CN116813960A - 一种高反射可调液晶薄膜及其制备方法 - Google Patents
一种高反射可调液晶薄膜及其制备方法 Download PDFInfo
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- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 8
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- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 claims description 4
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- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
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Abstract
本发明公开了一种高反射可调液晶薄膜及其制备方法,原料包括液晶分子、光引发剂、阻聚剂、手性添加剂,质量比为89.8‑86.4:3‑5:0.1‑0.3:4‑8。其制备方法是S1:将原料溶于混合有机溶剂中,于40℃下搅拌混合;S2:将液晶材料,用OSP10#线棒,控制湿膜厚度为6μm均匀涂布在50μm的PET上;S3:将湿膜放到烘箱锡纸或铁板上,烘烤除去溶剂;S4:将膜取出经过UV固化机,固定螺距梯度,得到成型的薄膜;S5、同样的方法在薄膜的另一面涂上掺杂不同旋向的手性添加剂的混合溶液,得到高反射的液晶薄膜。本发明通过光聚合分子本身就可以交联,不需要外加交联剂,能得到规整的液晶排列。
Description
技术领域
本发明涉及液晶技术领域,尤其涉及一种高反射可调液晶薄膜及其制备方法。
背景技术
我国光学膜行业正处在快速发展期,未来还有很大的提升空间。我国反射型光学薄膜需求量与日俱增,发展迅速。
反射型光学薄膜亟待解决以下三方面问题:一是材料分子的精准设计合成原理和技术;二是功能基团、分子链段和凝聚态等不同尺度结构协同取向和三维折光指数精确调控的科学原理;三是光学膜精密流延、拉伸的原理和技术。
从自组装纳米复合高分子功能材料的设计、制备和机理研究的发展进程及现状,我们可以看到鲜有报道。David M.Makow和C.Leroy Sanders在1978年首次提出了采用叠加具有不同反射波带的CLC薄膜的方法来制备具有多个反射波带的液晶薄膜材料。这为CH的应用开创了一个全新的领域。而在实际制备过程中,关键在于如何在不破坏每层CLC薄膜平行取向的前提下来实现不同层CLC的叠加。
发明内容
针对现有技术的不足,本发明提供一种高反射可调液晶薄膜及其制备方法。
为了实现上述目的,本发明的技术方案是:
一种高反射可调液晶薄膜,所述高反射可调液晶薄膜的原料至少包括液晶分子、光引发剂、阻聚剂、手性添加剂,所述液晶分子、光引发剂、阻聚剂、手性添加剂质量比为89.8-86.4:3-5:0.1-0.3:4-8;其中,所述液晶分子为液晶分子A和/或液晶分子B;
所述液晶分子A结构式为:
其中n为3-6;
所述液晶分子B结构式为:
其中m为3-6;
n、m均为整数。
作为对上述技术方案的改进,所述高反射可调液晶薄膜还包括流平剂,所述液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂质量比为89.8-86.4:3-5:0.1-0.3:0.1-0.3:4-8。
作为对上述技术方案的改进,本发明并提供了上述高反射可调液晶薄膜的制备方法,包括如下步骤:
S1:将液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂溶于混合有机溶剂中,于40℃下搅拌混合;
S2:将上述制备好的液晶材料,用OSP10#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有HC或primer的PET上;OSP10#线棒的湿膜间隙为10μm;
S3:涂布完成后,将湿膜放到烘箱锡纸或铁板上,于60℃下烘烤15秒至1min,除去溶剂;
S4:最后将膜取出经过40mj/cm2-800 mj/cm2的UV固化机,固定螺距梯度,得到成型的薄膜;
S5、同样的方法在薄膜的另一面涂上掺杂不同旋向的手性添加剂的混合溶液,得到高反射的液晶薄膜。
作为对上述技术方案的改进,所述光引发剂为光引发剂184、907、1220或MBZ中的一种或多种以任意比混合的混合物。
作为对上述技术方案的改进,所述流平剂为EFKA-3600、BYK355或BYK359。
作为对上述技术方案的改进,所述阻聚剂为对苯二酚或2,6二叔丁基对甲基苯酚。
作为对上述技术方案的改进,所述手性添加剂为S811或R5011。
作为对上述技术方案的改进,所述混合有机溶剂为环己酮、环戊酮和乙酸丁酯中的任意两种以任意比混合的混合物。
与现有技术相比,本发明具有的优点和积极效果是:
1、本发明所采用的丙烯酸酯的液晶化合物,通过光聚合分子本身就可以交联,不需要外加交联剂,能得到规整的液晶排列;2、本发明主要通过控制不同旋向手性添加剂,在薄膜两侧涂布,可得到高反射液晶薄膜,反射率可达80%,同时控制手性添加剂的含量可以调节色彩的变化,得到各种炫彩效果。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案,下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域普通技术人员来讲,在不付出创造性劳动性的前提下,还可以根据这些附图获得其他的附图。
图1为A1核磁图;
图2为B1核磁图;
图3为A2液相图;
图4为实施例1高反射薄膜反射曲线图;
图5为实施例3混合物DSC曲线图;
图6为实施例5制得的薄膜在偏光显微镜下的液晶分子取向图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
本申请先用表一将下述五个实施例的配方比例给以展示。
表一:配方表
实施例1
制备包含如下结构的材料1:
液晶分子A1,其核磁图如1所示,
引发剂184
(1)液晶分子A1的合成
将14.6g(0.05mol)4-(6-丙烯酰氧基己氧基)苯甲酸、12.5g(0.06mol)的N,N-二环己基碳二亚胺(DCC)和40mL二氯甲烷和添加到200mL的单口烧瓶中,室温搅拌并滴加含有3.7g(0.03mol)2-甲基-对羟基苯酚和0.7g(0.005mol)4-二甲胺基吡啶(DMAP)的二氯甲烷溶液100mL,搅拌反应48h之后抽滤除去不溶物,再用5%稀盐酸和5%碳酸氢钠水溶液分别洗涤,后用去离子水洗涤三遍,无水硫酸镁干燥过夜。抽滤除去硫酸镁,再配制二氯甲烷:乙酸丁酯=6:1的混合溶剂作为洗脱剂,通过柱层析法分离提纯得到的产物,真空干燥后得到白色晶体12g。
(2)高反射薄膜材料的制备
称取液晶分子A1(9.28)与光引发剂184(0.3g),流平剂EFKA-3600(0.01g),阻聚剂对苯二酚(0.01g),手性添加剂S811(0.4g)溶于环己酮和环戊酮(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。其反射曲线如图4所示。
实施例2
制备包含如下结构的材料2:
液晶分子A1
液晶分子B1
引发剂907
(1)液晶分子A1的合成
与实施例1中相同
(2)液晶分子B1的合成
29.2(0.1mol)4-(6-丙烯酰氧基己氧基)苯甲酸、16.74g(0.135mol)4-甲氧基酚13.5g(0.066mol)DCC、0.66g(0.006mol)DMAP溶于适量二氯甲烷中,在常温搅拌2天。反应结束后,将沉淀过滤除去,将体系浓缩,倒入正己烷中沉淀,并用正己烷重结晶,得到37.81g4-(6-丙烯酰氧基)己基苯甲酸-4’-甲氧基苯酚酯。
(3)高反射薄膜材料的制备
称取液晶分子A1(4.64g)、B1(4.64g)与光引发剂907(0.3g),流平剂BYK355(0.01g),阻聚剂2,6二叔丁基对甲基苯酚(0.01g),手性添加剂S811(0.4g)溶于环己酮和乙酸丁酯(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。
实施例3
制备包含如下结构的材料3:
液晶分子A2,其液相图如图3所示。
引发剂1220
(1)液晶分子A2的合成
将26.4g(0.1mol)4-(4-丙烯酰氧基丁氧基)苯甲酸、25.0g(0.12mol)的N,N-二环己基碳二亚胺(DCC)和80mL二氯甲烷和添加到200mL的单口烧瓶中,室温搅拌并滴加含有6.2g(0.06mol)2-甲基-对羟基苯酚和1.4g(0.01mol)4-二甲胺基吡啶(DMAP)的二氯甲烷溶液100mL,搅拌反应48h之后抽滤除去不溶物,再用5%稀盐酸和5%碳酸氢钠水溶液分别洗涤,后用去离子水洗涤三遍,无水硫酸镁干燥过夜。抽滤除去硫酸镁,再配制二氯甲烷:乙酸丁酯=6:1的混合溶剂作为洗脱剂,通过柱层析法分离提纯得到的产物,真空干燥后得到白色晶体18.4g。
(2)高反射薄膜材料的制备
称取液晶分子A2(9.28)与光引发剂1220(0.3g),流平剂BYK359(0.01g),阻聚剂对苯二酚(0.01g),手性添加剂S811(0.4g)溶于环戊酮和乙酸丁酯(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。混合物的DSC曲线如图5所示。
实施例4
制备包含如下结构的材料4:
液晶分子A2
液晶分子B2
引发剂BDK
(1)液晶分子A2的合成
与实施例3中相同
(2)液晶分子B2的合成
将26.4g(0.1mol)4-(4-丙烯酰氧基丁氧基)苯甲酸、
16.74g(0.135mol)4-甲氧基酚13.5g(0.066mol)DCC、0.66g(0.006mol)DMAP溶于适量二氯甲烷中,在常温搅拌2天。反应结束后,将沉淀过滤除去,将体系浓缩,倒入正己烷中沉淀,并用正己烷重结晶,得到35.15g白色晶体。
(3)高反射薄膜材料的制备
称取液晶分子A2(4.64g)、B2(4.64g)与光引发剂BDK(0.3g),流平剂BYK359(0.01g),阻聚剂2,6二叔丁基对甲基苯酚(0.01g),手性添加剂S811(0.4g)溶于环己酮和环戊酮(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。
实施例5
制备包含如下结构的材料5:
液晶分子A1
液晶分子B2
引发剂BDK
(1)液晶分子A1的合成
与实施例1中相同
(2)液晶分子B2的合成
与实施例4中相同
(3)高反射薄膜材料的制备
称取液晶分子A1(4.64g)、B2(4.64g)与光引发剂BDK(0.3g),流平剂BYK359(0.01g),阻聚剂对苯二酚(0.01g),手性添加剂S811(0.4g)溶于环戊酮和乙酸丁酯(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。制得的薄膜在偏光显微镜下的液晶分子取向如图6所示。
实施例6
制备包含如下结构的材料6:
液晶分子A2
液晶分子B1,其核磁图如图2所示。
引发剂907
(1)液晶分子A2的合成
与实施例3中相同
(2)液晶分子B1的合成
与实施例2中相同
(3)高反射薄膜材料的制备
称取液晶分子A2(4.64g)、B1(4.64g)与光引发剂907(0.3g),流平剂BYK359(0.01g),阻聚剂对苯二酚(0.01g),手性添加剂S811(0.4g)溶于环己酮和乙酸丁酯(4:1)(23.3g)混合溶剂中,制成固含量为30%的混合溶液。用RDS4#线棒(湿膜间隙10μm),控制湿膜厚度为6μm均匀涂布在50μm的没有任何HC或primer的PET上。60℃烘烤15秒至1min,进行紫外固化,得到液晶薄膜。同样的方法将手性添加剂换成R5011,在薄膜的另一面涂布得到最终高反射液晶薄膜。
将不同质量比例的液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂用以上方法混合,制得不同的高反射薄膜,配方如表1所示。
显然,上述实施例仅仅是为清楚地说明所作的举例,并非对实施方式的限定。对于所属领域的普通技术人员来说,在上述说明的基础上还可以做出其它不同形式变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引申出的显而易见的变化或变动仍处于本发明创造的保护范围之中。
Claims (8)
1.一种高反射可调液晶薄膜,其特征在于:所述高反射可调液晶薄膜的原料至少包括液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂,液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂质量比为89.8-86.4:3-5:0.1-0.3:0.1-0.3:4-8;其中,所述液晶分子为液晶分子A和/或液晶分子B;
所述液晶分子A结构式为:
其中n为3-6;
所述液晶分子B结构式为:
其中m为3-6;
n、m均为整数。
2.如权利要求1所述高反射可调液晶薄膜,其特征在于:所述高反射可调液晶薄膜还包括流平剂,所述液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂质量比为89.8-86.4:3-5:0.1-0.3:0.1-0.3:4-8。
3.一种如权利要求2所述高反射可调液晶薄膜的制备方法,其特征在于:
S1:将液晶分子、光引发剂、流平剂、阻聚剂、手性添加剂溶于混合有机溶剂中,于40℃下搅拌混合;
S2:将上述制备好的液晶材料,用OSP10#线棒,控制湿膜厚度为6μm均匀涂布在50μm的没有HC或primer的PET上;OSP10#线棒的湿膜间隙为10μm;
S3:涂布完成后,将湿膜放到烘箱锡纸或铁板上,于60℃下烘烤15秒至1min,除去溶剂;
S4:最后将膜取出经过40mj/cm2-800 mj/cm2的UV固化机,固定螺距梯度,得到成型的薄膜;
S5、同样的方法在薄膜的另一面涂上掺杂不同旋向的手性添加剂的混合溶液,得到高反射的液晶薄膜。
4.如权利要求3所述制备方法,其特征在于:所述光引发剂为光引发剂184、907、1220或MBZ中的一种或多种以任意比混合的混合物。
5.如权利要求3所述制备方法,其特征在于:所述流平剂为EFKA-3600、BYK355或BYK359。
6.如权利要求3所述制备方法,其特征在于:所述阻聚剂为对苯二酚或2,6二叔丁基对甲基苯酚。
7.如权利要求3所述制备方法,其特征在于:所述手性添加剂为S811或R5011。
8.如权利要求3所述制备方法,其特征在于:所述混合有机溶剂为环己酮、环戊酮和乙酸丁酯中的任意两种以任意比混合的混合物。
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