CN1204168C - 光学各向同性聚碳酸酯膜及其制备方法 - Google Patents
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Abstract
用冷却滚动挤压法将含聚碳酸酯的浇铸膜塑材料加工成光学各向同性的膜。用该光学各向同性膜作为保护数据记录媒体(CD-碟)的覆盖膜，使其免遭刮伤，或将它们用作信息层的载体材料。
Description
发明领域
本发明涉及纯度高、两侧光亮度都高的光学各向同性聚碳酸酯膜、经济地制备它们的挤压方法和本发明膜作为光学数据记录媒体覆盖膜的应用，例如袖珍唱片或DVD唱片。
本发明膜也可用作信息储存层的载体材料，为此，光学数据记录媒体应制得极薄。
现有技术
众所周知，由塑料制得的板和膜的要求是：它们应适合于制备或覆盖光学易读数据储存器，参见J.Hennig“用作光学板式储存器基体的聚合物”，《应用大分子化学》，第145/146卷，1986(第391-409页)。另外，这种板和膜不应含有颗粒大小超过10微米的杂质并且在加工时不应产生气泡和形成收缩孔。在成型时，它们的光学双折射应尽可能地低。
迄今为止，袖珍唱片形式的光学数据记录媒体主要是用压铸法制备的。也可采用其他的方法制备大型光学记录媒体，这种光学记录媒体的整块板由塑料制成，然后在其上涂覆信息储存层。
EP461485(Roehm GmbH)描述了经挤压制备的塑料整板或塑料膜及其制备方法。从挤压机的缝口模头喷嘴挤压出约290℃的聚碳酸酯熔融物，在轧机机架上压制，轧机机架由高光亮度的钢轧辊和棉絮填充的橡胶辊子构成。用这种方法可以制备单侧光亮度高的、而另一单侧无光泽的聚碳酸酯膜，膜的厚度为450微米。
EP351886(Bayer AG)描述了用浇铸法制备聚碳酸酯膜。将平均分子量为98000的聚碳酸酯溶解在二氯甲烷中，缓慢旋转加热溶液通过一个刮浆设备输送到抛光圆筒上。以此制备一种透明均匀的膜，膜的厚度为200微米。这种膜表现出强的双折射，具有的程差ΔG＝74纳米。固定以此制备的具有双折射的聚碳酸酯膜，借助于石英加热辐射体加热5-60秒。使不希望有的双折射降低到在不再成为干扰性的范围内。
JP07126375(Teijin Kasei股份有限公司)描述了双折射低的聚碳酸酯膜的制备方法。通过使用一种聚烯烃保护层，使得这种聚碳酸酯膜的双折射特别的低。
现有技术的缺点
光学各向同性聚碳酸酯薄膜的常规制备方法要么采用的是费用昂贵的浇铸法，要么采用的是不经济的挤压法，采用浇铸法时，为了避免逸出有毒的有机溶剂，必须采用昂贵的设备，而采用挤压法时，或是在第一步中制备出一侧无光泽的聚碳酸酯膜，或者制备出一侧光学各向异性的聚碳酸酯膜。
这后一种已知的光学各向异性挤压膜必须在后续步骤中转变成两侧都具有光亮度的光学各向同性挤压膜。两步挤压法的花费极其昂贵。虽然这种膜是相当光学各向同性的，但是膜的表面特性不理想。
任务
本发明的任务是提供一种两侧都具有光亮度的光学各向同性聚碳酸酯膜，这种膜克服了现有技术描述的生产工艺上的和经济上的缺点。这种膜应该是光学-和机械各向同性的，表面质量优越，具有尽可能高的光学纯度。
解决方案
令人惊奇地，借助于冷却滚动熔融浇铸法(Chill-RollSchmelzegieβVerfahren)可以制备出具有所要求的性能特征的光学上高价值的聚碳酸酯挤压膜，膜的厚度＜200微米，优选15-150微米，更优选30-100微米，特别优选60-90微米。为了获得高水平的光学纯度，最好采用分子量较低的聚碳酸酯压铸材料，正如在大规模制备压铸的光学信息储存器所使用的材料。
所使用的聚碳酸酯模制材料的分子量Mw为10000-40000，优选约15000-20000(压铸材料)。特别令人惊奇地是，不是供挤压法使用的压铸材料可以借助冷却滚动法挤压出具有所要求的性能特征的膜，这种方法的经济效率高，而且避免了有毒的有机溶剂(参见图1)。
本发明的实施方式
本发明主要采用的是熔融浇铸法，即所谓的冷却滚动法(Chill-Roll Verfahren)。将经喷嘴挤出的熔融膜通过冷却辊(冷却滚动轧辊)，在冷却辊上冷却。用此方法可制备出极薄的光学各向异性弱的膜(几乎是各向同性的膜，膜厚在15微米以下)。
“几乎各向同性”是指能透过此膜介质的光射线只存在几乎可以忽略不计的偏差，例如程差最大为50纳米，优选最大为35纳米，更优选最大为25纳米。
聚碳酸酯模制材料的加工温度为210-260℃，优选220-240℃。
为了避免在喷嘴上产生晶粒沉积，挤压装置最好在250-260℃的加工温度下开始运行。为了尽可能少地形成胶体，在约10分至1小时的起始阶段之后，逐渐将加工温度降低到220-240℃。
为了防止在挤压膜上出现喷嘴线纹或挤压条纹，应使挤压喷嘴的内表面、特别是喷嘴的边缘区域变得平滑，最好的方式是镀上一层铬。按照DIN(德国工业标准)4768标准，挤压喷嘴边缘区域的粗糙深度RA为0.025-0.002，优选0.015-0.002，更优选0.01-0.002。分配器通道的粗糙度最高达0.1较为适宜。
如果在挤压喷嘴的内表面上涂覆一种与聚碳酸酯不相容的试剂，就可以进一步改进挤压膜的质量，特别是防止出现喷嘴线纹或挤压条纹。可在洁净的喷嘴内表面上涂覆一种诸如硅油这样的试剂。这种试剂总体上不应提高表面的粗糙度，或者仅略有提高，但最好是使之降低。
还会影响挤压聚碳酸酯膜质量的其他因素是聚碳酸酯熔融物中存在的少量杂质。因此，最好在挤压圆筒和挤压喷嘴之间安装一个熔融物过滤器。过滤器芯子的筛号为5-50微米。
另一种有助于提高聚碳酸酯膜质量的措施是向模制材料配方中同时混入一种润滑剂。其常规用量占模制材料的0.01-1重量％。合适的润滑剂实例是部分氧化的聚乙烯，硬脂酸季戊四醇酯或C10-C20脂肪酸酯。
高光学纯度和高光学各向同性是薄膜投入所说应用的最基本的要求。
根据本发明的方法制备光学上高价值的聚碳酸酯膜。术语“光学上高价值的”主要指：双折射低，透射度高，形成的挤压条纹或喷嘴线纹的数量少(通过线性偏振光的少量偏差可测定)以及每单位面积的胶体数少。
本发明的膜最好没有一个表面区域的线性偏振光的偏差大于2角分。
通过记录偏差角进行这种测定，偏差角是透过膜的激光束产生的。为此，可以采用所谓的激光偏差法。在整个的挤压宽度上，借助于任一个步进电动机驱动的移动来测定角偏差，在膜的垂直透射光束与挤压方向交截时，632.8纳米的激光束获得角偏差。此后，透射的激光束为了放大偏差角而透过望远镜并照射在对位置敏感的数字光学传感器上。这就确定了照射在传感器上的光点的中心位置，通过X和Y坐标系上一系列的交叉点得出该位置。在评价喷嘴线纹时，只有Y值是相关的。
本发明的膜可用作光学数据记录媒体的抗刮痕保护膜，作为光学数据记录媒体的载体材料，作为制备显示器和荧光屏覆盖膜的基础材料。
实施例
实施例1
通过冷却滚动挤压聚碳酸酯模制材料制备本发明的膜，这种聚碳酸酯是在光学压铸法中使用的。
将借助于单螺旋式或双螺旋式挤压机产生的熔融物(为了确保熔融料流的稳定性，任选地可使用一个熔融泵)通过一个用于挤压膜的可自动调节的喷嘴输送到冷却滚动辊(粗糙深度RA＝0.002-0.006，RT＝0.02-0.004，根据DIN 4768测定)中。挤压喷嘴边缘区域的粗糙深度RA为0.02。喷嘴的内表面涂覆有与聚碳酸酯熔融物不相容的硅油。熔融料流的温度为235℃±5℃。熔融的膜与辊表面相切并缠绕辊大约180°。在缠绕其他的辊后，通过一个横向设置的、无接触的测量***测量膜带的厚度，借助于电子处理的信息和一个弹性螺栓***在整个范围内调节喷嘴的熔融物分配。对应的膜具有高的光学和机械各向同性。这后一项特性对于加工性能尤为重要，例如冲压成CD大小的唱片，因为PC压铸材料因其分子量低而比PC挤压材料显得明显易碎。
对比例1
用砑光法制备聚碳酸酯膜，膜厚为0.13毫米
将借助于单螺旋式或双螺旋式挤压机产生的熔融物(为了确保熔融料流的稳定性，任选地可使用一个熔融泵)通过一个用于挤压膜的喷嘴输送到砑光机中。在限定的辊距上确定熔融物的尺寸，通过升温的、抛成反光高光亮度的辊表面(粗糙深度RA＝0.002-0.006，RT＝0.02-0.004，根据DIN 4768测定)砑光并冷却。这样与圆筒形状不一致的一根或两根辊的几何形状进行弯曲砑光。卷边的尺寸占辊直径的0.1-0.2毫米。该卷边对于膜带的整个宽度上厚度的均匀分布十分重要。
基于用于该方法的通常高的辊距力，聚合物分子在挤压方向上拉长。产生的定向作用导致清晰、明显高的光学各向异性。
对比例2
按下列方法，制备浇铸的聚碳酸酯膜，膜厚为0.08毫米：
在一个用搅拌器搅拌的混合容器中，将聚碳酸酯溶解在由丙酮和二氯甲烷组成的溶剂混合物中。
接着用一个2微米高精密薄膜式压滤机除去聚碳酸酯溶液中的大颗粒杂质。接着将聚碳酸酯溶液倒入一个浇铸机中，加工成80微米厚的膜，浇铸机由23米滚转驱动的48米长的钢带构成。将随后干燥步骤中蒸发的溶剂再返回到该过程中。
制成的PC浇铸膜尽管具有足够低的光学各向异性，但是不能免于干扰性的光学缺陷，例如胶粒和条纹。
用有机溶液制备浇铸膜的方法花费昂贵，对技术的安全性要求也很高。所制成的膜难免含有高毒性的有机溶剂，因此，从毒理学的角度考虑是令人担心的。
制备具有光学上高价值状态的大面积钢带或制得有本发明熔融浇铸法的冷却滚动辊这样明显较小的表面是很困难的。因此，在膜表面上产生了不允许的较大数量的条纹。尽管使用了2微米高精密薄膜式压滤机，但是并不能避免使激光信号强度减弱的胶体状聚集。与挤压装置中的熔融物加工不同，在“溶液浇铸”中没有剪切场，因此，很难分解的聚碳酸酯的高分子成分基于“微观布朗式运动”的可能性，即产生尽可能低的界面能，而会发生聚集。
胶体条纹和拉制的条纹使激光信号强度减弱到不允许的低水平，因此，在放奏如此保护的CD***时会出现大量的信号故障。
参考标记
10--熔融膜
15--由熔融膜形成的膜
20--冷却滚动辊
30--喷嘴
| 特性实施例 | 收缩量190℃/30分钟[％]MD*/TD* | 光雾[％]ASTM-D1003 | 程差[纳米] | 双折射Δn | 拉力试验ISO 527-3断裂伸长[％]MD*/TD* |
| 本发明膜用于压铸光学数据记录媒体的冷却滚动挤压PC模制材料厚度：0.08毫米 | ＜1/＜1 | 0.5 | 31 | 4·10-4 | 39/35 |
| 对比例1·在砑光法中制备的PC膜挤压模制材料厚度：0.13毫米 | 31/-7 | 0.3 | 360 | 3·10-3 | 145/99 |
| 对比例2·由有机溶液浇铸的PC膜(商品名Pokalon)厚度：0.08毫米 | 3 | 1.2 | 29 | 4·10-4 | 未测量 |
*MD：机械方向
*TD：横向
说明：“收缩量”确定了本发明与对比例1的界限。
光雾确定了本发明与对比例2的界限。
双折射和程差确定了本发明与对比例1的界限。
断裂伸长确定了本发明与对比例1的界限。
Claims (5)
1.一种光学几乎各向同性的塑料膜的制备方法，由直链或支链的聚碳酸酯制成，其特征在于，用冷却滚动法熔融浇铸聚碳酸酯熔融物，其中，所使用的聚碳酸酯的平均分子量在10000-40000之间，挤压喷嘴内表面的挤压喷嘴边缘区域的粗糙深度RA，根据DIN 4768标准，为0.025-0.002，和挤压喷嘴的内表面涂覆有与聚碳酸酯熔融物不相容的试剂。
2.按权利要求1的方法制备的其厚度低于200微米的聚碳酸酯膜。
3.权利要求2聚碳酸酯膜的用途，用作光学数据记录媒体的抗刮痕膜。
4.权利要求2聚碳酸酯膜的用途，用作光学数据记录媒体的载体材料。
5.权利要求2聚碳酸酯膜的用途，用作制备显示器和荧光屏覆盖膜的基础材料。
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| DK1060209T3 (da) * | 1997-12-05 | 2004-10-04 | Roehm Gmbh | Fremgangsmåde til fremstilling af overfladehårde PMMA-folier, som kan håndteres i "Film-Insert-Moulding"-fremgangsmåden, har höjglans på begge sider og er frie for gellegemer |
| DE19836800A1 (de) | 1998-08-14 | 2000-02-17 | Roehm Gmbh | Optisch isotrope Polycarbonat-Folien sowie Verfahren zu deren Herstellung |
| JP2002074749A (ja) | 2000-08-30 | 2002-03-15 | Sony Corp | 光学記録媒体およびその製造方法 |
| JP2003123323A (ja) * | 2001-10-03 | 2003-04-25 | Sony Corp | 光情報媒体 |
| US20030214070A1 (en) * | 2002-05-08 | 2003-11-20 | General Electric Company | Multiwall polycarbonate sheet and method for its production |
| DE10238188A1 (de) * | 2002-08-15 | 2004-03-04 | Panta Gmbh | Verfahren zur Herstellung klebstofffreier Flachleiter-Bandkabel |
| DE10354546A1 (de) * | 2003-11-21 | 2005-06-23 | Bayer Materialscience Ag | Polycarbonat-Massivformkörper mit verbesserten optischen und verarbeitungstechnischen Eigenschaften |
| US20050274247A1 (en) * | 2004-06-14 | 2005-12-15 | Sean Talkington | Stripper apparatus and methods for rotary dies |
| DE102005020424A1 (de) * | 2005-04-29 | 2006-11-02 | Röhm Gmbh | Verfahren zur Herstellung einer Folie aus thermoplastischem Kunststoff, Folie und Verwendung der Folie |
| US20070013100A1 (en) * | 2005-07-13 | 2007-01-18 | Capaldo Kevin P | Method for producing plastic film |
| DE102006025481A1 (de) * | 2006-05-30 | 2007-12-06 | Röhm Gmbh | Verfahren zur Herstellung einer eingefärbten Folie aus thermoplastischem Kunststoffen, Folie und Verwendung der Folie |
| DE102010062900A1 (de) | 2010-12-13 | 2012-06-14 | Evonik Röhm Gmbh | Verfahren zur Herstellung von Lichtleitkörpern und deren Verwendung in Beleuchtungseinheit |
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| DE2729763A1 (de) * | 1977-07-01 | 1979-01-18 | Bayer Ag | Thermoplastisch verarbeitbare polycarbonatmischungen |
| DE3347684A1 (de) * | 1983-12-31 | 1985-08-29 | Bayer Ag, 5090 Leverkusen | Verfahren zur herstellung von kunststoff-folien mit verbesserten optischen eigenschaften |
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