CN1028239C - 可用激活能射线固化的组合物及其用途 - Google Patents

可用激活能射线固化的组合物及其用途 Download PDF

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CN1028239C
CN1028239C CN88108507A CN88108507A CN1028239C CN 1028239 C CN1028239 C CN 1028239C CN 88108507 A CN88108507 A CN 88108507A CN 88108507 A CN88108507 A CN 88108507A CN 1028239 C CN1028239 C CN 1028239C
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compound
acrylate
ester
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CN1033822A (zh
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时田卓
山根健次
稻垣始
粟栖正吉
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Mitsui Chemical Industry Co Ltd
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Mitsui Petrochemical Industries Ltd
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Abstract

一种可用激活能射线固化的组合物，包括(A)一种环氧树脂，(B)一种选自锍盐和环戊二烯合铁类的化合物，(C)一种选自丙烯酸酯、甲基丙烯酸酯及其低聚物的化合物，(D)一种有机过氧化物，以及任选的(E)橡胶组分。所述组合物可用作光学记录介质的粘合层。

Description

本发明涉及一种可用激活射线固化的组合物，该组合物可通过诸如紫外线（UV）、电子射束（EB）或各种放射线之类的激活能射线进行固化，还涉及一种含有该组合物的固化产物作为粘合层的光学记录介质，例如光学记录盘或光学存储卡。
在现有技术中，光盘是借助光致固化剂将一种在基片上形成的记录层粘合到一种透光性保护材料上而制备的。用于此目的的光致固化剂最好在短时间内即能起到固化粘合作用，并且不含可能危害该记录层的组分，此外也不应该对基片的光学性质（如透明度）产生不利的影响。
目前已经知道一些环氧树脂组合物是可以用激活能射线固化的。然而，许多这类组合物在固化初始阶段的粘合性都很差，而且由于它们的固化时间较长，使得无法提高光盘生产线的生产速度。此外，在潮湿条件下许多这类组合物的粘合强度都较低。
已知有许多种树脂制成的基片已用于光学记录介质中。然而，本行业所寻求的是由这样一些树脂所制备的基片，即这些树脂要具有优异的耐热性、熔融模塑时固化以后收缩率很低、使用条件下具有长期尺寸稳定性、尤其是要求在高温高湿度条件下吸收水分后尺寸变化很小。
本发明的目的是提供一种具有各组分新型组合形式的可用激活能射线固化的组合物。
本发明的目的还包括提供一种可用激活能射线固化的组合物，这种组合物在激活能射线辐照下可以极迅速地固化。
本发明的目的还包括提供一种可用激活能射线固化的组合物，这种组合物在固化初期具有极好的粘合性，还具有优异的耐水分粘合力。
本发明的目的还包括提供一种新型光学记录介质，其中含有上述本发明的组合物的固化产物作为粘合层。
本发明的目的进一步包括提供含有这样一种粘合层和基片层的光学记录介质;所述粘合层具有很高的粘合强度和优异的耐水性及耐潮湿性，并且不会损害基片的光学性质;所述基片层在使用条件下，尤其的在高温高湿度条件下具有极好的尺寸稳定性。
本发明的其它目的及其优点通过以下的介绍将会更加明了。
根据本发明，这些目的和优点首先是通过一种可用激活能射线固化的组合物而实现的，所述组合物含有：
（A）一种环氧树脂，
（B）一种选自锍盐和环戊二烯合铁类的化合物，
（C）一种选自丙烯酸酯、甲基丙烯酸酯及它们的低聚物的化合物，
（D）一种有机过氧化物。
在附图中，图1示出通过磁力紧固的方法固定 在转盘1上的光盘3;图2示出用来测定本发明的组合物在固化过程中的粘合力的试样组合形式;图3示出的是测定光盘粘合强度所用装置的示意图;图4是一张粗略的断面图，示出测定光盘基片与一种毂盘之间粘合强度的试验方法。
本发明的组合物中所含的环氧树脂（A）最好是在其每个分子中至少含有两个环氧基团。特别优选的是脂族或脂环族环氧化合物。
上述环氧树脂（A）的具体例子包括多酚化合物[如双酚A、双酚F和1，1，2，2-四（4′-羟基苯基）乙烷]的缩水甘油醚;多元酚（如儿茶酚、间苯二酚、氢醌和间苯三酚）的缩水甘油醚;多元醇（如乙二醇、丁二醇、丙三醇、赤藓醇和聚氧化亚烷基二醇）的缩水甘油醚;可溶可熔型酚醛环氧树脂;脂环族环氧树脂，如二氧化乙烯基环己烯，二氧化苎烯和二氧化二聚环戊二烯;多元羧酸（如邻苯二甲酸和环己烷-1，2-二甲酸）的酯缩合产物的多缩水油酯;多缩水甘油基胺型环氧树脂。其中优选的是多酚化合物的缩水甘油醚和可溶可熔型酚醛环氧树脂，更为优选的是双酚A和双酚F的缩水甘油醚，最优选的是双酚A的缩水甘油醚。
本发明的组合物中含有一种锍盐或一种环戊二烯合铁化合物（B）。
优选的锍盐是三芳基锍盐，特别优选的是三苯基锍盐。例如，所述锍盐的阴离子部分是AsF- 6或BF- 4。
上述锍盐的例子有三苯基锍盐，如
三（4-甲基苯基）锍盐，如
Figure 881085073_IMG1
三（4-甲氧基苯基）锍盐，如
Figure 881085073_IMG2
所述环戊二烯合铁化合物可以在其分子中含有两个环戊二烯基或含有一个环戊二烯基和一个芳族基团（如苯基或异丙苯基）;后者是优选的。结合有一个环戊二烯基和一个异丙苯基的铁化合物尤为理想。
环戊二烯含铁化合物的例子有环戊二烯基异丙苯基铁（Ⅱ）盐，如
Figure 881085073_IMG3
作为本发明的组合物中的化合物（B），上述锍盐和环戊二烯合铁化合物既可单独使用，也可合用。作为化合物（B），上述化学式的环戊二烯基异丙苯基铁（Ⅱ）盐尤其适用。
本发明组合物中的化合物（C）是选自丙烯酸酯、甲基丙烯酸酯和它们的低聚物。
所用的丙烯酸酯或甲基丙烯酸酯可以是羟基化合物或二羟基及多羟基化合物与丙烯酸或甲基丙烯酸所成的酯。这些酯可以是丙烯酸或甲基丙烯酸与下列羟基化合物所成的酯，如C1-20脂族一元醇，C1-30脂环醇，C1-20脂族二元醇，C1-20脂环二元醇，C3-20三元醇和带有羟端基的聚酯。
这些酯的具体例子包括;丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸丁酯、丙烯酸环己酯、丙烯酸降冰片烷酯、丙烯酸联环戊基酯、丙烯酸联环戊烯基酯、丙烯酸异冰片基酯、甲基丙烯酸环己酯、如下式的六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-丙烯酸酯：
Figure 881085073_IMG4
12-甲基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-丙烯酸酯、11-甲基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-丙烯酸酯、12-乙基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-丙烯酸酯、11-乙基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-丙烯酸酯、具下式的八环[8，8，12，9，14，9，111，18，113，16，0，03，8，012，17]二十二烷基-5-丙烯酸酯：
Figure 881085073_IMG5
15-甲基八环[8，8，12，9，14，7，111，18，113，16，0，03，8，012，17]二十二烷基-5-丙烯酸酯、2，7-二甲基四环[4，4，0，12，5，17，10]十二烷基-3-丙烯酸酯、2，10-二甲基四环[4，4，0，12，5，17，10]二十烷基-3-丙烯酸酯、11，12-二甲基四环[4，4，0，12，5，17，10]二十烷基-3-丙烯酸酯、具下式的四环[4，4，0，12，5，17，10]十二烷基-3-丙烯酸酯：
Figure 881085073_IMG6
9位取代的四环[4，4，0，12，5，17，10]十二烷基-3-丙烯酸酯（9位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟）、8位取代的四环[4，4，0，12，5，17，10]十二烷基-3-丙烯酸酯（8位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟）、8，9位二取代的四环[4，4，0，12，5，17，10]十二烷基-3-丙烯酸酯（8位和9位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟）、六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-甲基丙烯酸酯、12-甲基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-甲基丙烯酸酯、11-甲基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-甲基丙烯酸酯、12-乙基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-甲基丙烯酸酯、11-乙基六环[6，6，1，13，6，110，13，02，7，09，14]十七烷基-4-甲基丙烯酸酯、八环[8，8，12，9，14，9，111，18，113，16，0，03，18，012，17]二十二烷基-5-甲基丙烯酸酯、15-甲基八环[8，8，12，9，14，9，111，18，113，16，0，03，18，012，17]二十二烷基-5-甲基丙烯酸酯、2，7-二甲基四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯、2，10-二甲基四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯、11，12-二甲基四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯、9位取代的四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯（9位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟）、8位取代的四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯（8位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟）、8，9位二取代的四环[4，4，0，12，5，17，10]十二烷基-3-甲基丙烯酸酯（8位和9位上的取代基：甲基、乙基、丙基、异丁基、己基、环己基、硬脂酰基、溴、氟），
如式（Ⅰ）所示两端均由丙烯酸封端的聚酯：
Figure 881085073_IMG7
其中A表示一个丙烯酸残基，M代表一个二价脂族或脂环族醇残基，N代表一个二元酸残基，n是一个正整数，以及如式（Ⅱ）所示两端均由丙烯酸封端且分子链中的羟基亦被丙烯酸所封闭的聚酯：
Figure 881085073_IMG8
其中A的定义同上，X代表一个三元或三元以上的脂族或脂环族醇残基，Y代表一个二元或多元酸的残基，m是正整数。
上述丙烯酸酯或甲基丙烯酸酯，某些已在日本专利公告号136529/1986中予以公开。这些丙烯酸酯或甲基丙烯酸酯可采用已知的方法预聚成低聚物后再使用。
作为本发明组合物的组分（C），优选的是（甲基）丙烯酸烷基酯和式（Ⅰ）、（Ⅱ）所示化合物的混合物。
本发明的组合物中还含有一种有机过氧化物（D）。所述过氧化物的例子包括过氧化苯甲酰、过氧化二氯苯甲酰、氢过氧化异丙苯、过氧化二异丙苯、过氧化二叔丁基、2，5-二甲基-2，5-二（过氧化苯甲酸酯）-3-己炔、1，4-双（叔丁基过氧异丙基）苯、过氧化月桂酰、过乙酸叔丁酯、2，5-二甲基-2，5-二（叔丁基过氧）-3-己炔、2，5-二甲基-2，5-二（叔丁基过氧）己烷、过苯甲酸叔丁酯、苯基过乙酸叔丁酯、过异丁酸叔丁酯、过仲辛酸叔丁酯、过新戊酸叔丁酯、过新戊酸异丙基酯和二乙基过乙酸叔丁酯。
其中优选的是二烷基过氧化物，如过氧化二异 丙苯、过氧化二叔丁基、2，5-二甲基-2，5-二（叔丁基过氧）-3-己炔、2，5-二甲基-2，5-二（叔丁基过氧）己烷和1，4-双（叔丁基过氧异丙基）苯。
本发明的组合物包含组分（A）、（B）、（C）和（D）作为基本组分。本发明的组合物最好含有100份（重量）（A），1-10份，特别是2-5份（重量）（B），15-35份，特别是20-30份（重量）（C），和1-10份，特别是2-15份（重量）（D）。
在本发明的组合物中不必在所有情况下都添加光致聚合引发剂。然而，如果使用能量较低的激活能射线，如紫外线，最好添加上述引发剂。所述光致聚合引发助剂可以是任何一种已知的引发剂，但要求它们一旦经受到UV等类辐照时，应能够分解而产生自由基，或者其中的氢原子经辐照后可被移去从而产生自由基。上述光致聚合引发剂的具体例子包括苯偶姻及它的醚，如苯偶姻甲醚、苯偶姻乙醚、苯偶姻异丙醚和苯偶姻丁醚;二苯酮类化合物，如二苯酮、对-氯二苯酮和对一甲氧基二苯酮;苯偶酰类化合物，如苯偶酰、苯偶酰二甲基缩酮;羟烷基苯基酮类化合物，如1-（4-异丙基苯基）-2-羟基-2-甲基-1-丙酮、1-苯基-2-羟基-2-甲基-1-丙酮和1-（4-叔丁基苯基）-2-羟基-2-甲基-1-丙酮。
可用于本发明的增感剂的例子包括烃类，如蒽、萘、
Figure 881085073_IMG9
和菲;硝基化合物，如对-二硝基苯、对-硝基苯胺、1，3，5-三硝基苯和对硝基联苯;氨基化合物，如正丁基胺、二正丁基胺、三乙胺、甲基丙烯酸二乙基氨基乙基酯、对-硝基苯胺和N-乙酰-4-硝基-1-萘胺;酚类化合物，如苯酚、对-硝基酚、2，4-二硝基酚和2，4，6-三硝基酚;酮类，如苯甲醛、9-蒽醛、苯乙酮、二苯酮、二亚苄基丙酮、苯偶酰、对′，对-二氨基二苯酮和对′，对-四甲基二氨基二苯酮;醌类，如蒽醌、1，2-苯并蒽醌、苯醌、1，2-萘醌和1，4-萘醌;蒽酮类，如蒽酮、1，9-苯并蒽酮、2-氧代-3-氮杂-1，9-苯并蒽酮、6-苯基-1，9-苯并蒽酮、3-苯基-1，9-苯并蒽酮和3-甲基-1，3-二氮杂-1，9-苯并蒽酮。
本发明的组合物基本上是无溶剂的，但有时也可含在溶剂。此外，本发明的组合物还可以含有一些能够在普通无溶剂粘合剂中使用的组分，如反应活性稀释剂、增感剂、增稠剂、防流淌剂、贮存稳定剂和增塑剂。
还可以在本发明组合物中添加一种橡胶组分，以提高粘合强度，用作为胶粘剂时可使上述组合物具有一定的屈挠性。
举例讲，适于加用的上述橡胶组分可以是苯乙烯/（二）烯烃的二嵌段或三嵌段共聚物或其氢化产物。具体例子包括苯乙烯/异戊二烯共聚物、苯乙烯/丁烯共聚物、苯乙烯/乙烯共聚物、苯乙烯/丁二烯共聚物、苯乙烯/丁烯/苯乙烯共聚物、苯乙烯/异戊二烯/苯乙烯共聚物，苯乙烯/乙烯/丁烯/苯乙烯共聚物、苯乙烯/乙烯/丙烯共聚物和苯乙烯/乙烯/丙烯/苯乙烯共聚物。聚异戊二烯、丁基橡胶、氯丁橡胶、丁腈橡胶、有机硅橡胶、丙烯酸类橡胶也可作上述橡胶组分。最优选的是含苯乙烯的橡胶组分。
橡胶组分的加入量相对于（A）、（B）、（C）、（D）各组分总重量100份而言，可达50份（重量），较好是0.05-50份，更好是0.1-30份，最好是0.2-10份（重量）。
本发明的组合物适用于涂覆和粘合各类基材，尤其适用于透明材料，最主要是适用于光学材料，如用于粘合透镜或光盘。尤其是当一种材料中所含的基片容易与化学物质起反应而发生变性（如在一个光盘的记录层中的情况）时，若用本发明的组合物粘合这种材料，组分（C）最好以所述低聚物的形式使用，而且如果需要的话，可添加一种光致聚合引发剂。
准备用本发明组合物涂覆的基片可以是由任何材料制成的。聚碳酸酯聚合物、（甲基）丙烯酸酯聚合物、乙烯/环烯烃共聚物和含有4-甲基-1-戊烯作为主要成分的烯烃共聚物尤为适用，因为本发明的组合物对这些材料的粘合性很好。
根据本发明，提供了一种含有本发明组合物的固化产物作为粘合层的光学记录介质，并将其做为特别推荐的用途。
具体讲，本发明还提供了一种光学记录介质，它包括：
（Ⅰ）由一种乙烯/环烯烃共聚物制成的光盘基片，所述共聚物主要成分如下：
（1）式（1）所示的重复单元
Figure 881085073_IMG10
其中R1、R2、R3、R4、R5、R6、R7、R8、R9、R10、R11和R12各自独立地代表氢原子、卤原子或C1-20烷基，R9可以键合到R11或R12上，形成3元-6元环，R10可以键合到R11或R12上，形成3元-6元环，n是正整数，当n至少为2时，R5、R6、R7或R8中的两个或两个以上基团可以相同，也可不同，
（2）式（2）所示的重复单元
-CH2CH2- （2）
（Ⅱ）由前述含有组分（A）、（B）、（C）和（D）的组合物的固化产物构成的粘合层。
构成上述光学记录介质的该光盘基片（Ⅰ）是由该乙烯/环烯烃共聚物制成的。
该乙烯/环烯烃共聚物最好基本上由10-60%（摩尔）式（1）所示单元和90-40%（摩尔）式（2）所示单元所组成。
式（1）所示单元是由下面的式（1）′所代表的环烯烃（单体）衍生而得到的
Figure 881085073_IMG11
其中所有符号的含意均与式（1）相同。
式（2）所示单元是由乙烯得到的。
在式（1）′中，R1-R12所代表的囟素可以是氟、氯、溴或碘，以氯或溴为好。
所述C1-20烷基可以是直链的或支链的。具体例子有甲基、乙基、丙基、异丙基、丁基、异丁基和正己基。
R9可以键合到R11或R12上形成3元-6元环，R10可以键合到R11或R12上形成3元-6元环。该环最好是碳环。
n是一个正整数。当n为零时，上述式（1）′可改写为
Figure 881085073_IMG12
其中所有符号的含意均与式（1）′相同。
当n是1时，上述式（1）′可改写为
Figure 881085073_IMG13
其中所有符号含意同上。
当n是2时，式（1）′可改写为
Figure 881085073_IMG14
其中所有符号含意同上，式中出现了两次的R5、R6、R7和R8各自可相同或不同。
式（1）′所示的环烯烃中，以式（1）′2的环烯烃为好，因为它们易于制备也容易得到。式（1）′2中R1-R12所有基团都是氢原子的那些环烯烃尤为理想，因为由它们制得的聚合物具有优异的耐热性或耐溶剂性。
式（1）′化合物的例子如下所示：
Figure 881085073_IMG15
Figure 881085073_IMG16
Figure 881085073_IMG17
例如，上述环烯烃可应用在美国专利3，557，072（相当于日本专利公开号14910/1971）或日本专利公告号154133/1982中所公开的方法制备。
式（1）′所示单体和乙烯的共聚物可以在熟知的齐格勒催化剂、尤其是含钒的齐格勒催化剂存在下，将所述单体聚合而制备。例如，这类催化剂和聚合方法已在日本专利公告号168，708/1985中公开。
制备上述共聚物时还可以将另一种单体与之共聚，其用量以不损害该共聚物的性质为度，例如相对于每摩尔乙烯，所述另一种单体的用量不多于1摩尔。所述另一种单体可以是一种α-烯烃或另一种环烯烃。其实例包括一般具有3-20个碳原子的α-烯烃，最好含3-10个碳原子，如丙烯、1-丁烯、3-甲基-1-丁烯、1-戊烯、3-甲基-1-戊烯、4-甲基-1-戊烯、1-己烯、1-辛烯、1-癸烯、1-十二碳烯、1-十四碳烯、1-十六碳烯和1-二十碳烯。所述环烯烃可以是未交联的环烯或一种苯乙烯。其实例是环戊烯、环己烯、3，4-二甲基环戊烯、3-甲基环己烯、2（2-甲基丁基）-1-环己烯、苯乙烯和α-甲基苯乙烯。多烯化合物，如二聚环戊二烯、亚乙基降冰片烯和乙烯基降冰片烯，同样可用来共聚。不饱和羧酸，如马来酸或马来酸酐，也可用来共聚。
本发明所用的乙烯/环烯烃共聚物最好具有0.03-10dl/g，特别是0.1-5dl/g的特性粘度[η]值（在萘烷中于135℃测定）;不大于10%、最好不大于5%的结晶度（由X射线衍射计测定）;不大于5，最好不大于1的碘值;以及50-250℃，最好60-200℃的玻璃化温度（Tg）。
本发明所用的乙烯/环烯烃共聚物的特征在于，式（1）′的单体组分在该共聚物中主要呈式（1）所示的结构。结果该聚合物的碘值一般不大于5，大多数情况下不大于1。这种结构亦为C13-NMR所证实。
由于具有这种结构，使得该共聚物化学性质很稳定，且具有极好的耐水性、耐化学（如碱或酸）性、耐溶剂性、耐热性和耐候性。它的含水量极低，而且尺寸精确性极高。
举例讲，可以按下列步骤制备本发明的光学记录介质;将本发明的组合物在一种有机溶剂（如丙酮、甲乙酮或甲基异丁基酮）中的溶液涂覆到一块基片（Ⅰ）的表面上，再将另一块基片（Ⅰ）叠放在上述涂覆过的表面上，然后用紫外线、电子射束、放射线或γ射线，最好用紫外线或电子射束的辐射线辐照该组合件，从而将该组合物固化成为粘合层。
本发明的光学记录介质，既可以通过将两块都带有光学记录层的基片借助所述粘合层彼此粘合在一起而制成，也可以通过将一块带有光学记录层的基片与另一块不带光学记录层的基片借助所述粘合层彼此粘合在一起而制成。
可用已知的方法在上述基片上提供一层光磁记录层或相变型记录层。如果需要的话，可以在该光学记录层上再形成一种由金属膜等组成的反射层。还可以在所述基片和光学记录层之间或在光学记录层表面上提供一种由介电物质组成的增强层。
本发明提供的可用激活能射线固化的新型组合物，当用诸如紫外线、电子射束、放射线、γ射线（最好是用紫外线、电子射束或放射线）之类的激活能射线进行辐照时，可以在短时间内固化。它的粘合强度很高，而且不损害基片的光学性质。此外由于该组合物不含溶剂，所以不会对环境造成污染。本发明的组合物还具有极高的初始粘合性及耐潮湿粘合性。
本发明的组合物特别适合用于光学记录介质。
本发明可用激活能射线固化的组合物特别适于在制备光盘过程中用作将毂盘与光盘和光盘基片粘合为一体的胶粘剂。
在用于记录和再现信息的光学驱动装置中，采用了一种磁灯法，其中将一个光盘固定在此装置的一个转盘上，并随该转盘高速旋转。图1是一个粗略的剖面图，示出一个转盘和一个光盘，光盘3紧固在转盘1上。用这样的方法将光盘3装在转盘1上，在转盘1的凹陷部位装有一个磁路2，光盘随该转盘一同旋转。在转盘上放上该光盘后，所述光盘是靠磁力吸引而固定在转盘上，该转盘的旋转中心轴要与该光盘的旋转中心轴对中。为此目的，要装到转盘上的该光盘带有可被磁力吸引的部分5以及定位于旋转中心的孔4。上述可被磁力吸引的部分在本发明中称为毂盘。
最好使用本发明的可用激活能固化的组合物作为胶粘剂，将该毂盘粘合到基片6上构成所述的光 盘。
该毂盘可用塑料材料（如聚碳酸酯）、金属材料或陶瓷材料制造。该毂盘至少在其嵌入光盘的末端部分是由磁性材料构成的。所述磁性材料可以本身就是磁性体，也可以是磁性体与另一种材料的复合物。具体讲，所述磁性材料主要包括下列几类：（1）一种磁性金属，（2）一种其中混有磁性的塑料材料，或（3）一种在其嵌入光盘的末端部分具有磁性金属的塑料材料。从强度和吸引力的角度考虑，最好采用磁性金属构成该磁性材料。
下列实例进一步详细介绍本发明。
下列实例中拉伸粘合强度是用以下方法测定和评价的。将一种树脂注塑成试样A（30×1.27×3毫米）和试样B（25×12×6.3毫米）。用渍有异丙醇的纱布轻轻擦拭上述试样的表面。将本发明的组合物涂布在试样A的表面上，再将试样B叠放在试样A经涂覆的表面上并稍加扰动，以保证该组合物均匀地分布在试样B的整个粘合表面上（粘合面积为0.8平方厘米）。将上述组件夹持在石英玻璃片之间使之固定。用一种激活能射线辐照该组件，将所涂布的组合物固化。粘合的组合试样的外观示于图2，其中d＝30毫米，e＝12.7毫米，f＝3毫米，g＝25毫米，h＝12毫米，i＝6.3毫米。
用一台拉伸试验机（Instron    CO.，Ltd出产，型号为1123）以50毫米/分钟的速度拉伸上述组合试样，记录所用拉力。用粘合面积除拉力值即得到试样的拉伸强度。
实例1
制备胶粘剂
将一种双酚A型环氧树脂（EPOMIK    R-140，Mitsui    Petrochemical    Industries，Ltd出产）与一种丙烯酸酯单体（Aromix    M-5700，Toa    Sunthitic    Chemical    Industry，Co.Ltd出产）和三种丙烯酸酯低聚物（Aromix    M-6100、M-6300和M-8030，Toa    Synthitic    Chemical    Industry，Co.Ltd出产）相混合，其重量混合比环氧树脂/M-5700/M-6100/M-6300/M-8030为80/7/5/3/5。将100份（重量）上述混合物与2份（重量）环戊二烯基异丙苯基铁（Ⅱ）盐（Ciba-Geigy    Co.，Ltd出产）、0.25份（重量）蒽（Wako    Pure    Chemicals    CO.，Ltd）和3.1份（重量）氢化氧化异丙基苯（Kayaku    Noury    Corporation出产，70%级）相混合，得到一种本发明的组合物（胶粘剂）。
粘合强度
用本发明的上述胶粘剂组合物，如图2所示将一种聚碳酸酯试样（AD-5503，Teijin    Chemical    Co.，Ltd.出产）和下文将要介绍的一种乙烯/环烯烃共聚物试样粘合在一起。在紫外线下以160毫瓦/平方厘米的照度将上述组件辐照15秒。用上述方法测定该组件的拉伸粘合强度。结果示于表1。将另一组同样的试样在80℃和85%湿度的恒温恒湿箱中放置200小时，然后测其粘合强度。结果也示于表1。
制备乙烯/环烯烃共聚物
在一个装有搅拌叶片的2升容积的玻璃聚合容器中，将乙烯和1，3，5，8-二甲桥-1，2，3，4，4a，5，8，8a-八氢化萘（结构式为
Figure 881085073_IMG19
的多环烯烃，简称为DMON）连续共聚。具体做法是将DMON的环己烷溶液、VO（OC2H5）Cl2（催化剂）的环己烷溶液和倍半氯化乙基铝（Al（C2H5）1.5Cl1.5）的环己烷溶液，从该聚合容器的顶部连续地喂入，各种原料的用量是这样的，使该聚合容器中DMON的浓度为60克/升，钒的浓度为0.9毫摩尔/升，铝的浓度为7.2毫摩尔/升。同时聚合溶液连续地从该聚合容器的下部排出，从而使聚合溶液在聚合容器中的量总保持在1升。此外，乙烯、氢气和氮气分别以每小时85升、6升和45升的流量从该聚合容器的顶部送入。冷却剂通过装在该聚合容器外部的夹套进行循环，使上述共聚反应保持在10℃进行。
通过上述条件下的共聚反应得到一种含有乙烯/DMON共聚物的聚合反应混合物。将少量异丙醇加入从上述聚合容器下部排出的聚合反应混合物以停止聚合反应。将所述聚合反应混合物倒入一个盛有三倍于该混合物重量的丙酮的自制混合器中，同时加以搅拌。滤集所生成的沉淀的共聚物，以约50克/升的浓度将该共聚物分散在丙酮中。然后在丙酮的沸点温度再令该共聚物反应2小时。经此处理后，滤集该共聚物，并于120℃减压干燥一昼夜。
最终所得的乙烯/DMON无规共聚物的乙烯含量为59%（摩尔）（以C13-NMR分析法测定）， 特性粘度[η]为0.42dl/g（于135℃在萘烷中测定），玻璃化温度为136℃。
实例2
用聚甲基戊烯（TRX
Figure 881085073_IMG20
RT18，Mitsui Pertrochemical Industries，Ltd出产）和聚碳酸酯做基片，用与实例1同样的方法粘合。测定粘合试样的粘合强度，结果示于表1。
实例3
用与实例1同样的方法粘合上述聚碳酸酯和乙烯/环烯烃共聚物试样，不同之处是在制备实例3的胶粘剂组合物时用的是1，2-苯并蒽醌（Aldlich    Company的产品）而不是蒽。结果示于表1。
实例4
将2份（重量）的甲基异丁基酮（Wako    Pure    Chemicals    Co.，Ltd出产）加入100份（重量）实例1中制备的胶粘剂组合物中。按实例1的方法用这种组合物粘合上述聚碳酸酯和乙烯/环烯烃共聚物试样。结果示于表1。
实例5
按实例1的方法制备胶粘剂组合物，不同之处是用三苯基锍盐替代环戊二烯基异丙苯基铁（Ⅱ）盐。按实例1的方法用这种胶粘剂组合物粘合上述乙烯/环烯烃共聚物和聚碳酸酯试样。结果示于表1。
对照例1
按实例1的方法制备胶粘剂组合物，不同之处是没有添加该丙烯酸酯单体和丙烯酸酯低聚物。按实例1的方法用所得的粘合剂组合物粘合上述乙烯/环烯烃共聚物和聚碳酸酯试样。结果示于表1。
实例6
按实例1的方法制备胶粘剂组合物，不同之处是其中未加蒽。按实例1的方法用所得的胶粘剂组合物粘合上述乙烯/环烯烃共聚物和聚碳酸酯试样。结果示于表1。
表1
拉伸粘合强度
耐潮湿试验之前    耐潮湿试验之后
实例1    16    18
实例2    14    13
实例3    17    15
实例4    18    16
实例5    16    14
对照例1    14    4
实例6    10    8
实例7
制备涂布料
将一种双酚A型环氧树脂（EPOMIC    R-140）、一种丙烯酸酯单体（M-5700）和三种丙烯酸酯低聚物（M-6100、M-6300和M-8030）按环氧树脂/M-5700/M-6100/M-6300/M-8030之重量比为80/7/5/3/5的比例混合。将上述混合物、环戊二烯基异丙苯基铁（Ⅱ）盐、蒽和环己基过氧化氢以100/2/0.25/2.5（按上述顺序）的重量比相混合。用7倍于该混合物量的丙酮将其稀释制成一种涂布料。
制备光盘
用实例1中制备的同样的乙烯/环烯烃共聚物制成一批厚度为12毫米、直径为130毫米的光盘基片。用常规方法在这些基片的表面上形成一个光磁记录层。
涂布和粘合
将2毫升上述涂布料滴加在所述光盘的表面上，并用旋涂器将其涂布均匀。将两块涂布过的光盘在压力下（20千克/平方厘米）粘合在一起，用紫外线辐照此组合件（160毫瓦/平方厘米，30秒）。
测定光盘的性能
上述光盘的粘合强度用图3所示的装置测定。如图3所示，上述粘合在一起的光盘放置在上下两个夹具之间。将该盘紧固在上部和下部夹具上，同时施以真空，向上下两个方向拉开该夹具，记录下拉力值。测定初始强度及耐水和耐潮湿试验（80℃，85%湿度，200小时）后的强度。结果示于表2。此阶段该盘未出现翘曲，也没观察到该粘合层有任何变化。
实例8
按实例7的方法制备涂布料，不同之处是用1，2-苯并蒽醌替代蒽。按实例7的方法用上述涂布料粘合光盘，测定粘合强度。结果示于表2。
实例9
按实例7的方法制备涂布料，不同之处是用下式所示的四氟硼酸三苯基锍盐替代环戊二烯基异丙苯基铁（Ⅱ）盐：
Figure 881085073_IMG21
按实例7的方法用上述涂布料粘合光盘，测定 粘合强度。结果示于表2。
表2
粘合强度（千克/平方厘米）
实例    耐水耐潮湿试验前耐水耐潮湿试验后
7    ＞100    ＞100
8    ＞100    99
9    ＞100    96
实例10
制备胶粘剂
将0.5克苯乙烯/乙烯/丙烯共聚物（KL-1001，Kurauay    Inc.出产，分子量为100，000，苯乙烯含量为35%（重量））溶于120克甲苯和四氢呋喃的1∶1混合物。然后，将100克双酚A型环氧树脂（EPOMIK    R-140）溶于上述溶液。此溶液在一蒸发器中蒸发3-5小时以除去溶剂。将余留物在一个真空干燥器中于100℃、400毫米汞柱条件下干燥12小时。将80份（重量）所得的组合物与7份、5份、3份和5份（重量）的一种丙烯酸酯单体（Aronix    MK-5700）及三种丙烯酸酯低聚物（M-6100，M-6300和M-8030）相混合（比例关系与所述原料的顺序一致）。将100份所得的组合物与2份环戊二烯基异丙苯基铁（Ⅱ）盐（Ciba-Geigy公司出产）、0.25份蒽（Wako    Pure    Chemical    Co.Ltd.出产）和3.1份氢过氧化异丙基苯（70%品级，Kayaku    Noury    Corporation出产）相混合，得到一种可用激活能射线固化的组合物。上述份数均以重量计。
用最终得到的组合物将聚碳酸酯（AD-5503，Teijin    Chemical    Co.Ltd.出产）样品A和上述乙烯/环烯烃共聚物的样品B如图2那样粘合。用紫外线以160毫瓦/平方厘米的照度对上述组合试件辐照15秒。用所得的粘合组件作为试样，测定该胶粘剂的拉伸粘合强度。
还测定了该试样在70℃和85%湿度的恒温恒湿容器中储放200小时以后的粘合强度。结果示于表3。
实例11
用实例10中制备的胶粘剂将一个不锈钢（SUS430）样品和一个乙烯/环烯烃共聚物样品粘合在一起。用此粘合的组件作为试样，按实例10的方法测定该胶粘剂的拉伸粘合强度。结果示于表3。
实例12
按实例10的方法制备胶粘剂，不同之处是用一种苯乙烯/异戊二烯/苯乙烯共聚物（Shell    Chemical    Co.出产，分子量为115，000，苯乙烯含量为14%（重量））替代苯乙烯/乙烯/丙烯共聚物。用所得的胶粘剂粘合与实例10相同的样品。用此粘合组件作为试样，按实例10的方法测定此胶粘剂的拉伸粘合强度。结果示于表3。
实例13
用实例12的胶粘剂粘合与实例11相同的样品。用此粘合组件作为试样，按实例10的方法测定此胶粘剂的粘合强度。结果示于表3。
实例14
按实例10的方法制备胶粘剂，不同之处是用苯乙烯/丁烯/苯乙烯共聚物（Shell    Chemical    Co.出产，分子量为72，000，苯乙烯含量为28%（重量））替代苯乙烯/乙烯/丙烯共聚物，用三苯基锍盐替代环戊二烯合铁（Ⅱ）盐。用所得的胶粘剂粘合与实例11相同的样品。用此粘合组件作为试样，按实例10的方法测定此胶粘剂的拉伸粘合强度。结果示于表3。
对照例3
按实例10的方法制备胶粘剂，不同之处是未添加氢过氧化异丙基苯。用此胶粘剂粘合与实例11相同的样品。用此粘合组件作为试样，按实例10的方法测定该胶粘剂的拉伸粘合强度。结果示于表3。
实例15
向100份（重量）实例10中制备的胶粘剂中添加1份（重量）甲苯。用这种胶粘剂粘合与实例11相同的样品。用此粘合组件作为试样，按实例10的方法测定该胶粘剂的拉伸粘合强度。结果示于表3。
表3
拉伸粘合强度（千克/平方厘米）
耐潮湿试验前    耐潮湿试验后
实例10    17    17
实例11    22    21
实例12    16    17
实例13    19    20
实例14    17    17
对照例15    24    23
对照例3    0    -
制备光盘基片
用按实例1制备的乙烯/环烯烃共聚物制成一种厚1.2毫米、直径为86毫米的光盘基片，并用常规方法在其上形成一种光磁记录层。
制备毂盘
由不锈钢（SUS    430）冲压成一种毂盘。
粘合该毂盘
用一台带有旋转盘的分配器（SHOTHMATIC    D3，Iwashita    Engineering    Company制造）将本发明的组合物涂布到所述光盘基片上。将所述毂盘叠置在上述光盘基片上，并在其上加一负载（200克）。然后以与实例10相同的照度用紫外线进行辐射，将此胶粘剂固化。
拉伸粘合强度。
图4是夹具9和试样10的粗略的剖面图。
如图4所示，光盘基片11和毂盘12被固定在夹具中以便测定拉伸粘合强度。用一台拉伸试验机（Motel    1123，Instron    Co.制造）以50毫米/分钟的速率沿X和Y两个方向拉伸该试样，从而测得该胶粘剂的拉伸强度，用所测得的拉伸强度值除以粘合面积即为该胶粘剂的拉伸粘合强度。
实例16
用与实例10相同的胶粘剂粘合所述光盘基片11和毂盘12。用此粘合组件作为试样，按上述方法测定此胶粘剂的粘合强度。结果示于表4。
实例17
用与实例12相同的胶粘剂粘合与实例16相同的光盘基片和毂盘。用此粘合组件作为试样，按上述方法测定该胶粘剂的粘合强度。结果列于表4。
实例18
用与实例15相同的胶粘剂粘合与实例16相同的光盘基片和毂盘。用此粘合组件作为试样，按上述方法测定该胶粘剂的粘合强度。结果示于表4。
表4
拉伸粘合强度（千克/平方厘米）
实例    耐潮湿试验前    耐潮湿试验后
16    13    13
17    13    12
18    15    13

Claims (8)

1、一种可用激活能射线固化的组合物，其中含有：
(A)一种环氧树脂，
(B)一种环戊二烯合铁类化合物，该化合物亦可与一种锍盐组合在一起使用，
(C)一种选自丙烯酸酯、甲基丙烯酸酯及它们的低聚物的化合物，
(D)一种有机过氧化物，亦可含有：
(E)一种橡胶组分。
2、按权利要求1的组合物，其中环氧树脂（A）是一种脂族或脂环族环氧树脂。
3、按权利要求1的组合物，其中环氧树脂（A）是含有双酚A组分的一种双酚A型环氧树脂。
4、按权利要求1的组合物，其中（B）所述的锍盐是三芳基锍盐。
5、按权利要求1的组合物，其中环戊二烯合铁类化合物（B）是环戊二烯基异丙苯基铁盐。
6、按权利要求1的组合物，其中化合物（C）是一种丙烯酸或甲基丙烯酸与带有环烃基团的羟基化合物所成的酯，或该酯的低聚物。
7、按权利要求1的组合物，其中化合物（C）一种聚酯多羟基化合物的单或多丙烯酸酯或多甲基丙烯酸酯，或者是所述丙烯酸酯或甲基丙烯酸酯的低聚物。
8、权利要求1-7所述组合物的用途，用作为形成光学记录介质的粘合剂。
CN88108507A 1987-12-08 1988-12-08 可用激活能射线固化的组合物及其用途 Expired - Fee Related CN1028239C (zh)

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JP309,428/87 1987-12-09
JP62309428A JPH01150529A (ja) 1987-12-09 1987-12-09 光記録媒体
JP63211084A JP2545119B2 (ja) 1988-08-25 1988-08-25 活性エネルギ―光線硬化型組成物およびこの組成物を用いた光ディスク基板とハブとの接着方法
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MY106951A (en) 1995-08-30
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EP0320237A3 (en) 1990-10-10
EP0320237A2 (en) 1989-06-14
DE3880642D1 (de) 1993-06-03
EP0320237B1 (en) 1993-04-28
CN1033822A (zh) 1989-07-12
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US5445855A (en) 1995-08-29
DE3880642T2 (de) 1993-11-18

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