CN104379645A - 用于降低全氟弹性体制品的静电电势的方法 - Google Patents
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Abstract
本发明为用于降低全氟弹性体制品的静电电势的方法,其中所述全氟弹性体制品用萘钠溶液处理;洗涤并用氢氧化铵处理。
Description
技术领域
本发明涉及用于降低全氟弹性体制品的静电电势的方法。更具体地,本发明涉及其中用还原剂处理全氟弹性体制品的表面的方法。
背景技术
全氟弹性体已实现了优异的商业成功并用于遭遇恶劣环境的多种应用,具体地讲发生暴露于高温和腐蚀性化学品的那些最终用途中。例如,这些聚合物常常用于飞机发动机的密封件、油井钻探设备、以及高温下使用的工业设备用密封元件中。
全氟氟弹性体的优异特性很大程度上归因于构成这些组合物中聚合物主链的主要部分的共聚全氟化单体单元的稳定性和惰性。此类单体包括四氟乙烯和全氟化乙烯基醚。为了充分开发弹性体特性,通常将全氟弹性体交联,即硫化。为此,通常将少量固化位点单体与全氟单体单元共聚。尤其优选包含至少一个腈基团的固化位点单体,例如全氟-8-氰基-5-甲基-3,6-二氧杂-1-辛烯。此类组合物描述于美国专利4,281,092;4,394,489;5,789,489;以及5,789,509中。
在某些最终应用中,如在半导体晶片制造设备中,典型的全氟弹性体制品的相对高(即>500V)的静电电势可能存在问题。已知静电电势可通过将导电填料掺入全氟弹性体制品中来降低。然而,此类填料可能是半导体晶片制造设备中的不可取的污染源。因此,将期望降低全氟弹性体制品的静电电势的另一种方法。
发明内容
本发明的一个方面是用于降低全氟弹性体制品的静电电势的方法,所述方法包括:
A)用还原剂处理全氟弹性体制品,以还原所述全氟弹性体制品的至少一个表面;
B)洗涤经还原的全氟弹性体制品以除去任何过量的还原剂;以及
C)用氢氧化铵溶液处理洗涤过的经还原的全氟弹性体制品。
本发明的另一方面是一种包含固化的全氟弹性体的制品,所述制品具有小于500V的静电电势和如由ESCA所测量的1.3∶1至0.9∶1的氟原子与碳原子的重量比,并且其中所述制品不含导电炭黑。
具体实施方式
全氟弹性体为聚合物组合物,其具有至少两个主要的全氟化单体的共聚单元。一般来讲,主要共聚单体中的一个为全氟烯烃,而另一个为全氟乙烯醚。代表性的全氟化烯烃包括四氟乙烯和六氟丙烯。合适的全氟化乙烯基醚包括由下式表示的那些
CF2=CFO(Rf′O)n(Rf″O)mRf (I)
其中Rf′和Rf″是不同的具有2-6个碳原子的直链或支化的全氟亚烷基基团,m和n独立地为0-10,并且Rf为具有1-6个碳原子的全氟烷基基团。
优选的全氟化乙烯基醚的类别包括由下式表示的组合物:
CF2=CFO(CF2CFXO)nRf (II)
其中X为F或CF3,n为0-5,并且Rf为1-6个碳原子的全氟烷基基团。
最优选的全氟化乙烯基醚为其中n为0或1并且Rf包含1-3个碳原子的那些。此类全氟化醚的例子包括全氟(甲基乙烯基)醚和全氟(丙基乙烯基)醚。其它可用的单体包括由下式表示的化合物
CF2=CFO[(CF2)mCF2CFZO]nRf (III)
其中Rf为具有1-6个碳原子的全氟烷基基团,
m=0或1,n=0-5,并且Z=F或CF3。该类别的优选的成员是其中Rf为C3F7,m=0并且n=1的那些。另外的全氟化乙烯基醚单体包括由下式表示的化合物:
CF2=CFO[(CF2CFCF3O)n(CF2CF2CF2O)m(CF2)p]CxF2x+1 (IV)
其中m和n=1-10,p=0-3,并且x=1-5。该类别的优选的成员包括其中n=0-1,m=0-1,并且x=1的化合物。
可用的全氟化乙烯基醚的另外的例子包括:
CF2=CFOCF2CF(CF3)O(CF2O)mCnF2n+1 (V)
其中n=1-5,m=1-3,并且其中优选地n=1。
优选的全氟弹性体共聚物包含四氟乙烯和至少一个全氟化乙烯基醚作为主要的单体单元。在此类共聚物中,共聚的全氟化醚单元占聚合物中单体单元总量的约15-50摩尔%。
全氟弹性体还包含至少一个固化位点单体的共聚单元,所述共聚单元的含量通常为0.1-5摩尔%。所述范围优选地介于0.3-1.5摩尔%之间。尽管可存在多于一类的固化位点单体,但最常使用一种固化位点单体,并且其包含至少一个腈取代基基团。合适的固化位点单体包括含腈氟化烯烃、含腈氟化乙烯基醚。可用的含腈固化位点单体包括由下面所示出的式表示的那些。
CF2=CF-O(CF2)n-CN (VI)
其中n=2-12,优选2-6;
CF2=CF-O[CF2-CFCF3-O]n-CF2-CFCF3-CN (VII)
其中n=0-4,优选0-2;以及
CF2=CF-[OCF2CFCF3]x-O-(CF2)n-CN (VIII)
其中x=1-2,并且n=1-4。
优选式(VIII)的那些。尤其优选的固化位点单体为具有腈基团和三氟乙烯基醚基团的全氟化聚醚。最优选的固化位点单体为
CF2=CFOCF2CF(CF3)OCF2CF2CN (IX)
即全氟(8-氰基-5-甲基-3,6-二氧杂-1-辛烯)或8-CNVE。
其它固化位点单体包括由式R1CH=CR2R3表示的烯烃,其中R1和R2独立地选自氢和氟并且R3独立地选自氢、氟、烷基和全氟烷基。所述全氟烷基基团可包含至多约12个碳原子。然而,优选至多4个碳原子的全氟烷基基团。此外,所述固化位点单体优选具有不超过三个氢原子。此类烯烃的例子包括乙烯、偏二氟乙烯、乙烯基氟化物、三氟乙烯、1-氢五氟丙烯和2-氢五氟丙烯,以及溴化或碘化的烯烃诸如4-溴代-3,3,4,4-四氟丁烯-1和溴化三氟乙烯。另选地,或除了固化位点单体的共聚单元之外,还可通过含溴或含碘链转移剂在聚合期间的反应将含溴或含碘端基的固化位点引入到全氟弹性体聚合物链上。
可掺入用于本发明的全氟弹性体中的固化位点单体的另一种类型为全氟(2-苯氧基丙基乙烯基醚)和相关的单体,如在美国专利3,467,638中所公开的。
尤其优选的全氟弹性体包含53.0-79.9摩尔%四氟乙烯、20.0-46.9摩尔%全氟(甲基乙烯基)醚和0.1至1.5摩尔%含腈固化位点单体。
可用于包含含腈固化位点的全氟弹性体的优选的固化体系利用由下式表示的双(氨基酚)和双(氨基硫代苯酚):
以及由下式表示的四胺:
其中A为SO2、O、CO、1-6个碳原子的烷基,1-10个碳原子的全氟烷基,或连接两个芳环的碳-碳键。上式X和XI中的氨基基团和羟基基团或硫代基团在苯环上彼此邻近,并且可相对于基团A在间位和对位互换。优选地,固化剂为选自下列的化合物:4,4′-[2,2,2-三氟-1-(三氟甲基)亚乙基]双(2-氨基苯酚);4,4′-磺酰基双(2-氨基苯酚);3,3′-二氨基联苯胺;以及3,3′,4,4′-四氨基二苯甲酮。这些中的第一种是最优选的,并且将被称为双(氨基苯酚)AF。固化剂可如授予Angelo的美国专利号3,332,907中所公开的制备。双(氨基苯酚)AF可通过以下方法制备:优选用硝酸钾和三氟乙酸将4,4′-[2,2,2-三氟-1-(三氟甲基)亚乙基]-双酚(即双酚AF)硝化,然后用乙醇作为溶剂和催化量的碳载钯作为催化剂进行催化氢化。应选择固化剂的含量以优化期望的硫化橡胶特性。一般来讲,使用比与全氟弹性体中存在的所有固化位点反应所需的量略微过量的固化剂。通常,每100份弹性体需要0.5-5.0重量份的固化剂。优选的范围为1.0-2.0phr。
还可将过氧化物用作固化剂,尤其是当固化位点为腈基团或碘基团或溴基团时。可用的过氧化物是在固化温度下产生自由基的那些。尤其优选在超过50℃的温度下分解的二烷基过氧化物或双(二烷基过氧化物)。在许多情况下,优选的是使用具有连接到过氧氧的叔碳原子的二特丁基过氧化物。这一类别的最有用的过氧化物为2,5-二甲基-2,5-二(叔丁基过氧基)3-己炔和2,5-二甲基-2,5-二(叔丁基过氧基)己烷。其它过氧化物可选自诸如过氧化二异丙苯、过氧化二苯甲酰、过苯甲酸叔丁酯和碳酸二[1,3-二甲基-3-(叔丁过氧基)丁基]酯的化合物。一般来讲,每100份全氟弹性体使用约1-3份过氧化物。通常与作为过氧固化剂体系的一部分的组合物共混的另一种材料为助剂,所述助剂由能够与过氧化物协同作用以提供可用固化的多不饱和化合物构成。这些助剂可以介于0.1和10份每100份全氟弹性体之间,优选介于2-5phr之间的量添加。典型的助剂包括但不限于氰尿酸三烯丙酯;异氰脲酸三烯丙酯;异氰脲酸三(甲基烯丙基)酯;三(二烯丙基胺)-s-三嗪;亚磷酸三烯丙酯;N,N-二烯丙基丙烯酰胺;六烯丙基磷酰胺;N,N,N′,N′-四烷基邻苯二甲酰胺;N,N,N′,N′-四烯丙基丙二酰胺;异氰脲酸三乙烯基酯;2,4,6-三乙烯基甲基三硅氧烷以及三(5-降冰片-2-亚甲基)氰尿酸酯。尤其可用的是异氰脲酸三烯丙酯。
适用于固化具有腈固化位点的全氟弹性体的其它固化剂包括如美国专利5,565,512中所公开的氨、无机或有机酸的铵盐(例如,全氟辛酸铵),如美国专利6,281,296 B1中所公开的分解以产生氨的化合物(例如脲),以及如美国专利6,638,999 B2中所公开的含氮亲核化合物(例如二苯胍)。
取决于存在的固化位点单体,还可使用双固化体系。例如,具有含腈固化位点单体的共聚单元的全氟弹性体可使用包含过氧化物与氨生成固化剂以及助剂组合的混合物的固化剂。一般来讲,使用0.3-5份过氧化物、0.3-5份助剂、以及0.1-10份氨生成固化剂。
可将添加剂,诸如填料(例如非原纤化和原纤化含氟聚合物、非导电炭黑、硫酸钡、二氧化硅、氧化铝、铝硅酸盐、以及二氧化钛)、稳定剂、增塑剂、润滑剂以及通常用于全氟弹性体配混的加工助剂掺入本发明的组合物中,前体条件是它们对于预期使用条件具有足够的稳定性。
用于本发明的固化的全氟弹性体制品通过将上述全氟弹性体组合物成形,然后固化制成。固化可通过加热或通过辐射引发。随后可将所述制品在升高的温度下后固化一段时间。此类制品的例子包括密封件、垫圈、O形环和复合材料部件(例如,粘合的门密封件)。
本发明的一个方面是用于降低不含导电炭黑的全氟弹性体制品的静电电势的方法。所述方法包括A)用还原剂处理全氟弹性体制品以还原所述全氟弹性体制品的至少一个表面;B)洗涤经处理过的全氟弹性体制品以除去任何过量的还原剂;以及C)用氢氧化铵溶液处理洗涤过的经还原的全氟弹性体制品。
合适的还原剂的例子包括但不限于萘基碱金属(alkali metal naphthalides)(例如萘钠、萘钾和苊烯钠)、液体碱金属(例如钠/钾合金)、以及还原性等离子体(例如氢等离子体)。萘钠是优选的还原剂。其通常为有机溶剂诸如四氢呋喃或二甲氧基乙烷。(购自ActonTechnologies)为适用于本发明方法的可商购获得的还原剂的例子。
在步骤A)中,处理优选在惰性气氛诸如氮气或氩气中进行。全氟弹性体制品的表面的充分还原通常在所述全氟弹性体制品暴露于还原剂后约5分钟之后在室温下进行。
在步骤B)中,然后洗涤具有还原表面的全氟弹性体制品以除去过量的还原剂。洗涤不需要在惰性气氛中进行。洗涤通常为多步方法,其中首先用有机溶剂(例如丙酮),然后用去离子水,然后用稀酸溶液(例如,0.1M HCl)冲洗经还原的全氟弹性体制品。然后再次用丙酮冲洗所述制品。
在步骤C)中,用氢氧化铵溶液(约1M)处理经洗涤和还原的全氟弹性体制品并使其风干。
优选地,用足量去离子水,并且然后优选用最终的氢氧化铵溶液进一步洗涤所述全氟弹性体制品,以从制品的表面除去痕量金属离子。
所得的具有还原表面的全氟弹性体制品具有低静电电势,即小于500V,优选小于100V,并且尤其适用于半导体晶片制造设备。如由ESCA所测量的,制品的表面至至少10微米的深度具有1.3∶1至0.9∶1(优选1∶1)的氟原子与碳原子的重量比。这与由于还原剂的作用而在制品表面附近形成的多个C-C双键一致。所述制品不含导电炭黑。
实例
测试方法
在Shishido Electrostatic Ltd.,STATIRON DS-3型静电电势计中对K314型全氟弹性体O形环进行静电电势测量。传感器和O形环之间的距离为5mm。在实例中记录沿O形环表面在3个点处所测量的静电电势的平均值。
用Physical Electronics Quantera Scanning ESCA微探针,使用在20kV和100W下操作的聚焦(100mm)单色Al X射线(1486.6eV)束对经处理过的和未经处理的(即对照)O形环进行ESCA表面分析。X-射线束使用电子枪产生并在~1400mm×~200mm范围内扫描以限定分析区域。表面充电通过用低能量离子和电子(分别为~8eV和~1eV)溢流样品来中和。在恒定能量模式下操作电子能量分析仪,其中传递能量为55eV并且数据点之间的步长大小为0.2eV,以进行高分辨率扫描(通常对于每个元件在20-50eV之间扫描)。飞离角相对于样品法线为45°。
实例1
用于该实例的全氟弹性体制品为K-314型O形环,其由已用双(氨基苯酚)AF固化的包含四氟乙烯、全氟(甲基乙烯基)醚和全氟(8-氰基-5-甲基-3,6-二氧杂-1-辛烯)的共聚单元的全氟弹性体制成。所述O形环不含导电炭黑。
在处理之前O形环的静电电势测量为1085V。ESCA示出处理之前氟原子与碳原子的重量比为1.8∶1。
将待用本发明方法处理的O形环置于氮气吹扫箱中。然后用萘钠的二甲氧基乙烷溶液()处理O形环。轻轻搅拌样品以确保充分覆盖。5分钟之后,从绿色溶液中取出O形环并从吹扫箱中移出。然后用丙酮、接着用去离子水,然后用0.1M HCl,并且最后再次用丙酮洗涤O形环的还原表面。在所述方法的这一阶段,O形环的静电电势测量为399V。
然后将经洗涤的O形环浸入1M氢氧化铵溶液中并使其风干。然后在足量去离子水中对O形环进行洗涤。所得的O形环上的静电电势测量为52V。ESCA示出所得的O形环上的氟原子与碳原子的重量比为0.98∶1。
Claims (8)
1.用于降低全氟弹性体制品的静电电势的方法,所述方法包括:
A)用还原剂处理全氟弹性体制品,以还原所述全氟弹性体制品的至少一个表面;
B)洗涤经处理过的全氟弹性体制品以除去任何过量的还原剂;以及
C)用氢氧化铵溶液处理洗涤过的经处理过的全氟弹性体制品。
2.根据权利要求1所述的方法,其中所述还原剂选自萘基碱金属、液体碱金属和还原性等离子体。
3.根据权利要求2所述的方法,其中所述萘基碱金属选萘钠、萘钾和苊烯钠。
4.根据权利要求3所述的方法,其中所述萘基碱金属为萘钠。
5.根据权利要求4所述的方法,其中所述萘钠为有机溶剂中的溶液。
6.包含固化的全氟弹性体的制品,所述制品具有小于500V的静电电势和如由ESCA所测量的1.3∶1至0.9∶1的氟原子与碳原子的重量比,并且其中所述制品不含导电炭黑。
7.根据权利要求6所述的制品,其中所述静电电势小于100V。
8.根据权利要求6所述的制品,其中氟原子与碳原子的所述重量比为1∶1。
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JPH0859864A (ja) * | 1994-08-18 | 1996-03-05 | Fujitsu Ltd | フッ素樹脂製品とその製造方法 |
CN1659028A (zh) * | 2002-04-18 | 2005-08-24 | 3M创新有限公司 | 含有氟化聚合物层的多层制品粘合和粘结 |
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GB1399268A (en) * | 1972-08-29 | 1975-07-02 | Cosid Kautasit Werke Veb | Packing elements |
JPS609734A (ja) * | 1983-06-30 | 1985-01-18 | Toray Ind Inc | フツ素樹脂成型体 |
GB2302693B (en) * | 1995-06-26 | 1999-03-10 | Tokuyama Corp | Fluorine-containing resin molded articles |
JP2000034380A (ja) * | 1998-07-17 | 2000-02-02 | Daikin Ind Ltd | 架橋性エラストマー組成物、該組成物から製造されるシール材およびそれに用いるフィラー |
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- 2013-06-27 CN CN201380033208.7A patent/CN104379645A/zh active Pending
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JPH0859864A (ja) * | 1994-08-18 | 1996-03-05 | Fujitsu Ltd | フッ素樹脂製品とその製造方法 |
CN1659028A (zh) * | 2002-04-18 | 2005-08-24 | 3M创新有限公司 | 含有氟化聚合物层的多层制品粘合和粘结 |
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