了一种兼具高强高韧、高修复效率、温和修复条件及多通道修复特性的基于多重可逆作用的自修复聚氨酯弹性体，大大提高了材料的韧性。
2.在聚氨酯基体中加入了W-Eu双掺杂VO2纳米粉体，与单一元素掺杂的VO2相比，双金属掺杂VO2的相变温度大幅度降低，同时还能保持对红外透过的高效的调节能力。减小了室温下红外光的透过率，降低了室内和室外的热交换，从而达到了减小能耗的目的。
具体实施方式
下面结合实施例对本发明做进一步的阐述。
实施例1：
一种自修复温敏变色窗贴，原料以重量份为：25份聚己二酸丁二醇酯、8份异佛尔酮二异氰酸酯、0.6份二月桂酸二丁基锡、1份4,4'二氨基二苯二硫醚、0.5份硼酸、3份热致变色材料。
其制备方法包括如下步骤：
(1)取聚己二酸丁二醇酯置于密炼机中，在真空环境下110℃熔融搅拌2h，搅拌完成后保持真空停止加热并将温度降至80℃，通入干燥的N2，依次加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡和热致变色材料，继续搅拌反应3h，制得聚氨酯预聚物。
(2)恒定温度80℃在N2保护下向聚氨酯预聚物中加入扩链剂4,4'二氨基二苯二硫醚搅拌至混合均匀搅拌扩链2h，停止加热加入扩链剂硼酸溶搅拌10min，混合均匀后，将反应液倒入聚四氟乙烯模具中真空排气泡约30min，于80℃固化10h，得到聚氨酯弹性体。
(3)将所得聚氨酯弹性体用于压延机，制得自修复温敏变色膜。再将温敏变色膜、PET离型膜、聚丙烯酸压敏胶用于涂布机制得自修复温敏变色窗贴。
实施例2：
一种自修复温敏变色窗贴，原料以重量份为：30份聚己二酸丁二醇酯、9份异佛尔酮二异氰酸酯、0.9份二月桂酸二丁基锡、1.2份4,4'二氨基二苯二硫醚、0.5份硼酸、4份热致变色材料。
其制备方法包括如下步骤：
(1)取聚己二酸丁二醇酯置于密炼机中，在真空环境下110℃熔融搅拌2h，搅拌完成后保持真空停止加热并将温度降至80℃，通入干燥的N2，依次加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡和热致变色材料，继续搅拌反应3h，制得聚氨酯预聚物。
(2)恒定温度80℃在N2保护下向聚氨酯预聚物中加入扩链剂4,4'二氨基二苯二硫醚搅拌至混合均匀搅拌扩链2h，停止加热加入扩链剂硼酸溶搅拌10min，混合均匀后，将反应液倒入聚四氟乙烯模具中真空排气泡约30min，于80℃固化10h，得到聚氨酯弹性体。
(3)将所得聚氨酯弹性体用于压延机，制得自修复温敏变色膜。再将温敏变色膜、PET离型膜、聚丙烯酸压敏胶用于涂布机制得自修复温敏变色窗贴。
实施例3：
一种自修复温敏变色窗贴，原料以重量份为：20份聚己二酸丁二醇酯、5份异佛尔酮二异氰酸酯、0.5份二月桂酸二丁基锡、0.6份4,4'二氨基二苯二硫醚、0.4份硼酸、4份热致变色材料。
其制备方法包括如下步骤：
(1)取聚己二酸丁二醇酯置于密炼机中，在真空环境下110℃熔融搅拌2h，搅拌完成后保持真空停止加热并将温度降至80℃，通入干燥的N2，依次加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡和热致变色材料，继续搅拌反应3h，制得聚氨酯预聚物。
(2)恒定温度80℃在N2保护下向聚氨酯预聚物中加入扩链剂4,4'二氨基二苯二硫醚搅拌至混合均匀搅拌扩链2h，停止加热加入扩链剂硼酸溶搅拌10min，混合均匀后，将反应液倒入聚四氟乙烯模具中真空排气泡约30min，于80℃固化10h，得到聚氨酯弹性体。
(3)将所得聚氨酯弹性体用于压延机，制得自修复温敏变色膜。再将温敏变色膜、PET离型膜、聚丙烯酸压敏胶用于涂布机制得自修复温敏变色窗贴。
数据测试：
将实施例1-3根据ASTM D3359进行自修复膜附着力测试；自修复膜铅笔硬度测试根据ASTM D3363。
自修复膜自修复性能测试步骤：选取载重200g/cm2的细黄铜刷在自修复膜表面来回刮擦30次，使用50℃热水进行修复。
将实施例1-3所制备的自修复温敏变色窗贴裁切为15cm×2.5cm的长条，采用万能拉伸试验机测试其断裂伸长率。
定义修复效率(％)＝修复后断裂伸长率/修复前断裂伸长率
测试结果如表1所示
表1性能测试结果
Figure BDA0002928221130000061
将实施例1-3所制得温敏变色窗贴裁剪为10cm×10cm的方形膜片，将其贴附与11cm×11cm的方形玻璃片，采用GB/T 2680-1994测试可见光原始透射比；置于烘箱中进行耐候性测试；依据GB/T 36403-2018测试红外透过率；测试结果如表2所示。
表2性能测试结果
Figure BDA0002928221130000062
表1和表2结果说明，本发明的一种自修复温敏变色窗贴具有较高的可见光透过率，随着温度的变化能对太阳光中能量较高的红外线的透过率进行调节。耐候性测试表明本发明的自修复温敏变色窗贴附着力好、耐老化。铅笔硬度测试结果表明本发明耐洗刷性强，并且具有优秀的自修复性能，最大自修复效率可达到93.2％。

Claims (7)

1.一种自修复温敏变色窗贴，其特征在于，所述自修复温敏变色窗贴的原料以重量份计为：20-30份聚己二酸丁二醇酯、5-10份异佛尔酮二异氰酸酯、0.5-1份二月桂酸二丁基锡、0.5-1.5份4,4'二氨基二苯二硫醚、0.2-1份硼酸、2-5份热致变色材料。
2.根据权利要求1所述的一种自修复温敏变色窗贴，其特征在于，所述热致变色材料为W-Eu双掺杂VO2纳米粉体。
3.根据权利要求1所述的一种自修复温敏变色窗贴，其特征在于，所述热致变色材料的制备方法为：将钨酸(H2WO4)和硝酸铕(Eu(NO3)3)加入到稍过量的双氧水中超声分散10min作为A液待用；取V2O5和CH3COOH超声分散于70ml去离子水，再加入3ml浓盐酸作为B液；将B液快速倒入A液中并于80℃水浴下搅拌60min，随后将混合溶液移入聚四氟乙烯反应釜中水热反应4h，反应温度为200℃；待反应完成冷却至室温后将产物取出，经过去离子水和无水乙醇数次洗涤、离心后收集后，在80℃烘箱中干燥8h；最后将干燥好的产物在氩气保护下进行高温退火处理，得到W-Eu双掺杂VO2纳米粉体。
4.根据权利要求3所述的热致变色材料的制备方法，其特征在于，钨酸和硝酸铕的配料比为0.5-2.5mmol:0.5-2.5mmol。
5.根据权利要求3所述的热致变色材料的制备方法，其特征在于，V2O5和CH3COOH的配料比为0.4-0.6g:0.5-0.7g。
6.根据权利要求3所述的热致变色材料的制备方法，其特征在于，高温退火处理条件为：退火温度450℃-550℃、升温速率5℃/min、退火时间4h。
7.根据权利要求1所述的一种自修复温敏变色窗贴的制备方法，其特征在于，所述方法由以下步骤组成：
(1)取聚己二酸丁二醇酯置于密炼机中，在真空环境下110℃熔融搅拌2h，搅拌完成后保持真空停止加热并将温度降至80℃，通入干燥的N2，依次加入异佛尔酮二异氰酸酯、二月桂酸二丁基锡和热致变色材料，继续搅拌反应3h，制得聚氨酯预聚物；
(2)恒定温度80℃在N2保护下向聚氨酯预聚物中加入扩链剂4,4'二氨基二苯二硫醚搅拌至混合均匀搅拌扩链2h，停止加热加入扩链剂硼酸溶搅拌10min，混合均匀后，将反应液倒入聚四氟乙烯模具中真空排气泡约30min，于80℃固化10h，得到聚氨酯弹性体；
(3)将所得聚氨酯弹性体用于压延机，制得自修复温敏变色膜；再将温敏变色膜、PET离型膜、聚丙烯酸压敏胶用于涂布机制得自修复温敏变色窗贴。
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Publication number Priority date Publication date Assignee Title
CN115960545A (zh) * 2022-12-05 2023-04-14 苏州易昇光学材料股份有限公司 一种高抗黄变级耐候型自修复gpu保护膜

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115960545A (zh) * 2022-12-05 2023-04-14 苏州易昇光学材料股份有限公司 一种高抗黄变级耐候型自修复gpu保护膜
CN115960545B (zh) * 2022-12-05 2023-09-05 苏州易昇光学材料股份有限公司 一种高抗黄变级耐候型自修复gpu保护膜

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