CN116515340A - 一种胆甾相液晶/高分子复合体系微胶囊及其制备方法 - Google Patents
一种胆甾相液晶/高分子复合体系微胶囊及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种胆甾相液晶/高分子复合体系微胶囊及其制备方法,属于柔性液晶显示领域,其方法如下:以可聚合液晶单体/小分子向列相液晶/手性剂/光引发剂为复合芯材,通过复凝聚法对复合芯材进行包覆,通过紫外固化得到内部液晶分子被聚合网络锚定的胆甾相液晶/高分子复合体系微胶囊。该液晶微胶囊利用高分子网络固定内部体系,优化了液晶微胶囊在力学和光学方面的性能,适用于柔性显示。
Description
技术领域
本发明涉及一种胆甾相液晶/高分子复合体系微胶囊及其制备方法,属于柔性液晶显示技术领域。
背景技术
胆甾相液晶具有颜色鲜艳,反射亮度高,温/电致变色、响应速率快、可调节全光谱显色等优势。但是,液晶材料对环境因素非常敏感,暴露在空气中会造成液晶性能的改变,而且,液晶本身具有流动性,无法直接固着在基材表面,从而限制了液晶的应用范围。
为了保护液晶不受外界污染,防止液晶泄露,研究液晶封装技术对拓宽液晶应用范围并实现液晶产业化具有重要意义。目前,液晶的封装技术主要有液晶盒、液晶聚合物混合体系以及液晶微胶囊化。
液晶盒有尺寸过大、依赖表面处理和制备工艺以达到显色目的、刚性过大等缺陷,无法应用于柔性设备。液晶聚合物混合体系结合了液晶的响应特性和聚合物易于进行机械加工的优势,但是,聚合物网络会干扰液晶分子的理想排布,产生强烈的光散射,影响其颜色性能。因此,近年来在液晶的显示方面,微胶囊技术逐渐成为液晶显示的关键技术。
微胶囊可以保护内部液晶不受污染,同时,由于尺寸小,可以排除角度各向异性,实现全角度显示。但是,液晶被包覆后,会干扰其反射强度,造成显色性能大幅下降。
如何在保护液晶内容物的同时保持其鲜艳的颜色,是液晶微胶囊技术新的研究热点。因此,提供一种胆甾相液晶/高分子复合体系微胶囊,利用微胶囊内部的聚合网络,优化其机械性能与光学性能,提高微胶囊的综合性能,用于柔性液晶显示技术领域,就成为该技术领域亟需解决的技术难题。
发明内容
本发明的目的之一是提供一种胆甾相液晶/高分子复合体系微胶囊,利用微胶囊内部的聚合网络,优化其机械性能与光学性能,提高微胶囊的综合性能,可用于柔性液晶显示领域。
本发明的上述目的是通过以下技术方案达到的:
一种胆甾相液晶/高分子复合体系微胶囊,包括内部的液晶复合体系和外部的明胶-树胶团聚物,内部的复合体系为小分子向列相液晶/手性剂/可聚合液晶单体/光引发剂。
优选地,所述内部的液晶复合体系和外部的明胶-树胶团聚物之间的添加量为5:4-2:3。
优选地,所述明胶与树胶之间的重量比为1:1。
优选地,所述手性剂的质量百分数为2.25%-3.1%,所述可聚合液晶单体的质量百分数为1%-5%,所述光引发剂的质量百分数为0.5%,余量为小分子向列相液晶。
优选地,所述可聚合液晶单体的质量百分数为2%,所述光引发剂的质量百分数为0.5%。
优选地,所述小分子向列相液晶的质量百分数为91.4%-96.25%。
优选地,所述小分子向列相液晶/手性剂/可聚合液晶单体/光引发剂具体为HNG717200-000(江苏和成显示材料有限公司)/S5011/C6M/IGM651。
优选地,所述C6M的质量百分数为1%-5%,S5011的质量百分数为2.25%-3.1%,IGM651的质量百分数为0.5%,余量为HNG717200-000(江苏和成显示材料有限公司)。
优选地,所述HNG717200-000(江苏和成显示材料有限公司)的质量百分数为91.4%-96.25%。
优选地,所述C6M的添加量为2%。
本发明的另一目的是提供上述液晶微胶囊的制备方法。
本发明的上述目的是通过以下技术方案达到的:
一种胆甾相液晶/高分子复合体系微胶囊的制备方法,包括以下步骤:
(1)将手性剂、可聚合液晶单体与小分子向列相液晶按比例混合,水浴加热溶解,或添加二氯甲烷后,烘箱蒸发溶解,得到液晶复合体系;
(2)烧瓶中添加阿拉伯树胶水溶液和PVA水溶液;
(3)称取明胶,水浴加热并搅拌至完全溶解,制备明胶水溶液;
(4)向步骤(1)得到的液晶复合体系中加入光引发剂和二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加,加热搅拌;向烧瓶中加入步骤(3)制得的明胶水溶液,搅拌均匀后,调节pH至3-5;紫外灯照射烧瓶内的反应液,保持加热温度及搅拌速度不变;停止加热,直至反应液降至室温,0-10℃冰水浴,滴加戊二醛或甲醛溶液;
(5)取出反应液,pH调节至8-10,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到液晶微胶囊。
优选的,步骤(1)中,所述手性剂为S5011,所述可聚合液晶单体为C6M,所述小分子向列相液晶为HNG717200-000(江苏和成显示材料有限公司)。
优选的,步骤(4)中,所述紫外灯照射的光照强度为30-120mW/cm2。
有益效果:
本发明的胆甾相液晶/高分子复合体系微胶囊,利用微胶囊内部的聚合网络,优化其机械性能与光学性能,提高微胶囊的综合性能,可用于柔性液晶显示领域。
具体如下:
1,手性剂S5011的添加量不同会使得液晶体系呈现不同的颜色,当添加量为2.25wt%时,体系呈现红色;当添加量为2.70wt%时,体系呈现绿色;当添加量为3.10wt%时,体系呈现蓝色。可通过调控S5011的含量,实现微胶囊在可见光范围内不同波段的显色。
2,可聚合液晶单体C6M对胆甾相液晶/高分子复合体系微胶囊的影响是有益的,在C6M协同胆甾相液晶的自组装中,其作用类似于小分子向列相液晶,与向列相液晶和手性剂共同组装成胆甾相的周期性螺旋结构,经紫外固化后,单体形成聚合物网络,起到稳定微胶囊内部结构的作用。
3,在机械强度方面,可聚合液晶单体的添加改善了微胶囊的坚固程度,破裂率明显减少;在光学性能方面,当体系中可聚合液晶单体添加到一定程度时,会显现出其对液晶的锚定取向作用,提高反射率。
为使本发明的目的、技术方案和优点更加清晰,以下结合附图和具体实施例,对本发明进一步详细说明,但并不意味着对本发明保护范围的限制。
附图说明
图1是本发明实例1中胆甾相液晶/高分子复合体系微胶囊制备流程示意图。
图2-1是仅包覆C6M的液晶微胶囊的偏光图。
图2-2是对比实施例1的微胶囊的偏光图。
图2-3是本发明实例1中胆甾相液晶/高分子复合体系微胶囊的偏光图。
图3是本发明实例1中胆甾相液晶/高分子复合体系微胶囊、C6M和对比实施例1的红外光谱。
图4是本发明实例1、实施例2、实施例3和对比实施例1的反射谱图。
具体实施方式
除非特别说明,本发明下述实施例中,所需原料和助剂均为本技术领域市场可购的常规原料和助剂,所需的反应设备均为常规反应设备,反应条件均为常规条件,所需测试设备和方法均为常规测试设备和方法。
对比实施例1
胆甾相液晶微胶囊的制备,其步骤如下:
(1)将0.054g手性剂S5011和1.946g小分子向列相液晶HNG717200-000(江苏和成显示材料有限公司)混合,60℃水浴加热5h溶解;或添加1ml二氯甲烷后,烘箱蒸发10h溶解,得液晶混合物;
(2)称取1.25g阿拉伯树胶粉末混合30ml去离子水制备阿拉伯树胶水溶液;向烧瓶中加入20ml质量分数为5wt%的PVA水溶液和配置好的阿拉伯树胶水溶液;
(3)称取1.25g明胶,混合30ml去离子水,35℃水浴加热并搅拌至完全溶解,制备得明胶水溶液;
(4)向步骤(1)的液晶混合物中加入1ml二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加,45℃加热搅拌,20min后,加入步骤(3)制备的明胶水溶液,搅拌均匀后,调节pH至4,保持搅拌速率不变,维持3h;停止加热,直至反应液降至室温,0-10℃冰水浴1h,冰水浴半小时后,滴加3ml质量分数为37wt%的戊二醛或甲醛溶液;
(5)取出反应液,pH调节至9,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到微胶囊。
实施例1
如图1所示,为本发明实施例1中胆甾相液晶/高分子复合体系微胶囊制备流程示意图;
胆甾相液晶/高分子复合体系微胶囊的制备,其步骤如下:
(1)将0.054g手性剂S5011、0.04g可聚合液晶单体C6M、0.01g光引发剂IMG651与1.896g小分子向列相液晶HNG717200-000(江苏和成显示材料有限公司)混合,水浴加热溶解或添加1ml二氯甲烷后,烘箱蒸发溶解,得到液晶复合体系,期间严格避光;
(2)称取1.25g阿拉伯树胶粉末混合30ml去离子水制备阿拉伯树胶水溶液。向烧瓶中加入20ml质量分数为5wt%的PVA水溶液和配置好的阿拉伯树胶水溶液;
(3)称取1.25g明胶,混合30ml去离子水,35℃水浴加热并搅拌至完全溶解,制备明胶水溶液;
(4)向步骤(1)得到的液晶复合体系中加入1ml二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加,45℃加热搅拌;20min后,向烧瓶中加入步骤(3)制得的明胶水溶液,搅拌均匀后,调节pH至4,保持搅拌速率不变,维持2h;紫外灯照射烧瓶内的反应液,保持加热温度及搅拌速度不变,时间1h,紫外灯固化前应严格避光反应;停止加热,直至反应液降至室温,0-10℃冰水浴1h,冰水浴0.5h时,滴加3ml质量分数为37wt%的戊二醛或甲醛溶液;
(5)取出反应液,pH调节至9,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到液晶微胶囊。
实施例2
胆甾相液晶/高分子复合体系微胶囊的制备,其步骤如下:
(1)将0.054g手性剂S5011、0.02g可聚合液晶单体C6M、0.01g光引发剂IMG651与1.916g小分子向列相液晶HNG717200-000(江苏和成显示材料有限公司)混合,水浴加热10h溶解或添加1ml二氯甲烷后,烘箱蒸发溶解,得到液晶复合体系,期间严格避光;
(2)称取1.25g阿拉伯树胶粉末混合30ml去离子水制备阿拉伯树胶水溶液;向烧瓶中加入20ml质量分数为5wt%的PVA水溶液和配置好的阿拉伯树胶水溶液;
(3)称取1.25g明胶,混合30ml去离子水,35℃水浴加热并搅拌至完全溶解,制备明胶水溶液;
(4)向步骤(1)得到的液晶复合体系中加入1ml二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加,45℃加热搅拌;20min后,向烧瓶中加入步骤(3)制得的明胶水溶液,搅拌均匀后,调节pH至4,保持搅拌速率不变,维持2h;紫外灯照射烧瓶内的反应液,保持加热温度及搅拌速度不变,时间1h,紫外灯固化前应严格避光反应;停止加热,直至反应液降至室温,0-10℃冰水浴1h,冰水浴0.5h时,滴加3ml质量分数为37wt%的戊二醛或甲醛溶液;
(5)取出反应液,pH调节至9,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到液晶微胶囊。
实施例3
胆甾相液晶/高分子复合体系微胶囊的制备,其步骤如下:
(1)将0.054g手性剂S5011、0.10g可聚合液晶单体C6M、0.01g光引发剂IMG651与1.836g小分子向列相液晶HNG717200-000(江苏和成显示材料有限公司)混合,水浴加热溶解或添加1ml二氯甲烷后,烘箱蒸发溶解,得到液晶复合体系,期间严格避光;
(2)称取1.25g阿拉伯树胶粉末混合30ml去离子水制备阿拉伯树胶水溶液;向烧瓶中加入20ml质量分数为5wt%的PVA水溶液和配置好的阿拉伯树胶水溶液;
(3)称取1.25g明胶,混合30ml去离子水,35℃水浴加热并搅拌至完全溶解,制备明胶水溶液;
(4)向步骤(1)得到的液晶复合体系中加入1ml二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加,45℃加热搅拌;20min后,向烧瓶中加入步骤(3)制得的明胶水溶液,搅拌均匀后,调节pH至4,保持搅拌速率不变,维持2h;紫外灯照射烧瓶内的反应液,保持加热温度及搅拌速度不变,时间1h,紫外灯固化前应严格避光反应;停止加热,直至反应液降至室温,0-10℃冰水浴1h,冰水浴0.5h时,滴加3ml质量分数为37wt%的戊二醛或甲醛溶液;
(5)取出反应液,pH调节至9,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到液晶微胶囊。
用LEICA DM2700 M偏振光学显微镜,在室温环境下,对待测样品进行表征。如图2-1所示,是仅包覆可聚合液晶单体C6M的微胶囊的偏光图;如图2-2所示,是对比实施例1的微胶囊的偏光图;如图2-3所示,是本发明实例1中胆甾相液晶/高分子复合体系微胶囊的偏光图;当芯材仅为可聚合液晶单体C6M时,微胶囊的内部呈白色,没有出现马耳他十字交叉条纹现象,而在图像中可以观察到明显的双折射现象,这是因为C6M也具有液晶性,但并不具有小分子向列相液晶的流动性所致;对比实施例1内部有明显的马耳他十字交叉条纹,并且微胶囊内部的颜色更加明亮;而本发明实施例1内部同时具有C6M和小分子液晶HNG717200-000(江苏和成显示材料有限公司)的特点,微胶囊中心呈白色,且内部有明显的马耳他十字条纹;证明C6M被包覆在微胶囊中。
用Nicolet IS10傅里叶变换红外光谱仪,将待测样品与溴化钾(KBr)粉末共混研磨均匀,压制成原片后测量微胶囊样品(对比实施例1和实施例1)和可聚合液晶单体C6M的红外光谱。如图3所示,是本发明实例1中胆甾相液晶/高分子复合体系微胶囊、C6M和对比实施例1的红外光谱;实施例1和C6M在1607cm-1处和1513cm-1处有相同特征峰,该峰是由C6M中苯环的骨架振动引起,而对比实施例1在此处没有特征峰,说明C6M被成功封装在实施例1中。
用AvaSpec-2048FT-SPU光纤光谱仪对实施例1、实施例2、实施例3和对比实施例1的样品进行测试,如图4所示,是本发明实例1、实施例2、实施例3和对比实施例1的反射波谱图;从反射波谱图中可以看出,C6M参与后,提高了微胶囊的反射率,这是由于C6M聚合后对液晶分子有锚定取向作用,固定住液晶分子,使得微胶囊反射率有大幅提高;但C6M添加量过高,当添加至5wt%时,由于C6M本身呈白色,反而降低了反射率,但聚合网络稳定了微胶囊的内部结构,机械性能有大幅提升。
应用实施例1
胆甾相液晶/高分子复合体系微胶囊在柔性显示器件方面的应用
本发明实施例1中的液晶微胶囊具有良好的可塑性,可附着在柔性基板上进行使用,可将微胶囊混合PVA水溶液和明胶水溶液,涂敷在PET薄膜或其他柔性基材固化成液晶薄膜,且基于胆甾相液晶特有的光学性质,可实现反射式、双稳态彩色显示,在柔性显示方面拥有广阔的应用前景。
应用实施例2
胆甾相液晶/高分子复合体系微胶囊在防伪油墨方面的应用
液晶油墨是构成防伪油墨的基础,可用于包装、证件防伪、广告画册等。本发明实施例1中的液晶微胶囊可用于制造油墨或具有偏振效果的光变颜料。通过加入油墨粘接剂即可制成在室温下稳定存在、颜色亮丽、具有特殊防伪效果的高级油墨。将微胶囊与水溶性的树脂、连接料、助剂等混合,可组成具有一定触变性和流变性的印刷油墨。
本发明的胆甾相液晶/高分子复合体系微胶囊将可聚合液晶单体添加至胆甾相液晶中,形成液晶复合体系,然后通过复凝聚法将其包覆成微胶囊。由于C6M相当于小分子向列相液晶,所以,本发明人设计将小分子向列相液晶和可聚合液晶单体协同组装成胆甾相螺旋结构进行反应,在不改变其内部结构和反射波段的基础上,制备出改良的液晶微胶囊。
本发明通过可聚合液晶单体的聚合网络改良液晶微胶囊,以此提高其机械性能与光学性能。
本发明的主要创新点为将可聚合液晶单体引入微胶囊的芯材中,采用小分子向列相液晶/可聚合液晶单体/手性剂/引发剂复合体系,通过复凝聚法,将制备的微胶囊作为微反应器,通过紫外自由基聚合法将芯材制备成胆甾相液晶/高分子网络复合体系,调控微胶囊中液晶的取向,提高其光学反射率,提高其力学强度,最终得到兼顾高反射率和力学性能的胆甾相液晶/高分子复合体系微胶囊,该材料可用于反射式液晶显示器、光增亮膜、滤色片等。
以上所述具体实施例,对本发明的目的、技术方案和有益效果进行了进一步详细说明,但并不限制本发明,凡在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (10)
1.一种胆甾相液晶/高分子复合体系微胶囊,包括内部的液晶复合体系和外部的明胶-树胶团聚物,内部的复合体系为小分子向列相液晶/手性剂/可聚合液晶单体/光引发剂。
2.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述手性剂的质量百分数为2.25%-3.1%,所述可聚合液晶单体的质量百分数为1%-5%,所述光引发剂的质量百分数为0.5%,余量为小分子向列相液晶。
3.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述可聚合液晶单体的质量百分数为2%,所述光引发剂的质量百分数为0.5%。
4.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述小分子向列相液晶的质量百分数为91.4%-96.25%。
5.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述小分子向列相液晶/手性剂/可聚合液晶单体/光引发剂具体为HNG717200-000/S5011/C6M/IGM651。
6.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述C6M的质量百分数为1%-5%,S5011的质量百分数为2.25%-3.1%,IGM651的质量百分数为0.5%,余量为HNG717200-000。
7.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述HNG717200-000的质量百分数为91.4%-96.25%。
8.根据权利要求1所述胆甾相液晶/高分子复合体系微胶囊,其特征在于:所述C6M的添加量为2%。
9.权利要求1-8中任一项所述胆甾相液晶/高分子复合体系微胶囊的制备方法,其步骤如下:
(1)将手性剂、可聚合液晶单体、光引发剂与小分子向列相液晶按比例混合,水浴加热溶解,或添加二氯甲烷后,烘箱蒸发溶解,得到液晶复合体系;
(2)烧瓶中添加阿拉伯树胶水溶液和PVA水溶液;
(3)称取明胶,水浴加热并搅拌至完全溶解,制备明胶水溶液;
(4)向步骤(1)得到的液晶复合体系中加入二氯甲烷,溶解至澄清后,将吸管伸入步骤(2)中烧瓶内液体的液面以下,缓慢滴加并加热搅拌;向烧瓶中加入步骤(3)制得的明胶水溶液,搅拌均匀后,调节pH至3-5;紫外灯照射烧瓶内的反应液,保持加热温度及搅拌速度不变;停止加热,直至反应液降至室温,0-10℃冰水浴,滴加戊二醛或甲醛溶液;
(5)取出反应液,pH调节至8-10,多次水洗,直待溶液澄清后,用吸管吸取上层清液,即可得到液晶微胶囊。
10.根据权利要求9所述胆甾相液晶/高分子复合体系微胶囊的制备方法,其特征在于:步骤(1)中,所述手性剂为S5011,所述可聚合液晶单体为C6M,所述小分子向列相液晶为HNG717200-000,所述光引发剂为IGM651;步骤(4)中,所述紫外灯照射的光照强度为30-120mW/cm2。
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