CN102264792A - 热塑性聚氨酯制成的光导向装置 - Google Patents
热塑性聚氨酯制成的光导向装置 Download PDFInfo
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- CN102264792A CN102264792A CN2009801531113A CN200980153111A CN102264792A CN 102264792 A CN102264792 A CN 102264792A CN 2009801531113 A CN2009801531113 A CN 2009801531113A CN 200980153111 A CN200980153111 A CN 200980153111A CN 102264792 A CN102264792 A CN 102264792A
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- Prior art keywords
- thermoplastic polyurethane
- photoconduction
- aforesaid right
- vulcabond
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Classifications
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Abstract
本发明涉及适合用于生产光导向装置的热塑性聚氨酯(下文称TPU)，涉及其生产方法，并涉及基于TPU的光导向装置。
Description
本发明涉及适用于生产光导体的热塑性聚氨酯(下文称TPU)，涉及其生产的方法，还涉及基于TPU的光导体。
已知光波导向装置可用于传输大量数据，并且该数据传输不受干扰，即不受电磁场的影响。存在的已知光导体由玻璃纤维组成，但也有已知光导体由塑料组成。塑料组成的光导体特别已知于机械工程领域、汽车构造领域和办公领域。这类光导体也称作“聚合物光纤”，其可具有由传输光的聚合物组成的光芯、光学覆盖层材料和保护套。工业上使用的主要聚合物的实例对于芯而言有聚甲基丙烯酸甲酯，对于覆盖层材料而言有含氟聚合物(例如聚偏二氯乙烯或聚四氟乙烯)。
US-A-4 836 646已公开使用具体的保护层(“覆盖层”)，并且关于所述光学芯此处一般性地提及了聚苯乙烯、聚甲基丙烯酸甲酯、聚碳酸酯、聚氨酯，或者苯乙烯与甲基丙烯酸甲酯、苯乙烯与丙烯酸甲酯、甲基丙烯酸甲酯与丙烯酸乙酯、苯乙烯与α-甲基苯乙烯或苯乙烯与乙烯基甲苯的共聚物。US 2008/0117639 A1公开了具有聚光效果的光导板，其可在光传输期间使其变化。为此使用的塑料意欲为TPU、PC、硅氧烷、PMMA或PET。
WO 94/09048 A1已公开玻璃状的交联聚氨酯和聚氨酯网络，并且这些聚氨酯可用于生物医药应用，一个实例为光学纤维。该文件旨在化学计量地使用羟基基团和异氰酸酯基团并且所述多元醇具有低分子量。
然而，基于柔性、弹性且高度透明的塑料的已知光导材料不能可靠地提供足够的光传输以用于长度大于3m的发射器/接收器设备。此外，光导塑料(例如聚甲基丙烯酸甲酯)对于柔性连接而言太硬且太脆，并且使用玻璃纤维的无机光导体不适合窄弯曲半径。已知的光导体吸收损耗过度和/或机械性质不足。
本发明的一个目的是提供这样的改进的光导体，其具有柔性、弹性且高度透明，并且其即使在长度较高时也可靠提供足够的光传输。
本发明提供一种光导热塑性聚氨酯，其可获自
A)至少一种二异氰酸酯
B)至少一种多元醇
C)至少一种异氰酸酯-反应性的增链剂，其中在所述热塑性聚氨酯中，
a)芳族化合物和共轭π-电子体系的含量是至多40重量％、优选至多25重量％、特别优选至多10重量％，基于包括存在的任意添加剂的所述热塑性聚氨酯计，
b)热塑性聚氨酯的折射率是至少1.50、优选至少1.52，并且
c)总的不透度小于10％、优选小于7％。
在a)中芳族化合物和共轭π-电子体系的含量是基于芳族化合物(不含氢H)、不饱和碳原子和作为π-电子体系的部分的杂原子(但此处不包括氧原子)的重量计。
折射率是在20℃的温度下测定，并且总的不透度优选通过实施例中所述的方法确定。优选在均匀层厚度为2mm的试件上测量折射率，所述试件通过将液态光导热塑性聚氨酯倾倒在平坦的水平取向的光滑表面上制成，下文也称作注射模塑板。然后对该铸造板冲压或切割得到合适尺寸的试件。
本发明还提供本发明的TPU用作光导体——特别是纤维——中的光导元件的用途。
本发明还提供一种生产光导体的方法，其包括使用本发明的TPU作为光导材料，特别是纤维和管中的光导材料。
本发明还提供一种生产本发明TPU的方法，其包括使至少一种有机二异氰酸酯A)、至少一种优选线性的羟基封端的多元醇B和至少一种基于二元醇的短链增链剂反应，其包括：
-使用的NCO基团与全部异氰酸酯-反应性基团的当量比为0.9∶1.0至1.2∶1.0、优选0.95∶1.0至1.10∶1.0
-不引入散射中心
-以及，不引入或基本不引入吸收UV辐射和/或VIS辐射的添加剂。
本发明的其他实施方案可见于权利要求、说明书和实施例中。当然，在不超过本发明范围的情况下，本发明制品/方法/用途的上述特征不仅可以各种所述的组合使用，还可以其他组合使用，这也同样适用于下文所述的本发明特征。
热塑性聚氨酯TPU是这样的聚氨酯，其在一定温度范围内可反复经受加热软化和冷却硬化，并在软化状态中可反复经由铸造以模塑部件、挤出物、或成形部件的形式进行模塑，从而得到半成品或得到制品。所述TPU是嵌段共聚物；这些共聚物在分子内具有硬的和软的链段。在一个优选的实施方案中，对于脂族TPU而言，硬质相的比例基于全部TPU计，优选为15至65重量％、特别是40至65重量％，其中硬质相比例通过下式定义：
其中定义如下：
MCEx：增链剂x的摩尔质量，以g/mol计
mCEx：增链剂x的质量，以g计
Miso：所使用的异氰酸酯的摩尔质量，以g/mol计
mtot：所有起始材料的总质量，以g计
k：增链剂的数目。
此外，优选避免使用任何这样的添加剂，即在约280至800nm范围内具有显著吸收或由散射中心产生的散射的类型。
在本发明的上下文中，“无显著吸收”意指2mm注射模塑板在280nm至800nm范围内的透射比是大于80％、优选大于85％、更优选大于90％、特别优选大于95％。
在本发明的上下文中，散射中心是在所使用的波长下在垂直于入射的方向上造成光散射的任何粒子。如果散射中心的最大尺寸是所使用光波长的4/2、优选1/1、更优选1/2、特别优选1/4，则光散射的发生随在透明TPU上入射光波长的变化而变化。
相应地，称作散射中心的粒子是最长空间尺寸为光导体上入射光波长的小于4/2、优选1/1、更优选1/2、特别优选1/4的那些粒子。
散射中心极特别优选最大直径的空间尺寸为大于0.7μm、优选大于0.6μm、特别优选大于0.5μm的粒子。
本发明热塑性聚氨酯通过使异氰酸酯A与多元醇B和任选地对异氰酸酯具有反应性的其它化合物、以及与增链剂C反应而生产，所述反应任选在催化剂D和/或常规助剂E的存在下进行。
常用于聚氨酯生产的组分A、B、C以及任选地D和/或E将示例说明如下：
a)使用的有机异氰酸酯A可包括熟知的芳族、脂族、脂环族和/或芳脂族异氰酸酯，优选二异氰酸酯，实例有：二苯基甲烷-2，2’-、2，4’-和/或4，4’-二异氰酸酯(MDI)、亚萘基-1，5-二异氰酸酯(NDI)、甲苯-2，4-和/或2，6-二异氰酸酯(TDI)、二苯基甲烷二异氰酸酯、3，3’-二甲基二苯基二异氰酸酯、1，2-二苯基乙烷二异氰酸酯、和/或亚苯基二异氰酸酯、三-、四-、五-、六-、七-和/或八亚甲基二异氰酸酯、2-甲基五亚甲基-1，5-二异氰酸酯、2-乙基亚丁基-1，4-二异氰酸酯、五亚甲基-1，5-二异氰酸酯、亚丁基-1，4-二异氰酸酯、1-异氰酸根合-3，3，5-三甲基-5-异氰酸根合甲基环己烷(异佛尔酮二异氰酸酯，IPDI)、1-异氰酸根合-4-[(4-异氰酸根合环己基)甲基]环己烷(H12MDI)、2，6-二异氰酸根合己烷羧酸酯、1，4-和/或1，3-双(异氰酸根合甲基)环己烷(HXDI)、环己烷-1，4-二异氰酸酯、1-甲基环己烷-2，4-和/或2，6-二异氰酸酯、和/或二环己基甲烷-4，4’-、2，4’-和2，2’-二异氰酸酯，优选二苯基甲烷2，2’-、2，4’-和/或4，4’-二异氰酸酯(MDI)、亚萘基-1，5-二异氰酸酯(NDI)、甲苯-2，4-和/或2，6-二异氰酸酯(TDI)、六亚甲基二异氰酸酯、1-异氰酸根合-4-[(4-异氰酸根合环己基)甲基]环己烷、和/或IPDI。
特别优选的异氰酸酯是脂族异氰酸酯，例如六亚甲基二异氰酸酯以及特别是H12MDI。
b)使用的对异氰酸酯具有反应性的化合物(b)可包括熟知的对异氰酸酯具有反应性的化合物，实例有聚酯醇、聚醚醇和/或聚碳酸酯二醇，其也经常统称为“多元醇”，其数量平均摩尔质量(Mn)为500g/mol至8000g/mol、优选600g/mol至6000g/mol、特别是800g/mol至小于3000g/mol，并且优选地，其相对于异氰酸酯的平均官能度为1.8至2.3、优选1.9至2.2、特别是2。
优选使用聚醚多元醇，实例是基于熟知的起始物质和基于常规环氧烷的那些，所述环氧烷例如环氧乙烷、环氧丙烷和/或环氧丁烷；优选基于1，2-环氧丙烷和环氧乙烷的聚醚醇，并且特别是聚氧基四亚甲基二醇。所使用的聚醚醇还可包括已知作为低不饱和聚醚醇的那些。就本发明而言，低不饱和多元醇特别是不饱和化合物的含量小于0.02meq/g、优选小于0.01meq/g的聚醚醇。该类聚醚醇大部分通过使环氧烷(特别是环氧乙烷、环氧丙烷及其混合物)在高活性催化剂的存在下加合至上述二元醇或三元醇上而反应生成。
该类高活性催化剂的实例是氢氧化铯和多金属氰化物催化剂，也称作DMC催化剂。经常使用的DMC催化剂是六氰钴酸锌。DMC催化剂可在反应后存留于聚醚醇中，但通常将其除去，例如通过沉降或过滤除去。
也可使用多种多元醇的混合物来代替使用一种多元醇。特别优选地，作为组分(b)的本发明的热塑性聚氨酯基于聚四氢呋喃，其数量平均摩尔质量(Mn)为600g/mol至2000g/mol、优选800g/mol至1400g/mol、特别优选950g/mol至1050g/mol。
c)使用的增链剂C可包括熟知的脂族、芳脂族、芳族和/或脂环族化合物，其数量平均摩尔质量为50g/mol至499g/mol，优选双官能的化合物，实例是在亚烷基基团中具有2至10个碳原子的烷二醇，优选1，4-丁二醇、1，6-己二醇，和/或具有3至8个碳原子的二-、三-、四-、五-、六-、七-、八-、九-和/或十亚烷基二醇，优选未支化的烷二醇，特别是1，3-丙二醇和1，4-丁二醇。
d)特别加速二异氰酸酯A的NCO基团与组分B之间反应的合适的催化剂D为：常规的且现有技术已知的叔胺，实例有三乙胺、二甲基环己基胺、N-甲基吗啉、N，N’-二甲基哌嗪、2-(二甲基氨基乙氧基)乙醇、二氮杂二环[2.2.2]辛烷等；并且还特别是有机金属化合物，例如钛酸酯(titanic ester)，铁化合物优选乙酰丙酮酸铁(III)，锡化合物优选二乙酸亚锡、二辛酸亚锡、二月桂酸亚锡，或在另一个优选的实施方案中，脂族羧酸的二烷基锡盐，更优选二乙酸二丁锡、二月桂酸二丁锡等。催化剂的常用量为0.00001至0.1重量份/100重量份多羟基化合物(b)。
e)也可将常规助剂E与催化剂D一起加入结构组分A至C中。可提及的实例有发泡剂、表面活性剂、阻燃剂、成核剂、润滑剂和脱模剂、染料、以及颜料、稳定剂(例如用于保护避免水解、光、热或脱色的稳定剂)、无机和/或有机填充剂、增强剂、增塑剂和金属钝化剂。优选使用的水解稳定剂是低聚和/或多聚脂族或芳族碳二亚胺。
然而，在一个优选实施方案中，这类助剂的用量基于包括添加剂的热塑性聚氨酯的总重量计，至多1重量％、特别是至多0.1重量％。一个特别优选的实施方案不使用所述助剂。
特别优选基于氢化MDI和至少一种聚醚醇的TPU，基于包括存在的任何添加剂的热塑性聚氨酯计，其芳族化合物和共轭π-电子体系的最大比例为25重量％、优选至多10重量％，特别是不包括芳族化合物的TPU。
“不包括芳族化合物”是指，在0.25μm至0.35μm的光波长范围内，由厚度为2mm的注射模塑板制成的试件的透射率大于30％、更优选大于50％、特别优选大于70％。
TPU可通过已知的方法分批或连续地生产，例如使用反应挤出机(reactive extruder)法或带式机法以一步法过程或以预聚物过程生产，优选以一步法过程生产。在这些方法中，反应组分A、B和任选地C、D和/或E可相继或同时彼此混合，由此立即开始反应。在挤出机法中，将结构组分A、B以及任选地C、D和/或E单独地或以混合物的形式加入挤出机中，并且优选在100℃至280℃、更优选140℃至250℃的温度下反应，并且将生成的热塑性聚氨酯挤出、冷却并粒化。
为了优化TPU，可改变多元醇组分B和增链剂C。一个优选的实施方案设定多元醇B与待使用的全部增链剂C的重量比为20至2、特别是8至3。
在一个优选的实施方案中，异氰酸酯A与异氰酸酯-反应性组分的反应以950至1050、特别优选970至1010、特别是980至1000的指数发生。此处的指数通过反应期间组分A中所使用的全部异氰酸酯基团与异氰酸酯-反应性基团(即特别是基团B和C)的比例定义。如果指数是1000，则对于组分A的每个异氰酸酯基团存在一个活性氢原子。如果指数大于1000，则存在比OH基团更多的异氰酸酯基团。
本发明的光导TPU可直接拉制以生产线材、管或纤维，它们用于光导体应用中。在一个优选的实施方案中，本发明的TPU用于复合导体中，所述复合导体包含光导体形式的本发明的TPU，其优选还具有其他层(覆盖层)以改进光导体内的全反射。在一个更优选的实施方案中，覆盖层可具有一个环绕外层以保护免受机械损害。
覆盖层是光导体上的附加层，在本案中是在热塑性聚氨酯上的附加层，该层的折射率与光导体不同。当不具有覆盖层时，光导体边界层的反射由光导体与空气之间的折射率差确定，而当具有包覆层时，相应的反射行为由光导体的折射率与覆盖层的折射率的比例确定。由于光在边界层发生反射的最大角度取决于折射率差，因而当光导体弯曲时，光导体与覆盖层之间的折射率差特别重要。光导体的芯的折射率优选大于1.45、更优选大于1.5。这样，光会保持在该半径内，即使光导体经受弯曲也不会逃逸出去。随着光导体和覆盖层之间的折射率差变得更大，光导体弯曲的程度也可变得更大。光导体和覆盖层之间的折射率差优选大于0.1、更优选大于0.15、特别优选大于0.2。
在另一个实施方案中，本发明的TPU可用于复合导体中，所述复合导体包括中心电导体(例如铜线)以及一个由本发明的光导TPU组成的环形环绕层，其中TPU环本身具有一个环绕覆盖层。在一个更优选的实施方案中，覆盖层一个环绕涂层以保护免受机械损害。这类结构优选适用于汽车中信号传输。
本发明材料作为光导体的具体应用可存在于汽车构造中，其中传输距离为3至5m。另一个可考虑的应用是用在部件具有高移动自由度的能源供应体系中，特别是当传输距离是3至5m时。此处，柔性透明的光导TPU可用于对柔性能量电缆进行覆盖。可能的汽车应用不仅为预防性地检测对具有安全功能的线(ABS电缆、制动软管)的损害，而且还为快速进行数据传输以在没有任何干扰电压的情况下实现控制和测量目的。另一个应用的实例是用于仪器背景照明的柔性体系。
合适的覆盖层优选含氟聚合物、含氟弹性体和已知于US-A-4836646的聚氨酯-硅氧烷共聚物。
实施例
1.组分
以下组分用于下述实施例中：
表1
2.测定方法
使用热塑性聚氨酯以挤出直径为2mm的线材作为光导体。
为测定透光率，将线材的输入端(即光入射到光导体上的位置)通过连接套管连接至“超亮白色”LED(发光二极管)(直径5mm)上或连接至激光二极管(LD)上。此处连接位点设计为使激光二极管与与其轴垂直交切的光导体表面垂直接触。光导体末端也与所述光导体轴垂直交切。这样，来自LED或LD的光信号就输入至(即入射至)测试部分(即光导体)。测量使用这样的方法进行，即，使来自LED或LD和getSpec 2048小型分光计的380nm至780nm的范围内的光信号的直接入射，并使用以下光功率或照度：
LED(白色)光功率＝47μW，
照度＝1000lux
激光二极管LD(红色)光功率＝450μW，
照度＝3450lux
在测试样品部分的末端(即由直径为2mm的热塑性聚氨酯制成的光导体)存在一个已通过市售光导体(直径为200μm/置于光学检测器囊内的中央)连接至getSpec 2048分光计上的光学检测器。测试的光导体的长度最高达8m。
总的不透度按照如下测定：
测色设备用于测量试件的颜色，首先用光阱作为背景然后用白色贴图(white tile)作为背景，在反射中，排除镜面反射。亮度(根据DIN 6174的L值)以比例形式计算，并表示为以％计的不透度。
使用购自HunterLab的“UltraScan”测色设备或等同设备。样本根据AA E-10-132-002生产。测色设备在达到操作温度进行标准化，一般持续30分钟的时间，并且按以下参数运行：
模式：RSEX(排除镜面反射(Reflection Specular Excluded))，使用排除了镜面反射的反射，打开光泽阱(gloss trap)
视图面积(area view)：大
口径：25.4
UV滤光器：关闭
以下公式用于计算总的不透度：
不透度＝(黑色的L值/白色的L值)×100％
如此，0％的不透度值意指样本完全透明，100％的值意指完全不透明。
折射率是使用折射计和日光-光谱光测定。
3.生产TPU的方法的一般说明
测试挤出物在以下条件下生产，直径为约2mm：
表2
| 挤出机： | 同向旋转双螺杆挤出机，APV MP19 |
| 温度分布： | HZ1(进料)175℃至185℃ |
| HZ2 180℃至190℃ | |
| HZ3 185℃至195℃ | |
| HZ4 185℃至195℃ | |
| HZ5(停止)180℃至190℃ | |
| 螺旋旋转速率： | 100rpm |
| 压力： | 约10至30bar |
| 挤出物冷却： | 水浴(10℃) |
4.具体实施例
以下TPU使用以上给出的起始组分以所述的方法生产(除非另外说明，数据以g计)。
表3
表中数据未给出单位的，该数据以克[g]计。
可能的传输距离的测量
样本线材在上述方法中使用以传输来自LED和LD的可见光谱区的光，同时检测或确定能提供足以适合应用的脉冲传输的最大可能传输距离。
表4
| TPU | RT(LED) | RT(LD) | |
| TPU1 | 1.5 | 2.6 | |
| TPU2 | 1.4 | 2.5 | |
| TPU3 | 2.9 | 4.0 | |
| TPU4 | 4.0 | 6.0 |
RT：能提供足以适合应用的脉冲传输的最大相对传输距离[m]
使用的光源如下：
LED(白色)光功率47μW，照度1000lux
激光二极管LD(红色)光功率450μW，照度3450lux
Claims (9)
1.一种光导热塑性聚氨酯，获自
A)至少一种二异氰酸酯
B)至少一种多元醇
C)至少一种异氰酸酯-反应性的增链剂，其中在所述热塑性聚氨酯中，
a)芳族化合物和共轭π-电子体系的含量为至多40重量％、优选至多25重量％、特别优选至多10重量％，基于包括存在的任意添加剂的所述热塑性聚氨酯计，
b)所述热塑性聚氨酯的折射率为至少1.50、优选至少1.52，且
c)总的不透度是小于10％、优选小于7％。
2.权利要求1的光导热塑性聚氨酯，其中所使用的二异氰酸酯A)包括脂族二异氰酸酯，且所使用的多元醇包括聚醚醇。
3.上述权利要求中至少一项的光导热塑性聚氨酯，其中所述二异氰酸酯A)是1-异氰酸根合-4-[(4-异氰酸根合环己基)甲基]环己烷。
4.上述权利要求中至少一项的光导热塑性聚氨酯，其中所述多元醇是平均分子量为600至2000的聚醚醇。
5.上述权利要求中至少一项的光导热塑性聚氨酯，其中所使用的多元醇包括聚四氢呋喃。
6.上述权利要求中至少一项的光导热塑性聚氨酯，其中所述增链剂C是1，4-丁二醇。
7.上述权利要求中至少一项的光导热塑性聚氨酯用作光导体中的光导元件的用途，特别是用作光导纤维和光导管中的光导元件的用途。
8.一种用于生产光导体的方法，其包括使用上述权利要求中至少一项的光导热塑性聚氨酯作为光导材料。
9.一种生产上述权利要求中至少一项的光导热塑性聚氨酯的方法，其包括使至少一种有机二异氰酸酯A)、至少一种优选线性的羟基封端的多元醇B和至少一种基于二元醇的短链增链剂反应，其包括
-使用的NCO基团与全部异氰酸酯-反应性基团的当量比为0.9∶1.0至1.2∶1.0、优选0.95∶1.0至1.10∶1.0
-不引入散射中心
-以及，不引入或基本不引入吸收UV辐射和/或VIS辐射的添加剂。
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| CN114690307A (zh) * | 2020-12-31 | 2022-07-01 | 三芳化学工业股份有限公司 | 热塑性聚氨酯导光纤维及其制造方法 |
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| AU782220B2 (en) | 2000-10-13 | 2005-07-14 | Talex Optical Co., Ltd. | Polyurethane resin composition and optical lens having impact resistance |
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| CN114690307A (zh) * | 2020-12-31 | 2022-07-01 | 三芳化学工业股份有限公司 | 热塑性聚氨酯导光纤维及其制造方法 |
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