CN111732749B - 一种聚乙烯醇光学薄膜的制备方法 - Google Patents

一种聚乙烯醇光学薄膜的制备方法 Download PDF

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CN111732749B
CN111732749B CN202010795047.7A CN202010795047A CN111732749B CN 111732749 B CN111732749 B CN 111732749B CN 202010795047 A CN202010795047 A CN 202010795047A CN 111732749 B CN111732749 B CN 111732749B
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吴福胜
唐成宏
刘密密
向学毅
吴云柱
葛继承
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Anhui Wanwei Updated High Tech Material Industry Co Ltd
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Abstract

本发明公开了一种聚乙烯醇光学薄膜的制备方法，是将膜用PVA树脂及辅料经溶解、脱泡、流延成型、预干燥、热处理、收卷制备而成。本发明将热处理分预热、热处理、冷却三个过程进行，并严格控制薄膜在热处理各段的温度、停留时间和张力，可以使薄膜在横向和纵向的收缩率近似，横纵向膨润度趋同，膨润比在1‑1.02％之间，减少下游生产中因膨润比过大导致染色不均匀问题。

Description

一种聚乙烯醇光学薄膜的制备方法
技术领域
本发明属于聚乙烯醇薄膜技术领域，具体涉及一种偏光片用聚乙烯醇光学薄膜的制备方法。
背景技术
目前聚乙烯醇光学薄膜的生产方法是将PVA树脂及辅料溶解于超纯水中，配置成铸膜原液，铸膜原液经挤出机脱泡、模头流延成型、干燥导辊预干燥、热处理烘箱烘干定型，收卷获得聚乙烯醇光学薄膜成品。
聚乙烯醇光学膜主要用于偏光片的生产，终端产品为各类液晶显示器。聚乙烯醇光学膜的性能，决定了偏光片的偏振度、透光率、色调等光学性能。聚乙烯醇光学薄膜经过膨润、拉伸、染色，并与TAC膜贴合后制成偏光片，其中，薄膜在膨润时，横向和纵向均发生延伸，延伸的程度可用薄膜膨润前后尺寸变化的比值，即横向膨润度和纵向膨润度来表示。实际生产中，以横向膨润度与纵向膨润度的比值，即膨润比来表示薄膜的膨润性能。若薄膜的膨润比过大，则说明薄膜在膨润过程中，横向和纵向的延伸程度不均，在后续的拉伸和染色过程中，极易形成色斑、条纹等染色不均的现象，严重影响偏光片的光学性能。
纵向因受牵引力的作用无法自由收缩，即在同等工艺环境下，薄膜横向和纵向的收缩程度不同聚乙烯醇光学膜在热处理时，薄膜横向为自由收缩，，是造成薄膜膨润比变化的主要因素。
传统方法中，薄膜的热处理过程往往为单一的加热升温过程，而薄膜在受热的各个阶段中，横向和纵向的收缩程度并不相同。因此，需要一种更加精准可控的方法，针对薄膜在不同受热状态下，进行准确的调控，以降低膨润比，提高偏光片的光学性能。
发明内容
基于上述现有技术所存在的不足之处，本发明提供了一种聚乙烯醇光学薄膜的制备方法，旨在解决该光学膜在后续偏光片生产加工时，因膨润不佳导致的染色不均问题。
本发明为实现发明目的，采用如下技术方案：
一种聚乙烯醇光学薄膜的制备方法，是将膜用PVA树脂及辅料溶解于超纯水中，配置成质量浓度为25-35％的铸膜原液；所述铸膜原液经挤出机脱泡后，通过模头流延成型，再经干燥导辊进行预干燥，然后进入热处理烘箱烘干定型，收卷获得聚乙烯醇光学薄膜成品。
上述热处理可为热风气流式、真空式、热硅油式等干燥方法，干燥所用介质可以是氮气、压缩空气、硅油类等。热处理分预热、热处理、冷却三个过程进行，其中：预热过程可分为1至多段，优选1-3段，更优选2段；热处理过程可分为1至多段，优选1-3段，更优选2段；冷却过程可分为1至多段，优选1-3段，更优选1段。
本发明通过调整薄膜在热处理各段的温度、停留时间和张力，以控制薄膜横向和纵向的收缩，降低薄膜膨润比。以5段热处理为例：
当所述热处理为5段时，各段温度范围为：Ⅰ段温度50-90℃，Ⅱ段60-110℃，Ⅲ段80-150℃，Ⅳ段60-130℃，Ⅴ段30-70℃；其中，Ⅰ段优选60-80℃，Ⅱ段优选70-100℃，Ⅲ段优选90℃～130℃，Ⅳ段优选90-110℃，Ⅴ段优选40-60℃。
当所述热处理为5段时，薄膜在热处理各段中停留时间为：Ⅰ段10-40s，Ⅱ段10-30s，Ⅲ段5-20s，Ⅳ段10-30s，Ⅴ段20-50s；其中，Ⅰ段优选15-35s，Ⅱ段优选10-25s，Ⅲ段优选5-15s，Ⅳ段优选10-20s，Ⅴ段优选20-40s。
当所述热处理为5段时，热处理各段张力为：Ⅰ段30-100N/m，Ⅱ段40-90N/m，Ⅲ段20-70N/m，Ⅳ段40-90N/m，Ⅴ段30-120N/m；其中，Ⅰ段优选60-90N/m，Ⅱ段优选40-80N/m，Ⅲ段优选20-50N/m，Ⅳ段40-60N/m，Ⅴ段优选60-100N/m。
热处理的预热过程温度较低，停留时间稍长，目的是使薄膜均匀受热失水，此时薄膜收缩较小，因此张力可以稍高；热处理过程温度较高，为了控制薄膜含水率，此过程停留时间不宜过长，且热处理过程薄膜收缩较大，因此张力最低，以长度收缩弥补宽度收缩；冷却过程的目的是使膜冷却，完成最后的干燥，此时薄膜的收缩率较低，张力较高。因此，以热处理为5段为例，在设定时应保证：Ⅲ段温度最高，且停留时间最短、张力最小；Ⅴ段温度最低，且停留时间最长、张力最大。
与现有工艺相比，本发明的有益效果体现在：
本发明将热处理分预热、热处理、冷却三个过程进行，并严格控制薄膜在热处理各段的温度、停留时间和张力，可以使薄膜在横向和纵向的收缩率近似，横纵向膨润度趋同，膨润比在1-1.02％之间，减少下游生产中因膨润比过大导致染色不均匀问题，且本发明的方法操作简单、经济可行。
具体实施方式
下面对本发明的实施例作详细说明，本实施例在以本发明技术方案为前提下进行实施，给出了详细的实施方式和具体的操作过程，但本发明的保护范围不限于下述的实施例。
实施例1
将PVA 1799膜用树脂500Kg、增塑剂甘油50Kg、表面活性剂椰子油二乙醇酰胺2.7Kg、抗氧化剂1098共1.3Kg溶于超纯水中，配置成质量浓度为30％的铸膜原液。铸膜原液经挤出机脱泡后，通过模头流延成型，再经数根干燥导辊进行预干燥，然后进入热处理烘箱烘干定型，收卷获得聚乙烯醇光学薄膜成品。
本实施例中热处理不分段，温度为110℃、热处理时间为90s,、热处理段张力控制为50N/m。
实施例2
按照与实施例1相同的方式制液、脱泡、流延、预干燥，然后进入热处理烘箱干燥定型。区别在于本实施例中热处理分5段，各段温度、停留时间及张力如表1所示。
表1
项目 Ⅰ段 Ⅱ段 Ⅲ段 Ⅳ段 Ⅴ段
温度(℃) 65 90 115 100 50
停留时间(S) 30 15 10 15 25
张力(N/m) 70 60 30 45 85
实施例3
按照与实施例1相同的方式制液、脱泡、流延、预干燥，然后进入热处理烘箱干燥定型。区别在于本实施例中热处理分5段，各段温度、停留时间及张力如表2所示。
表2
项目 Ⅰ段 Ⅱ段 Ⅲ段 Ⅳ段 Ⅴ段
温度(℃) 65 85 130 95 55
停留时间(S) 30 20 5 10 20
张力(N/m) 70 55 20 60 80
对比例1
按照与实施例1相同的方式制液、脱泡、流延、预干燥，然后进入热处理烘箱干燥定型。区别在于本对比例中热处理分5段，各段温度、停留时间及张力如表3所示。
表3
项目 Ⅰ段 Ⅱ段 Ⅲ段 Ⅳ段 Ⅴ段
温度(℃) 65 115 100 90 50
停留时间(S) 30 10 15 15 25
张力(N/m) 70 30 45 60 85
对比例2
按照与实施例1相同的方式制液、脱泡、流延、预干燥，然后进入热处理烘箱干燥定型。区别在于本对比例中热处理分5段，各段温度、停留时间及张力如表4所示。
表4
项目 Ⅰ段 Ⅱ段 Ⅲ段 Ⅳ段 Ⅴ段
温度(℃) 65 90 115 100 50
停留时间(S) 30 15 30 25 25
张力(N/m) 70 60 30 45 85
对比例3
按照与实施例1相同的方式制液、脱泡、流延、预干燥，然后进入热处理烘箱干燥定型。区别在于本对比例中热处理分5段，各段温度、停留时间及张力如表5所示。
表5
项目 Ⅰ段 Ⅱ段 Ⅲ段 Ⅳ段 Ⅴ段
温度(℃) 65 90 115 100 50
停留时间(S) 30 15 10 15 25
张力(N/m) 70 60 60 70 85
聚乙烯醇光学膜膨润度和膨润比的测定方法是：取长宽各为10cm的光学膜，在30℃纯水中浸没膨润10分钟后，薄膜横向(纵向)尺寸与原横向尺寸比值为横向(纵向)膨润度，横向与纵向膨润度比值称之为膨润比。各实施例与对比例所得薄膜膨润比数据如表6所示。
表6
实施例1 实施例2 实施例3 对比例1 对比例2 对比例3
膨润比 1.077 1.004 1.009 1.052 1.022 1.027
从表6可以看出，本发明提供的工艺条件生产的PVA光学薄膜可以明显降低薄膜的膨润比。
将各实施与对比例制得的PVA薄膜浸入35℃纯水中浸润1min，在含120.5g/L、KI20g/L的30℃的染色槽中浸染100s，边染色边拉伸，拉伸至原长的5倍，在固色槽(HBO3-KI40g/L)中固色1min后，在100℃的条件干燥3min，在PVA膜两侧贴合上三醋酸纤维素膜，干燥得到偏光片。分别测试制得偏光片的性能指标，偏振度与透光率，结果如表7所示。
表7
Figure BDA0002625235650000041
Figure BDA0002625235650000051
由实施例和对比例可以看出，热处理各部分温度以及停留时间控制不当、热处理各部分张力设置不适宜会导致薄膜横、纵向膨润度出现差异，膨润比较大。本发明将PVA膜进行多段热处理，并严格控制各段的温度、停留时间和张力，可以使薄膜在横向和纵向的膨润度趋同，膨润比在1-1.02％之间，解决了因膨润比较大导致的染色不均问题。
以上所述仅为本发明的示例性实施例而已，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、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (1)

1.一种聚乙烯醇光学薄膜的制备方法，其特征在于：将膜用PVA树脂及辅料溶解于超纯水中，配置成铸膜原液；所述铸膜原液经挤出机脱泡后，通过模头流延成型，再经干燥导辊进行预干燥，然后进入热处理烘箱烘干定型，收卷获得聚乙烯醇光学薄膜成品；
热处理分为预热、热处理、冷却三个过程；所述热处理的预热过程分为2段、热处理过程分为2段、冷却过程为1段，从而使热处理共包括5段；
当所述热处理为5段时，各段温度范围为：Ⅰ段60-80℃，Ⅱ段70-100℃，Ⅲ段90℃-130℃，Ⅳ段90-110℃，Ⅴ段40-60℃；
当所述热处理为5段时，薄膜在热处理各段中停留时间为：Ⅰ段15-35s，Ⅱ段10-25s，Ⅲ段5-15s，Ⅳ段10-20s，Ⅴ段20-40s；
当所述热处理为5段时，热处理各段张力为：Ⅰ段60-90N/m，Ⅱ段40-80N/m，Ⅲ段20-50N/m，Ⅳ段40-60N/m，Ⅴ段60-100N/m；
同时保证：Ⅲ段温度最高，且停留时间最短、张力最小；Ⅴ段温度最低，且停留时间最长、张力最大。
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