CN114960238A - 一种基于全波段光蓄热热致变色织物的制备方法及应用 - Google Patents
一种基于全波段光蓄热热致变色织物的制备方法及应用 Download PDFInfo
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Abstract
本发明公开了一种基于全波段光蓄热热致变色织物的制备方法，该方法构建了具有全波段光热转化效应的复合材料；以纳米铯钨粉、吲哚菁绿、石墨烯为芯材，三聚氰胺‑甲醛树脂/改性SiO2杂化层为壁材，制备光蓄热微胶囊染料；以温变隐色染料为芯材，SiO2为壁材，制备温敏变色微胶囊染料；将光蓄热染料和温变染料分别采用不同的粘合剂制备成印花浆作用于棉织物的正反面上；选用的两种粘合剂分别是双组分聚氨酯的两种组分PPG‑2000与MDI；因此经其之间的交联作用使两种染料结合；纳米铯钨粉在光的照射下，入射光光子与其表面的自由电子相互作用，吸收入射光并产生大量热；使温变微胶囊变色以间接达到光致变色，能够实时监控热量释放状态。
Description
技术领域
本发明涉及光蓄热热致变色材料的制备方法及应用，尤其涉及一种基于全波段光蓄热热致变色织物的制备方法及应用。
背景技术
太阳能可以通过光伏、光化学和光热过程被利用并转化为各种能源形式，包括电力、化学(燃料)和热能。在太阳能转化形式中，光热是一个直接的转换过程，具有最高的可实现转换效率。光热效应是由光激发产生的，从而将部分或完全的光能转化为热能。其中太阳能光谱能量的分布为：紫外(UV)区域(300～400nm)占功率的3％，可见光范围 (400～700nm)占功率的45％，近红外(NIR)区域(700～2500nm)占功率的52％。如果光吸热材料在300至2500nm波长处有较高的吸光度，同时反射率/透射率可忽略不计，就能够以最大限度地利用太阳的能量，并将其转化为热能。具有光热效应的材料主要分无机材料和有机材料两大类，其中无机材料有贵金属和半导体，有机材料有碳基材料、染料和共轭聚合物。在高效太阳能集热器材料的设计中，阳光的吸收及其转化为热能的效率都有助于整体的光热性能。具有全波段太阳能吸收的材料能够更加有效地实现对太阳能能源的应用。
热致变色材料是利用变色染料热致变色来测量物体表面温度及温度分布的一种特殊功能性材料，也称为变色材料或热敏材料。其应用范围从简单的示温作用拓展到印刷、涂料、防伪和生活用品等日常生活的各个方面。光诱导温敏变色织物是指织物在光照的调控下，实现温度的可控稳定变化，以呈现颜色的变化，它们的各种潜在应用，如加热器、电子显示、军事、保护、传感等领域。常用的变色纤维基本实现通过紫外线、温度和化学物质刺激变色溶剂。然而，在大多数情况下，颜色的变化是被动的，无法进行自主的控制。与这些刺激物相比，光致变色效应更为明显通过施加光照来调节纤维表面温度来实现。光致变色是指通过吸收电磁辐射使化学物质在两种形式之间进行可逆的转化，且两种形式具有不同的吸收光谱。通常，这可以描述为暴露于光线时颜色的可逆变化。目前光致变色织物都是通过某种处理手段使有机光致变色化合物附着在织物表面或者纤维里面，使其具有光致变色功能。然而，颜色变化区域很小。而且光致变色染料的转换速度受染料周围环境的刚性大小影响。
发明内容
发明目的：本发明的目的在于提供一种基于全波段光蓄热热致变色织物的制备方法，制备得到的全波段光蓄热热致变色织物光储能性能好、能量密度高、稳定性能优异。本发明的另一目的是提供该基于全波段光蓄热热致变色织物在应用中对光照强度的监控。
技术方案：本发明的基于全波段光蓄热热致变色织物的制备方法，包括以下步骤：
(1)温敏变色微胶囊染料的制备：以热致变色隐色染料为芯材，二氧化硅为壁材，用溶胶-凝胶法制备出具有温敏变色性能的微胶囊；将温敏变色微胶囊与增稠剂、粘合剂、水按一定比例在机械搅拌的作用下进行共混，制得温敏变色染料；
(2)光蓄热微胶囊染料的制备：以纳米铯钨粉、吲哚菁绿、石墨烯为芯材，三聚氰胺-甲醛树脂/改性SiO2杂化层为壁材，采用原位聚合法制备出具有光蓄热性能的微胶囊；将光蓄热微胶囊与分散剂按一定比例在机械搅拌的作用下分散制得分散液；向其中加入适量的粘合剂、增稠剂和水再进行机械搅拌制得纳米铯钨粉印花浆料；
(3)基于全波段光蓄热热致变色织物的制备：将光蓄热微胶囊染料通过丝网印花的方式印在棉织物的一面上；再通过丝网印花的方式将温敏变色微胶囊染料印在棉织物的另一面上；将印花后的织物在一定温度下焙烘一定时间，得到光蓄热热致变色织物。
进一步地，步骤(1)中，所述温敏变色微胶囊为聚苯乙烯温变微胶囊、脲醛树脂温变微胶囊、聚甲基丙烯酸酯温变微胶囊、二氧化硅温变微胶囊中的一种。
进一步地，步骤(1)中，所述增稠剂选用HF-202增稠剂、粘合剂选用MDI增稠剂；温变色微胶囊、增稠剂HF-202与粘合剂MDI的摩尔比为1:1:2-2:2:3。
进一步地，步骤(2)中，所述光蓄热微胶囊芯材中的纳米铯钨粉的粒径为20-5000nm。
进一步地，步骤(2)中，所述增稠剂选用HF-202增稠剂、所述粘合剂选用PPG-2000粘合剂；光蓄热微胶囊染料、增稠剂HF-202与粘合剂PPG-2000的摩尔比为1:2:1-1:3:1。
进一步地，步骤(2)中，所述机械搅拌的速度为2-4rad/s，时间为5-10min。
进一步地，步骤(3)中，所述印花方式为平网印花和圆网印花的一种。
进一步地，步骤(3)中，所述焙烘温度为150-200℃，焙烘时间为5-10min。
本发明还提供通过上述制备方法所制得的基于全波段光蓄热热致变色织物的应用，包括以下步骤：为全波段光蓄热热致变色织物选择合适的变色温度，在不同光源下进行照射，观察该织物变色现象；通过监控全波段光蓄热热致变色织物的颜色变化，来预防穿着由该织物所制成纺织品的实验者身体被强光灼伤。
进一步地，所述光为紫外光，可见光与红外光。
本发明为了使光蓄热热致变色织物获得更好的光热转换效果，选择将纳米铯钨粉浆料与温敏变色染料分别印在棉织物的正反面，实现光蓄热热致变色效率的最大化。
本发明通过选用纳米铯钨粉作为光热转换材料，该光热转换材料有着特殊的阳离子嵌入结构和氧空位缺陷，粒子中存在大量自由电子，会产生局部表面等离子共振(LSPR)效应，即当光线入射到纳米颗粒上时，如果入射光的振动频率与金属粒子表面的自由电子谐振频率相同时产生的相干振荡，会触发电子的集体激发。激发的热电子和入射的电磁场形成共振，使颗粒内部的自由电子气体振荡，强烈吸收入射光，并转化为热。光子 -电子及电子-光子间的相互作用使纳米铯钨粉粒子在近红外光和可见光的照射下产生大量的热。
基于光蓄热微胶囊表面产生LSPR效应释放大量热对织物的影响，本发明针对在光热转换过程中热量释放的监控引入三芳甲烷类温变染料，从而有效地实现实时监控与警示作用。三芳甲烷类温变染料为有机可逆温变材料，主要由发色剂、显色剂和溶剂三部分组成。该温变染料变色是由电子给予与接受所发生的平衡移动产生的不同颜色的物质之间发生的变化而引起的。其中，发色剂作为电子给体，显色剂作为电子受体，溶剂作为温度调节剂，决定材料的变色温度。当纳米铯钨粉释放出的热量达到某一定值时，该染料会发生颜色变化，从而达到监控警示的效果。
通过选用粘合剂PPG-2000与粘合剂MDI，经其之间发生的化学反应产生的交联作用，使光蓄热微胶囊染料与温变色微胶囊染料结合，以达到光蓄热热致变色得目的。同时因为两种粘合剂之间的交联作用可以形成一种聚氨酯胶粘剂，使织物的色牢度得到较大的改善。PPG-2000与MDI之间的化学反应原理如下图式所示：
有益效果：与现有技术相比，本发明具有如下显著优点：
(1)本发明的光蓄热微胶囊染料对于光是全波段的吸收，光热转换效率较高，尤其是在可见光区有着较强吸收与优秀的光热转换效率；(2)纳米铯钨粉释放的热量会使温变染料升温变色，起到警示的作用；(3)本发明选用双组分聚氨酯胶粘剂的两个组分分别作为温敏变色微胶囊染料与光蓄热微胶囊染料的粘合剂，通过其之间的化学反应产生的交联作用，可以使两种染料结合，同时使染料的色牢度显著提升。
附图说明
图1为本发明PPG-2000与MDI之间的化学反应原理图；
图2为本发明实施例6的光蓄热热致变色染料变色前后颜色性能分析图。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
一、基于光蓄热热致变色织物的制备
实施例1
合成聚苯乙烯温变微胶囊变色染料
将温变色微胶囊与增稠剂HF-202、粘合剂MDI、水按摩尔比2:2:3在机械搅拌并以2rad/s的速度作用下进行共混，制成聚苯乙烯温变微胶囊变色浆料。
实验发现，聚苯乙烯化学性质稳定，成膜性好，但聚苯乙烯本身具有绝热的特性，导致热至变色的效果较差。
实施例2
合成脲醛树脂温变微胶囊变色染料
将温变色微胶囊与增稠剂HF-202、粘合剂MDI、水按摩尔比2:2:3在机械搅拌并以2rad/s的速度作用下进行共混，制成脲醛树脂温变微胶囊变色浆料。
实验发现，以脲醛树脂为壁材制成微胶囊不是表面光滑的球体，并且相互之间严重粘连。
实施例3
合成聚甲基丙烯酸酯温变微胶囊变色染料
将温变色微胶囊与增稠剂HF-202、粘合剂MDI、水按摩尔比2:2:3在机械搅拌并以2rad/s的速度作用下进行共混，制成聚甲基丙烯酸酯温变微胶囊变色浆料。
实验发现，以聚甲基丙烯酸酯为壁材制得的微胶囊成膜性和化学稳定性均较好，但与以脲醛树脂为壁材的微胶囊一样，产物均为表面不光滑的球体，且粘连现象严重。
实施例4
合成二氧化硅温变微胶囊变色染料
将温变色微胶囊与增稠剂HF-202、粘合剂MDI、水按摩尔比2:2:3在机械搅拌并以2rad/s的速度作用下进行共混，制成二氧化硅温变微胶囊变色浆料。
实验发现，相较于合成高分子类壁材，利用二氧化硅作为壁材成膜性较差，制成的温变微胶囊性能不如前者。
实施例5
合成光蓄热微胶囊染料
将光蓄热微胶囊与分散剂HLD-106按一定比例在机械搅拌的作用下分散制得分散液。向其中加入适量的粘合剂PPG-2000、增稠剂HF-202和水。纳米铯钨粉、增稠剂与粘合剂的摩尔比为1:3:1。再进行机械搅拌并以2rad/s的速度作用下制得纳米铯钨粉印花浆料。
实施例6
制备基于全波段光蓄热热致变色织物
将纳米铯钨粉浆料通过丝网印花的方式印在真丝织物的一面上。再通过丝网印花方式将温敏变色染料印在真丝织物的另一面上。将印花后的织物在焙烘温度为150℃焙烘5min，得到基于全波段光蓄热热致变色织物。
实验发现，制备出的织物在模拟一个太阳光辐射光照强度下进行照射，在2min时温度达到平衡，平衡温度为38℃，证明织物具有光热转换性能。随之对织物的颜色性能进行测试，，如图2所示，将图2中曲线(a)与曲线(b)进行比较，发现(a)曲线在波长为545nm处出现一个较强的吸收峰，且在此波长处曲线(a)与曲线(b)的K/S 差值在1.5～1.7之间，因此所制备的光蓄热热致变色织物可以出现明显的颜色的变化。
实施例7
对比染料中添加与未添加双组分聚氨酯粘合剂的织物的耐皂洗牢度性能
将染料中添加双组分聚氨酯粘合剂的织物与染料中未添加双组分聚氨酯粘合剂的织物分别与浓度为5g/L的皂液进行混合置于水洗罐中，摇匀，在40℃水温中水洗30min，水洗结束后洗净试样，自然晾干，用灰色样卡对试样贴衬物进行评级，用Photoshop软件对试样进行测色评级。
实验表明，添加了双组分聚氨酯粘合剂的织物的色牢度评级为5级，未添加双组分聚氨酯粘合剂的织物的色牢度评级为4级。由此表明制备织物的过程中使用双组分聚氨酯的两个组分作为粘合剂，会提高织物的耐皂洗牢度。
Claims (10)
1.一种基于全波段光蓄热热致变色织物的制备方法，其特征在于，包括以下步骤：
(1)温敏变色微胶囊染料的制备：以热致变色隐色染料为芯材，二氧化硅为壁材，用溶胶-凝胶法制备出具有温敏变色性能的微胶囊；将温敏变色微胶囊与增稠剂、粘合剂、水按一定比例在机械搅拌的作用下进行共混，制得温敏变色染料；
(2)光蓄热微胶囊染料的制备：以纳米铯钨粉、吲哚菁绿、石墨烯为芯材，三聚氰胺-甲醛树脂/改性SiO2杂化层为壁材，采用原位聚合法制备出具有光蓄热性能的微胶囊；将光蓄热微胶囊与分散剂按一定比例在机械搅拌的作用下分散制得分散液；向其中加入适量的粘合剂、增稠剂和水再进行机械搅拌制得纳米铯钨粉印花浆料；
(3)基于全波段光蓄热热致变色织物的制备：将光蓄热微胶囊染料通过丝网印花的方式印在棉织物的一面上；再通过丝网印花的方式将温敏变色微胶囊染料印在棉织物的另一面上；将印花后的织物在一定温度下焙烘一定时间，得到光蓄热热致变色织物。
2.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(1)中，所述温敏变色微胶囊为聚苯乙烯温变微胶囊、脲醛树脂温变微胶囊、聚甲基丙烯酸酯温变微胶囊、二氧化硅温变微胶囊中的一种。
3.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(1)中，所述增稠剂选用HF-202增稠剂、粘合剂选用MDI增稠剂；温变色微胶囊、增稠剂HF-202与粘合剂MDI的摩尔比为1:1:2-2:2:3。
4.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(2)中，所述光蓄热微胶囊芯材中的纳米铯钨粉的粒径为20-5000nm。
5.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(2)中，所述增稠剂选用HF-202增稠剂、所述粘合剂选用PPG-2000粘合剂；光蓄热微胶囊染料、增稠剂HF-202与粘合剂PPG-2000的摩尔比为1:2:1-1:3:1。
6.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(2)中，所述机械搅拌的速度为2-4rad/s，时间为5-10min。
7.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(3)中，所述印花方式为平网印花和圆网印花的一种。
8.根据权利要求1所述的基于全波段光蓄热热致变色织物的制备方法，其特征在于，步骤(3)中，所述焙烘温度为150-200℃，焙烘时间为5-10min。
9.权利要求1～8任一项所述制备方法所制得的基于全波段光蓄热热致变色织物的应用，其特征在于，包括以下步骤：为全波段光蓄热热致变色织物选择合适的变色温度，在不同光源下进行照射，观察该织物变色现象；通过监控全波段光蓄热热致变色织物的颜色变化，来预防穿着由该织物所制成纺织品的实验者身体被强光灼伤。
10.根据权利要求9所述的基于全波段光蓄热热致变色织物的应用，其特征在于，所述光为紫外光，可见光与红外光。
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