CN115491903A - 一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法 - Google Patents
一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法 Download PDFInfo
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Abstract
本发明涉及辐射制冷技术领域,尤其涉及一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法。将聚合物PMMA薄膜浸泡在海藻酸钠溶液中,随后分别依次浸泡在氯化钙、钠盐溶液中、晾干,重复4~7次,最终制得钙盐增强型高性能辐射制冷聚合物薄膜。本发明基于海藻酸钠与Ca2+的静电作用引入具有高发射特性的钙盐,使聚合物薄膜实现降温性能的显著提升。增强型聚合物薄膜具有优异的辐射制冷性能,在建筑降温、节能环保、可穿戴热管理等领域具有广阔应用前景,且该制备方法简单、原料便宜,易于规模批量化生产。
Description
技术领域
本发明涉及辐射制冷技术领域,尤其涉及一种钙盐(CaHPO4、CaSiO3、CaSO3等)增强型高性能辐射制冷聚合物薄膜的制备方法。增强型聚合物薄膜具有优异的辐射制冷性能,在建筑降温、节能环保、可穿戴热管理等领域具有广阔应用,且该制备方法简单、原料便宜,易于规模批量化生产。
背景技术
随着温室效应和全球变暖等问题的加剧,制冷技术在各领域的需求日益增加。其中,作为零能耗、环境友好的一种新技术,辐射制冷技术引发人们的广泛关注,其基本原理是将地球的热量以热辐射的形式释放到宇宙太空中去。地面上的热量以电磁波形式在穿越大气层时,部分电磁波被吸收或重返到地面。存在一个大气透明窗口,即8~13μm的电磁波在穿透大气层时只有少量被吸收,大部分以红外线的形式到达宇宙,因此达到降温的目的。辐射制冷技术可广泛应用于建筑物降温、冷凝水收集、太阳能电池冷却、户外设备散热、农业大棚降温等。
根据辐射制冷基本原理,材料不仅要满足在大气透明窗口(8~13μm)范围内高辐射,而且需要具备热红外高发射。然而,现有技术中存在的问题主要是:(1)薄膜结构调控性差,自身难以获得高辐射;(2)高分子薄膜材料自身的红外发射率低。因此,通过组分复合和微纳结构的设计,在不影响聚合物薄膜其他性能的情况下,提升聚合物薄膜的辐射制冷性能是一种有效的途径。海藻酸钠具有优异的成膜性,分子中含有大量聚阴离子基团,它们与一些带正电荷的阳离子基团相互作用,改变薄膜表面结构,从而影响光学性能。
本发明专利提出,基于海藻酸钠和高发射特性的钙盐(CaHPO4、CaSiO3、CaSO3,等),提出一种实现对聚合物薄膜辐射制冷性能提升的方法,获得高性能辐射制冷的聚合物薄膜。
发明内容
本发明的目的:本发明旨在解决现有技术中存在的技术问题之一。为此,本发明的目的在于提供一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法。
本发明的技术方案是:为了解决上述问题,本发明采用的技术方案如下:
一种钙盐增强型高性能辐射制冷聚甲基丙烯酸甲酯(PMMA)薄膜的制备方法。首先,将PMMA溶解于溶剂中变成PMMA溶液,通过静电纺丝技术制备得到PMMA膜,把PMMA膜浸泡于SA溶液中,获得海藻酸钠修饰的PMMA膜(SA@PMMA);然后,将SA@PMMA膜分别在CaCl2、去离子水、钠盐溶液(Na2HPO4、Na2SiO3、Na2SO3)中依次浸渍、晾干,整个过程重复多次,最后得到钙盐修饰的PMMA膜(CaHPO4@PMMA、CaSiO3@PMMA、CaSO3@PMMA等)。具体的制备步骤为:
(1)将PMMA溶解于N,N-二甲基甲酰胺(DMF)和甲酸混合溶液中,通过静电纺丝技术制备得到PMMA膜;
(2)将PMMA膜浸泡到海藻酸钠溶液中,浸渍一定时间后得到SA@PMMA膜;
(3)将SA@PMMA膜分别在CaCl2、去离子水、钠盐溶液(Na2HPO4、Na2SiO3、Na2SO3)中依次浸渍、晾干,整个过程重复多次,最后得到钙盐修饰的PMMA膜(CaHPO4@PMMA、CaSiO3@PMMA、CaSO3@PMMA,等)。
优选的是,步骤(1)中,DMF和甲酸的优选质量比为2∶1,优选的PMMA溶液质量浓度为10wt%~20wt%。
优选的是,步骤(1)中,静电纺丝电压为14kV,喷速为0.1~0.2mL/s。
优选的是,步骤(2)中,海藻酸钠溶液质量浓度为45~55wt%,浸泡时间为3~6h。
优选的是,步骤(3)中,CaCl2溶液、钠盐溶液(分别为Na2HPO4、Na2SiO3、Na2SO3)浓度均为0.15~0.25mol/L,浸泡时间为2~5min,整个浸泡、晾干过程的重复次数为4~7次。
本发明提供了一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,这种制备方法可应用于多种聚合物薄膜,制备工艺简单、原料便宜,无需大型设备,可规模化,得到的高发射聚合物薄膜,辐射制冷性能优异,应用广泛。
有益效果:
(1)本发明提供了一种高发射钙盐增强PMMA膜辐射制冷性能的方法,钙盐(CaHPO4、CaSiO3、CaSO3等)的添加使PMMA膜在大气窗口附近具有高发射性能。
(2)本发明将不同的钙盐(CaHPO4、CaSiO3、CaSO3等)添加到PMMA膜,其原理相同,不受薄膜种类的限制,因此可以应用于多种聚合物薄膜,提升其在大气窗口的发射率。
(3)降温效果显著:在太阳光模拟器AM1.5G的光照强度为100mW/cm2且光照时长为1000s时,CaHPO4@PMMA膜、CaSiO3@PMMA膜和CaSO3@PMMA膜温度相比原始PMMA膜温度分别低5.2℃、3.4℃、11.7℃。
(4)与其他辐射制冷薄膜相比,该聚合物薄膜具有以下优点:
①制备过程简单,操作方便,重复性高;
②辐射制冷薄膜具有高发射性;
③辐射制冷薄膜制冷性能优异;
④成本较低,实用性强,具有良好的工业化应用前景。
附图说明:
图1为实施例1、例2、例3、例4产物的红外光谱图
图2为实施例1、例2、例3、例4产物的中红外发射率谱图
图3为实施例1、例2、例3、例4产物在一个太阳光照下的温度-时间曲线
图4为实施例1产物在不同光照强度下的温度-时间曲线
图5为实施例2、例3、例4产物在户外光照强度下温度-时间曲线
具体实施方式:
本发明中制备材料的具体实施方式如下:
实施例1
将PMMA溶于DMF和甲酸混合溶液(DMF与甲酸质量比为2∶1)获得15wt%的PMMA溶液,在电压14kV,喷速0.146mL/s条件下静电纺丝制备得到PMMA膜;将SA溶于去离子水中制得50wt%的SA溶液,将PMMA膜浸泡于SA溶液中4h获得SA@PMMA膜。配置浓度为0.2mol/L的CaCl2、Na2HPO4溶液,将PMMA膜交替浸渍CaCl2、去离子水、Na2HPO4溶液中,浸泡时间3min,重复浸泡次数5次,最后获得CaHPO4@PMMA膜。
实施例2
将Na2HPO4溶液换成Na2SiO3溶液,其他条件和实施例1相同,得到CaSiO3@PMMA膜。
实施例3
将Na2HPO4溶液换成Na2SO3溶液,其他条件和实施例1相同,得到CaSO3@PMMA膜。
实施例4
将PMMA溶于DMF和甲酸混合溶液(DMF与甲酸质量比为2∶1)获得15wt%的PMMA溶液,在电压为14kV,喷速为0.146mL/s条件下静电纺丝制备得到PMMA膜。
图1是实施例1、例2、例3、例4产物红外性能表征。测试不同钙盐修饰的PMMA膜、PMMA膜和对应的钙盐,测试范围为250-1500nm。在CaHPO4@PMMA红外图中1212cm-1、1122cm-1、1062cm-1、988cm-1、876cm-1是由PO4 2-振动引起的,表明CaHPO4成功负载在PMMA膜上。在CaSiO3@PMMA红外图中,1033cm-1附近出现的特征峰是由Si-O-Si振动引起的,表明CaSiO3成功负载在PMMA膜上。在CaSO3@PMMA红外图中,981cm-1附近出现的特征峰是由SO3 2-振动引起的,表明CaSO3成功负载在PMMA膜上。
图2实施例1、例2、例3、例4产物中红外发射性能表征。具体步骤为,测试负载不同钙盐的PMMA膜和PMMA膜,测试范围为2.5-15μm。可以看到,在8-13μm范围内,CaHPO4@PMMA膜、CaSiO3@PMMA膜、CaSO3@PMMA膜和PMMA膜的发射率分别为0.955、0.967、0.947和0.939,钙盐改性后的PMMA膜普遍具有较高的发射率,高发射钙盐的添加提升了PMMA膜在8~13μm的发射率。
图3是实施例1、例2、例3、例4产物在室内模拟一个太阳光照下降温性能表征。具体步骤为,将不同钙盐修饰的PMMA膜放在同一平面上,调节太阳光模拟器AM1.5G的光照强度为100mW/cm2,用热成像FOTRIC 323Pro记录膜表面温度随时间的变化。可以看到,当光照时长1000s时,CaHPO4@PMMA膜、CaSiO3@PMMA膜和CaSO3@PMMA膜温度比原始PMMA膜温度分别低5.2℃、3.4℃、11.7℃,钙盐改性后的PMMA膜降温效果普遍比未添加钙盐的PMMA膜降温效果更佳。
图4是实施例1产物在室内模拟不同光照强度下膜表面温度-时间曲线。具体步骤为,将CaHPO4@PMMA膜放在太阳光模拟器AM1.5G下,调节太阳光模拟器AM1.5G的光照强度依次为100mW/cm2、200mW/cm2、300mW/cm2和600mW/cm2,用热成像FOTRIC 323Pro记录膜表面温度随时间的变化。可以看到,当光照时间为1000s时,CaHPO4@PMMA膜表面温度分别为48.4℃、53.3℃、63.6℃和67.3℃。
图5是实施例2、例3、例4产物在户外光照强度下温度-时间图。具体步骤为,将CaSiO3@PMMA膜、CaSO3@PMMA膜和PMMA膜在户外日照,用热成像FOTRIC 323Pro记录膜表面温度随时间的变化。可以看到,日照时间1200秒,CaSiO3@PMMA膜、CaSO3@PMMA膜和PMMA膜的温度分别为48.3℃、45.6℃和46.6℃。由此可见,在户外条件下,钙盐改性的PMMA膜,降温效果普遍比未添加钙盐的PMMA膜降温效果更突出。
Claims (6)
1.一种钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,其特征在于,包括以下步骤:
(1)制备聚甲基丙烯酸甲酯(PMMA)膜:将PMMA溶解于N,N-二甲基甲酰胺(DMF)和甲酸混合溶液中,通过静电纺丝技术制备得到PMMA膜。
(2)制备海藻酸钠(SA)修饰的PMMA膜:将海藻酸钠溶于去离子水溶液中得到SA溶液,然后把PMMA膜浸泡于SA溶液中,获得海藻酸钠修饰的PMMA膜(SA@PMMA)。
(3)将SA@PMMA膜分别在CaCl2、去离子水、钠盐溶液(Na2HPO4、Na2SiO3、Na2SO3)中依次浸渍、晾干,整个过程重复多次,最后得到钙盐修饰的PMMA膜(CaHPO4@PMMA、CaSiO3@PMMA、CaSO3@PMMA等)。
2.根据权利要求1所述的钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,其特征在于,步骤(1)中,DMF和甲酸的优选质量比为2∶1,优选的PMMA溶液质量浓度为10wt%~20wt%。
3.根据权利要求1所述的钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,其特征在于,步骤(1)中,静电纺丝条件为:电压为14kV,喷速为0.1~0.2mL/s。
4.根据权利要求1所述的钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,其特征在于,步骤(2)中,海藻酸钠溶液质量浓度为45~55wt%,浸泡时间为3~6h。
5.根据权利要求1所述的钙盐增强型高性能辐射制冷聚合物薄膜的制备方法,其特征在于,步骤(3)中,CaCl2溶液、钠盐溶液(分别为Na2HPO4、Na2SiO3、Na2SO3)浓度均为0.15~0.25mol/L,浸泡时间为2~5min,整个浸泡、晾干过程的重复次数为4~7次。
6.根据权利要求5所述的制备方法,最后分别获得CaHPO4@PMMA、CaSiO3@PMMA、CaSO3@PMMA三种薄膜材料。钙盐修饰的PMMA膜具有高发射性能,其中CaSiO3@PMMA膜发射率最高。
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