CN106893127B - 一种高阻隔性光学薄膜及其制备方法和应用 - Google Patents
一种高阻隔性光学薄膜及其制备方法和应用 Download PDFInfo
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Abstract
本发明涉及光学膜制备领域，具体涉及一种高阻隔性光学薄膜及其制备方法和应用。该光学薄膜由光学基膜、氧气阻隔膜和水汽阻隔膜复合而成，所述光学基膜的上表面涂有所述氧气阻隔膜，所述氧气阻隔膜的上表面涂有所述水汽阻隔膜，所述氧气阻隔膜位于所述光学基膜与所述水汽阻隔膜之间。其制备方法包括：S1.疏水改性PVA阻隔液及隔水阻隔液的制备；S2.疏水改性PVA阻隔液的涂布及干燥；S3.隔水阻隔液的涂布及干燥。本发明提供的高阻隔性光学薄膜产品由光学基膜、氧气阻隔膜和水汽阻隔膜三层复合而成，得到产品具有极低的透氧透水性，可用作量子点膜的外层阻隔膜或用作要求阻隔外界氧气和水汽的食品包装膜等；制备方法简单，生产成本低。
Description
技术领域
本发明涉及光学膜制备领域，具体涉及一种高阻隔性光学薄膜及其制备方法和应用。
背景技术
将通过量子点纳米材料制备的量子点膜应用在显示器的背光模组中，可以提高色域值和色彩饱和度，是近年来兴起的一项热门技术。但是量子点材料对高温、强光、氧气、湿度及酸等有害环境极为敏感，非常容易衰减，故在量子点膜的实际应用中，需要良好的阻隔性能，以保证产品在使用过程中的稳定性。目前，在电学、包装等领域一般多采用无机物或无机物与有机物复合制备阻隔涂层，其具有良好的阻隔性能；目前也已经开发出高度透明的阻隔涂层应用于光学膜领域。但是现有的阻隔层一般通过化学气相沉积、等离子体增强化学气相沉积、溅射和真空工艺等制备，成本高且工艺复杂。
发明内容
本发明所要解决的技术问题是提供一种高阻隔性光学薄膜及其制备方法和应用，该薄膜由有机高分子材料制成，制备时采用简单方便的涂膜工艺依次在基膜上形成氧气阻隔层和水汽阻隔层，得到的薄膜具有较好的阻隔性能，可用作量子点膜的外层阻隔膜或用作要求阻隔外界氧气和水汽的食品包装膜等。
本发明解决上述技术问题的技术方案如下：一种高阻隔性光学薄膜，其由光学基膜、氧气阻隔膜和水汽阻隔膜复合而成，所述光学基膜的上表面涂有所述氧气阻隔膜，所述氧气阻隔膜的上表面涂有所述水汽阻隔膜，所述氧气阻隔膜位于所述光学基膜与所述水汽阻隔膜之间。
在上述技术方案的基础上，本发明还可以有如下进一步的具体选择。
上述的氧气阻隔膜和水汽阻隔膜均由有机高分子材料制成，有机高分子材料被用作阻隔材料时，小分子物质是通过高分子材料的分子间自由体积渗透的，因此具有阻隔性的高分子材料应具有以下特征：
①阻隔非极性小分子(如氧气)时，阻隔高分子材料应具有某种程度的极性，如含有羟基，腈，氯，氟，丙烯酸或酯等基团；阻隔极性小分子(如水)时，阻隔高分子材料应具有非极性结构，分子结构对称或者具有能平均电子结构的大π键；②分子链具有一定的刚性，不易发生热运动，可以阻碍小分子的渗透；③不与渗透分子发生反应；④分子对称有序，利于结晶、取向等。结晶和取向会让分子链排列紧密，密切堆积，分子间自由体积小，不利于小分子的渗透；⑤分子链间或分子之间有较强的相互作用力，如氢键等；⑥具有较小的自由体积与较高的玻璃化转变温度(Tg)。
具体的，所述光学基膜为光学PET膜或光学PC膜。
具体的，所述氧气阻隔膜为疏水改性PVA膜，所述疏水改性PVA膜由PVA水溶液和戊二醛水溶液在盐酸催化作用下发生缩醛化反应交联后再流延烘干而成。
PVA分子具有规整的线性结构，分子内含有大量的羟基，因此PVA具有极强的亲水性，是一种水溶性高分子材料。由于大量羟基的存在，PVA容易形成大量的分子内和分子间氢键，强大的分子间相互作用力会提高PVA的结晶能力，使其具有高度的结晶性、化学稳定性、热稳定性、透光性、良好的光泽和高的机械强度。同时由于高度的结晶性，PVA分子间自由体积较小，因此对于非极性小分子如氧气等，具有极为优越的阻隔能力；但是对极性小分子如水汽的阻隔能力较差，且若PVA长时间暴露在水汽中，会吸附水分子并溶胀，溶胀之后PVA的阻隔性会急剧下降，因此需要对PVA进行适当的疏水改性，保留其阻隔氧气的能力的同时，防止吸水溶胀。PVA的羟基决定了其亲水性能，为了将PVA改性为疏水聚合物，需要从醇解后的羟基(-OH)入手。可以通过共聚改性(如内酯化改性)和后期改性(如缩醛化反应、酯化反应等)来改变PVA大分子的化学结构，获得疏水性的PVA疏水材料。此外，也可以通过在PVA层上涂布隔水层，隔绝PVA与水的接触，来保留PVA较好的隔氧能力。
具体的，所述水汽阻隔膜为PE膜、PC膜、PMMA膜和PS膜中的任意一种。PE、PC、PMMA和PS均为低透水性聚合物，其中PE是晶态聚合物，需要加热到熔点以上才能熔融或者溶解，PS、PC和PMMA是非晶态聚合物，在常温下即可溶解在适当的溶剂中。
具体的，所述光学基膜的厚度为10-250μm，所述氧气阻隔膜的厚度为0.4-14.5μm，所述水汽阻隔膜的厚度为0.4-14.5μm。
本发明还提供一种高阻隔性光学薄膜的制备方法，其包括如下步骤：
S1.将PVA水溶液、戊二醛水溶液和盐酸混合配制成疏水改性的PVA阻隔液，备用；将PE、PC、PMMA和PS中的任一种溶于有机溶剂配制成隔水阻隔液，备用；
S2.将所述疏水改性的PVA阻隔液涂布于由光学PET膜或光学PC膜制成的光学基膜的上表面，烘干，在所述光学基膜的上表面形成氧气阻隔膜，得光学基膜与氧气阻隔膜的复合膜；工业上生产PVA膜的方法通常是在传送带或平面上流延成膜，具体的，是将PVA以水溶液形式流延到传送带或平面上，再加热烘干成膜。由于PVA的氢键作用导致分子间作用力非常强，其熔点大于分解温度，故不能采用熔融加工。
S3.将所述隔水阻隔液涂布于所述氧气阻隔膜的上表面，干燥，在所述氧气阻隔膜的上表面形成水汽阻隔膜，得由光学基膜、氧气阻隔膜和水汽阻隔膜复合而成的高阻隔性光学薄膜。
在上述制备方法的基础上，本发明还可以做如下进一步的具体选择。
具体的，S1中所述PVA水溶液中PVA的质量分数为3-25％，所述戊二醛水溶液中戊二醛的质量分数为8-12％，所述盐酸的质量分数为2-6％,所述疏水改性的PVA阻隔液由所述PVA水溶液、戊二醛水溶液和盐酸按照100:0.1-10:0.2-2的重量比例充分混合并反应0.5-1h制成。PVA和戊二醛在盐酸的催化作用下，发生缩醛化反应，双醛基团使PVA分子形成交联结构，提高耐水能力。
具体的，S1中所述隔水阻隔液中相应的PE、PC、PMMA或PS的质量分数为3-25％，所述有机溶剂为二氯甲烷或二甲苯。
具体的，S2和S3中涂布所述疏水改性的PVA阻隔液和隔水阻隔液时，使用规格为10-50μm的线棒涂布器刮涂。规格为10-50μm的线棒涂布器刮涂出的湿膜厚度为10-50μm，待阻隔液中的溶剂或水分挥发完之后，即得干膜，干膜的厚度由阻隔液中的固体含量确定。
本发明还提供一种高阻隔性光学薄膜的应用，其可用作量子点膜的外层阻隔膜或用作要求阻隔外界氧气和水汽的食品包装膜。
与现有技术相比，本发明的有益效果是：
1)本发明提供的高阻隔性光学薄膜产品由光学基膜、氧气阻隔膜和水汽阻隔膜三层复合而成，三层膜均由有机高分子材料制成，得到产品具有极低的透氧透水性，可用作量子点膜的外层阻隔膜或用作要求阻隔外界氧气和水汽的食品包装膜等；
2)本发明提供的制备方法简单，制备相应的高分子溶液，然后依次在光学基膜上直接涂膜并干燥成相应的隔膜即可，工艺简单，生产成本低。
附图说明
图1为本发明提供的一种高阻隔性光学薄膜的结构示意图；
图2为本发明提供的一种高阻隔性光学薄膜制备方法的流程图；
附图中，各标号代表的意义如下：
1.光学基膜；2.氧气阻隔膜；3.水汽阻隔膜。
具体实施方式
以下结合附图及具体实施例对本发明的原理和特征进行描述，所举实例只用于解释本发明，并非用于限定本发明的范围。
如图1所示，本发明提供一种高阻隔性光学薄膜，其由光学基膜1、氧气阻隔膜2和水汽阻隔膜3复合而成，所述光学基膜1的上表面涂有所述氧气阻隔膜2，所述氧气阻隔膜的上表面涂有所述水汽阻隔膜3，所述氧气阻隔膜2位于所述光学基膜1与所述水汽阻隔膜3之间。
如图2所示，本发明提供一种高阻隔性光学薄膜的制备方法，其包括如下步骤:
S1.将PVA水溶液、戊二醛水溶液和盐酸混合配制成疏水改性的PVA阻隔液，备用；将PE、PC、PMMA和PS中的任一种溶于有机溶剂配制成隔水阻隔液，备用；
S2.将所述疏水改性的PVA阻隔液涂布于由光学PET膜或光学PC膜制成的光学基膜的上表面，烘干，在所述光学基膜的上表面形成氧气阻隔膜，得光学基膜与氧气阻隔膜的复合膜；
S3.将所述隔水阻隔液涂布于所述氧气阻隔膜的上表面，干燥，在所述氧气阻隔膜的上表面形成水汽阻隔膜，得由光学基膜、氧气阻隔膜和水汽阻隔膜复合而成的高阻隔性光学薄膜。
以下实施例中用到的PVA水溶液是将分子量40000-120000、醇解度88-98％的PVA粉末或者颗粒溶解于去离子水中制备得到，PVA水溶液中PVA的质量分数为3-25％。以下实施例中使用的PE、PC、PS、PET等均为市售产品，其中用作光学基膜的PET或PC均为光学级。
实施例1
一种高阻隔性光学薄膜，其制备方法包括如下步骤:
S1.将15wt％的PVA水溶液、10wt％的戊二醛水溶液和4wt％的盐酸按照100：5：1的重量比例混合配制成疏水改性的PVA阻隔液，备用；将PE溶于二氯甲烷中配制成15wt％的PE隔水阻隔液，备用；
S2.用规格为25μm的线棒涂布器将所述疏水改性的PVA阻隔液刮涂于厚75μm的PET光学基膜的上表面，烘干，在所述光学PET基膜的上表面形成厚约4.0μm的PVA氧气阻隔膜，得到复合膜PET+PVA；
S3.用规格为25μm的线棒涂布器将所述PE隔水阻隔液刮涂于所述PVA氧气阻隔膜的上表面，干燥，在所述PVA氧气阻隔膜的上表面形成厚约4.0μm的PE水汽阻隔膜，得三层复合膜PET+PVA+PE，即为目标产品——高阻隔性光学薄膜。
实施例2
一种高阻隔性光学薄膜，其制备方法包括如下步骤:
S1.将3wt％的PVA水溶液、8wt％的戊二醛水溶液和2wt％的盐酸按照100：0.1：0.2的重量比例混合配制成疏水改性的PVA阻隔液，备用；将PE溶于二氯甲烷中配制成3wt％的PE隔水阻隔液，备用；
S2.用规格为10μm的线棒涂布器将所述疏水改性的PVA阻隔液刮涂于厚10μm的PET光学基膜的上表面，烘干，在所述光学PET基膜的上表面形成厚约0.4μm的PVA氧气阻隔膜，得到复合膜PET+PVA；
S3.用规格为10μm的线棒涂布器将所述PE隔水阻隔液刮涂于所述PVA氧气阻隔膜的上表面，干燥，在所述PVA氧气阻隔膜的上表面形成厚约0.4μm的PE水汽阻隔膜，得三层复合膜PET+PVA+PE，即为目标产品——高阻隔性光学薄膜。
实施例3
一种高阻隔性光学薄膜，其制备方法包括如下步骤:
S1.将25wt％的PVA水溶液、12wt％的戊二醛水溶液和6wt％的盐酸按照100：10：2的重量比例混合配制成疏水改性的PVA阻隔液，备用；将PE溶于二氯甲烷中配制成25wt％的PE隔水阻隔液，备用；
S2.用规格为50μm的线棒涂布器将所述疏水改性的PVA阻隔液刮涂于厚250μm的PET光学基膜的上表面，烘干，在所述光学PET基膜的上表面形成厚约14.5μm的PVA氧气阻隔膜，得到复合膜PET+PVA；
S3.用规格为50μm的线棒涂布器将所述PE隔水阻隔液刮涂于所述PVA氧气阻隔膜的上表面，干燥，在所述PVA氧气阻隔膜的上表面形成厚约14.5μm的PE水汽阻隔膜，得三层复合膜PET+PVA+PE，即为目标产品——高阻隔性光学薄膜。
实施例4
与实施例1相比，本实施例用PS代替PE，其余参数及步骤均保持不变，最终得到三层复合膜PET+PVA+PS。
实施例5
与实施例4相比，本实施例用PC代替PET，其余参数及步骤均保持不变，最终得到三层复合膜PC+PVA+PS。
对比例1
以75μm厚的PET膜，作为对照薄膜。
对比例2
在75μm厚的PET膜的表面刮涂实施例1制成的疏水改性的PVA阻隔液，形成二层复合膜PET+PVA，不涂水汽阻隔膜，作为对照薄膜。
对比例3
在75μm厚的PC膜的表面刮涂实施例1制成的疏水改性的PVA阻隔液，形成二层复合膜PC+PVA，不涂水汽阻隔膜，作为对照薄膜。
分别使用实施例1至5和对比例1至3制备出的高阻隔性光学薄膜和对照薄膜作为量子点膜的外层阻隔膜，即将量子点层置于两张相同的所述高阻隔性光学薄膜或对照薄膜中间(量子点层与光学基膜接触)制成量子点膜片，测试量子发光效率；然后将制备得到的量子点膜片放入85老化箱(恒温85℃，恒湿85RH)中，85老化箱内为充有空气(与外界空气的氧气含量接近)，经过100h后再次测试量子发光效率；具体的测试结果如下表所示：
| 光学膜类型 | 初始发光效率 | 老化后发光效率 | 衰减率 | |
| 实施例1 | PET+PVA+PE | 93.05％ | 89.77％ | 3.52％ |
| 实施例2 | PET+PVA+PE | 92.85％ | 88.97％ | 4.18％ |
| 实施例3 | PET+PVA+PE | 92.54％ | 89.45％ | 3.34％ |
| 实施例4 | PET+PVA+PS | 92.66％ | 88.48％ | 4.51％ |
| 实施例5 | PC+PVA+PS | 92.45％ | 87.13％ | 5.75％ |
| 对比例1 | PET | 91.94％ | 76.03％ | 17.30％ |
| 对比例2 | PET+PVA | 93.40％ | 86.81％ | 7.06％ |
| 对比例3 | PC+PVA | 90.57％ | 83.22％ | 8.12％ |
由上表可知，本发明依次在光学基膜表面涂覆氧气阻隔膜和水汽阻隔膜得到三层复合的高阻隔性光学薄膜，以此光学薄膜封装量子点层得到的量子点膜片的初始发光效率和老化试验后的发光效率均较高，老化试验前后发光效率的衰减率低，表明本发明得到的高阻隔性光学薄膜具有很好的阻隔氧气和水汽渗透的能力。另外，从对比例可知：仅以光学基膜封装量子点层时，其老化试验后的发光效率较低，即发光效率衰减很快，其原因为氧气或/和水汽渗透光学基膜后对量子点层进行了破坏；仅以PVA阻隔液涂覆后光学基膜得到PET+PVA两层复合膜，以该两层复合膜封装量子点层后得到的量子点膜片产品在相应老化试验中发光效率的衰减率得到了一定体程度的降低，但因缺少水汽阻隔膜，故其仍然比以本发明制备的高阻隔性光学薄膜的性能差。
以上所述仅为本发明的较佳实施例，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (4)
1.一种高阻隔性光学薄膜的制备方法，其特征在于，包括如下步骤：
S1.将PVA水溶液、戊二醛水溶液和盐酸混合配制成疏水改性的PVA阻隔液，备用；将PE、PC、PMMA和PS中的任一种溶于有机溶剂配制成隔水阻隔液，备用；
S2.将所述疏水改性的PVA阻隔液涂布于由光学PET膜或光学PC膜制成的光学基膜的上表面，烘干，在所述光学基膜的上表面形成氧气阻隔膜，得光学基膜与氧气阻隔膜的复合膜；
S3.将所述隔水阻隔液涂布于所述氧气阻隔膜的上表面，干燥，在所述氧气阻隔膜的上表面形成水汽阻隔膜，得由光学基膜、氧气阻隔膜和水汽阻隔膜复合而成的高阻隔性光学薄膜。
2.根据权利要求1所述的一种高阻隔性光学薄膜的制备方法，其特征在于，S1中所述PVA水溶液中PVA的质量分数为3-25％，所述戊二醛水溶液中戊二醛的质量分数为8-12％，所述盐酸的质量分数为2-6％，所述疏水改性的PVA阻隔液由所述PVA水溶液、戊二醛水溶液和盐酸按照100:0.1-10:0.2-2的重量比例充分混合并反应0.5-1h制成。
3.根据权利要求1至2任一项所述的一种高阻隔性光学薄膜的制备方法，其特征在于，S1中所述隔水阻隔液中相应的PE、PC、PMMA或PS的质量分数为3-25％，所述有机溶剂为二氯甲烷或二甲苯。
4.一种如权利要求1至3任一项所述的一种高阻隔性光学薄膜的应用，其特征在于，用作量子点膜的外层阻隔膜或用作要求阻隔外界氧气和水汽的食品包装膜。
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