CN108003368B - 一种变色片 - Google Patents
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- CN108003368B CN108003368B CN201711353718.9A CN201711353718A CN108003368B CN 108003368 B CN108003368 B CN 108003368B CN 201711353718 A CN201711353718 A CN 201711353718A CN 108003368 B CN108003368 B CN 108003368B
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Abstract
本发明公开了一种变色片,解决了现有变色片变色能力有待提高的问题,技术方案包括基材,在基材的外表面至少覆盖有下变色层和上变色层,所述上变色层的初始吸光率大于上变色层初始吸光率。本发明结构简单、易于生产制造、在不改变变色材料以及变色片的高分子材料种类的前提下,就可以有效地改善变色片的变色性。
Description
技术领域
本发明涉及一种光致变色制品,具体的说是一种变色片。
背景技术
光致变色材料变色的机理是光变材料吸收紫外光后,发生分子状态改变,以另一种结构或者聚集态存在。同时对可见光的吸收率大幅增加。然后在热作用或者其它方式下,可逆地回到初始状态,同时对可见光的吸收率大幅缩小。已知的某些光致变色装置,如光致变色眼镜、调光玻璃,是将变色材料分散在聚合物中,以渗透、镀膜、浇铸等方式形成具有变色能力的装置(此类装置基本上是平面状,因此本文称为变色片)。由于某些原因,光致变色材料在不变色时也具有较浅颜色,因此需要通过调配变色材料的种类以及固定色调染料来调整变色片初始颜色(初始颜色:指不变色时的颜色)。通过这些方法使得变色片看上去是无色透明。
但是实际上,在不变色时,变色片对光有明显吸收,多数的产品经过测试,在不计算光线反射损失时,对可见光吸收率约9%-12%。为了不使该吸收率过高,不得加入过多变色材料。
另一方面,为了保证变色片的变色能力,变色材料的添加量不可以过少,否则变色性能不足。变色片曝露于日照下。若可见光(400-650nm)平均透过率小于20%时,则可看出变色非常良好。若可见光平均透过率大于40%,则会感觉变色片变色功能弱。尤其是当气温较高时,变色材料性能有所下降,常常会使得变色片变色能力弱。
研究人员希望在不增加变色片初始吸光率的情况下,增强变色片的变色性能。为了解决上述问题,大部分研究者集中于考虑设计一种更加优秀的变色材料如更浅的初始吸光率或者更强的变色强度、更好的可溶解性、更佳紫外吸收区间等,或者使用性能优异的变色片高分子材料与变色材料匹配使用,以达到变色片初始颜色变浅同时变色性增强的目的,显然,这种新材料的研发是一个工作量大、漫长且困难重重的过程。
目前,变色片的结构通常包括基材及覆盖在基材上的变色层,目前已有报导在基材上覆盖单层或多层变色层,如公开号CN101668714A公开了一种多层光致变色板,包括氧或水分防护阻隔隔膜,和至少两层或者更多层的光致变色膜,其通过对不同功能层的组合和原料的选择,以获得优异耐久性好和外观的光致变色玻璃。又如公开号为CN105017698B公开了一种光热响应型智能节能复合膜,可用于制备一层或多层交替复合的变色膜,其原料中使用了含螺吡喃可逆光致变色和含二氧化钒基可逆致变色物质组成,具有变色效果好、抗老色性能好的优点。综上,现有公开的各种结构的变色片大多基于解决耐久性或新材料方法的研发,并无更好的方法,在不改变变色材料以及变色片的高分子材料种类的前提下,就可以有效地改善变色片的变色性。
发明内容
本发明的目的是为了解决上述技术问题,提供一种结构简单、易于生产制造、在不改变变色材料以及变色片的高分子材料种类的前提下,就可以有效地改善变色片的变色性的变色片。
技术方案在基材的外表面至少覆盖有下变色层和上变色层,所述上变色层的吸光率大于下变色层吸光率。
所述下变色层初始吸光率为0-5%,上变色层初始吸光率为5-25%,且两层变色片初始吸光率之差大于1%。这里所述吸光率为:以不含有变色膜层的基材CR39作测试参照,测量可见光在400-650nm波长的平均吸收率。
所述下变色层初始吸光率为1-5%,上变色层初始吸光率为5-10%,上变色层减下变色层的吸光率之差大于1%。
所述上、下变色层至少由聚合物材料和有机光致变色材料混合而成,其中,所述聚合物材料为聚氨酯。
所述聚氨酯为预聚体和扩链剂反应生成的-NCO封端的聚合物,其中,所述扩链剂至少包含-OH或者-SH基团中一种。
所述预聚体中-NCO的摩尔量相对于所述扩链剂中-OH或者-SH的摩尔量≥5%。
所述预聚体由多官能二异氰酸酯和多元醇混合反应而成;
其中,所述多官能二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、六亚甲基二异氰酸酯三聚体中的一种或多种;
其中,所述多元醇为聚丙二醇、聚四氢呋喃、聚碳酸酯多元醇、聚酯多元醇、聚酯多元醇中的一种或多种。
所述有机光致变色材料为萘并吡喃类化合物。
所述聚氨酯具有在涂覆30微米厚度时,能够对320-400nm紫外线的吸收率小于50%性能。
所述上、下变色层的固化成膜温度为90-120摄氏度。
针对背景技术中存在的问题,发明人改变思路,在材料种类不变的情况下,分析影响变色强度的因素分别为:紫外线强度、变色材料的量、紫外线在不同变色材料间的分配、温度等。在其它条件不变的前提下,得出合理地给不同的变色材料分配紫外线,就能够强化变色片的变色效果的结论。而为了实现不同的变色材料分配紫外线的目的,可以考虑采用在基材上覆盖不同初始吸光率的变色层的方法实现。
基上述研究,发明人将初始吸光率较低变色材料置于下变色层,初始吸光率较高的变色材料置于上变色层(接触光照层)。其目的是让上变色层获得更多光照,增强变色能力,而下变色层的变色材料初始吸光率低,两者的互补作用,会使变色片的初始透光率不会降低,从而达到不降低变色片的初始透光率,而增加变色能力的目的。
进一步的,为了尽可能提高其变色能力,上变色片和下变色片的初始吸光率最好保持在限定的差度范围内,即至少大于1%的初始吸光率差,优选的是大于2%吸光率差。否则难以起到提升变色强度的效果。
本发明并不对各层材料及制备工艺进行特别限定,可使用现有领域中常用的材料及制备方法制造。
所述基材应为可接受光致变色涂层的基材,其原料可以根据应用领域和环境条件不同进行合理选择,包括但不仅限于PET、聚硫氨酯、PC、尼龙、CR-39中的至少一种。可以采用例如模具浇铸法制备,上、下变色层的固化成膜温度优选为90-120摄氏度,过高会使变色材料分解,过低会因为长时间未固化而缩边。包括上变色层和下变色层在内的变色层含有聚合物材料和有机光致变色材料,聚合物材料优选聚氨酯,进一步优选满足在涂覆30微米厚度时,能够对320-400nm紫外线的吸收率小于50%性能,这类聚氨酯具有不影响变色材料利用紫外线的特点,能进一步提高变色片的变色能力。具体地,所述聚氨酯为预聚体和扩链剂反应生成的异氰酸酯封端的聚合物,其中,所述扩链剂至少包含-OH或者-SH基团中一种。所述扩链剂可以列举出:2,2-二羟甲基丁醇、1,2-丙二醇、巯基乙醇、三硫代二乙二醇、2,3-二硫代(2-巯基)-1-丙烷硫醇、巯基丙酸季戊四醇酯、丙二硫醇、丁二硫醇等。
所述预聚体中-NCO的摩尔量相对于所述多元醇中-OH的摩尔量≥5%。其中,预聚体由多官能二异氰酸酯和多元醇混合反应而成。所述多官能二异氰酸酯可以列举出:异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、六亚甲基二异氰酸酯三聚体等;优选异佛尔酮二异氰酸酯,这是由于异佛尔酮二异氰酸酯具有独特的化学结构,它与其他的脂肪/环脂族二异氰酸酯不同,异佛尔酮二异氰酸酯具有一个环己酮体系,三个甲基和两个不同的异氰酸酯基团,三个甲基使异佛尔酮二异氰酸酯几乎与各种树脂溶剂互溶,使用异佛尔酮二异氰酸酯制备的变色片具有良好的丰满度和较强的那化学性能。
所述多元醇可以列举出:聚丙二醇、聚四氢呋喃、聚碳酸酯多元醇、聚酯多元醇等;优选聚丙二醇、聚四氢呋喃,最优选聚丙二醇,这是由于聚丙二醇对制备聚氨酯稳定性有明显的影响,使用聚丙二醇作为多元醇制备的变色片不存在缩水、黑点、白雾、水纹、晶点、麻点、垂流、积液等不良现象。
所述有机光致变色材料为萘并吡喃类化合物,优选螺吡喃、俘精酸酐、螺吡嗪等,在制备所述上、下变色层时,还可加入溶剂溶解原料,所述溶剂可以列举出二甲基甲酰胺、N-甲基吡咯烷酮、乙酸乙酯、二乙二醇二甲醚、乙二醇二甲醚、乙酸丁酯、二氯乙烷、丙二醇二甲醚等,所述变色材料:聚氨酯材料:溶剂三者的质量比优选为2-10:100:10-30。还可根据需要添加各种添加剂,如抗氧剂、抗光老化剂、催化剂或表面活性剂等。变色层可通过渗透、镀膜、浇铸等方式涂覆在基材上。除上变色层和下变色层外,在基材上还可根据需要添加隔离层、粘合层、保护层、变色层、染色层等,此为现有技术,在此不作详述。本发明也不限定在上、下变色层之间再增加新的变色层的可能。所述上、下变色层具体颜色的选择在满足上述吸光率条件下,可根据产品需求合理设置,以满足不同产品功能及外观上的要求。
本发明结构极为简单、构思巧妙、易于生产制造、可完全利用现有的材料和工艺方法,在不改变变色材料以及变色片的高分子材料种类的前提下,有效地改善变色片的变色性,达到不降低变色片的初始透光率,而增加变色能力的目的,本发明变色片可用于光致变色眼镜、调光玻璃等涉及需要具有变色能力的装置,具有广阔的市场应用前景。
附图说明
图1为本发明结构示意图。
其中,1-基材、2-下变色层、3-上变色层。
具体实施方式
参见图1,本发明变色片至少包括供变色层附着的基材1、覆盖在基材1上表面的下变色层2,和覆盖在下变层2上的上变色层。其中,所述下变色层初始吸光率为0-5%,上变色层初始吸光率为5-25%,且上变色层初始吸光率减去下变色层初始吸光率大于1%。作为优选,所述下变色层初始吸光率为1-5%,上变色层初始吸光率为5-10%,且上变色层初始吸光率减去下变色层初始吸光率大于1%。
作为示例,提供变色片的制造实施例,但该实施例并非限定了本发明变色片的制造,本领域技术人员还可根据需要选择其它合适的制造方法。
实施例1(所述百分数为质量百分数,比值为质量比):
使用了CR-39圆片作为基材,使用5%氢氧化钾水溶液在60摄氏度浸泡10分钟进清洗,然后用肥皂水、去离子水清洗,使用压缩空气干燥。将该基材用等离子清洗机清洗:在50ml/mi n的氧气流,小于0.5mm汞柱的压强下,处理60秒。然后在该基材上旋涂下变色层的涂覆液,通过控制转速,使涂层厚度为18μm,旋涂成膜后,将此圆片放于氮气烘箱中100摄氏度干燥4小时。取出圆片,冷却后,旋涂第二光致变色层涂覆液,涂覆厚度为12μm,旋涂成膜后,将此圆片放于氮气烘箱中100摄氏度干燥4小时即得变色片1。
所述变色层涂覆液制备方法为:将光致变色材料、聚氨酯材料和溶剂混合制成聚氨酯溶液,然后加入聚氨酯溶液质量(100%计)1%的抗氧剂245、0.5%的抗光老化剂622、0.05%的催化剂二丁基二氯化锡、0.1%硅氧烷表面活性剂DC-57。
涂覆液中聚氨酯材料由预聚体和扩链剂反应生成,预聚体由异佛尔酮二异氰酸酯(IPDI)与聚丙二醇(PPG1000)摩尔比为2:1混合反应而成,扩链剂为2,2-二羟甲基丁醇(TMP),预聚体中-NCO相对于扩链剂TMP中-OH的摩尔量的羟基过量5%。涂覆液中有机光致变色材料为萘并吡喃类化合物。
上、下变色层的制备方法均与上述相同,所不同的是:上变色层制备时,聚氨酯溶液中变色材料:聚氨酯材料:溶剂=1:22:5,上变色层使用的变色材料初始吸光率高。下变色层制备时聚氨酯溶液中变色材料:聚氨酯材料:溶剂=1:22:5,下变色层使用的变色材料初始吸光率低。应当指出的是,下变色层中的变色材料用量最好要满足变色后获得中性颜色。此处中性颜色指在CI E颜色体系中,颜色的CIE坐标(x,y)x值为0.2至0.5,y值为0.2至0.4,呈现灰色、棕色以及类似于灰色或棕色的颜色。
将试样放置在光具座上,使用FLAME光纤光谱仪测试该试样透过率(400-650nm),为85%。使用中教金源提供的摸拟日光氙灯,调整UVA强度为3W/m2(使用UVA光度计确保紫外强度)。在22摄氏度下照射试样,试样变为黑灰色,透光率下降。当透过率降至恒定值时,读取光纤光谱仪的透过率,为饱和透过率。
实施例2-6的方法与实施例1相同,所不同之处见表1、2。
表1实施例1-6聚氨酯材料制备原料
表2实施例1-6变色片工艺参数及表征结果
对比实施例1
使用了CR-39(折射率为1.49)圆镜片作为基材,使用5%氢氧化钾水溶液在60摄氏度浸泡10分钟进清洗,然后用肥皂水、去离子水清洗,使用压缩空气干燥。将该基材用等离子清洗机清洗:在50ml/min的氧气流,小于0.5mm汞柱的压强下,处理60秒,然后在该层上旋涂光致一层变色层,涂覆厚度为27μm。旋涂成膜后,将此圆片放于氮气烘箱中100摄氏度干燥4小时。
所述变色层制备方法为:将光致变色材料(注:变色材料种类与实施例1相同,但是比例不同,其比例为1:1.2,其变色后的色调和实施例1一致)溶于DMF,然后加入总质量的1%的抗氧剂245、0.5%的抗光老化剂622、0.05%的催化剂二丁基二氯化锡、0.1%的硅氧烷表面活性剂DC-57、聚氨酯材料。其中,所述聚氨酯溶液中变色材料:聚氨酯材料:溶剂=1:22:5。
对比实施例2
与对比实施例1相同,不同在于:烘箱干燥温度为80℃。
对比实施例3
与对比实施例1相同,不同在于:将变色层增厚至31μm以期望增加变色强度。
对实施例和对比例的通过率和变化能力进行测试,测试结果见表3。
表3
实施例编号 | 初始透过率 | 饱和透过率 | 有无缩边 |
对比实施例1 | 84.3% | 25.8% | 缩边可忽略 |
对比实施例2 | 84.3% | 25.8% | 明显缩边 |
对比实施例3 | 83.1% | 23.9% | 缩边可忽略 |
通过测试,实施例1与对比实施例1-3的初始透过率均接近。在模拟日光条件下,饱和变色后,实施例1的饱和透过率为22.1%,而对比实施例1、2、3分别为25.8%、25.8%、23.9%,且对比实施例2有明显缩边情况发生。相比于对比实施例,本发明变色片的变色能力明显增强,无缩边问题。
Claims (9)
1.一种变色片,包括基材,其特征在于,在基材的外表面至少覆盖有下变色层和上变色层,所述下变色层初始吸光率为0-5%,上变色层初始吸光率为5-25%,所述上变色层的初始吸光率大于下变色层初始吸光率,且两层变色层初始吸光率之差大于1%。
2.如权利要求1所述的变色片,其特征在于,所述下变色层初始吸光率为1-5%,上变色层初始吸光率为5-10%,且两层变色层初始吸光率之差大于1%。
3.如权利要求1所述的变色片,其特征在于,所述上、下变色层至少由聚合物材料和有机光致变色材料混合而成,其中,所述聚合物材料为聚氨酯。
4.如权利要求3所述的变色片,其特征在于,所述聚氨酯为预聚体和扩链剂反应生成的-NCO封端的聚合物,其中,所述扩链剂至少包含-OH或者-SH基团中一种。
5.如权利要求4所述的变色片,其特征在于,所述预聚体中-NCO的摩尔量相对于所述扩链剂中-OH或者-SH的摩尔量≥5%。
6.如权利要求4或5所述的变色片,其特征在于,所述预聚体由多官能二异氰酸酯和多元醇混合反应而成;
其中,所述多官能二异氰酸酯为异佛尔酮二异氰酸酯、六亚甲基二异氰酸酯、苯二亚甲基二异氰酸酯、六亚甲基二异氰酸酯三聚体中的一种或多种;
其中,所述多元醇为聚丙二醇、聚四氢呋喃、聚碳酸酯多元醇、聚酯多元醇中的一种或多种。
7.如权利要求3所述的变色片,其特征在于,所述有机光致变色材料为萘并吡喃类化合物。
8.如权利要求3所述的变色片,其特征在于,所述聚氨酯具有在涂覆30微米厚度时,能够对320-400nm紫外线的吸收率小于50%的性能。
9.如权利要求1-3任一项所述的变色片,其特征在于,所述上、下变色层的固化成膜温度为90-120摄氏度。
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