CN111902442B - 树脂组合物、光纤用二次被覆材料及光纤 - Google Patents
树脂组合物、光纤用二次被覆材料及光纤 Download PDFInfo
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- CN111902442B CN111902442B CN201980022116.6A CN201980022116A CN111902442B CN 111902442 B CN111902442 B CN 111902442B CN 201980022116 A CN201980022116 A CN 201980022116A CN 111902442 B CN111902442 B CN 111902442B
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- 239000013307 optical fiber Substances 0.000 title claims description 33
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- 238000000576 coating method Methods 0.000 title claims description 26
- 239000000463 material Substances 0.000 title claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 126
- 229920005989 resin Polymers 0.000 claims abstract description 85
- 239000011347 resin Substances 0.000 claims abstract description 85
- 239000000178 monomer Substances 0.000 claims abstract description 57
- 239000002245 particle Substances 0.000 claims abstract description 40
- 229910052809 inorganic oxide Inorganic materials 0.000 claims abstract description 36
- 125000000951 phenoxy group Chemical group [H]C1=C([H])C([H])=C(O*)C([H])=C1[H] 0.000 claims abstract description 36
- 239000003999 initiator Substances 0.000 claims abstract description 13
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Abstract
本发明的树脂组合物包含:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、具有苯氧基的单体和光聚合引发剂的基础树脂;以及疏水性无机氧化物颗粒。该树脂组合物在45℃的粘度为300mPa·s至4200mPa·s。以基础树脂的总量为基准,具有苯氧基的单体的含量为1质量%至30质量%。
Description
技术领域
本公开涉及一种树脂组合物、光纤用二次被覆材料及光纤。
本申请要求基于2018年4月2日提交的日本专利申请No.2018-070649的优先权,并引用了该日本专利申请中所记载的全部内容。
背景技术
通常,光纤具有用于保护作为光传输体的玻璃纤维的被覆树脂层。为了减小对光纤施加侧压时发生的微小弯曲所引起的传输损耗的增加,要求光纤具有优异的侧压特性。
引用列表
专利文献
专利文献1:JP 2014-219550A
发明内容
根据本公开的一个实施方案的树脂组合物包含:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、具有苯氧基的单体和光聚合引发剂的基础树脂,以及疏水性无机氧化物颗粒,其中所述树脂组合物在45℃的粘度为300mPa·s以上4200mPa·s以下,并且以基础树脂的总量为基准,具有苯氧基的单体的含量为1质量%以上30质量%以下。
附图说明
[图1]图1为示出了根据本发明实施方案的光纤的一个实例的示意性截面图。
具体实施方式
[本公开待解决的问题]
含有填料的树脂组合物存在粘度高而涂布性差的倾向。另一方面,当为了调整树脂组合物的粘度而增加稀释性单体的添加量时,低聚物的比率降低,并且由树脂组合物形成的涂膜倾向于变脆。此外,当增加稀释性单体的添加量时,由树脂组合物形成的涂膜的杨氏模量增加或减少,或涂膜的厚度变薄从而使树脂层的强度降低。因此,对于光纤的被覆树脂层中所使用的树脂组合物,要求兼具涂布性与涂膜性。
本公开的目的在于提供一种能够兼具涂布性与涂膜性的树脂组合物,以及具有由该树脂组合物形成的被覆树脂层的光纤。
[本公开的有利效果]
本公开可提供一种能够兼具涂布性与涂膜性的树脂组合物,以及具有由该树脂组合物形成的被覆树脂层的光纤。
[本公开的实施方案的说明]
首先,将通过列举对本公开的实施方案的内容进行说明。根据本公开的一个实施方案的树脂组合物包含:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、具有苯氧基的单体和光聚合引发剂的基础树脂,以及疏水性无机氧化物颗粒,其中树脂组合物在45℃的粘度为300mPa·s以上4200mPa·s以下,并且以基础树脂的总量为基准,所述具有苯氧基的单体的含量为1质量%以上30质量%以下。
这样的树脂组合物能够兼具涂布性与涂膜性。此外,通过将上述树脂组合物用作光纤被覆用的紫外线固化型树脂组合物,能够制备具有优异侧压特性的光纤。
为调整涂布性与涂膜性之间的平衡,基础树脂可以进一步含有不具有苯氧基的单体。此外,当不具有苯氧基的单体在25℃的粘度为50mPa·s以下时,易于改善树脂组合物的涂布性。
具有苯氧基的单体可为选自由(甲基)丙烯酸2-苯氧基乙酯、(甲基)丙烯酸3-苯氧基苄酯、苯氧基二乙二醇(甲基)丙烯酸酯以及苯氧基聚乙二醇(甲基)丙烯酸酯所组成的组中的至少一种。因此,变得易于调整树脂组合物的涂布性与涂膜性之间的平衡。
上述无机氧化物颗粒可为选自由二氧化硅、二氧化锆、氧化铝、氧化镁、氧化钛、氧化锡以及氧化锌组成的组中的至少一种,因为这些颗粒在树脂组合物中的分散性优异,并且能够容易地形成硬质覆膜。
根据本公开的一个方面的光纤包括:包括芯部和包层的玻璃纤维;与玻璃纤维接触并被覆该玻璃纤维的初级树脂层;以及被覆初级树脂层的次级树脂层,并且次级树脂层包含树脂组合物的固化物。通过将根据本实施方案的树脂组合物应用于次级树脂层,能够提升光纤的侧压特性。
[本公开的实施方案的细节]
根据需要参照附图对根据本实施方案的树脂组合物、光纤用二次被覆材料以及光纤的具体例子进行说明。本发明不限于这些示例,而是由权利要求书表示,并且意图包括与权利要求书等同的意义和范围内的所有变化。在下述说明中,在附图的说明中对相同的要素赋予相同的参考数字,并且省略重复的说明。
<树脂组合物>
根据本实施方案的树脂组合物包含:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、具有苯氧基的单体和光聚合引发剂的基础树脂;以及疏水性无机氧化物颗粒。
(甲基)丙烯酸酯指的是丙烯酸酯或与其相对应的甲基丙烯酸酯。这也同样地适用于(甲基)丙烯酸等。
(基础树脂)
以根据本实施方案的基础树脂的总量为基准,基础树脂含有1质量%以上30质量%以下的具有苯氧基的单体。通过使基础树脂中具有苯氧基的单体的含量在这样的范围内,能够提升树脂组合物的涂布性,并且形成具有适合作为光纤的被覆用树脂的杨氏模量的涂膜。具有苯氧基的单体的含量优选为2质量%以上28质量%以下,更优选为3质量%以上25质量%以下。
具有苯氧基的单体的实例包括:(甲基)丙烯酸2-苯氧基乙酯、(甲基)丙烯酸3-苯氧基苄酯、苯氧基二乙二醇(甲基)丙烯酸酯、苯氧基聚乙二醇(甲基)丙烯酸酯以及壬基苯氧基聚乙二醇(甲基)丙烯酸酯。从调整树脂组合物的涂布性与涂膜性之间的平衡的观点出发,具有苯氧基的单体可以为选自由(甲基)丙烯酸2-苯氧基乙酯、(甲基)丙烯酸3-苯氧基苄酯、苯氧基二乙二醇(甲基)丙烯酸酯和苯氧基聚乙二醇(甲基)丙烯酸酯所组成的组中的至少一种。其中,作为具有苯氧基的单体,优选为(甲基)丙烯酸2-苯氧基乙酯或(甲基)丙烯酸3-苯氧基苄酯。具有苯氧基的单体可组合使用两种以上。
从改善树脂组合物的涂布性的观点出发,具有苯氧基的单体在25℃的粘度优选为50mPa·s以下,更优选为1mPa·s以上30mPa·s以下,还更优选为1mPa·s以上25mPa·s以下。
基础树脂还可以进一步包含不具有苯氧基的单体。不具有苯氧基的单体在25℃的粘度优选为50mPa·s以下,更优选为1mPa·s以上30mPa·s以下,还更优选为1mPa·s以上25mPa·s以下。因此,能够获得涂布性与涂膜性之间的平衡优异的树脂组合物。
不具有苯氧基的单体可为具有一个聚合性基团的单官能单体或具有两个以上聚合性基团的多官能单体。不具有苯氧基的单体可组合使用两种以上。
不具有苯氧基的单官能单体的实例包括:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸丙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸仲丁酯、(甲基)丙烯酸叔丁酯、(甲基)丙烯酸异丁酯、(甲基)丙烯酸正戊酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸己酯、(甲基)丙烯酸庚酯、(甲基)丙烯酸异戊酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸异辛酯、(甲基)丙烯酸异癸酯、(甲基)丙烯酸月桂酯、4-叔丁基环己醇(甲基)丙烯酸酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸苄酯、(甲基)丙烯酸二环戊烯酯、(甲基)丙烯酸二环戊烯氧基乙酯、(甲基)丙烯酸二环戊酯、(甲基)丙烯酸壬基酚聚乙二醇酯、(甲基)丙烯酸异冰片酯等(甲基)丙烯酸酯类单体;(甲基)丙烯酸、(甲基)丙烯酸二聚物、(甲基)丙烯酸羧基乙酯、(甲基)丙烯酸羧基戊酯和ω-羧基-聚己内酯(甲基)丙烯酸酯等含羧基的单体;N-丙烯酰基吗啉、N-乙烯基吡咯烷酮、N-乙烯基己内酰胺、N-丙烯酰基哌啶、N-甲基丙烯酰基哌啶、N-丙烯酰基吡咯烷、3-(3-吡啶)丙基(甲基)丙烯酸酯、环三羟甲基丙烷甲缩醛丙烯酸酯等含杂环的(甲基)丙烯酸酯;马来酰亚胺、N-环己基马来酰亚胺、N-苯基马来酰亚胺等马来酰亚胺系单体;(甲基)丙烯酰胺、N,N-二甲基(甲基)丙烯酰胺、N,N-二乙基(甲基)丙烯酰胺、N-己基(甲基)丙烯酰胺、N-甲基(甲基)丙烯酰胺、N-异丙基(甲基)丙烯酰胺、N-丁基(甲基)丙烯酰胺、N-羟甲基(甲基)丙烯酰胺、N-羟甲基丙烷(甲基)丙烯酰胺等酰胺系单体;(甲基)丙烯酸氨基乙酯、(甲基)丙烯酸氨基丙酯、(甲基)丙烯酸N,N-二甲基氨基乙酯、(甲基)丙烯酸叔丁基氨基乙酯等(甲基)丙烯酸氨基烷基酯系单体;N-(甲基)丙烯酰基氧基亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-6-氧基六亚甲基琥珀酰亚胺、N-(甲基)丙烯酰基-8-氧基八亚甲基琥珀酰亚胺等琥珀酰亚胺系单体。
作为单官能单体,从调整由树脂组合物形成的涂膜的杨氏模量的观点出发,优选为(甲基)丙烯酸异冰片基酯或4-叔丁基环己醇(甲基)丙烯酸酯,更优选为(甲基)丙烯酸异冰片基酯。
不具有苯氧基的多官能单体的实例包括:乙二醇二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、三丙二醇二(甲基)丙烯酸酯、双酚A的环氧烷加成物的二(甲基)丙烯酸酯、四乙二醇二(甲基)丙烯酸酯、羟基新戊酸新戊二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、1,9-壬二醇二(甲基)丙烯酸酯、1,12-十二烷二醇二(甲基)丙烯酸酯、1,14-十四烷二醇二(甲基)丙烯酸酯、1,16-十六烷二醇二(甲基)丙烯酸酯、1,20-二十烷二醇二(甲基)丙烯酸酯、异戊二醇二(甲基)丙烯酸酯、3-乙基-1,8-辛二醇二(甲基)丙烯酸酯、双酚A的EO加成物二(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、三羟甲基辛烷三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚丙氧基三(甲基)丙烯酸酯、三羟甲基丙烷聚乙氧基聚丙氧基三(甲基)丙烯酸酯、三[(甲基)丙烯酰氧基乙基]异氰脲酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇聚乙氧基四(甲基)丙烯酸酯、季戊四醇聚丙氧基四(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、二三羟甲基丙烷四(甲基)丙烯酸酯、二季戊四醇四(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯和己内酯改性三[(甲基)丙烯酰氧基乙基]异氰脲酸酯。
作为多官能单体,从降低树脂组合物的粘度并形成具有所需的杨氏模量的涂膜的观点出发,可以使用三丙二醇二(甲基)丙烯酸酯、1,6-己二醇(甲基)丙烯酸酯和三羟甲基丙烷三(甲基)丙烯酸酯。其中,作为多官能单体,优选为三丙二醇二(甲基)丙烯酸酯。
以基础树脂的总量为基准,基础树脂包含的单体(具有苯氧基的单体以及不具有苯氧基的单体)优选为21质量%以上45质量%以下,更优选为22质量%以上43质量%以下。通过包含在上述范围内的单体,使得易于制备涂布性与涂膜性之间的平衡更优异的树脂组合物。
根据本实施方案的树脂组合物包含氨基甲酸酯(甲基)丙烯酸酯低聚物。作为氨基甲酸酯(甲基)丙烯酸酯低聚物,可以使用使多元醇化合物、多异氰酸酯化合物以及含羟基的(甲基)丙烯酸酯化合物反应所获得的低聚物。
多元醇化合物的实例包括:聚四亚甲基二醇、聚丙二醇及双酚A-环氧乙烷加成二醇。多元醇化合物的数均分子量可以为400至1000。多异氰酸酯化合物的实例包括:2,4-甲苯二异氰酸酯、2,6-甲苯二异氰酸酯、异佛尔酮二异氰酸酯和二环己基甲烷4,4’-二异氰酸酯。含羟基的(甲基)丙烯酸酯化合物的实例包括:(甲基)丙烯酸2-羟乙酯、(甲基)丙烯酸2-羟丁酯、1,6-己二醇单(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、(甲基)丙烯酸2-羟丙酯和三丙二醇单(甲基)丙烯酸酯。
通常使用有机锡化合物作为合成氨基甲酸酯(甲基)丙烯酸酯低聚物的催化剂。有机锡化合物的实例包括:二月桂酸二丁基锡、二乙酸二丁基锡、马来酸二丁基锡、双(巯基乙酸2-乙基己酯)二丁基锡、双(巯基乙酸异辛酯)二丁基锡和二丁基氧化锡。从易得性或催化性能方面来看,优选使用二月桂酸二丁基锡或二乙酸二丁基锡作为催化剂。
在合成氨基甲酸酯(甲基)丙烯酸酯低聚物时,可以使用碳原子数为5以下的低级醇。低级醇的实例包括:甲醇、乙醇、1-丙醇、2-丙醇、1-丁醇、2-丁醇、2-甲基-2-丙醇、1-戊醇、2-戊醇、3-戊醇、2-甲基-1-丁醇、3-甲基-1-丁醇、2-甲基-2-丁醇、3-甲基-2-丁醇和2,2-二甲基-1-丙醇。
根据本实施方案的树脂组合物还可以进一步包含环氧(甲基)丙烯酸酯低聚物。作为环氧(甲基)丙烯酸酯低聚物,可以使用使具有(甲基)丙烯酰基的化合物与具有两个以上缩水甘油基的环氧树脂进行反应所获得的低聚物。
可以从已知的自由基光聚合引发剂中适当选择光聚合引发剂并使用。光聚合引发剂的实例包括:1-羟基环己基苯基酮、2,2-二甲氧基-2-苯基苯乙酮、1-(4-异丙基苯基)-2-羟基-2-甲基丙烷-1-酮、2,4,4-三甲基戊基氧化膦、2,4,4-三甲基苯甲酰基二苯基氧化膦、2-甲基-1-[4-(甲硫基)苯基]-2-吗啉基-丙烷-1-酮(Omnirad 907,IGM Resins公司制)、2,4,6-三甲基苯甲酰基二苯基氧化膦(Omnirad TPO,IGM Resins公司制)和双(2,4,6-三甲基苯甲酰基)苯基氧化膦(Omnirad 819,IGM Resins公司制)。
(无机氧化物颗粒)
根据本实施方案的无机氧化物颗粒为表面经过疏水处理的球状颗粒。根据本实施方案的疏水处理是指在无机氧化物颗粒的表面引入疏水性基团。引入有疏水性基团的无机氧化物颗粒在树脂组合物中的分散性优异。疏水性基团可以为(甲基)丙烯酰基等反应性基团、或烃基(例如烷基)或芳基(例如苯基)等非反应性基团。在无机氧化物颗粒具有反应性基团的情况下,易于形成杨氏模量高的树脂层。
根据本实施方案的无机氧化物颗粒分散于分散介质中。通过使用分散于分散介质中的无机氧化物,能够使无机氧化物颗粒均匀地分散于树脂组合物中,由此可以提高树脂组合物的保存稳定性。对于分散介质,只要其不妨碍树脂组合物的固化,则没有特别的限制。分散介质可以为反应性的或者为非反应性的。
作为反应性的分散介质,可以使用诸如(甲基)丙烯酰基化合物、环氧化合物之类的单体。(甲基)丙烯酰基化合物的实例包括:1,6-己二醇二(甲基)丙烯酸酯、EO改性双酚A二(甲基)丙烯酸酯、聚乙二醇二(甲基)丙烯酸酯、PO改性双酚A二(甲基)丙烯酸酯、聚丙二醇二(甲基)丙烯酸酯及聚四亚甲基二醇二(甲基)丙烯酸酯。作为(甲基)丙烯酰基化合物,可以使用上述的单体中所例示的化合物。
非反应性的分散介质可包括:诸如甲基乙基酮(MEK)之类的酮溶剂、诸如丙二醇单甲醚(PGME)之类的醇溶剂、或诸如丙二醇单甲醚乙酸酯(PGMEA)之类的酯溶剂。在非反应性的分散介质的情况下,可以通过将基础树脂与分散在分散介质中的无机氧化物颗粒混合,并去除分散介质的一部分来制备树脂组合物。当利用光学显微镜(放大倍率约100倍)观察包含无机氧化物颗粒的分散介质,并且未观察到颗粒时,可以将无机氧化物颗粒视为以一次粒子的形式分散。
由于在树脂组合物中的分散性优异且易形成硬质覆膜,因此上述无机氧化物颗粒优选为选自由二氧化硅(Silica)、二氧化锆(Zirconia)、氧化铝(Alumina)、氧化镁(Magnesia)、氧化钛(Titania)、氧化锡以及氧化锌所组成的组中的至少一种。从优异的廉价性、易进行表面处理、具有紫外线透过性、以及易赋予树脂层适当的硬度等观点出发,更优选使用疏水性的二氧化硅颗粒作为根据本实施方案的无机氧化物颗粒。
从提高树脂层的杨氏模量的观点出发,无机氧化物颗粒的平均一次粒径优选为200nm以下,更优选为5nm以上200nm以下,进一步优选为10nm以上100nm以下。平均一次粒径例如可以通过电子显微镜照片的图像分析、光散射法和BET法进行测定。在一次粒子的粒径较小的情况下,分散有无机氧化物的一次粒子的分散介质在目视下看起来是透明的。在一次粒子的粒径比较大(40nm以上)的情况下,分散有一次粒子的分散介质看起来是白浊的。但没有观察到沉淀物。
以树脂组合物的总量为基准,无机氧化物颗粒的含量优选为1质量%以上60质量%以下,更优选为7质量%以上50质量%以下,还更优选为9质量%以上40质量%以下。当无机氧化物颗粒的含量为1质量%以上时,易于形成侧压特性优异的树脂层。当无机氧化物颗粒的含量为60质量%以下时,使得易于提升树脂组合物的涂布性。
树脂组合物可以进一步包含硅烷偶联剂、光致酸产生剂、流平剂、消泡剂、防氧化剂等。
对于硅烷偶联剂,只要其不妨碍树脂组合物的固化,则没有特别地限定。硅烷偶联剂的实例包括:硅酸四甲酯、硅酸四乙酯、巯基丙基三甲氧基硅烷、乙烯基三氯硅烷、乙烯基三乙氧基硅烷、乙烯基三(β-甲氧基-乙氧基)硅烷、β-(3,4-环氧环己基)-乙基三甲氧基硅烷、二甲氧基二甲基硅烷、二乙氧基二甲基硅烷、3-丙烯酰氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二乙氧基硅烷、γ-甲基丙烯酰氧基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲氧基硅烷、N-(β-氨基乙基)-γ-氨基丙基三甲基二甲氧基硅烷、N-苯基-γ-氨基丙基三甲氧基硅烷、γ-氯丙基三甲氧基硅烷、γ-巯基丙基三甲氧基硅烷、γ-氨基丙基三甲氧基硅烷、双-[3-(三乙氧基甲硅烷基)丙基]四硫化物、双-[3-(三乙氧基甲硅烷基)丙基]二硫化物、γ-三甲氧基甲硅烷基丙基二甲基硫代氨甲酰基四硫化物和γ-三甲氧基甲硅烷基丙基苯并噻唑基四硫化物。
作为光致酸产生剂,可以使用具有A+B-结构的鎓盐。光致酸产生剂的实例包括:UVACURE1590(Daicel-Cytec制造)、CPI-100P、110P、210S(San-Apro制造)等锍鎓盐;Omnicat 250(IGM Resins制造)、WPI-113(FUJIFILM Wako Pure Chemical Corporation制造)、Rp-2074(Rhodia-Japan Ltd.制造)等碘鎓盐。
根据本实施方案的树脂组合物在45℃的粘度为300mPa·s以上4200mPa·s以下,优选为400mPa·s以上4000mPa·s以下,更优选为500mPa·s以上3500mPa·s以下。通过使树脂组合物的粘度处于上述范围,能够改善树脂组合物的涂布性。
<光纤>
图1为表示根据本实施方案的光纤的一个例子的示意性剖面图。光纤10包括:包括芯部11和包层12的玻璃纤维13;以及包括设置在玻璃纤维13的外周的初级树脂层14、以及次级树脂层15的被覆树脂层16。
包层12包围着芯部11。芯部11和包层12主要包含石英玻璃等玻璃,例如,芯部11中可以使用添加有锗的石英,包层12中可以使用纯石英或添加有氟的石英。
在图1中,例如,玻璃纤维13的外径(D2)为约125μm,构成玻璃纤维13的芯部11的直径(D1)为约7μm至15μm。
被覆树脂层16的厚度通常为约60μm至70μm。初级树脂层14和次级树脂层15的各自的厚度可以为约10μm至50μm,例如,初级树脂层14的厚度可以为35μm,并且次级树脂层15的厚度可以为25μm。光纤10的外径可以为约245μm至265μm。
根据本实施方案的树脂组合物可以应用于次级树脂层。可以通过使含有上述基础树脂和无机氧化物的树脂组合物固化而形成次级树脂层。根据本实施方案的树脂组合物适合作为光纤用二次被覆材料。因此,能够提高光纤的侧压特性。
次级树脂层的杨氏模量在23℃优选为1300MPa以上,更优选为1300MPa至2600MPa,还更优选为1300MPa至2500MPa。当次级树脂层的杨氏模量为1300MPa以上时,容易提高侧压特性,当杨氏模量为2600MPa以下时,能够赋予次级树脂层以适度的韧性,因而在次级树脂层中难以产生裂纹等。
分散在分散介质中的无机氧化物颗粒即使在树脂层固化后还是以分散在树脂层中的状态存在。当使用反应性的分散介质时,无机氧化物颗粒与分散介质一起混合到树脂层中,并保持分散状态而引入至树脂层中。当使用非反应性的分散介质时,分散介质的至少一部分从树脂组合物中挥发而消失。但是无机氧化物颗粒仍然以分散状态残留在树脂组合物中,并且在固化后的树脂层中仍然以分散状态存在。利用电子显微镜的观察显示,树脂层中存在的无机氧化物颗粒的一次粒子是分散的状态。
初级树脂层14可以是通过使包含氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂的树脂组合物固化而形成的。初级树脂层用的树脂组合物可以使用现有公知的技术。作为氨基甲酸酯(甲基)丙烯酸酯低聚物、单体、光聚合引发剂以及硅烷偶联剂,可以适当地选自上述基础树脂中所示例的化合物。构成初级树脂层的树脂组合物与形成次级树脂层的基础树脂具有不同的组成。
[实施例]
以下,示出使用根据本公开的实施例及比较例的评价试验的结果,并进一步详细地说明本公开。本发明并不限定于这些实施例。
(低聚物)
作为低聚物,准备通过使分子量为600的聚丙二醇、2,4-甲苯二异氰酸酯和丙烯酸羟基乙酯进行反应所获得的氨基甲酸酯丙烯酸酯低聚物(UA)、以及环氧丙烯酸酯低聚物(EA)。
(具有苯氧基的单体)
作为具有苯氧基的单体,准备丙烯酸3-苯氧基苄酯(Kyoeisha Chemical Co.,Ltd.制,商品名“Light Acrylate POB-A”)、丙烯酸2-苯氧基乙酯(Kyoeisha ChemicalCo.,Ltd.制,商品名“Light Acrylate PO-A”)、苯氧基二乙二醇丙烯酸酯(KyoeishaChemical Co.,Ltd.制,商品名“Light Acrylate P2H-A”)、以及苯氧基聚乙二醇丙烯酸酯(Kyoeisha Chemical Co.,Ltd.制,商品名“Light acrylate P-200A”)。
(不具有苯氧基的单体)
作为不具有苯氧基的单体,准备丙烯酸异冰片基酯(Osaka Organic ChemicalIndustry Co.,Ltd.制,商品名“IBXA”)以及三丙二醇二丙烯酸酯(Daicel-Allnex Co.,Ltd.制,商品名“TPGDA”)。
(光聚合引发剂)
作为光聚合引发剂,准备1-羟基环己基苯基酮及2,4,6-三甲基苯甲酰基二苯基氧化膦。
(无机氧化物颗粒)
作为无机氧化物颗粒,准备平均粒径为70nm至100nm的疏水性二氧化硅颗粒、平均粒径为40nm至60nm的疏水性二氧化硅颗粒、以及平均粒径为10nm至15nm的疏水性二氧化硅颗粒。这些二氧化硅颗粒具有甲基丙烯酰基,且分散于甲基乙基酮(MEK)中。
[树脂组合物的制备]
混合上述低聚物、单体以及光聚合引发剂从而制备基础树脂。将基础树脂与二氧化硅颗粒混合,然后在减压下将作为分散介质的大部分MEK去除,以制备各树脂组合物。树脂组合物中的MEK的含量为5质量%以下。
在表1及表2中,单体的数值为以基础树脂的总量为基准的含量,低聚物的数值为以单体、低聚物及二氧化硅颗粒的总量为基准的含量,二氧化硅颗粒的数值为以树脂组合物的总量为基准的含量。
使用实施例及比较例中所获得的树脂组合物进行以下评价。将结果示于表1及表2。
(粘度)
使用作为B型粘度计的Brookfield Co.,Ltd.制“数字粘度计DV-II”(使用的转子:No.18,转速:10rpm)测定树脂组合物在45℃的粘度。
(杨氏模量)
利用旋涂机,将各树脂组合物涂布在聚对苯二甲酸乙二醇酯(PET)膜上,然后使用Heraeus制的无电极UV灯系统“VPS6(D灯泡)”,在1000±100mJ/cm2的条件下进行固化,从而在PET膜上形成厚度为200±20μm的树脂层(涂膜)。将树脂层从PET膜上剥离,从而得到了树脂膜。
将树脂膜冲切成JIS K 7127Type5的哑铃状,并在23±2℃、50±10%RH的条件下,使用拉伸试验机以1mm/分钟的拉伸速度和25mm的标距长度进行拉伸,从而得到应力-应变曲线。由2.5%割线确定杨氏模量。
[光纤的制备]
将75质量份的氨基甲酸酯丙烯酸酯低聚物、12质量份的壬基苯氧基聚乙二醇丙烯酸酯、6质量份的N-乙烯基己内酰胺、2质量份的1,6-己二醇二丙烯酸酯、1质量份的2,4,6-三甲基苯甲酰基二苯基氧化膦(Omnirad TPO)以及1质量份的3-巯基丙基三甲氧基硅烷(MPTS)混合,从而得到了树脂组合物A1,其中氨基甲酸酯丙烯酸酯低聚物由分子量为2000的聚丙二醇、2,4-甲苯二异氰酸酯和丙烯酸羟乙酯和甲醇反应而得。
通过使用树脂组合物A1,在由芯部和包层构成的直径为125μm的玻璃纤维的外周形成厚度为35μm的初级树脂层,进一步将实施例或比较例中制作的各树脂组合物涂布在初级树脂层的外周,以形成次级树脂层,从而制作光纤。线速度设为1500m/分钟。
(涂布性)
针对所制作的光纤,通过确认有无断线而评价树脂组合物的涂布性。将无断线的情况视为“OK”,将确认有断线的情况视为“NG”。当树脂组合物的粘度过高时,形成次级树脂层时的被覆直径不稳定而易发生断线。另一方面,当树脂组合物的粘度过低时,自动调心力难以起作用而易于产生厚度不均匀。
[表1]
[表2]
经证实,实施例的树脂组合物能够兼具涂布性与涂膜性。
附图标记列表
10:光纤、11:芯部、12:包层、13:玻璃纤维、14:初级树脂层、15:次级树脂层、16:被覆树脂层。
Claims (8)
1.一种用于光纤的次级树脂层的树脂组合物,包含:含有氨基甲酸酯(甲基)丙烯酸酯低聚物、具有苯氧基的单体和光聚合引发剂的基础树脂,以及疏水性无机氧化物颗粒,其中
所述基础树脂还包含环氧(甲基)丙烯酸酯低聚物,
所述树脂组合物在45℃的粘度为500mPa·s以上3500mPa·s以下,并且
以所述基础树脂的总量为基准,所述具有苯氧基的单体的含量为1质量%以上30质量%以下,
所述具有苯氧基的单体为选自由(甲基)丙烯酸2-苯氧基乙酯、(甲基)丙烯酸3-苯氧基苄酯、苯氧基二乙二醇(甲基)丙烯酸酯和苯氧基聚乙二醇(甲基)丙烯酸酯所组成的组中的至少一种,
所述疏水性无机氧化物颗粒是通过在无机氧化物颗粒的表面引入疏水性基团而得到的。
2.根据权利要求1所述的树脂组合物,其中所述基础树脂还含有不具有苯氧基的单体。
3.根据权利要求2所述的树脂组合物,其中所述不具有苯氧基的单体在25℃的粘度为50mPa·s以下。
4.根据权利要求1至3中任一项所述的树脂组合物,其中所述无机氧化物颗粒为选自由二氧化硅、二氧化锆、氧化铝、氧化镁、氧化钛、氧化锡和氧化锌所组成的组中的至少一种。
5.根据权利要求1至3中任一项所述的树脂组合物,其中所述无机氧化物颗粒的平均一次粒径为200nm以下。
6.根据权利要求1至3中任一项所述的树脂组合物,其中以所述树脂组合物的总量为基准,所述无机氧化物颗粒的含量为1质量%以上60质量%以下。
7.一种光纤用二次被覆材料,其包含根据权利要求1至6中任一项所述的树脂组合物。
8.一种光纤,包括:
包括芯部和包层的玻璃纤维,
与所述玻璃纤维接触并被覆该玻璃纤维的初级树脂层;以及
被覆所述初级树脂层的次级树脂层,
其中所述次级树脂层包含根据权利要求1至6中任一项所述的树脂组合物的固化物。
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