CN110294831A - 一种用于智能窗户的弹性热致变色材料制备方法及其产物和应用 - Google Patents
一种用于智能窗户的弹性热致变色材料制备方法及其产物和应用 Download PDFInfo
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Abstract
本发明公开了一种用于智能窗户的弹性热致变色材料制备方法及其产物和应用。使多异氰酸酯和聚醚多元醇在一定温度下进行反应，得到聚氨酯预聚物，再将交联剂和扩链剂按一定比例加入聚氨酯预聚物中，充分反应后得到聚氨酯复合物，最后将该聚氨酯复合物放入水中溶胀即得弹性热致变色材料。所得弹性热致变色材料具有弹性大，相变温度低，对温度响应灵敏，太阳光透过率调节能力强、低温下透过率高等优点，可应用于智能窗户的制造等；其制备方法具有原料易得，反应条件温和，制备工艺简单等优点，可用于工业化大规模生产。
Description
技术领域
本发明属于智能材料以及响应型聚合物技术领域。具体涉及一种用于智能窗户的弹性热致变色材料制备方法及其产物和应用。
背景技术
在多光照地区的建筑能耗中，制冷和供暖占据主要部分，以调节室内温度至舒适区间。而窗户吸收阳光并透过红外光是造成办公室、汽车和其他类似空间过热的原因之一，因此控制透过窗户的阳光是调节室内温度的一种重要手段。智能窗户被广泛应用于太阳光能量的调节，其包括热致变色、光致变色和电致变色等类型。其中热致变色智能窗户，是一系列在温度变化刺激下发生变色响应的智能窗户。这一类智能窗户可用于光学节能系统，吸收光热能量，达到降低空调能耗的效果。
目前已有多种可阻挡阳光以调节室内温度的方法，如静态调节太阳光的百叶窗和玻璃贴膜，动态调节太阳光透过的相变材料、热致变色材料和聚合物分散液晶等。掺有氧化钒(VO2)的无机涂料因具有热致变色特性，引起了科学家的极大兴趣。然而，由于含VO2的无机涂料具有相对较高的转变温度(67℃)和复杂的制备工艺，很难在工业上实现大规模生产。三氧化钨(WO3)是电致变色智能窗中最常用的材料，但其需要一个透明的导电层来实现变色功能。因此，目前在实际应用中，能动态调节太阳光在窗户中透过率的技术较为复杂，并且存在响应温度高、响应速度不灵敏、太阳光透过率调节能力低等问题。
有机热致变色材料因其制备工艺简单，响应灵敏，柔性可拉伸，可动态调节窗户的透明度等优点而受到青睐。这些材料的热致变色原理，通常是基于最低临界共溶温度(LCST)或最高临界共溶温度(UCST)的相变。Fang(Xinhao Li，Chang Liu，Shien-PingFeng，Nicholas Xuanlai Fang，Joule 2018，3，1-13.)等人注入聚(N-异丙基丙烯酰胺)-2-氨基甲基丙烯酸乙酯水凝胶微粒至封闭的玻璃容器，制作成智能窗户，在低温下呈现透明状态，遇热则变白。Chung(Thanh-Giang La，Xinda Li，Amit Kumar，Yiyang Fu，Shu Yang，Hyun-Joong Chung，Acs Applied Materials&Interfaces 2017，9，33100-33106.)等人报道了一种在UCST附近从乳白色(低温)到透明(高温)的可拉伸聚多孔水凝胶，该水凝胶可在寒冷天气中用作智能窗口。但目前可供选择用于智能窗户的有机热致变色材料有限，并且存在响应温度高的缺点，同时材料的拉伸延展性能也需要进一步提高。
发明内容
发明目的：针对现有技术存在的上述问题，本发明的目的在于提供一种用于智能窗户的弹性热致变色材料制备方法，原料易得，反应条件温和，工艺简单。本发明的另一目的在于提供用于智能窗户的弹性热致变色材料，具有弹性大，相变温度低，对温度响应灵敏，太阳光透过率调节能力强、低温下透过率高等优点，可作为制造智能窗户的智能响应材料。
技术方案：为了解决上述问题，本发明所采用的技术方案如下：
一种用于智能窗户的弹性热致变色材料制备方法，包括如下步骤：
1)将质量比为1∶3～1∶30的多异氰酸酯和聚醚多元醇在25-90℃下进行反应1-10h，得到聚氨酯预聚物；
2)将交联剂和扩链剂按一定比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为25-90℃，反应时间为0.5-10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀1～24h，得到弹性热致变色材料。
优选地，步骤1)中所述的多异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、赖氨酸二异氰酸酯和二环己基甲烷二异氰酸酯中的一种或几种的混合。
优选地，步骤1)中所述的聚醚多元醇(分子量为400-10000)为聚丙二醇、聚乙二醇、聚环氧丙烷二元醇、聚四氢呋喃醚二元醇和聚丙二醇-乙二醇-丙二醇中的一种或几种的混合。
优选地，步骤2)中所述的交联剂为苯胺甲基倍半硅氧烷、环己烷基倍半硅氧烷、γ-氨丙基倍半硅氧烷、苯胺丙基倍半硅氧烷、丙三醇和三羟甲基丙烷中的一种或几种的混合。
优选地，步骤2)中所述的扩链剂为1，4-丁二醇、乙二醇、二甘醇、乙二胺和N，N-二羟基(二异丙基)苯胺中的一种或多种的混合。
优选地，所述的一种用于智能窗户的弹性热致变色材料制备方法，包括如下步骤：
1)将质量比为1∶5.75的甲苯二异氰酸酯和聚丙二醇-乙二醇-丙二醇在85℃下进行反应3h，得到聚氨酯预聚物；
2)将苯胺丙基倍半硅氧烷按1.28％的比例和乙二醇按2.56％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀5h，得到弹性热致变色材料。
优选地，所述的一种用于智能窗户的弹性热致变色材料制备方法，包括如下步骤：
1)将质量比为1∶2.19∶2.19的赖氨酸二异氰酸酯和聚乙二醇和聚环氧丙烷二元醇在30℃下进行反应10h，得到聚氨酯预聚物；
2)将γ-氨丙基倍半硅氧烷按1.63％的比例和1，4-丁二醇按1.63％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为6h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀24h，得到弹性热致变色材料。
优选地，所述的一种用于智能窗户的弹性热致变色材料制备方法，包括如下步骤：
1)将质量比为1∶3.82的二环己基甲烷二异氰酸酯和聚乙二醇在60℃下进行反应5h，得到聚氨酯预聚物；
2)将三羟甲基丙烷按1.58％的比例和乙二醇按2.38％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀10h，得到弹性热致变色材料。
所述的用于智能窗户的弹性热致变色材料制备方法得到的弹性热致变色材料。
所述的弹性热致变色材料在智能窗户、智能温度检测或指纹采集领域的应用。
有益效果：相比于现有技术，本发明的优点为：
(1)本发明提供的一种用于智能窗户的弹性热致变色材料制备方法，原料易得，反应条件温和，制备工艺简单，可用于工业化大规模生产；
(2)本发明提供用于智能窗户的弹性热致变色材料，具有弹性大，相变温度低，对温度响应灵敏，太阳光透过率调节能力强、低温下透过率高等优点，除可以广泛应用于建筑玻璃，汽车窗户等采光系统外，在智能温度检测以及指纹采集等领域也有着潜在的应用。
附图说明
图1为弹性热致变色材料做成的智能窗户材料进行变温条件下的近红外-可见光-紫外光透过率测试结果图；
图2为弹性热致变色材料做成的智能窗户在低温和高温条件下透明度变化图。
具体实施方式
下面结合具体实施例对本发明进一步进行描述。
实施例1：
将2.22g异佛尔酮二异氰酸酯和5g聚丙二醇和5g聚乙二醇混合，加热到85℃反应1h，继而加入0.2g丙三醇和0.40g 1，4-丁二醇，并在80℃下反应2h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡1h，得到弹性热致变色材料。
实施例2：
将2.22g异佛尔酮二异氰酸酯和66.6g聚丙二醇-乙二醇-丙二醇混合，加热到85℃反应2h，继而加入0.15g苯胺甲基倍半硅氧烷和0.40g 1，4-丁二醇，并在25℃下反应2h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡2h，得到弹性热致变色材料。
实施例3：
将2.5g二苯基甲烷二异氰酸酯和5g聚四氢呋喃醚二元醇和2.5g聚乙二醇混合，加热到25℃反应10h，继而加入0.1gγ-氨丙基倍半硅氧烷和0.3g乙二胺，并在90℃下反应0.5h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡2h，得到弹性热致变色材料。
实施例4：
将1.74g甲苯二异氰酸酯和10g聚丙二醇-乙二醇-丙二醇混合，加热到85℃反应3h，继而加入0.15g苯胺丙基倍半硅氧烷和0.3g乙二醇，并在60℃下反应10h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡5h，得到弹性热致变色材料。
实施例5：
将1.68g六亚甲基二异氰酸酯和10g聚丙二醇-乙二醇-丙二醇混合，加热到50℃反应10h，继而加入0.1g环己烷基倍半硅氧烷和0.40g二甘醇，并在50℃下反应10h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡24h，得到弹性热致变色材料。
实施例6：
将1.68g六亚甲基二异氰酸酯和5g聚四氢呋喃醚二元醇和5g聚环氧丙烷二元醇混合，加热到80℃反应3h，继而加入0.15g丙三醇和0.20g N，N-二羟基(二异丙基)苯胺，并在65℃下反应5h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡6h，得到弹性热致变色材料。
实施例7：
将2.28g赖氨酸二异氰酸酯和5g聚乙二醇和5g聚环氧丙烷二元醇混合，加热到30℃反应10h，继而加入0.2gγ-氨丙基倍半硅氧烷和0.20g 1，4-丁二醇，并在60℃下反应6h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡24h，得到弹性热致变色材料。
实施例8：
将2.28g赖氨酸二异氰酸酯和10g聚四氢呋喃醚二元醇，加热到70℃反应5h，继而加入0.15g苯胺丙基倍半硅氧烷和0.60g乙二胺，并在60℃下反应6h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡12h，得到弹性热致变色材料。
实施例9：
将2.62g二环己基甲烷二异氰酸酯和5g聚乙二醇和5g聚环氧丙烷二元醇混合，加热到90℃反应2h，继而加入0.3g环己烷基倍半硅氧烷和0.20g 1，4-丁二醇，并在80℃下反应6h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡5h，得到弹性热致变色材料。
实施例10：
将2.62g二环己基甲烷二异氰酸酯和10g聚乙二醇混合，加热到60℃反应5h，继而加入0.2g三羟甲基丙烷和0.30g乙二醇，并在60℃下反应10h，得到聚氨酯复合物。将上述复合物浸在纯水中浸泡10h，得到弹性热致变色材料。
实施例11：
取实施例1-10中制备的弹性热致变色材料，进行拉伸性能测试和在10℃、20℃、25℃和30℃等温度下的阳光透过率测试。测试结果如表1所示，所得材料拉伸至原始长度的5～20倍后才断裂，在实际拉伸过程中，小于断裂伸长率范围的拉伸都可恢复，表明所得弹性热致变色材料弹性性能良好；表1同时显示，所得材料的透光率在10℃时可达87％～98％，在20℃有84～95％，在25℃时下降为48％～76％，在30℃时只有18％～40％，表明所得材料具有相变温度低，对温度响应灵敏，太阳光透过率调节能力强等优点。
表1：材料拉伸性能测试和透光率测试结果
实施例12：
取实施例1-10制备的弹性热致变色材料做成的智能窗户材料，进行变温条件下的近红外-可见光-紫外光透过率测试，结果如图1所示(以实施例2产品为例)，随着温度升高，材料透过率逐渐降低至一定值，其在2500nm-300nm下的透过率在15℃和40℃下具有较大的差别，表明材料对太阳光的透射有极强的调节能力；图2显示，用弹性热致变色材料做成的智能窗户，在低温时高度透明，在高温时则呈现不透明的白色，因此，本申请制备的产品在低温下使阳光透过率高，高温下使阳光透过率低，自动地根据温度调节阳光的透过率。
Claims (10)
1.一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，包括如下步骤：
1)将质量比为1∶3～1∶30的多异氰酸酯和聚醚多元醇在25-90℃下进行反应1-10h，得到聚氨酯预聚物；
2)将交联剂和扩链剂按一定比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为25-90℃，反应时间为0.5-10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀1～24h，得到弹性热致变色材料。
2.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，步骤1)中所述的多异氰酸酯为异佛尔酮二异氰酸酯、甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯、赖氨酸二异氰酸酯和二环己基甲烷二异氰酸酯中的一种或几种的混合。
3.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，步骤1)中所述的聚醚多元醇为聚丙二醇、聚乙二醇、聚环氧丙烷二元醇、聚四氢呋喃醚二元醇和聚丙二醇-乙二醇-丙二醇中的一种或几种的混合。
4.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，步骤2)中所述的交联剂为苯胺甲基倍半硅氧烷、环己烷基倍半硅氧烷、γ-氨丙基倍半硅氧烷、苯胺丙基倍半硅氧烷、丙三醇和三羟甲基丙烷中的一种或几种的混合。
5.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，步骤2)中所述的扩链剂为1，4-丁二醇、乙二醇、二甘醇、乙二胺和N，N-二羟基(二异丙基)苯胺中的一种或多种的混合。
6.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，包括如下步骤：
1)将质量比为1∶5.75的甲苯二异氰酸酯和聚丙二醇-乙二醇-丙二醇在85℃下进行反应3h，得到聚氨酯预聚物；
2)将苯胺丙基倍半硅氧烷按1.28％的比例和乙二醇按2.56％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀5h，得到弹性热致变色材料。
7.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，包括如下步骤：
1)将质量比为1∶2.19∶2.19的赖氨酸二异氰酸酯和聚乙二醇和聚环氧丙烷二元醇在30℃下进行反应10h，得到聚氨酯预聚物；
2)将γ-氨丙基倍半硅氧烷按1.63％的比例和1，4-丁二醇按1.63％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为6h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀24h，得到弹性热致变色材料。
8.根据权利要求1所述的一种用于智能窗户的弹性热致变色材料制备方法，其特征在于，包括如下步骤：
1)将质量比为1∶3.82的二环己基甲烷二异氰酸酯和聚乙二醇在60℃下进行反应5h，得到聚氨酯预聚物；
2)将三羟甲基丙烷按1.58％的比例和乙二醇按2.38％的比例加入步骤1)得到的聚氨酯预聚物中充分反应，反应温度为60℃，反应时间为10h，得到聚氨酯复合物；
3)将步骤2)得到的聚氨酯复合物放入水中溶胀10h，得到弹性热致变色材料。
9.权利要求1-8所述用于智能窗户的弹性热致变色材料制备方法得到的弹性热致变色材料。
10.权利要求9所述的弹性热致变色材料在智能窗户、智能温度检测或指纹采集领域的应用。
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| CN113388052B (zh) * | 2021-06-28 | 2022-09-02 | 绍兴迪飞新材料有限公司 | 智能动态调光膜及其制备工艺及调光玻璃及调光玻璃系统 |
| CN115268160A (zh) * | 2022-08-08 | 2022-11-01 | 安徽华菱汽车有限公司 | 一种汽车及变色玻璃 |
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