CN111716843B - 一种3d显影高分子薄膜及其制备方法 - Google Patents

一种3d显影高分子薄膜及其制备方法 Download PDF

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CN111716843B
CN111716843B CN202010594586.4A CN202010594586A CN111716843B CN 111716843 B CN111716843 B CN 111716843B CN 202010594586 A CN202010594586 A CN 202010594586A CN 111716843 B CN111716843 B CN 111716843B
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polyacrylonitrile
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刘鉴联
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Guangzhou Xinglianda Plastic Products Co ltd
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Abstract

本发明公开一种3D显影高分子薄膜，包括第一发光层、第二发光层、第三发光层和基材层，第一发光层、第二发光层、第三发光层和基材层从上往下依次安装，第三发光层安装在基材层上表面，第二发光层安装在第三发光层一侧表面，第一发光层一侧与第二发光层连接；本发明还公开了一种3D显影高分子薄膜的制备方法；热处理过程中聚氨酯融在聚丙烯腈表面，聚丙烯腈表面形成致密结构，光照射在复合膜表面后反射作用减弱，光损失率降低，所以该复合膜具有优异的透明度，解决了现有技术中通过聚丙烯腈制备透明纤维膜，但是制备过程中由于自身限制，透明膜的透光性能较低，无法满足高清晰3D显影的要求等技术问题。

Description

一种3D显影高分子薄膜及其制备方法
技术领域
本发明属于高分子薄膜技术领域，具体为一种3D显影高分子薄膜及其制备方法。
背景技术
透明投影屏幕是使观众隔着屏幕能看到屏幕后面的景物，又能看清屏幕上投影图像的特殊投影屏幕，具有隔空悬物魔幻成像的3D神奇效果。现有的透明投影屏幕技术主要是全息投影膜，这种膜是在塑料基材上用精密加工技术压印出微观的“坑坑点点”，使入射投影光在其表面的透射、反射和散射有个合理分布，要求其透明性好，则其成像性就差，反之要求其成像性好，则其透明性自然就差，譬如说入射投影光有50％的光透射，则可能有30％的光前散射，20％的光背散射，成像效果正投和背投都差不多。
中国发明专利CN108628080A一种全息投影膜及其制备方法和应用，所述全息投影膜自上而下依次包括第一导电层、聚合物分散液晶层和第二导电层，所述聚合物分散液晶层中分散有光扩散粒子。所述制备方法包括在第一导电层上涂布聚合物分散液晶，贴合第二导电层后，聚合物分散液晶固化为聚合物分散液晶层，即得。本发明所述的全息投影膜通过在聚合物分散液晶层中添加光扩散粒子，使得所述全息投影膜在通电透明状态下的雾度可调，使得所述全息投影膜在通电和不通电的状态下均可投影显示。
发明内容
为了克服上述的技术问题，本发明提供一种3D显影高分子薄膜及其制备方法。
本发明所要解决的技术问题：
(1)通过膨润土和纳米二氧化硅制备扩散粒子时，由于膨润土自身层间距较小，导致复合后结构不稳定，而且不具有阻燃性能，不能对显影膜进行保护。
(2)现有技术中通过聚丙烯腈制备透明纤维膜，但是制备过程中由于自身限制，透明膜的透光性能较低，无法满足高清晰3D显影的要求。
本发明的目的可以通过以下技术方案实现：
一种3D显影高分子薄膜，包括第一发光层、第二发光层、第三发光层和基材层，第一发光层、第二发光层、第三发光层和基材层从上往下依次安装，第三发光层安装在基材层上表面，第二发光层安装在第三发光层一侧表面，第一发光层一侧与第二发光层连接；
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35-45℃水浴加热并磁力搅拌20-30min，之后加入连二亚硫酸钠，升温至55-65℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶35-40∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10％的N,N-二甲基甲酰胺和浓度为15％的N,N-二甲基甲酰胺中，35-45℃下超声10-12h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜。
第一步中先将聚丙烯腈通过10％碳酸钠溶液和连二亚硫酸钠进行初步处理，之后第二步中将聚丙烯腈粉末和聚氨酯粉末在不同浓度的N,N-二甲基甲酰胺中混合，制备出不同浓度的纺丝液，之后将按照2∶1的重量比混合后进行静电纺丝，制得复合纤维膜，之后通过对该复合纤维膜进行热处理制得复合透明纤维膜，该复合纤维膜以聚丙烯腈为内层，聚氨酯为表层，热处理过程中聚氨酯融在聚丙烯腈表面，聚丙烯腈表面形成致密结构，光照射在复合膜表面后反射作用减弱，光损失率降低，所以该复合膜具有优异的透明度。
进一步地，第二步中热处理的具体步骤为：将复合纤维膜固定，之后转移至真空干燥箱中，控制真空干燥箱的温度为180-200℃，干燥时间为4h，之后升温至200-220℃，在此温度下干燥6h，之后升温至220-230℃，在此温度下保温10h。
进一步地，所述第一发光层表面安装有扩散粒子，所述扩散粒子为纳米复合粒子，该纳米复合粒子的粒径为200-800nm。
进一步地，所述纳米复合粒子由如下方法制成：
步骤S1、将膨润土、尿素和乙醇按照3∶5∶1的重量比混合均匀，之后加入三口烧瓶中，45-55℃水浴加热并以120r/min的转速搅拌3-4h，制得混合浆料，抽滤并用35-40℃去离子水洗涤三次，之后用无水乙醇洗涤三次，烘干，研磨，制得改性膨润土；
步骤S2、将改性膨润土和纳米二氧化硅混合，以1000r/min的转速搅拌40min，制得复合粒子前驱体，之后加入六甲基二硅氮烷，磁力搅拌15-30min后升温至100℃，在此温度下反应4-5h，过滤，用去离子水洗涤三次，制得纳米复合粒子，控制改性膨润土、纳米二氧化硅、六甲基二硅氮烷的重量比1∶2∶50-60。
步骤S1中膨润土、尿素和乙醇按照3∶5∶1的重量比混合，对膨润土进行插层改性，通过将尿素作为插层剂，一方面能够增大膨润土中蒙脱石的层间距，为其它分子进入蒙脱石提供空间，另一方面当制得的改性高岭土燃烧时能够分解出氨气，对燃烧过程进行阻碍，赋予第一发光层表面一定的阻燃性能；步骤S2中将改性高岭土和纳米二氧化硅混合，通过六甲基二硅氮烷进行修饰，二氧化硅表面的羟基能够与六甲基二硅氮烷发生脱水缩合反应，二氧化硅均匀吸附在改性高岭土表面，形成一种改性高岭土为核，纳米二氧化硅为壳的微米/纳米核壳结构，该微粒能够作为光散射粒子，促进光通过第一发光层。
进一步地，第一发光层为铕/PVB复合材料，第一发光层的发射波长为可见光波段。
进一步地，第二发光层为铽掺杂聚乙烯，第二发光层的发射波长为300-510nm。
进一步地，第三发光层为为钆掺杂聚乙烯，第三发光层的发射波长300-560nm。
进一步地，第一发光层、第二发光层、第三发光层和基材层从上往下依次安装，第三发光层安装在基材层上表面，第二发光层一侧与在第三发光层侧表面连接，第二发光层另一侧与第一发光层侧表面连接，第一发光层上均匀安装有扩散粒子。
本发明的有益效果：
(1)本发明一种3D显影高分子薄膜，包括第一发光层、第二发光层、第三发光层和基材层，所述第一发光层表面安装有扩散粒子，步骤S1中膨润土、尿素和乙醇按照3∶5∶1的重量比混合，对膨润土进行插层改性，通过将尿素作为插层剂，一方面能够增大膨润土中蒙脱石的层间距，为其它分子进入蒙脱石提供空间，另一方面当制得的改性膨润土燃烧时能够分解出氨气，对燃烧过程进行阻碍，赋予第一发光层表面一定的阻燃性能；步骤S2中将改性膨润土和纳米二氧化硅混合，通过六甲基二硅氮烷进行修饰，二氧化硅表面的羟基能够与六甲基二硅氮烷发生脱水缩合反应，二氧化硅均匀吸附在改性膨润土表面，形成一种改性膨润土为核，纳米二氧化硅为壳的微米/纳米核壳结构，该微粒能够作为光散射粒子，促进光通过第一发光层，解决了通过膨润土和纳米二氧化硅制备扩散粒子时，由于膨润土自身层间距较小，导致复合后结构不稳定，而且不具有阻燃性能，不能对显影膜进行保护的技术问题；
(2)所述基材层为复合透明纤维膜，制备过程中第一步中先将聚丙烯腈通过10％碳酸钠溶液和连二亚硫酸钠进行初步处理，之后第二步中将聚丙烯腈粉末和聚氨酯粉末在不同浓度的N,N-二甲基甲酰胺中混合，制备出不同浓度的纺丝液，之后将按照2∶1的重量比混合后进行静电纺丝，制得复合纤维膜，之后通过对该复合纤维膜进行热处理制得复合透明纤维膜，该复合纤维膜以聚丙烯腈为内层，聚氨酯为表层，热处理过程中聚氨酯融在聚丙烯腈表面，聚丙烯腈表面形成致密结构，光照射在复合膜表面后反射作用减弱，光损失率降低，所以该复合膜具有优异的透明度，解决了现有技术中通过聚丙烯腈制备透明纤维膜，但是制备过程中由于自身限制，透明膜的透光性能较低，无法满足高清晰3D显影的要求等技术问题。
附图说明
为了便于本领域技术人员理解，下面结合附图对本发明作进一步的说明。
图1为本发明一种3D显影高分子薄膜的结构示意图。
图中：1、第一发光层；2、第二发光层；3、第三发光层；4、基材层。
具体实施方式
下面将结合本发明实施例，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作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
一种3D显影高分子薄膜，包括第一发光层1、第二发光层2、第三发光层3和基材层4，第一发光层1、第二发光层2、第三发光层3和基材层4从上往下依次安装，第三发光层3安装在基材层4上表面，第二发光层2安装在第三发光层3一侧表面，第一发光层1一侧与第二发光层2连接；
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35℃水浴加热并磁力搅拌20min，之后加入连二亚硫酸钠，升温至55℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶35∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10％的N,N-二甲基甲酰胺和浓度为15％的N,N-二甲基甲酰胺中，35℃下超声10h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜。
纳米复合粒子由如下方法制成：
步骤S1、将膨润土、尿素和乙醇按照3∶5∶1的重量比混合均匀，之后加入三口烧瓶中，45℃水浴加热并以120r/min的转速搅拌3h，制得混合浆料，抽滤并用35℃去离子水洗涤三次，之后用无水乙醇洗涤三次，烘干，研磨，制得改性膨润土；
步骤S2、将改性膨润土和纳米二氧化硅混合，以1000r/min的转速搅拌40min，制得复合粒子前驱体，之后加入六甲基二硅氮烷，磁力搅拌15min后升温至100-110℃，在此温度下反应4h，过滤，用去离子水洗涤三次，制得纳米复合粒子，控制改性膨润土、纳米二氧化硅、六甲基二硅氮烷的重量比1∶2∶50。
实施例2
一种3D显影高分子薄膜，包括第一发光层1、第二发光层2、第三发光层3和基材层4，第一发光层1、第二发光层2、第三发光层3和基材层4从上往下依次安装，第三发光层3安装在基材层4上表面，第二发光层2安装在第三发光层3一侧表面，第一发光层1一侧与第二发光层2连接；
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35℃水浴加热并磁力搅拌20min，之后加入连二亚硫酸钠，升温至55℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶38∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10％的N,N-二甲基甲酰胺和浓度为15％的N,N-二甲基甲酰胺中，35℃下超声10h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜。
其余同实施例1。
实施例3
一种3D显影高分子薄膜，包括第一发光层1、第二发光层2、第三发光层3和基材层4，第一发光层1、第二发光层2、第三发光层3和基材层4从上往下依次安装，第三发光层3安装在基材层4上表面，第二发光层2安装在第三发光层3一侧表面，第一发光层1一侧与第二发光层2连接；
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35℃水浴加热并磁力搅拌20min，之后加入连二亚硫酸钠，升温至55℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶39∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10％的N,N-二甲基甲酰胺和浓度为15％的N,N-二甲基甲酰胺中，35℃下超声10h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜。
其余同实施例1。
实施例4
一种3D显影高分子薄膜，包括第一发光层1、第二发光层2、第三发光层3和基材层4，第一发光层1、第二发光层2、第三发光层3和基材层4从上往下依次安装，第三发光层3安装在基材层4上表面，第二发光层2安装在第三发光层3一侧表面，第一发光层1一侧与第二发光层2连接；
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35℃水浴加热并磁力搅拌20min，之后加入连二亚硫酸钠，升温至55℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶40∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10％的N,N-二甲基甲酰胺和浓度为15％的N,N-二甲基甲酰胺中，35℃下超声10h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜。
其余同实施例1。
对比例1
本对比例与实施例1相比，未加入聚氨酯粉末，制备方法如下所示：
所述基材层为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10％碳酸钠溶液中，35℃水浴加热并磁力搅拌20min，之后加入连二亚硫酸钠，升温至55℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10％碳酸钠溶液和连二亚硫酸钠的重量比为1∶35∶0.5；
第二步、分别将聚丙烯腈粉末加入浓度为10％的N,N-二甲基甲酰胺，35℃下超声10h，制得聚丙烯腈纺丝液，之后将聚丙烯腈纺丝液静电纺丝，制得纤维膜，之后进行热处理，制得所述透明纤维膜。
对比例2
本对比例与实施例1相比，未对膨润土进行改性，制备方法如下所示：
纳米复合粒子由如下方法制成：
将膨润土和纳米二氧化硅混合，以1000r/min的转速搅拌40min，制得复合粒子前驱体，之后加入六甲基二硅氮烷，磁力搅拌15min后升温至100-110℃，在此温度下反应4h，过滤，用去离子水洗涤三次，制得纳米复合粒子，控制膨润土、纳米二氧化硅、六甲基二硅氮烷的重量比1∶2∶50。
对比例3
本对比例为市场中一种3D显影高分子薄膜。
对实施例1-4和对比例1-3的光透过率、雾度和散射率进行检测，结果如下表所示；
光透过率(％) 雾度(％) 散射率(％)
实施例1 88.56 2.6 41.55
实施例2 88.58 2.5 41.40
实施例3 87.96 2.6 41.25
实施例4 88.35 2.7 41.88
对比例1 75.65 2.9 41.08
对比例2 79.85 2.8 35.67
对比例3 74.65 2.8 33.85
从上表中能够看出实施例1-4的光透过率为88.35-88.58％，雾度为2.5-2.7％，散射率为41.25-41.88％，对比例1-3的光透过率为74.65-79.85％，雾度为2.8-2.9％，散射率为33.85-41.08％；复合纤维膜以聚丙烯腈为内层，聚氨酯为表层，热处理过程中聚氨酯融在聚丙烯腈表面，聚丙烯腈表面形成致密结构，光照射在复合膜表面后反射作用减弱，光损失率降低，所以该复合膜具有优异的透明度，解决了现有技术中通过聚丙烯腈制备透明纤维膜，但是制备过程中由于自身限制，透明膜的透光性能较低，无法满足高清晰3D显影的要求等技术问题。
在本说明书的描述中，参考术语“一个实施例”、“示例”、“具体示例”等的描述意指结合该实施例或示例描述的具体特征、结构、材料或者特点包含于本发明的至少一个实施例或示例中。在本说明书中，对上述术语的示意性表述不一定指的是相同的实施例或示例。而且，描述的具体特征、结构、材料或者特点可以在任何的一个或多个实施例或示例中以合适的方式结合。
以上内容仅仅是对本发明所作的举例和说明，所属本技术领域的技术人员对所描述的具体实施例做各种各样的修改或补充或采用类似的方式替代，只要不偏离发明或者超越本权利要求书所定义的范围，均应属于本发明的保护范围。

Claims (6)

1.一种3D显影高分子薄膜，其特征在于，包括第一发光层（1）、第二发光层（2）、第三发光层（3）和基材层（4），第一发光层（1）、第二发光层（2）、第三发光层（3）和基材层（4）从上往下依次安装，第三发光层（3）安装在基材层（4）上表面，第二发光层（2）安装在第三发光层（3）一侧表面，第一发光层（1）一侧与第二发光层（2）连接；
所述基材层（4）为复合透明纤维膜，该复合透明纤维膜由如下方法制成：
第一步、将聚丙烯腈加入10%碳酸钠溶液中，35-45℃水浴加热并磁力搅拌20-30min，之后加入连二亚硫酸钠，升温至55-65℃，继续搅拌30min，取出、研磨，过滤，制得聚丙烯腈粉末，控制聚丙烯腈、10%碳酸钠溶液和连二亚硫酸钠的重量比为1∶35-40∶0.5；
第二步、分别将聚丙烯腈粉末和聚氨酯粉末加入浓度为10%的N,N-二甲基甲酰胺和浓度为15%的N,N-二甲基甲酰胺中，35-45℃下超声10-12h，制得聚丙烯腈纺丝液和聚氨酯纺丝液，之后将聚丙烯腈纺丝液和聚氨酯纺丝液按照2∶1的重量比混合，静电纺丝，制得复合纤维膜，之后进行热处理，制得所述复合透明纤维膜；
所述第一发光层（1）表面安装有扩散粒子（11），所述扩散粒子（11）为纳米复合粒子，该纳米复合粒子的粒径为200-800nm；
所述纳米复合粒子由如下方法制成：
步骤S1、将膨润土、尿素和乙醇按照3∶5∶1的重量比混合均匀，之后加入三口烧瓶中，45-55℃水浴加热并以120r/min的转速搅拌3-4h，制得混合浆料，抽滤并用35-40℃去离子水洗涤三次，之后用无水乙醇洗涤三次，烘干，研磨，制得改性膨润土；
步骤S2、将改性膨润土和纳米二氧化硅混合，以1000-1200r/min的转速搅拌40-50min，制得复合粒子前驱体，之后加入六甲基二硅氮烷，磁力搅拌15-30min后升温至100-110℃，在此温度下反应4-5h，过滤，用去离子水洗涤三次，制得纳米复合粒子，控制改性膨润土、纳米二氧化硅、六甲基二硅氮烷的重量比1∶2∶50-60。
2.根据权利要求1所述的一种3D显影高分子薄膜，其特征在于，第二步中热处理的具体步骤为：将复合纤维膜固定，之后转移至真空干燥箱中，控制真空干燥箱的温度为180-200℃，干燥时间为4h，之后升温至200-220℃，在此温度下干燥6h，之后升温至220-230℃，在此温度下保温10h。
3.根据权利要求1所述的一种3D显影高分子薄膜，其特征在于，第一发光层（1）为铕/PVB复合材料，第一发光层（1）的发射波长为可见光波段。
4.根据权利要求1所述的一种3D显影高分子薄膜，其特征在于，第二发光层（2）为铽掺杂聚乙烯，第二发光层（2）的发射波长为300-510nm。
5.根据权利要求1所述的一种3D显影高分子薄膜，其特征在于，第三发光层（3）为钆掺杂聚乙烯，第三发光层（3）的发射波长300-560nm。
6.根据权利要求1所述的一种3D显影高分子薄膜的制备方法，其特征在于，第一发光层（1）、第二发光层（2）、第三发光层（3）和基材层（4）从上往下依次安装，第三发光层（3）安装在基材层（4）上表面，第二发光层（2）一侧与在第三发光层（3）侧表面连接，第二发光层（2）另一侧与第一发光层（1）侧表面连接，第一发光层（1）上均匀安装有扩散粒子（11）。
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