CN110709467B - 氟橡胶组合物和氟橡胶交联体 - Google Patents

氟橡胶组合物和氟橡胶交联体 Download PDF

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CN110709467B
CN110709467B CN201880037566.8A CN201880037566A CN110709467B CN 110709467 B CN110709467 B CN 110709467B CN 201880037566 A CN201880037566 A CN 201880037566A CN 110709467 B CN110709467 B CN 110709467B
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fluororubber
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vinylethoxysilane
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CN110709467A (zh
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吉田卓
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Nok Corp
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Abstract

本发明提供一种蒸汽环境下的压缩永久变形优异、防止蒸汽环境下的硬度变化、并且粘接性优异的氟橡胶组合物和氟橡胶交联体。该氟橡胶组合物的特征在于，含有由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物、二氧化硅‑硅酸铝的乙烯基乙氧基硅烷反应物、和水滑石，并基本上不含氧化镁和氢氧化钙，且相对于100重量份的三元系氟橡胶聚合物，含有2～55重量份的二氧化硅‑硅酸铝的乙烯基乙氧基硅烷反应物、0.5～10重量份的水滑石。

Description

氟橡胶组合物和氟橡胶交联体
技术领域
本发明涉及氟橡胶组合物和氟橡胶交联体，更详细地说，涉及蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的氟橡胶组合物和氟橡胶交联体。
背景技术
以往，已知将从内燃机的燃烧室排出的排出气体的一部分再循环至内燃机的吸气系统的排气再循环(Exhaust Gas Recirculation；EGR)阀(专利文献1)。
在EGR阀中设置有用于防止所述排出气体(也称为EGR气体)的泄漏的油封。
EGR阀的内部由于是接触排出气体、冷凝水的严酷的环境，因此在上述的油封中使用有耐热、耐化学品性优异的氟橡胶。
另外，上述的油封由于还暴露于蒸汽，因此还要求耐蒸汽性。通常多元醇交联的氟橡胶由于作为吸酸剂配合的MgO，而导致耐蒸汽性差。因此，在蒸汽环境下使用过氧化物交联系的氟橡胶。
(现有技术文献)
(专利文献)
专利文献1：日本特开2015-124640号公报
专利文献2：WO2006/006468(氟橡胶组合物)
发明内容
(发明要解决的问题)
在过氧化物硫化系的氟橡胶中，为了提高粘接性，使用金属氧化物，但由于金属氧化物，出现蒸汽环境中的固化劣化和油封的弹性减弱(压缩永久变形降低)。
因此，对于现有的氟橡胶组合物，希望有蒸汽环境下的压缩永久变形优异，蒸汽环境下的硬度变化被防止，并且粘接性优异的组合物。
因此，本发明的课题是提供一种蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的氟橡胶组合物和氟橡胶交联体。
另外，本发明的其他课题通过以下的记载来阐明。
用于解决课题的手段
上述课题通过以下的各发明解决。
1.一种氟橡胶组合物，其特征在于，含有由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物、和二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，所述氟橡胶组合物基本上不含氧化镁和氢氧化钙，并相对于100重量份的所述三元系氟橡胶聚合物，含有8～60重量份的所述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物。
2.一种氟橡胶组合物，其特征在于，含有由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物、二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物、和水滑石，所述氟橡胶组合物基本上不含氧化镁和氢氧化钙，并相对于100重量份的所述三元系氟橡胶聚合物，含有2～55重量份的所述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物、0.5～10重量份的所述水滑石。
3.上述1或2所述的氟橡胶组合物，其特征在于，所述三元系氟橡胶聚合物的氟含量为64～67重量％。
4.一种氟橡胶交联体，其特征在于，将上述1～3中任一项所述的氟橡胶组合物交联而成。
(发明效果)
根据本发明，能够提供蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的氟橡胶组合物和氟橡胶交联体。
具体实施方式
以下对用于实施本发明的方式进行详细说明。
首先，对本发明的第一方案所涉及的氟橡胶组合物进行说明。
第一方案所涉及的氟橡胶组合物含有由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物、和二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，并基本上不含氧化镁和氢氧化钙。
在此，所谓氟橡胶组合物基本上不含氧化镁和氢氧化钙是指不含氧化镁和氢氧化钙，或者相对于100重量份的三元系氟橡胶聚合物，它们的合计的含量为0.1重量份以下、优选0.05重量份以下。
相对于100重量份的上述三元系氟橡胶聚合物，第一方案所涉及的氟橡胶组合物含有8～60重量份、优选10～50重量份的上述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物。
由此，可获得蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的效果。
三元系氟橡胶聚合物，从显著发挥本发明的效果的观点出发，优选氟含量为64～67重量％。
作为三元系氟橡胶聚合物中的聚合成分的全氟乙烯醚能够用通式CF2＝CFORf(式中，Rf表示碳原子数1～10的全氟烷基)表示。作为上述碳原子数1～10的全氟烷基，例如可列举全氟甲基等。
三元系氟橡胶聚合物优选可进行过氧化物交联，并且优选在分子中含有碘和/或溴作为交联位点。
作为这样的三元系氟橡胶聚合物，例如可使用杜邦公司制“Viton GLT600S”(氟含量64重量％)、“Viton GTL200S”(氟含量64重量％)、Solvay Solexis公司制“TecnoflonPL855”(氟含量64重量％)等市售品。三元系氟橡胶聚合物可将2种以上混合使用。
二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物只要是使二氧化硅-硅酸铝与乙烯基乙氧基硅烷反应而得到的反应物，则并无特别限定。作为二氧化硅-硅酸铝，例如可使用Hoffmann Mineral GMBH制“Sillitin Z86”等市售品。另外，作为二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，例如可使用Hoffmann Mineral GMBH制“AKTISIL VM”等市售品。
接下来，对本发明的第二方案所涉及的氟橡胶组合物进行说明。
第二方案所涉及的氟橡胶组合物含有由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物、二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物和水滑石，并且基本上不含氧化镁和氢氧化钙。
在第二方案所涉及的氟橡胶组合物中，相对于100重量份的上述三元系氟橡胶聚合物，含有2～55重量份、优选3～50重量份的上述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，并且含有0.5～10重量份、优选1～9重量份的上述水滑石类。
由此，可获得蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的效果。
对于第二方案中使用的三元系氟橡胶聚合物和二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，能够援用针对第一方案的说明。
作为第二方案中使用的水滑石，例如可列举Mg4.3Al2(OH)12.6CO3·mH2O、Mg6Al2(OH)16CO3·4H2O、Mg4.5Al2(OH)13CO3·3.5H2O等。作为水滑石类，例如可使用协和化学工业株式会社制“DHT-4A”等市售品。
以上说明的第一方案或第二方案所涉及的氟橡胶组合物优选进行过氧化物交联而使用。
在过氧化物交联中，能够优选使用有机过氧化物交联剂。
对有机过氧化物交联剂无特别限制，例如可列举2,5-二甲基-2,5-二(叔丁基过氧基)己烷等。
就有机过氧化物交联剂而言，相对于100重量份的三元系氟橡胶聚合物，优选以0.5～5重量份的比例使用，更优选以1～3重量份的比例使用。
在氟橡胶交联体中，除了以上说明的成分以外，可在不损害本发明的目的的范围适当添加作为橡胶的通常配合剂使用的交联助剂、白炭黑等增强剂、MT炭黑、FEF炭黑等炭黑、石墨等填充剂、硬脂酸、棕榈酸、石蜡等加工助剂、防老剂、增塑剂、氧化锌等。
本发明的氟橡胶交联体通过将以上说明的氟橡胶组合物交联而成。交联如上所述优选为过氧化物交联。采用本发明的氟橡胶交联体，可获得蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的效果。
在制造氟橡胶交联体的优选的方法中，首先，使用捏合机、肖氏密炼机、班伯里混炼机等密闭式混炼机或开炼辊将氟橡胶组合物的各成分混炼。接下来，将混炼物压成片状，或者使用挤出机、鲍尔装置等制成规定的形状。接下来，使用压缩压机、铸塑成型机、注射成型机等，在规定温度(优选100～180℃)、规定时间(优选1～30分钟)的条件下进行交联成型。进而，能够在规定温度(优选200～220℃)、规定时间(优选1～10小时)的条件下使用空气烘箱等进行二次交联。
本发明的氟橡胶交联体适合用作各种密封构件、特别是EGR阀用油封。由本发明的氟橡胶交联体构成的EGR阀用油封，由于蒸汽环境下的压缩永久变形优异，蒸汽环境下的硬度变化被防止，并且粘接性优异，因此在EGR阀的严酷的环境下能够实现良好的密封。
实施例
以下对本发明的实施例进行说明，但本发明并不限于所涉及的实施例。
以下为与第一方案有关的例证。
(实施例1)
1.氟橡胶组合物的制备
在下述100重量份的三元系氟橡胶聚合物C中配合10重量份的二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物(Hoffmann Mineral GMBH制“AKTISIL VM”)、3重量份的MT炭黑(CANCARB LIMITED公司制“THERMAX N-990LSR”)、0.1重量份的氧化锌(相当于JIS标准“第1种”的品质)，进而配合2重量份的有机过氧化物交联剂(2,5-二甲基-2,5-二(叔-丁基过氧基)己烷)(日本油脂株式会社制“PERHEXA25B-40”)以及规定的配合剂，并进行混炼，而得到未交联的氟橡胶组合物。
·三元系氟橡胶聚合物A：由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；氟含量64重量％(杜邦公司制“Viton GLT600S”)
·三元系氟橡胶聚合物B：由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；氟含量64重量％(杜邦公司制“Viton GTL200S”)
·三元系氟橡胶聚合物C：由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；氟含量64重量％(Solvay Solexis公司制“Tecnoflon PL855”)
2.试验片的制作
使用上述氟橡胶组合物，采用以下的方法制作粘接性评价用的试验片、蒸汽环境下的压缩永久变形评价用的试验片、蒸汽环境下的硬度变化防止评价用的试验片。
(1)粘接性评价用的试验片
将上述氟橡胶组合物成型为φ85mm的油封的形状，将其对于钢板在180℃下进行3分钟加压交联粘接，从而得到粘接性评价用的试验片。
(2)蒸汽环境下的压缩永久变形评价用的试验片
将上述氟橡胶组合物成型为线径3.1mm的O型环的形状，将其在180℃下加压交联3分钟，然后，在200℃的气氛下保持5小时，从而得到蒸汽环境下的压缩永久变形评价用的试验片。
(3)蒸汽环境下的硬度变化防止评价用的试验片
将上述氟橡胶组合物成型为2mm厚的片材，将其在180℃下加压交联3分钟，然后，在200℃的气氛下保持5小时，从而得到蒸汽环境下的硬度变化防止评价用的试验片。
3.评价方法
(1)粘接性
在上述粘接性评价用的试验片中，将粘接的油封用钳子剥离，作为橡胶残留的面积率，测定R残留率(％)。基于测定的R残留率(％)，用以下的评价标准进行评价。
＜评价标准＞
AA：R残留率(％)为80％以上且100％以下。
A：R残留率(％)为60％以上且不到80％。
B：R残留率(％)为45％以上且不到60％。
C：R残留率(％)为0％以上且不到45％。
(2)蒸汽环境下的压缩永久变形
按照JIS K6262：2013测定了蒸汽环境下的压缩永久变形(％)。试验环境设为湿度95％的蒸汽环境，试验温度设为80℃，试验时间设为96小时。基于测定的压缩永久变形(％)，用以下的评价标准进行评价。
＜评价标准＞
AA：压缩永久变形(％)为0％以上且25％以下。
A：压缩永久变形(％)超过25％且28％以下。
B：压缩永久变形(％)超过28％且31％以下。
C：压缩永久变形(％)超过31％且100％以下。
(3)蒸汽环境下的硬度变化防止
按照JIS K6258：2010测定蒸汽环境下的硬度变化。试验环境设为湿度95％的蒸汽环境，试验温度设为80℃，试验时间设为192小时。基于测定的硬度变化(Hw)(点数)，用以下的评价标准进行评价。
＜评价标准＞
AA：硬度变化(Hw)(点数)为±0。
A：硬度变化(Hw)(点数)为-5以上且-1以下。
B：硬度变化(Hw)(点数)为+1以上且+5以下。
C：硬度变化(Hw)(点数)为超过+5且+10以下。
(4)综合评价
基于上述(1)～(3)的评价结果，用以下的评价标准进行综合评价。
＜评价标准＞
AA：上述(1)～(3)的评价只是A以上。
A：作为上述(1)～(3)的评价，包含A以上，不含C。
B：上述(1)～(3)的评价只是B。
C：作为上述(1)～(3)的评价，包含C。
将以上的结果示于表1。
(实施例2)
在实施例1中，除了将二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物的配合量变为15重量份以外，与实施例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
(实施例3)
在实施例1中，除了将二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物的配合量变为30重量份以外，与实施例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
(实施例4)
在实施例3中，除了代替MT炭黑而配合2重量份的FEF炭黑(东海碳株式会社制“SEAST GS-O”)，并省略氧化锌的配合以外，与实施例3同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1中。
(比较例1)
在实施例1中，除了代替上述三元系氟橡胶聚合物C而使用由50重量份的三元系氟橡胶聚合物A和50重量份的上述三元系氟橡胶聚合物B组成的100重量份的聚合物，并将二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物的配合量变为5重量份，进而配合3重量份的水滑石(Mg4.3Al2(OH)12.6CO3·mH2O)(协和化学工业株式会社制“DHT-4A”)、6重量份的氧化镁(协和化学工业株式会社制“KYOWAMAG 150”)和3重量份的氢氧化钙(近江化学工业株式会社制“CALDIC 2000”)以外，与实施例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
(比较例2)
在比较例1中，除了省略了氧化镁的配合以外，与比较例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
(比较例3)
在比较例1中，除了省略了水滑石、氧化镁和氢氧化钙的配合以外，与比较例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
(比较例4)
在实施例1中，除了将二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物的配合量变为5重量份以外，与实施例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表1。
[表1]
Figure BDA0002304778150000081
＜评价＞
由表1可知，根据本发明的第一方案所涉及的氟橡胶组合物(实施例1～4)，可获得蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的效果。
与此相对，可知在含有氧化镁、氢氧化钙的比较例1、2中，蒸汽环境下的压缩永久变形差，不能防止蒸汽环境下的硬度变化。
另外，可知与本发明的第一方案所涉及的氟橡胶组合物(实施例1～4)相比，在二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物的含量不在8～60重量份的范围的比较例3、4中，粘接性差。
以下为与第二方案有关的例证。
(实施例5)
在由50重量份的下述三元系氟橡胶聚合物A和50重量份的下述三元系氟橡胶聚合物B组成的100重量份的聚合物中配合5重量份的二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物(Hoffmann Mineral GMBH制“AKTISIL VM”)、6重量份的水滑石(Mg4.3Al2(OH)12.6CO3·mH2O)(协和化学工业株式会社制“DHT-4A”)、3重量份的MT炭黑(CANCARB LIMITED公司制“THERMAX N-990LSR”)、0.1重量份的氧化锌(相当于JIS标准“第1种”的品质)，进而配合2重量份的有机过氧化物交联剂(2,5-二甲基-2,5-二(叔丁基过氧)己烷)(日本油脂株式会社制“PERHEXA25B-40”)以及规定的配合剂，并进行混炼，得到未交联的氟橡胶组合物。使用得到的氟橡胶组合物，与实施例1同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表2中。
·三元系氟橡胶聚合物A：由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；氟含量64重量％(杜邦公司制“Viton GLT600S”)
·三元系氟橡胶聚合物B：由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；氟含量64重量％(杜邦公司制“Viton GTL200S”)
(实施例6)
在实施例5中，除了将水滑石的配合量变为9重量份以外，与实施例5同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表2中。
(比较例5)
在实施例5中，除了将水滑石的配合量变为3重量份，进而配合6重量份的氧化镁(协和化学工业株式会社制“KYOWAMAG 150”)和3重量份的氢氧化钙(近江化学工业株式会社制“CALDIC 2000”)以外，与实施例5同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表2中。
(比较例6)
在实施例5中，除了将水滑石的配合量变为3重量份，进而配合3重量份的氢氧化钙以外，与实施例5同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表2中。
(比较例7)
在实施例5中，除了将水滑石的配合量变为12重量份以外，与实施例5同样地制作各试验片，并与实施例1同样地进行评价。将结果示于表2中。
[表2]
Figure BDA0002304778150000101
＜评价＞
由表2可知，根据本发明的第二方案所涉及的氟橡胶组合物(实施例5、6)，可获得蒸汽环境下的压缩永久变形优异、蒸汽环境下的硬度变化被防止、并且粘接性优异的效果。
与此相对，可知在含有氧化镁、氢氧化钙的比较例5、6中，蒸汽环境下的压缩永久变形差，不能防止蒸汽环境下的硬度变化。
另外，可知与本发明的第二方案所涉及的氟橡胶组合物(实施例5、6)相比，在水滑石的含量不在0.5～10重量份的范围的比较例7中，蒸汽环境下的压缩永久变形差。

Claims (4)

1.一种氟橡胶组合物，其特征在于，含有：
由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；
二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物；和
炭黑，
基本上不含氧化镁和氢氧化钙，
相对于100重量份的所述三元系氟橡胶聚合物，含有8～60重量份的所述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物，
所述全氟乙烯醚由通式CF2＝CFORf表示，其中，Rf表示碳原子数1～10的全氟烷基。
2.一种氟橡胶组合物，其特征在于，含有：
由偏氟乙烯、全氟乙烯醚、四氟乙烯组成的三元系氟橡胶聚合物；
二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物；
水滑石；和
炭黑，
基本上不含氧化镁和氢氧化钙，
相对于100重量份的所述三元系氟橡胶聚合物，含有2～55重量份的所述二氧化硅-硅酸铝的乙烯基乙氧基硅烷反应物、0.5～10重量份的所述水滑石，
所述全氟乙烯醚由通式CF2＝CFORf表示，其中，Rf表示碳原子数1～10的全氟烷基。
3.根据权利要求1或2所述的氟橡胶组合物，其特征在于，
所述三元系氟橡胶聚合物的氟含量为64～67重量％。
4.一种氟橡胶交联体，其特征在于，
通过将权利要求1～3中任一项所述的氟橡胶组合物交联而形成。
CN201880037566.8A 2017-06-06 2018-05-21 氟橡胶组合物和氟橡胶交联体 Active CN110709467B (zh)

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