CN103402615B - 赋予了拒油性的透气过滤器 - Google Patents
赋予了拒油性的透气过滤器 Download PDFInfo
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- CN103402615B CN103402615B CN201280010856.6A CN201280010856A CN103402615B CN 103402615 B CN103402615 B CN 103402615B CN 201280010856 A CN201280010856 A CN 201280010856A CN 103402615 B CN103402615 B CN 103402615B
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- 239000005871 repellent Substances 0.000 title claims abstract description 66
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 41
- 230000035699 permeability Effects 0.000 claims abstract description 28
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 22
- 239000011737 fluorine Substances 0.000 claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- 239000012528 membrane Substances 0.000 claims abstract description 19
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 13
- 125000001118 alkylidene group Chemical group 0.000 claims abstract description 6
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- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims description 22
- 239000000178 monomer Substances 0.000 claims description 17
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- 229920000642 polymer Polymers 0.000 claims description 13
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 claims description 12
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- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 3
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- GVIVQCNNFDHBAG-UHFFFAOYSA-N 2,2-dimethyl-1,3-dioxole Chemical compound CC1(C)OC=CO1 GVIVQCNNFDHBAG-UHFFFAOYSA-N 0.000 description 1
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
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- 239000000853 adhesive Substances 0.000 description 1
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Abstract
本发明提供的透气过滤器为赋予了拒油性的透气过滤器,具备具有由拒油剂覆盖的表面的多孔膜,其中,拒油剂中含有的直链状含氟烃基由1)-R1C5F10CH2C4F9或2)-R2C6F13表示,多孔膜为聚四氟乙烯(PTFE)拉伸多孔膜。在此,R1和R2各自独立地为碳原子数1~12的亚烷基或亚苯基。该透气过滤器在不使透气性大幅降低的情况下赋予了拒油性。
Description
技术领域
本发明涉及赋予了拒油性的透气过滤器。
背景技术
汽车用车头灯、车尾灯、雾灯、转向灯、电动机、各种压力传感器、压力开关等汽车用电装部件、照相机、摄像机、手机等信息终端、电动剃刀、电动牙刷和室外用途的灯等各种设备的壳体上多设置有透气孔。设置透气孔的主要目的在于通过使设备的内部与外部连通来避免由设备的工作导致的设备壳体内的温度上升所伴随的内部压力的过度上升。另外,为了使电池工作时产生的气体排出,在电池壳上设置有透气孔。
为了防止水、尘埃等从设置在设备壳体上的透气孔侵入,有时在透气孔上配置透气过滤器。作为透气过滤器,多使用聚烯烃树脂或含氟树脂的多孔膜。特别是将聚四氟乙烯(以下称为“PTFE”)拉伸使其形成微多孔结构而得到的多孔膜作为拒水性优良的透气过滤器已知。但是,根据使用环境,皮脂、表面活性剂、油等也会接触到透气过滤器。即使使用拒水性优良的PTFE拉伸多孔膜作为透气过滤器,也不能充分防止表面张力低的液体的侵入。因此,根据透气过滤器的用途对其进行使用含有含氟聚合物的处理剂的拒油处理。
具有碳原子数为8以上的直链状全氟烷基(以下,有时将“直链状全氟烷基”表示为“Rf基”)的含氟聚合物适合赋予拒油性是公知的。碳原子数为8以上的Rf基的结晶性显著高于碳原子数少的(例如6以下的)Rf基的结晶性,认为该高度结晶性有助于显现优良的拒油性。并且还已知,基于高度结晶性,由具有碳原子数为8以上的Rf基的处理剂能够获得高的后退接触角(与前进接触角同为动态接触角)。该后退接触角随着结晶性的提高从碳原子数6至8急剧地增大。基于这样的情况,为了对透气过滤器赋予拒油性,惯例是使用含有具有碳原子数为8以上的Rf基的含氟聚合物的处理剂。
还已知与上述处理剂一同使用其他处理剂来对透气过滤器赋予拒油性的技术。例如,日本特开平7-126428号公报(专利文献1)中公开了利用含有具有Rf基的含氟聚合物、并且含有主链中具有含氟脂肪族环结构的含氟树脂的处理剂对透气过滤器进行处理的技术(权利要求1等)。具有含氟脂肪族环结构的含氟树脂的成膜性优良,可以通过例如将全氟(2,2-二甲基-1,3-二氧杂环戊烯)聚合而得到(第0009、0011段)。另外,专利文献1中记载了全氟烷基的碳原子数优选为4~16、特别优选为6~12(第0023段)。但是,在实施例栏中,按照上述惯例,使用了具有碳原子数平均为9的全氟烷基的含氟聚合物(第0049、0050段;各实施例)。
现有技术文献
专利文献
专利文献1:日本特开平7-126428号公报
发明内容
发明所要解决的问题
如上所述,以往,为了赋予高拒油性,一直认为必须利用碳原子数为8以上的Rf基的高结晶性。例如,如专利文献1的实施例栏中所示,即使仅使用具有含氟脂肪族环结构的含氟树脂,也无法对透气过滤器赋予充分的拒油性(各比较例)。从实用上而言,专利文献1中的拒油试验中使用的甲苯或IPA(异丙醇)接触后“瞬间润湿”的程度的特性也不能称为充分的拒油性。为了对透气过滤器赋予实用上充分的拒油性,实际情况是利用碳原子数为8以上的Rf基。
但是,使用含有具有碳原子数为8以上的Rf基的含氟聚合物的处理剂进行拒油处理时,有时会使透气过滤器的透气性大幅降低。该透气性降低的程度依赖于透气过滤器所具有的多孔结构。例如,对于聚烯烃、尼龙等无纺布而言,通常,由拒油处理导致的透气性的降低是有限的。另一方面,对于具有由原纤维和节点构成的特征性微多孔结构的PTFE拉伸多孔膜而言,利用上述处理剂的拒油处理所带来的透气性的降低有时会变得显著。
鉴于以上情况,本发明的目的在于在不使透气性大幅降低的情况下对PTFE拉伸多孔膜赋予拒油性。
用于解决问题的手段
本发明提供一种赋予了拒油性的透气过滤器,具备具有由拒油剂覆盖的表面的多孔膜,其中,拒油剂中含有的直链状含氟烃基由1)-R1C5F10CH2C4F9或2)-R2C6F13表示,多孔膜为PTFE拉伸多孔膜。在此,R1和R2各自独立地为碳原子数1~12的亚烷基或亚苯基。
发明效果
直链状含氟烃基由上述1)或2)表示的拒油剂能够在不使PTFE拉伸多孔膜的透气性大幅降低的情况下赋予能够满足实用上的要求的程度的拒油性。根据本发明,能够在不使透气性大幅降低的情况下对PTFE拉伸多孔膜赋予拒油性。
具体实施方式
本发明的透气过滤器具备具有由拒油剂覆盖的表面的PTEF拉伸多孔膜。PTFE拉伸多孔膜使用市售品即可,以下对制造方法的一例进行说明。
首先,对在PTFE细粉中添加液态润滑剂而得到的糊状混合物进行预成形。液态润滑剂只要能够将PTFE细粉的表面润湿并能够通过提取、干燥而除去则没有特别限制,可以使用例如液体石蜡、石脑油、白油等烃。液态润滑剂的添加量相对于PTFE细粉100重量份为约5重量份~约50重量份是适当的。预成形以不使液态润滑剂被挤出的程度的压力进行即可。
接着,通过糊料挤出或压延将预成形体成形为片状,将该PTFE成形体沿单轴或双轴方向拉伸而得到PTFE拉伸多孔膜。另外,PTFE成形体的拉伸优选在除去液态润滑剂后进行。
本说明书中,根据惯例,将对片状的PTFE成形体进行拉伸而形成有微多孔结构的PTFE的多孔膜称为“PTFE拉伸多孔膜”。PTFE拉伸多孔膜典型地具有由原纤维和节点构成的特征性的微多孔结构,表示其本身具有优良的拒水性。
另外,PTFE拉伸多孔膜可以是在PTFE的熔点以上的温度下煅烧而得到的煅烧品,也可以是未实施该煅烧的未煅烧品。
PTFE拉伸多孔膜的平均孔径优选0.005~10μm,更优选0.01~5μm,特别优选0.1~3μm。平均孔径过小时,有时透气过滤器的透气性会降低。平均孔径过大时,有时会发生异物的泄漏。另外,PTFE拉伸多孔膜的厚度优选5~5000μm,更优选10~1000μm,特别优选10~500μm。膜厚过小时,可能会使膜的强度不足或者因透气壳体的内外差压而使透气过滤器的变形过大。膜厚过大时,有时透气过滤器的透气性会降低。
透气过滤器可以是具有由拒油剂覆盖的表面的PTEF拉伸多孔膜与用于增强该膜的透气性支撑体的层叠体。使用透气性支撑体时,能够抑制由差压导致的透气过滤器的变形。透气性支撑体可以为单层,也可以为两个以上的层的层叠体。但是,为了显现拒油性,透气过滤器的至少一个主面应该由被拒油剂覆盖的PTFE拉伸多孔膜的表面构成。
作为透气性支撑体,可以使用超高分子量聚乙烯多孔膜、无纺布、织布、网、筛网、海绵、泡沫、金属多孔膜、金属网等。从强度、弹性、透气性、操作性和向容器上的焊接性等观点出发,作为透气性支撑体,优选无纺布和超高分子量聚乙烯多孔膜。
PTFE拉伸多孔膜与透气性支撑体可以只是单纯地叠合,也可以使用胶粘剂、热熔树脂等进行胶粘,还可以通过加热焊接、超声波焊接、振动焊接等进行焊接。
本发明中,使用具有1)-R1C5F10CH2C4F9或2)-R2C6F13作为直链状含氟烃基的拒油剂。在此,R1和R2各自独立地为碳原子数1~12、优选1~10的亚烷基或亚苯基。R1或R2为亚烷基时,上述1)或2)所示的含氟烃基为直链状氟烷基。另外,上述“直链状”的主旨在于明确含氟烃基的碳骨架不具有分支出的2个以上的末端,并不是将含有亚苯基作为R1或R2的情况排除在外的含义。
直链状全氟烷基(Rf基)是具有表现低表面自由能的CF3基且对覆盖表面赋予拒水拒油性的官能团。如上所述,已知碳原子数为8以上的Rf基的结晶性高,因此,使其显现优良的拒油性。含有具有碳原子数为8以上的Rf基的含氟聚合物的处理剂适合对皮革、纸、树脂等基材赋予拒水拒油性。但是,该处理剂应用于PTFE拉伸多孔膜这样的、具有微多孔结构的透气过滤器时,有时会带来透气性的大幅降低。另外,利用该处理剂赋予的拒水拒油性在要求高的动态接触角的用途中特别有用。但是,对于透气过滤器而言,一般只要能够赋予甲苯、癸烷等烃和以IPA为代表的低级醇不渗透的程度的拒油性即可。具有上述1)或2)作为直链状含氟烃基的拒油剂即使覆盖PTFE拉伸多孔膜的表面,也能够在不使透气度大幅降低的情况下赋予实用上充分的拒油性。
该拒油剂优选为具有直链状含氟烃基作为侧链的含氟聚合物。该含氟聚合物中,直链状含氟烃基通过例如酯基、醚基等官能团键合到主链上或者直接键合到主链上。
作为具有上述1)或2)作为直链状含氟烃基的含氟聚合物,可以列举例如以由a)CH2=CR3COOR1C5F10CH2C4F9或b)CH2=CR4COOR2C6F13表示的化合物作为单体的至少一部分的聚合物。在此,R1和R2如上所述。另外,R3和R4各自独立地为氢原子或甲基。
但是,在要求高拒油性的情况下,优选选择由上述a)表示的化合物或者上述b)中R4为甲基的化合物作为单体。即,本发明的优选实施方式中,使用以由a)CH2=CR3COOR1C5F10CH2C4F9或b’)CH2=C(CH3)COOR2C6F13表示的化合物作为单体的聚合物。在此,R1、R2和R3也如上所述。
该含氟聚合物可以是仅以由上述a)和/或b)表示的化合物为单体聚合而成的聚合物,但也可以是使上述化合物与其他单体共聚而成的聚合物。作为共聚时的单体,可以列举各种(甲基)丙烯酸类单体,但不限于此,也可以使用四氟乙烯等具有烯属不饱和键的各种单体。共聚物可以是无规共聚物,也可以是嵌段共聚物。但是,在采用共聚物的情况下,为了不妨碍拒油性的赋予,优选使由上述a)或b)表示的化合物在全部单体中所占的比率为60摩尔%以上,特别优选为90摩尔%以上。上述化合物的聚合方法依据作为丙烯酸类单体的聚合方法而公知的方法即可,可以通过溶液聚合或乳液聚合来实施。
上述含氟聚合物的平均分子量没有特别限制,利用数均分子量表示,例如为约1000~约500000。
作为利用拒油剂覆盖PTFE拉伸多孔膜的表面的方法,可以列举:将透气过滤器浸渍在将拒油剂溶解于溶剂而得到的溶液中的方法、将上述溶液涂布或喷雾在透气过滤器上的方法。利用拒油剂进行覆盖时,为了防止PTFE拉伸多孔膜的收缩,优选使用框等预先将PTFE拉伸多孔膜的端部固定。上述溶液中的拒油剂的适当浓度根据覆盖方法等而不同,对于将透气过滤器浸渍在溶液中的方法而言,为约0.1重量%~约10重量%。
拒油处理后的透气过滤器的透气度过低时,不能迅速地消除透气壳体内外的压力差。该透气度利用葛尔莱数表示优选为35秒/100ml以下(葛尔莱数越低则透气度越高)。如以下的实施例所示,根据本发明,能够提供具有葛尔莱数为35秒/100ml以下的透气性且具备具有实用的拒油性的表面的透气过滤器。该表面具备如下拒油性:滴加有机溶剂正癸烷或甲醇的直径5mm的液滴时,滴加后30秒以内液滴不渗透到表面中。根据本发明,还能够提供即使为了满足作为透气过滤器所要求的强度而使PTFE拉伸多孔膜的厚度为5μm以上、进而为10μm以上也具有低至上述程度的葛尔莱数且具备具有实用的拒油性的表面的透气过滤器。
实施例
以下,列举实施例和比较例对本发明进行详细说明,但本发明不受这些实施例的限制。
(实施例1)
作为PTFE拉伸多孔膜,准备日东电工株式会社制造的“TEMISH(注册商标)NTF1131”(大小15cm×15cm;厚度0.1mm;平均孔径1μm)。另外,用稀释剂(信越化学公司制造的“FSシンナー”)稀释信越化学公司制造的拒水拒油剂“X-70-041”以达到3.0重量%的浓度,从而制备拒油处理液。上述“X-70-041”是以含有由下式(a-1)表示的具有直链状氟烷基的化合物作为单体的聚合物作为拒油成分的拒水拒油剂。
CH2=CHCOOCH2CH2C5F10CH2C4F9(a-1)
将膜周围固定在20cm见方的框上以使其不收缩,在该状态下将上述PTFE拉伸多孔膜在保持20℃的上述拒油处理液中浸渍约3秒钟,接着在常温下放置约1小时使其干燥,得到拒油性的透气过滤器。
(实施例2)
除了使用含有以由下式(a-2)表示的具有直链状氟烷基的化合物作为单体的聚合物作为拒油成分的信越化学公司制造的拒水拒油剂“X-70-042”作为拒油剂以外,与实施例1同样地得到透气过滤器。
CH2=C(CH3)COOCH2CH2C5F10CH2C4F9(a-2)
(实施例3)
将由下式(b-1)表示的具有直链状氟烷基的化合物100g、作为聚合引发剂的偶氮二异丁腈0.1g、溶剂(信越化学公司制造的“FSシンナー”)300g投入装配有氮气导入管、温度计、搅拌器的烧瓶中,导入氮气后在70℃下搅拌的同时进行16小时的加成聚合,得到80g含氟聚合物。该聚合物的数均分子量为100000。用稀释剂(信越化学公司制造的“FSシンナー”)稀释该含氟聚合物以使浓度达到3.0重量%,从而制备拒油处理液。
CH2=CHCOOCH2CH2C6F13(b-1)
除了使用上述拒油处理液以外,与实施例1同样地得到透气过滤器。
(实施例4)
将由下式(b-2)表示的具有直链状氟烷基的化合物100g、作为聚合引发剂的偶氮二异丁腈0.1g、溶剂(信越化学公司制造的“FSシンナー”)300g投入装配有氮气导入管、温度计、搅拌器的烧瓶中,导入氮气后在70℃下搅拌的同时进行16小时的加成聚合,得到80g含氟聚合物。该聚合物的数均分子量为100000。用稀释剂(信越化学公司制造的“FSシンナー”)稀释该含氟聚合物以使浓度达到3.0重量%,从而制备拒油处理液。
CH2=C(CH3)COOCH2CH2C6F13(b-2)
除了使用上述拒油处理液以外,与实施例1同样地得到透气过滤器。
(比较例1)
将由下式(c)表示的具有直链状氟烷基的化合物100g、作为聚合引发剂的偶氮二异丁腈0.1g、溶剂(信越化学公司制造的“FSシンナー”)300g投入装配有氮气导入管、温度计、搅拌器的烧瓶中,导入氮气后在70℃下搅拌的同时进行16小时的加成聚合,得到80g含氟聚合物。该聚合物的数均分子量为100000。用稀释剂(信越化学公司制造的“FSシンナー”)稀释该含氟聚合物以使浓度达到3.0重量%,从而制备拒油处理液。
CH2=C(CH3)COOCH2CH2C8F17(c)
除了使用上述拒油处理液以外,与实施例1同样地得到透气过滤器。
对以上得到的拒油处理完毕的透气过滤器和未处理的上述PTFE拉伸多孔膜(未处理品)实施透气试验和拒油试验。透气试验通过JISP8117中规定的葛尔莱试验法来实施。另外,拒油试验依据ISO14419中规定的“织物-拒油性-烃耐性试验”来实施。具体而言,使用移液管将有机溶剂以直径约5mm的液滴的形式滴加到透气过滤器的表面上,通过目视确认滴加30秒后有无液滴的渗透。作为有机溶剂,使用正癸烷、甲醇和正己烷。另外,对于液滴的渗透,在液滴被多孔膜吸收或者因液滴的渗透而使多孔膜的色调发生变化的情况下判定为“渗透”。将结果示于表1中。
表1
比较例1中,与未处理品相比,葛尔莱数上升至5倍以上。碳原子数8以上的直链状全氟烷基(Rf基)具有高结晶性对于显现拒油性是有利的,但是,在维持如PTFE拉伸多孔膜所具有的微多孔结构的透气性方面成为障碍。与此相对,实施例1~4中,葛尔莱数的上升程度与未处理品相比停留于约1.6倍~约2.5倍。将实施例1~4与比较例进行对比时,葛尔莱数存在约2倍以上的差异。
另外,实施例1~4中,得到了以不使正癸烷(表面张力23.83dyn·cm-1)和甲醇(表面张力22.45dyn·cm-1)渗透的程度具有拒油性的表面。如果是不使这些有机溶剂渗透的程度的表面,则在作为透气过滤器的用途中满足实用上要求的特性。
另外,专利文献1中,公开了使用具有含氟脂肪族环结构的含氟树脂作为不具有碳原子数为8以上的直链状全氟烷基的拒油剂对PTFE拉伸多孔膜进行处理的例子(比较例3、4)。专利文献1的这些例子中处理后的表面对表面张力比正癸烷高的甲苯(表面张力28.52dyn·cm-1)和具有与甲醇同等程度的表面张力的异丙醇(IPA;表面张力21.32dyn·cm-1)的拒油性停留于“瞬间润湿”的程度。与这些例子进行对比时,可以理解具有1)-R1C5F10CH2C4F9或2)-R2C6F13作为直链状含氟烃基的拒油剂作为在不使PTFE拉伸多孔膜的透气性大幅降低的情况下赋予拒油性的拒油剂格外优良。
实施例1、2、4中,可以确认不使表面张力低于20dyn·cm-1的正己烷(表面张力18.40dyn·cm-1)发生渗透。可以理解,作为构成拒油剂的单体,a)CH2=CR3COOR1C5F10CH2C4F9或b’)CH2=C(CH3)COOR2C6F13特别优良。
Claims (2)
1.一种赋予了拒油性的透气过滤器,具备具有由拒油剂覆盖的表面的多孔膜,其中,
所述拒油剂中含有的直链状含氟烃基由-R1C5F10CH2C4F9表示,
所述多孔膜为聚四氟乙烯拉伸多孔膜,
在此,R1为碳原子数1~12的亚烷基或亚苯基。
2.一种赋予了拒油性的透气过滤器,具备具有由拒油剂覆盖的表面的多孔膜,其中,
所述拒油剂中含有的直链状含氟烃基由-R2C6F13表示,
所述多孔膜为聚四氟乙烯拉伸多孔膜,
所述拒油剂是以由CH2=C(CH3)COOR2C6F13表示的化合物作为单体的至少一部分的聚合物,
所述化合物在所述聚合物的全部单体中所占的比率为60摩尔%以上,
在此,R2为碳原子数1~12的亚烷基或亚苯基。
3.如权利要求1或2所述的透气过滤器,
其具有葛尔莱数为35秒/100ml以下的透气性,
向所述表面上滴加有机溶剂正癸烷或甲醇的直径5mm的液滴时,滴加后30秒以内所述液滴不渗透到所述表面中。
4.如权利要求3所述的透气过滤器,其中,所述聚四氟乙烯拉伸多孔膜的厚度为5μm以上。
5.如权利要求1所述的透气过滤器,其中,
所述拒油剂是以由CH2=CR3COOR1C5F10CH2C4F9表示的化合物作为单体的至少一部分的聚合物,
在此,R3为氢原子或甲基。
6.如权利要求5所述的透气过滤器,其中,
所述拒油剂是以由CH2=CR3COOR1C5F10CH2C4F9表示的化合物作为单体的聚合物。
7.如权利要求2或6所述的透气过滤器,其中,
向所述表面上滴加有机溶剂正己烷的直径5mm的液滴时,滴加后30秒以内所述液滴不渗透到所述表面中。
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KR20140016299A (ko) | 2014-02-07 |
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CN103402615A (zh) | 2013-11-20 |
JP2012236188A (ja) | 2012-12-06 |
BR112013021797B1 (pt) | 2020-12-29 |
US20140023895A1 (en) | 2014-01-23 |
WO2012117709A1 (ja) | 2012-09-07 |
EP2682178A1 (en) | 2014-01-08 |
TW201302283A (zh) | 2013-01-16 |
EP2682178B1 (en) | 2021-01-27 |
KR20180077289A (ko) | 2018-07-06 |
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