CN103189552A - 用于对润滑体系使用的亲水性组合物及使用其的装置和方法 - Google Patents
用于对润滑体系使用的亲水性组合物及使用其的装置和方法 Download PDFInfo
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- CN103189552A CN103189552A CN2011800514599A CN201180051459A CN103189552A CN 103189552 A CN103189552 A CN 103189552A CN 2011800514599 A CN2011800514599 A CN 2011800514599A CN 201180051459 A CN201180051459 A CN 201180051459A CN 103189552 A CN103189552 A CN 103189552A
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Abstract
用于对润滑体系使用的亲水性组合物包含直径为50nm~10μm且长度为直径至少5倍的亲水性纤维。所述亲水性纤维对水和/或其它亲水性流体具有强的亲和性并且可除去或消除在包含油和/或润滑流体的润滑体系中的游离或解离的水。
Description
交叉引用
本申请要求2010年10月25日提交的美国临时申请no.61/406,416、2010年11月30日提交的美国临时申请no.61/418,081、2010年12月10日提交的美国临时申请no.61/421,985和2010年12月22日提交的美国临时申请no.61/426,083的优先权,将其中的所有内容通过参考引入,如同在本文中完全阐述一样。
技术领域
本发明涉及用于对润滑体系使用的亲水性组合物以及使用其从所述润滑体系除去水或其它亲水性材料的装置和方法。
背景技术
US2005/0197260公开了一种环境友好的润滑脂组合物,其包含植物油和纤维素纤维、以及甘油、防锈剂和/或脂肪酸酯、卵磷脂和/或磷脂酰胆碱。
US6,482,780公开了用于滚柱轴承的润滑脂组合物,其包含引入在基础油中的含有具有至少3微米主轴长度的长纤维状材料的基于金属皂的增稠剂,其中该基础油包含组合共混的在其分子结构中具有极性基团的润滑剂和非极性润滑剂。
US5,874,391公开了聚合物增稠的润滑脂,其通过如下制备:将聚合物例如聚丙烯与基础油混合并加热所述混合物以使所述聚合物充分地溶解在所述基础油中。然后使经加热的混合物快速冷却或骤冷。
US5,415,791公开了用于埋置有固体润滑剂的滑动部件的润滑组合物,其包含5-78重量%的固体润滑剂粉末材料、5-30重量%的在常温下为液体或糊形式的润滑油、1-15重量%的用于吸收和保持所述润滑油的载体、和15-50重量%的热固性合成树脂粘合剂。所述载体可为亲油性纤维,例如纤维素纤维和聚丙烯纤维。
在通过已知的润滑体系润滑的设备的运行期间,当水或其它亲水性材料(流体)被不期望地引入到该体系中时,该润滑体系的性能受到负面影响。这样的不期望的水性材料可降低润滑剂的使用寿命和/或可导致设备的腐蚀。以前的用于从润滑体系除去和/或消除水或其它亲水性材料的解决方案是不足的。
发明内容
因此,本教导的目的是公开经改善的用于对润滑体系使用的亲水性组合物、利用所述亲水性组合物的装置以及用于从润滑体系除去水或其它亲水性材料的方法。
该目的分别通过权利要求1、20和23的发明实现。
本发明的进一步发展描述于从属权利要求中。
根据本教导的第一方面,公开亲水性组合物以对润滑体系使用且包含直径为50nm~10μm和长度为所述直径至少5倍的亲水性纤维。所述亲水性纤维对所述润滑体系中的水和/或其它亲水性流体具有强的亲和性,所述润滑体系优选包含油和/或其它润滑流体,例如,疏水性流体和/或物质,例如润滑脂。
这样的亲水性(优选吸湿性)纤维能够有利地消除、除去或吸收润滑体系中的任何游离水和/或任何解离的水,由此改善所述润滑体系的润滑性能,提高所述润滑体系的使用寿命和/或减少需要润滑的部件的腐蚀问题。
在本教导的另一方面中,所述亲水性纤维可设置在需要润滑的系统和/或机器上、附着到需要润滑的系统和/或机器、和/或埋置/引入到需要润滑的系统和/或机器中,例如,在其与油或其它润滑流体呈流体连通的表面上。这样的亲水性纤维可有利地用在轴承设备和/或包括或含有油或其它润滑流体作为润滑体系的组分的其它设备中。所述设备可包括含有油或其它润滑流体的密封部分。
另外或者替代地,根据本教导的亲水性纤维可设置成与需要润滑的表面流体连通,例如,接近于需要润滑的表面。在这种情况中,然后可使油或其它基础润滑流体与亲水性纤维接触,由此所述润滑体系中的水和/或其它亲水性成分可被所述亲水性纤维除去或吸收。
另外或替代地,所述亲水性纤维可以织物(fabric)材料例如无纺垫、毡或布的形式提供。所述织物材料可固定到暴露于润滑剂,即,与润滑剂呈流体连通的表面,或者埋置到该表面中,但优选与需要润滑的表面间隔开。此外,通过容许油或其它基础润滑流体接触所述亲水性表面/织物材料,水和/或其它亲水性物质可有效地从润滑剂除去。
由于所述亲水性纤维可由宽范围的材料制造,本教导有利地使得实现在亲水性(纤维或纤维状)材料的选择方面的宽的灵活性或选择。
如本教导中所利用的,术语“亲水性(的)”意指一片平坦的材料(即,将用于形成所述亲水性纤维或纤维状材料的材料)的表面将容易地被水覆盖(润湿),因为这将降低体系的总的表面能。材料越亲水,水滴在这样的材料的平坦光滑的表面上的“接触角”将越小,这使得接触角是根据本教导的亲水性程度的合适量度。大体上,如果当一小滴水落到材料上时呈现小于90度的内部接触角,这样的材料可被认为是亲水性的。根据本教导的亲水性纤维状材料的较高的亲水性程度(即较小的接触角)在一些实施方式中可为更有利的。
类似地,如在本教导中所利用的,术语“亲油性(的)”意指一片平坦的材料(即,用于形成亲油性纤维或纤维状材料的材料)的表面将容易地被油或另外的基础润滑流体覆盖(润湿),因为那将降低体系的总的表面能。亲油性材料的多孔结构将通过毛细作用像海绵那样吸收油。材料越亲油,油滴在这样的材料的平坦光滑的表面上的“接触角”将越小,这使得接触角是根据本教导的亲油性程度的合适量度。大体上,如果当落到材料上时,一小滴油呈现小于90度的内部接触角,这样的材料可被认为是亲油性的。根据本教导的亲油性纤维状材料的较高的亲油性程度(即较小的接触角)在一些实施方式中可为更有利的。
附图说明
唯一的图显示在滚柱轴承中用于布置一个或多个吸水结构的可能的位置的非限制性实例。
具体实施方式
首先,注意,根据本教导的亲水性纤维可对于在运行温度下呈现润滑性质以用于各种应用的范围广泛的流体例如油或其它基础润滑流体使用。
特别合适的润滑剂(油)包括,但不限于,由原油获得的矿物油,I、II和III类润滑剂,IV类润滑剂(聚α-烯烃“PAO”)和V类润滑剂(所有其它的)。
润滑油的更特别的但非限制性的列表包括矿物油、合成酯、以及基于植物的油和它们的衍生物,例如得自油菜籽、低芥酸菜籽(canola)、向日葵、低芥酸菜籽和棕榈的油。基于动物的油、它们的衍生物和合成润滑剂也可合适地用在本教导的一些方面中,包括,但不限于,聚乙二醇(PG)、聚亚烷基二醇(PAG)、白油、硅油、很高粘度指数油(VHVI)、水、甘油和蜡。
根据本教导的特别优选的油为矿物油、合成酯、PAO和合成烃。
所述润滑流体(油)的粘度的范围可从非常低(在40℃下低于1cSt)到非常高(在40℃下几千cSt)。最合适的粘度取决于应用温度、运行(例如,旋转)速度等,且本教导提供多种可能的润滑性质。然而,特别优选的是在40℃下具有10-300cSt的粘度的以上油类型的任一者。
大体上,根据本教导的亲水性(和/或亲油性)纤维可例如由可纺成纤维的任何类型的聚合物材料以及连同任选的添加剂制造。合适的聚合物包括,但不限于,聚酰胺(PA)、尼龙6,6、聚酰胺-6,6(PA-6,6)、聚酰胺-4,6(PA-4,6)、聚氨酯(PU)、聚苯并咪唑(PBI)、聚碳酸酯(PC)、聚丙烯腈(PAN)、丙烯腈橡胶(NBR)、聚乙烯醇(PVA)、聚乳酸(PLA)、聚乙烯-共-醋酸乙烯酯(PEVA)、聚甲基丙烯酸酯(PMMA)、四氢全氟辛基丙烯酸酯(TAN)、聚环氧乙烷(PEO)、胶原-PEO、聚苯胺(PANI)、聚苯乙烯(PS)、具有纤连蛋白官能性的丝状聚合物、聚乙烯基咔唑、聚对苯二甲酸乙二醇酯(PET)、聚丙烯酸(PAA)、聚丙烯甲醇(PM)、聚乙烯基苯酚(PVP)、聚氯乙烯(PVC)、醋酸纤维素(CA)、聚丙烯酰胺(PAA)、聚(乳酸-共-乙醇酸)(PLGA)、胶原、聚己内酯(PCL)、聚(甲基丙烯酸2-羟基乙酯)(HEMA)、聚(偏氟乙烯)(PVDF)、聚醚酰亚胺(PEI)、聚乙二醇(PEG)、聚(二茂铁基二甲基硅烷)(PFDMS)、聚(乙烯-共-乙烯醇)、聚乙烯基吡咯烷酮(PVP)、聚间苯二甲酰间苯二胺、聚丙烯(PP)、聚萘二甲酸乙二醇酯(PEN)、聚四氟乙烯(PTFE)、蜡、蜡状聚合物、聚烯烃、聚酯、聚砜和聚醚砜(PES)。
可使用固有地为亲水性的聚合物而没有进一步的处理。通过化学或物理后处理,或者通过在其表面上吸附两亲性物质,可使得不是亲水性的聚合物为亲水(吸湿)。通过类似的后处理可使得固有地亲水性的纤维更亲水以将亲水性和/或吸湿性调节到期望水平以用于特别的润滑剂和/或本教导的应用。
固有地亲水性的聚合物的实例包括,但不限于,丙烯酰胺类例如聚丙烯酰胺,丙烯酸类树脂例如聚丙烯酸,马来酸酐共聚物类,甲基丙烯酸酯,丙烯酸乙酯,胺官能聚合物例如聚烯丙基胺、乙烯亚胺、唑啉、和在其主链或侧链中含有胺基团的其它聚合物,醚,苯乙烯类例如聚苯乙烯磺酸盐和相关聚合物,乙烯基酸,和乙烯醇类例如聚乙烯醇。极性的但非水溶性的聚合物的实例为聚(乙烯基吡啶)。
优选的是在应用/使用条件下吸引水和/或其它亲水性物质并将它(它们)吸收到其纤维状网络中,使得不允许水和/或其它亲水性物质解离(溶解)或释放回到润滑流体中的聚合物或其变型。
PP和PA也是优选的且可通过合适的后处理适当地改性为亲水性的。
另外或替代地,得自天然或可生物降解来源的聚合物也适合用于制造可根据本教导利用的纤维。增加的益处是这样的聚合物中的许多是固有地亲水性的且可能不要求任何进一步的后处理以使得它们充分地亲水和/或吸湿以用于本教导的目的。这样的聚合物的代表性实例包括,但不限于,多糖例如纤维素、淀粉、甲壳质、壳聚糖、蛋白质、(多)肽和明胶。
当然,上述聚合物中的两种或更多种的混合物或共混物也是合适的。上述聚合物中的两种或更多种的所有可能的组合理解为被明确地列举以用于原始说明的目的。
在本教导的一个实施方式中,可将小分数(例如,0.1-5%)的一种类型的纤维添加到主要含有第二类型的纤维的润滑脂中以赋予所述润滑脂以特别的性质。例如,可将所述纤维设计成在升高的温度下熔化以形成润滑剂。另外或替代地,所述纤维可含有添加剂。另外或替代地,所述纤维可在润滑剂或润滑脂中提供结构功能。
可利用10:90-50:50的A:B比的两种类型的纤维A和B的混合物以赋予亲水性(例如,吸湿性)纤维状网络以独特的性质。
所述亲水性纤维可为最终材料的0.1-100重量%。更优选地,根据本教导的亲水性材料优选含有50-100重量%的亲水性纤维并且可为由所述纤维制成的织物或垫的形式,其可固定于在润滑体系内的位置并与润滑流体呈流体连通。
在本教导的另一优选的方面中,微米/纳米纤维网络可由天然地埋置、引入或吸收油或另外的合适的基础润滑流体的亲油性纤维制备,使得用于制造润滑剂的整个过程在很大程度上被简化。亲油性纤维可使用本质上固有地低成本的多种不同的现有方法由如上所述的多种不同的材料制造,且可如上所述调整或合适地选择所述纤维的长度/直径比、及其化学组成(本体或表面)。通过由本文中描述的亲油性纤维形成布、垫、织物、毡或海绵状网络或者通过将所述纤维适当地分散在合适的润滑剂中所得到的肥皂状或海绵状结构的构造也是可能的。
在本教导的另一方面中,布、垫、织物或毡材料可由多种不同的聚合物材料例如上述纤维材料制造。取决于所利用的聚合物和进行以改变布、垫、织物或毡材料的性质的任何制造后处理,所述布、垫、织物或毡材料可为亲水性的(例如,吸湿性的)或亲油性的。
在本教导的一个示例性实例中,亲油性织物或垫材料可设置在需要润滑的接触点(例如,滑动表面)处或附近以通过接触在润滑体系内的润滑流体(例如,油)而在接触点处现场(locally)形成增稠的润滑剂例如润滑脂或润滑脂状物质。另外,亲水性织物或垫材料可设置在与接触点(即在运行期间不需要润滑的在润滑体系内的位置)隔开但与润滑流体呈流体连通的位置处,以除去在润滑体系内的油或润滑流体中的任何水或其它亲水性物质。
另外,所述垫或织物材料也可使用包括在纤维状网络例如无纺纤维状网络的表面内或中的合适的润滑添加剂制造。这提供了在制造独特的低重量的结构体方面的灵活性,其仅需要在润滑体系内的方便位置中的布置,随后添加油或另外的基础润滑流体。可调整或合适地选择或处理所述纤维的性质以调节物理性质(例如,长度、直径、混合物等)和/或化学性质(表面处理,大块(bulk)材料、润湿行为等),该选择和/或处理使得所述纤维能够合适地适应于任何类型的润滑流体。
在另外的实施方式中,可将所述纤维切割到特定长度且因此所述纤维可以松散或可分散的状态利用。在用于制备在过去已是可得到的较短长度的纤维的另一方法中,可将由纤维制造的织物或布冻结,然后在它们处于脆性状态的同时将聚合物纤维粉碎。
这样的无纺纤维织物毡可例如通过熔喷微米或亚微米直径纤维、或者通过电纺丝制造。另外,可根据本教导有利地利用的纤维材料毡/布也可由商业来源例如Hills Inc.,W.Melbourne,Florida,U.S.A获得。
所述纤维网络可为有机的和/或无机的。可使所述纤维制造方法与非常大量的生产相适应。
所述纤维的直径优选在微米或纳米范围内,而所述纤维的长度优选在几到几十微米、最优选小于30微米(μm)的范围内。优选地,可避免纳米颗粒材料(即,长径比低例如约为1的纳米尺寸的颗粒),其可带来健康危害,这将限制其应用。
所述纤维直径为50nm-10μm,更优选100nm-1μm。此外,所述纤维具有为其直径至少5-10倍的长度。即,所述纤维优选具有至少5-10的长径比。可适当地调节所述纤维的长度以实现其结构性质、其机械稳定性和其本体(bulk)吸湿性质的期望的变化。因此,可优化所述纤维长度以用于特定的应用(使用)条件。
可制造和调整/调节用于所述纤维的基础材料以用于特定的应用。例如,所述基础材料也可作为布/织物材料或者预切割纤维的网络送至最终使用者。在这种情况中,最终使用者将仅需要添加油、润滑流体或润滑脂以制造具有水吸收能力的润滑剂体系。本教导的该方面提供大的灵活性程度,因为由于其低的重量(即,不同于相对重地油或润滑脂),所述基础材料可相对便宜地全球性运输。
根据本教导的亲水性纤维、由纤维制造的任何织物或网络状材料、润滑流体/油和/或增稠的润滑剂(例如,润滑脂)可包括一种或多种在润滑剂领域通常使用的已知添加剂。可包括所述添加剂以在下列方面向润滑剂提供特别的功能性:润滑剂的老化(例如,抗氧化剂)、减阻剂、抗磨损性质、抗极端压力性质等。
也可添加添加剂以通过使用合适的聚合物、蜡等将纤维连结或连接(例如,结合)以向润滑剂或润滑脂提供更强的结构。也可使用具有不同的性质的纤维作为添加剂。
其它合适的添加剂包括陶瓷颗粒(二氧化硅、氧化铝、氧化锆等)和金属颗粒。
所述添加剂可在制造所述纤维之前添加到聚合物本体基础物,但也可添加到干纤维。也可将少量的载体流体(非常合适的是具有或不具有添加剂的润滑剂)添加到干聚合物基础材料。然后可随后添加油或润滑流体以制造最终配方。
也可将所述添加剂添加到所述油,然后使其与所述纤维或纤维状材料(例如,由所述纤维制造的布/织物)接触。
在本教导的另一方面中,所述纤维本身可用作添加剂。例如,可将本文中公开的纤维添加到已知的润滑剂(例如,油、润滑脂和乳液)以改善其润滑和吸湿性能。
在本教导的另一方面中,可在相同的纤维中混合或合并不同的材料或材料性质,由此实现相分离和多相纤维。因此,可在单一的纤维中实现分化的或双重性能。这样的多性质或多相纤维可仿照具有两个脸的希腊神称作“JANUS纤维”。这样的多性质或多相纤维对于机械稳定性(当需要时)和亲水性材料的自愈能力的发展是高度有利的。即,在某种类型的破坏性机械作用(例如剪切)之后,纤维结构可优选再一次自愈(例如,重新自组装)成所需结构(网络)。
所述Janus纤维可根据多种方法制造。例如,可使所述纤维经历喷射处理、等离子体处理和/或沉积过程,其使一侧的纤维暴露。沉积材料可为金属,聚合物,小的陶瓷、金属或有机纳米颗粒,其在一侧例如经暴露的一侧埋置到所述纤维中或附着到所述纤维。这可在所述纤维的制造期间或者在其制造之后进行。所述沉积在经暴露的和未暴露的侧上产生具有不同性质的纤维。另一方式是平行制备两种不同类型的聚合物,然后使用现有的微米级挤出技术将它们成型为一种单一的纤维。这些有时被称作海中岛(Island-In-Sea)纤维,其中多个纳米或微米级(双组分)纤维在第三聚合物的基体中挤出。
本教导的另一方面涉及例如用于轴承、线性制动器、齿轮和任何其它机械座圈(滚道,raceway)、轨道或滑动表面的润滑体系。
例如,在这方面,可设置本教导的亲水性纤维,例如,将其附着到表面上或埋置/引入到表面中,以与设备例如轴承的座圈、齿轮或线性设备(马达)的滑动表面流体连通,以形成纤维的沉积物,其为接触到所述纤维的沉积物的润滑流体(例如,油)提供除水功能。然而,所述亲水性纤维优选不设置在位于需要润滑的设备内的接触/摩擦点处,以使已被所述亲水性材料吸收的任何水由于在接触点(即在设备的运行期间需要润滑的表面)存在的高压和/或高温条件而被释放回到润滑流体的可能性最小化。
所述纤维也可作为防腐措施应用以提供机械部件的更好的耐长期存储性。本教导的该特征提供在油润滑的体系(例如,如工业齿轮箱)中的脱水功能。因为该效果是原位实现的,其导致更长的使用寿命和水和/或其它亲水性物质从润滑流体的现场消除。
现在将在下面更详细地描述本教导的各种实施方式、特征和优点。
水吸收功能性
可熔体纺丝的纤维可具有非常不同的化学性质。例如,它们的行为也可调整为非常亲水的且在这种情况中,所述纤维将呈现非常高的对水的亲和性。这样的吸湿性纤维能够有利地消除(吸收)润滑体系中的任何游离水以及任何解离的水。如果置于密封件(seal)之中或之上,它们可担当用于工业润滑剂的主动水除去手段。
如将在下面进一步讨论的,这样的体系的一个特别有利的实例是其中密封件能够吸附水(否则该水对轴承体系将是非常有害的)的密封轴承。水可导致润滑剂的腐蚀和/或水解,例如,导致提早失效。
因此,在本教导的一些方面中,除了上述亲油性纤维之外或者代替上述亲油性纤维,亲水性和/或吸湿性纤维可设置在密封件的表面上。
固体润滑剂或固体油
过去,已知的“固体油”产品是通过将聚合物基体用油饱和而制造的。这样的固体油具有最高达70%的油含量,但是比润滑用润滑脂的通常情况硬得多。由于相对刚性的机械结构,它们可提供比润滑脂多的支持,而相对高的油含量提供比通过纯的聚合物材料可实现的更好的润滑。
纤维增稠的润滑脂可利用根据本教导的亲油性纤维制备,使得其具有可与已知的固体油和类似材料相比的刚度且因此具有相同的功能性。然而,在本教导的该方面中,与已知的固体油相比,也可改善性能,因为所述亲油性纤维本身也可用作润滑剂,即,所述亲油性纤维补充所述基础油的润滑性质。例如,在这样的实施方式中,纤维状材料在运行期间可折断,由此增大官能表面和所述“润滑脂”之间的间隙,这使摩擦减小。如果润滑纤维开始接触,它们可提供另外的润滑。
另外,通过调整目前的纤维的亲油性质,例如,通过对所述纤维进行涂覆或处理,可调整所得润滑脂的油渗析(bleed)速率,例如,以用于各种轴承应用。通过使用根据本教导的非常粘稠的纤维增稠的润滑脂制造固体油,可容易地配制不同的固体油产品以用于不同的轴承类型/运行条件。
这样的固体油优选具有聚合物纤维的基础材料的硬度的1%-100%的硬度值。
根据本教导的亲水性纤维或纤维状材料优选设置成与所述固体油呈流体连通以例如在润滑体系的运行期间从所述固体油除去水。由于所述固体油的类似固体的性质,在所述体系内布置多个亲水性纤维或亲水性材料的局部沉积物(例如,织物或垫)以提供充足的吸湿功能性可能是必需的。
增稠的润滑剂
在本教导的另一方面中,润滑剂以增稠的油和润滑脂的形式提供。更具体地,润滑流体或油优选可使用根据本教导的亲油性纤维增稠。然而,应理解,本亲水性纤维和由其制造的亲水性材料可对可用常规的皂材料或任何其它已知的润滑剂增稠剂增稠的多种润滑剂利用。
根据本教导的该方面,尽管最适当的稠度通常是通过增稠的润滑剂的应用或使用而测定的,但是NLGI等级或稠度(由National Lubricating GreaseInstitute设立或确定的标准)优选等于或大于00。更优选地,根据本教导的润滑剂可具有1-3,例如为2的稠度或NLGI等级。这样的增稠的润滑脂特别适合用在轴承中。
如果利用松散的亲油性纤维对润滑剂进行增稠,所述亲油性纤维在增稠的润滑剂中的最佳密度将取决于润滑剂用于特定应用的所需粘度和稠度、以及用于对润滑流体或油进行增稠的纤维的长度和直径。然而,注意,纤维增稠的润滑剂的优选的亲油性纤维重量密度(基于总的润滑剂重量)通常为约0.1-20%。纤维增稠的‘润滑脂’的优选纤维密度通常为约2-15%、更优选约5-12%。但是,在所述亲油性纤维连同其它增稠剂一起使用的情况中,纤维含量可相应降低。
此外,根据本教导的亲水性纤维可设置成与增稠的润滑剂呈流体连通以从基础润滑流体例如油中除去水。
改善的贮存期
当润滑脂长期存储在例如桶中时,油分离典型地发生。在这种情况中,油作为在润滑脂顶部的油层变得可见。通常,油比皂或其它增稠材料轻或不及皂或其它增稠材料致密,所以油漂浮在剩余的润滑脂上。该分离现象统治所述润滑脂的“贮存期”,即,在使用之前所述润滑脂可安全地存储的时间量。‘存储中(on the shelf)’的油的释放因此是不期望的,且这提出了挑战,因为润滑脂必须能够渗析充足的油以在运行期间用作良好的润滑剂。因此,需要适当地平衡贮存期和在使用期间的充足的渗析特性。
根据本教导的亲油性纤维增稠的润滑脂可以被制备成呈现较长的贮存期。特别地,可控制两个参数以影响贮存期。
首先,渐进性结构变化影响增稠剂(纤维)结构。这些受到所述结构保持油的能力的影响且因此受到油与所述结构之间的亲和性的影响。高度亲油性结构比疏油性结构更好地保持油。此外,如本说明书中的别处所描述的,所述结构的稳定性可优化。
其次,增稠材料在油中的浮力也影响贮存期。可设计增稠剂使得比质量(密度)几乎等于所述润滑脂中包含的油或润滑流体的比质量(密度)。在这种情况中,所述油或润滑流体不太能够漂浮在剩余的润滑脂的顶部,因为它们具有相等或基本上相等的比质量。
另外或替代地,可对纤维进行涂覆或处理或者因此以将所述基础油保持在所述纤维网络(亲油性质)内更长时间的方式进行选择。
所述纤维的亲油性可根据表面科学领域中已知的多种技术确定。例如,如上所述,油滴或润滑流体滴在与所述纤维相同的材料的光滑平坦的表面上的接触角可提供所述纤维的亲油性的一种指示。在这种情况中,内接触角越低或越浅,所述材料越亲油。当内接触角非常浅时,称所述油‘润湿’所述材料。用于指示亲油性的另一方法是测定由所述纤维制造的布或其它结构体(例如,织物)可吸收的油的体积。
此外,根据本教导的亲水性纤维可设置成与润滑剂呈流体连通以在润滑剂的存储期间除去水,由此进一步提高其贮存期。所述纤维可沉积例如在含有所存储的润滑剂的桶或槽的壁或其它表面上。
亲水性纤维网络
可设计根据本教导的亲水性聚合物纤维网络使得其将固体添加剂颗粒保持在所述纤维网络中且不受对所述纤维本身进行的任何处理的影响。这些颗粒的尺寸可为纳米、微米或介观(meso)级。具有数十微米的数量级的尺寸的颗粒称作介颗粒(mesoparticle)。在本教导的该方面中,可提供在所述纤维网络中的粒状“添加剂贮存所(reservoir)”的保持。
在“结构形成”(即纤维网络制造)过程中,可添加具有抗磨损性质(例如,通过掺混不溶解的二烷基二硫代磷酸锌,ZDDP)、抗摩擦或摩擦减小性质(例如,通过掺混MoS2、WS2和/或PTFE的一种或多种)、抗氧化性质和/或抗腐蚀性质的纳米、微米和介观级颗粒作为成分。还可将抗腐蚀添加剂和防腐剂引入到所述纤维网络中。
另外或替代地,如果处理纤维使得一些添加剂附着到其上,将得到引入所需的添加剂/化学性质的纤维结构。即,在润滑体系中存在所需要的或所期望的一种或多种性质,只要在所述润滑体系中含有所述纤维例如作为网络或作为悬浮体/分散体(例如糊)。
包括根据本教导的纤维的轴承和/或密封件
在本教导的另一方面中,根据本教导的纤维(例如,具有通常为约50nm~10μm的长度的亲水性纤维)可附着到或者引入到例如轴承或轴封的密封件、密封唇(seal-lip)或密封唇双层中,以吸收在用于轴承或轴封的润滑剂内的任何水或其它亲水性物质。
附图显示本教导的代表性轴承应用。在该示例性实施方式中,多个球轴承1(为了清楚的目的仅示出了一个)可移动地设置在轴承的两个环2(即外环和内环)之间。球轴承1可在环2中界定的各个轨道或座圈内导向。密封件3可设置在所述轴承的相反轴末端上以在所述轴承内界定密闭或密封的空间以保持润滑剂,例如适合用于轴承应用的润滑脂。
密封件3可由橡胶和/或弹性体聚合物,例如,腈橡胶(NBR)和聚氨酯(PU)材料制造,并且可根据本领域中已知的任何合适的技术制造。原则上,也可使用其它材料。
密封件3任选地可为多孔的以在其表面中界定贮油所(oil reservoir)。用于制造这样的多孔密封件3的一个代表性实例是在模塑之前向弹性体混合物中添加盐例如NaCl或CaCO3。在模塑该密封件之后,使用水溶液从密封唇中洗出所述盐,由此在能够于所述密封件的运行期间吸收、保持和/或存储油的表面中产生孔。
在优选实施方式中,然后可以通过使根据本教导的亲油性纳孔或微孔纤维网络附着到所述密封件材料,例如,附着到上述孔而制造油溶胀的多孔网络。附着力优选足够强以提供充足的抗磨损性。这可通过使用本领域中公知的合适的附着化学方法实现。该多孔网络也可附着到密封件对立面(相反)表面。
在另一实施方式中,较厚的包括根据本教导的纤维的‘垫’状结构(例如,布、织物、垫、毡等,如上面所讨论的)可附着到所述密封件或附着到对立面表面上。
在另一实施方式中,可利用油溶胀的纤维状网络和通常使用的密封件材料的多相混合物以将油溶胀的结构的小口袋(pocket)引入到所述密封件(或对立面)结构中。
由于仅在密封唇附近需要(一个或多个)贮油所,因此表面层(衬里)可为多孔的且可与标准密封件材料(例如NBR)组合。如果所述两种材料是相同的(例如,NBR或PU两者),它们在交联步骤期间可更容易地结合在一起。这在摩擦力向结合层施加应力时防止可能出现在该层中的粘附问题。
可将根据本教导的一种或多种亲水性材料4设置成优选与在部分地由密封件3界定的密封空间内的润滑剂呈流体连通。例如,亲水性垫4可设置例如附着到不接触球轴承1的轴承的环2之一或两者的一部分、密封件3的辐射状延伸的内部部分、或密封唇的非接触侧。亲水性材料4也可设置在密封空间的外部,例如密封件3的辐射状延伸的外部部分。
以这种方式,亲水性材料4与润滑剂例如润滑脂呈流体连通,且可在存储和/或轴承的运行期间有效地除去水和/或其它亲水性物质。
自然,本教导不限于球轴承,但可以任何类型的轴承利用,包括但不限于,圆柱形轴承、圆锥形轴承、球形轴承,等。
而且,本教导通常可应用于利用润滑剂(其在存储或运行期间可能变得被水或其它亲水性物质污染)的任何类型的系统或设备,包括但不限于可转动轴和轴封、齿轮箱、线性制动器等。
利用熔体纺丝过程施加到表面的亲水性纤维
替代将纤维状材料例如垫或织物附着到与润滑剂呈流体连通的表面,可使用熔体纺丝过程将根据本教导的亲水性纤维直接施加到金属导体的表面上,由此导致原位沉积和使用所述亲水性纤维的非常有成本效益的方式。所述纤维可直接喷射到生产线中的轴承环或密封件表面,然后让其冷却。该制造步骤可以不同方式进行,例如,通过控制喷射速度和目标表面的旋转速度两者。该过程产生涂覆在将吸附水的表面上的纤维。在一个实施方式中,使用将纤维直接施加到目标物体上的熔喷技术制造纤维。在替代性实施方式中,电纺丝过程可用于非常精确的纤维生产和至金属物体上的沉积控制。
在其一个实施方式中,所述纤维可起到轴承的防腐剂(防止腐蚀的物质)的作用。所述亲水性纤维(例如,根据上述的喷射(spray-on)方法施加的)可用于从润滑体系除去水。
这同样适用于根据在前的实施方式的导电密封件。
如果密封件聚合物不是导电性的,另一选择是使用过度冷却效应使得重叠模塑(overmolding)是可能的。
自生(self-generating)和自组装润滑脂
本教导的另一方面涉及使得油能够在润滑体系内泵送或除去,但是其中移动部件用润滑脂润滑的实施方式,例如在齿轮箱中。
在本教导的该方面的一个实施方式中,亲油性聚合物纤维增稠剂和油可单独地喷射在轴承内部以在轴承内部形成自生润滑脂。为了该目的,可将聚合物纤维加工成例如粒料或颗粒。随后可将油例如作为细的油雾单独地喷射到轴承中。所述油和聚合物纤维颗粒然后原位(再)组合以形成润滑脂。
在另一实施方式中,所述纤维可例如通过熔喷或电纺丝制造,然后沉积到齿轮、齿轮箱、轴承等的表面上。油单独地添加,或者刚好在施加到机械系统之前添加。
该实施方式的一个优点是油的泵送比稠润滑脂的泵送更容易(能量密集程度小),因为油的粘性较小。因此,可降低能耗而不牺牲润滑性能。
该实施方式的另一优点是可充分地控制润滑脂在轴承内部例如在壳体上、或者在滚动接触中的分布。
另一优点是取决于再润滑需要和运行条件的润滑脂配方的完全自由度和可变性。
另一优点是轴承可以用油润滑以确保滚动接触的补给,其中过量的油以润滑脂的形状和形式被吸附。
另一优点是所述亲水性材料可设置在润滑体系内的多种位置处。例如,所述亲水性材料可任选地设置在泵或过滤器附近且不需要在物理上位于需要润滑的设备内。
沉积在表面上的纤维
在上述的其中纤维沉积到与润滑剂呈流体连通的表面上(例如,附着到该表面上、埋置或引入在该表面中等)的实施方式的任一个中,所述纤维的厚度可为一个单层到数十层直到数百个层的纤维(或织物材料)。特别优选的范围为1-50层、更优选2-20层。
本文中公开的本教导的另外的实施方式包括,但不限于:
1.润滑脂,其包含油和/或润滑流体和具有在微米范围内的长度和在微米或纳米范围内的直径或宽度的增稠纤维,所述纤维是亲油性的。
2.根据实施方式1的润滑脂,其中所述纤维包含至少两个具有不同物理和/或化学性质的部分(portions)。
3.根据实施方式2的润滑脂,其中所述部分中的至少一个对类似部分的亲和性高于对所述油和/或润滑流体的亲和性,由此赋予所述增稠纤维以自组装性质。
4.根据前述实施方式中任一项的润滑脂,其中所述纤维具有100-500μm的长度。
5.根据实施方式4的润滑脂,进一步包含具有1-100μm的长度的亲油性增稠纤维。
6.根据前述实施方式1-3中任一项的润滑脂,其中所述纤维具有1-100μm的长度。
7.根据前述实施方式中任一项的润滑脂,其中所述纤维具有为其直径的至少约5-10倍的长度。
8.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维为有机纤维例如聚丙烯和无机物例如陶瓷例如氧化铝和/或二氧化硅的混合物。
9.根据前述实施方式中任一项的润滑脂,其中所述纤维也具有疏油和/或亲水性质。
10.根据前述实施方式中任一项的润滑脂,进一步包含具有疏油和/或亲水和/或吸湿性质的非亲油性纤维。
11.根据前述实施方式中任一项的润滑脂,其中所述纤维是可生物降解的。
12.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维包括纤维素和/或树胶。
13.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维用比所述增稠纤维更为极性的组合物涂覆,例如,无规涂覆。
14.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维包括Janus纤维。
15.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维由至少一种极性聚合物例如聚环氧乙烷(PEO)和至少一种非极性聚合物例如聚苯乙烯(PS)或聚丙烯(PP)构成。
16.根据实施方式15的润滑脂,其中所述纤维为嵌段共聚物。
17.根据前述实施方式中任一项的润滑脂,其中所述纤维对钢和/或聚合物表面具有强的亲和性。
18.根据前述实施方式中任一项的润滑脂,其中所述纤维形成海绵状网络,该海绵状网络吸收或保持所述润滑流体或油。
19.根据实施方式18的润滑脂,其中所述海绵状网络具有以下性质:其随着温度升高而收缩或紧缩,由此挤压出润滑流体或油。
20.根据前述实施方式中任一项的润滑脂,其中所述润滑脂包含至少两种类型的增稠纤维,其各自具有不同的熔融温度。
21.根据实施方式20的润滑脂,其中当使所述润滑脂达到高于所述增稠纤维的熔融温度的温度时,至少具有最低熔融温度的增稠纤维担当润滑剂。
22.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维由蜡形成和/或进一步包含蜡。
23.根据前述实施方式中任一项的润滑脂,进一步包含低分子量聚合物例如蜡,其交联具有较高分子量的增稠纤维。
24.根据实施方式22或23的润滑脂,其中所述蜡为天然蜡或烃蜡。
25.根据实施方式24的润滑脂,其中所述蜡为蜂蜡或石蜡。
26.根据前述实施方式中任一项的润滑脂,其中所述增稠纤维为增粘剂或进一步包含增粘剂。
27.根据前述实施方式中任一项的润滑脂,其中选择所述增稠纤维和所述润滑流体或油,使得当所述增稠纤维接触所述润滑流体或油时,所述增稠纤维能够自生纤维状海绵状网络。
28.根据前述实施方式中任一项的纤维(即不具有油或润滑流体),其优选构成最终材料的约0.1-100重量%、更优选约50-100重量%。
29.涂覆有根据实施方式28的纤维或者具有根据实施方式28的纤维埋置或引入到其中的轴承表面,所述轴承表面优选包含钢。
30.涂覆有根据实施方式28的纤维或者具有根据实施方式28的纤维埋置或引入到其表面中的密封件,所述密封件任选地包含设置在所述密封件中的弹性体材料例如NBR或聚氨酯和/或蜡纤维。
31.涂覆有根据实施方式28的纤维或者具有根据实施方式28的纤维埋置或引入到其表面中的轴承壳体(cage),所述壳体优选包含钢或聚酰胺。
32.分别根据实施方式29-31的轴承表面或密封件或轴承壳体,其分别具有在所述轴承表面或密封件表面或壳体表面中界定的多个贮油所,所述纤维和贮油所至少位于在运行期间相对于彼此移动的两个部件之间的初级(primary)接触点。
33.分别根据实施方式29-31的轴承表面或密封件或轴承壳体,其具有多孔表面结构和/或已被化学处理的表面结构以导致在规定的运行条件下润滑流体或油从所述润滑脂释放。
34.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述亲油性增稠纤维具有约50nm~10μm、和更优选约100nm~1μm的直径。
35.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述油和/或润滑流体包含以下的一种或多种:由原油获得的矿物油,I、II类和III类润滑剂,IV类润滑剂(聚α-烯烃“PAO”)和V类润滑剂(所有其它的)。
36.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述油和/或润滑流体包括以下的一种或多种:矿物油、合成酯、以及基于植物的油和它们的衍生物,例如得自油菜籽、低芥酸菜籽、向日葵、低芥酸菜籽和棕榈的油。
37.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述油和/或润滑流体包括以下的一种或多种:基于动物的油、它们的衍生物和合成润滑剂例如聚乙二醇(PG)、聚亚烷基二醇(PAG)、白油、硅油、很高粘度指数油(VHVI)、水、甘油和蜡。
38.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述油和/或润滑流体具有在40℃下约1~1000cSt的粘度。
39.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述纤维包括已被纺成纤维的聚合物材料。
40.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述纤维包括以下的一种或多种:聚酰胺(PA)、尼龙6,6、聚酰胺-6,6(PA-6,6)、聚酰胺-4,6(PA-4,6)、聚氨酯(PU)、聚苯并咪唑(PBI)、聚碳酸酯(PC)、聚丙烯腈(PAN)、丙烯腈橡胶(NBR)、聚乙烯醇(PVA)、聚乳酸(PLA)、聚乙烯-共-醋酸乙烯酯(PEVA)、PEVA、聚甲基丙烯酸酯(PMMA)、四氢全氟辛基丙烯酸酯(TAN)、聚环氧乙烷(PEO)、胶原-PEO、聚苯胺(PANI)、聚苯乙烯(PS)、具有纤连蛋白官能性的丝状聚合物、聚乙烯基咔唑、聚对苯二甲酸乙二醇酯(PET)、聚丙烯酸(PAA)、聚丙烯甲醇(PM)、聚乙烯基苯酚(PVP)、聚氯乙烯(PVC)、醋酸纤维素(CA)、聚丙烯酰胺(PAAm)、PLGA、胶原、聚己内酯(PCL)、聚(甲基丙烯酸2-羟基乙酯)(HEMA)、聚(偏氟乙烯)(PVDF)、聚醚酰亚胺(PEI)、聚乙二醇(PEG)、聚(二茂铁基二甲基硅烷)(PFDMS)、聚(乙烯-共-乙烯醇)、聚乙烯基吡咯烷酮(PVP)、聚间苯二甲酰间苯二胺、聚丙烯(PP)、聚萘二甲酸乙二醇酯(PEN)、聚四氟乙烯(PTFE)、蜡、蜡状聚合物、聚烯烃、聚酯和聚砜。
41.根据前述实施方式中任一项的润滑脂、纤维、密封件或轴承壳体,其中所述纤维包括得自天然或可生物降解来源的一种或多种聚合物,例如,多糖例如纤维素、淀粉、甲壳质、壳聚糖、蛋白质、(多)肽和明胶。
已经在最广泛的意义上结合对于实践本发明可能不是必需的特征和步骤在上面描述了优选实施方式和示例性实例,这样的详细组合仅出于具体描述本发明的代表性实例的目的进行描述。此外,以上描述的代表性实例的各种特征、以及各独立和从属权利要求可以不具体和明确列举的方式组合以提供本教导的另外的有用的实施方式。
说明书和/或权利要求中公开的所有特征、油、基础润滑流体、材料、聚合物、纤维、添加剂等意图彼此单独地和独立地公开以用于原始书面公开的目的、以及用于独立于实施方式和/或权利要求中的特征的组合而限制所要求保护的主题的目的。
另外,所有数值范围或实体组的指示意图公开每一个可能的中间数值或中间实体以用于原始的书面公开的目的、以及用于限制所要求保护的主题的目的。
Claims (23)
1.用于对润滑体系使用的亲水性组合物,其包含直径为50nm-10μm且长度为直径至少5倍的亲水性纤维,所述亲水性纤维对水和/或其它亲水性流体具有强的亲和性。
2.根据权利要求1的亲水性组合物,其中所述亲水性纤维设置在装置的元件(2,3)的表面上,该表面与润滑流体例如油呈流体连通,但与所述装置的任何摩擦接触表面间隔开。
3.根据权利要求2的亲水性组合物,其中所述亲水性纤维埋置到所述表面中或者物理引入到所述表面中。
4.根据权利要求2的亲水性组合物,其中所述亲水性纤维附着到所述表面。
5.根据权利要求2-4中任一项的亲水性组合物,其中所述表面为密封件(3)的表面,所述密封件(3)任选地由弹性体材料例如NBR或聚氨酯构成。
6.根据权利要求2-4中任一项的亲水性组合物,其中所述表面为轴承环(2)的表面,所述轴承环任选地由钢构成。
7.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维具有100nm~1μm的直径。
8.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维至少实质上包括吸湿性纤维。
9.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维为布、垫、织物或毡的形式。
10.根据权利要求9的亲水性组合物,其中所述亲水性纤维为无纺材料的形式。
11.根据前述权利要求中任一项的亲水性组合物,其中所述润滑体系包括选自以下的一种或多种的油和/或润滑流体:
由原油获得的矿物油,
I类、II类和III类润滑剂,IV类润滑剂,和
V类润滑剂。
12.根据权利要求11的亲水性组合物,其中所述油和/或润滑流体包括以下的一种或多种:矿物油、合成酯、以及基于植物的油和它们的衍生物,例如得自油菜籽、低芥酸菜籽、向日葵、低芥酸菜籽和棕榈的油,优选包括以下的一种或多种:矿物油、合成酯、PAO和合成烃。
13.根据权利要求11或12中任一项的亲水性组合物,其中所述油和/或润滑流体包括以下的一种或多种:基于动物的油、它们的衍生物和合成润滑剂例如聚乙二醇(PG)、聚亚烷基二醇(PAG)、白油、硅油、很高粘度指数油(VHVI)、水、甘油和蜡。
14.根据权利要求11-13中任一项的亲水性组合物,其中所述油和/或润滑流体具有在40℃为1~1000cSt、更优选在40℃为10~300cSt的粘度。
15.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维包括已被熔体纺丝成纤维的聚合物材料。
16.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维包括以下的一种或多种:聚酰胺(PA)、尼龙6,6、聚酰胺-6,6(PA-6,6)、聚酰胺-4,6(PA-4,6)、聚氨酯(PU)、聚苯并咪唑(PBI)、聚碳酸酯(PC)、聚丙烯腈(PAN)、丙烯腈橡胶(NBR)、聚乙烯醇(PVA)、聚乳酸(PLA)、聚乙烯-共-醋酸乙烯酯(PEVA)、PEVA、聚甲基丙烯酸酯(PMMA)、四氢全氟辛基丙烯酸酯(TAN)、聚环氧乙烷(PEO)、胶原-PEO、聚苯胺(PANI)、聚苯乙烯(PS)、具有纤连蛋白官能性的丝状聚合物、聚乙烯基咔唑、聚对苯二甲酸乙二醇酯(PET)、聚丙烯酸(PAA)、聚丙烯甲醇(PM)、聚乙烯基苯酚(PVP)、聚氯乙烯(PVC)、醋酸纤维素(CA)、聚丙烯酰胺(PAAm)、PLGA、胶原、聚己内酯(PCL)、聚(甲基丙烯酸2-羟基乙酯)(HEMA)、聚(偏氟乙烯)(PVDF)、聚醚酰亚胺(PEI)、聚乙二醇(PEG)、聚(二茂铁基二甲基硅烷)(PFDMS)、聚(乙烯-共-乙烯醇)、聚乙烯基吡咯烷酮(PVP)、聚间苯二甲酰间苯二胺、聚丙烯(PP)、聚萘二甲酸乙二醇酯(PEN)、聚四氟乙烯(PTFE)、蜡、蜡状聚合物、聚烯烃、聚酯、聚砜和聚醚砜(PES)。
18.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维包括得自天然或可生物降解来源的一种或多种聚合物,例如,多糖例如纤维素、淀粉、甲壳质、壳聚糖、蛋白质、(多)肽和明胶。
19.根据前述权利要求中任一项的亲水性组合物,其中所述亲水性纤维包括至少两个具有不同的物理和/或化学性质的部分。
20.一种装置,其包括:
至少两个处于彼此滑动和/或滚动接触的摩擦接触表面,
用于减小在所述摩擦接触表面处的摩擦的润滑流体,和
与所述润滑流体呈流体连通的根据前述权利要求中任一项的亲水性组合物。
21.根据权利要求20的装置,其中所述装置为轴承且所述亲水性组合物设置在至少一个与由滚动元件(1)和轴承环(2)界定的摩擦接触表面间隔开的位置处。
22.根据权利要求21的装置,其中所述亲水性组合物设置在所述轴承环(2)中的至少一个的表面上和/或密封件(3)的表面上,该表面不是摩擦接触表面。
23.用于吸收或除去润滑体系中的水或其它亲水性物质的方法,包括:
将根据权利要求1-19中任一项的亲水性组合物设置成与油和/或润滑流体呈流体连通,和
使所述亲水性组合物与所述油和/或润滑流体中的游离水和/或解离的水接触,由此所述亲水性组合物从所述油和/或润滑流体吸收或除去所述水或其它亲水性物质。
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EP2633016A1 (en) | 2013-09-04 |
EP2633014A1 (en) | 2013-09-04 |
EP2633013A1 (en) | 2013-09-04 |
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US20130302609A1 (en) | 2013-11-14 |
WO2012055882A1 (en) | 2012-05-03 |
US20130256065A1 (en) | 2013-10-03 |
CN103189485A (zh) | 2013-07-03 |
CN103180421B (zh) | 2015-07-22 |
US20130256064A1 (en) | 2013-10-03 |
CN103180421A (zh) | 2013-06-26 |
CN103282472A (zh) | 2013-09-04 |
WO2012055821A1 (en) | 2012-05-03 |
CN103180420A (zh) | 2013-06-26 |
EP2633015A1 (en) | 2013-09-04 |
CN103282472B (zh) | 2016-03-16 |
US9371498B2 (en) | 2016-06-21 |
WO2012055823A1 (en) | 2012-05-03 |
US20130274159A1 (en) | 2013-10-17 |
WO2012055827A1 (en) | 2012-05-03 |
WO2012055825A1 (en) | 2012-05-03 |
EP2633106A1 (en) | 2013-09-04 |
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