CN108350228A - 橡胶和包括由橡胶材料制备的内管的液压软管 - Google Patents
橡胶和包括由橡胶材料制备的内管的液压软管 Download PDFInfo
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- CN108350228A CN108350228A CN201680055632.5A CN201680055632A CN108350228A CN 108350228 A CN108350228 A CN 108350228A CN 201680055632 A CN201680055632 A CN 201680055632A CN 108350228 A CN108350228 A CN 108350228A
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- rubber
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Abstract
本发明涉及用于橡胶的固化组合物,其包含选自二丙烯酸锌和甲基丙烯酸锌的金属助剂、有机过氧化物、硫和水滑石化合物。本发明还涉及通过使用该固化组合物制备的未固化的和固化的橡胶组合物以及用于固化该未固化橡胶组合物的方法。而且,本发明还涉及由该橡胶制成的液压软管。
Description
本专利申请涉及一种固化组合物、一种包含该固化组合物的未固化橡胶组合物、一种可通过固化未固化橡胶组合物获得的固化橡胶和一种用于固化未固化橡胶组合物的方法。最后,其涉及一种包括由固化橡胶制备的内管的液压软管。
液压软管将压力下的流体从一个位置传送到另一位置。一般而言,软管由一种材料或多种不同材料的组合制成。使用的软管材料主要取决于软管需要的应用和性能。一些常用材料包括尼龙、聚氨酯、聚乙烯、PVC或合成橡胶或天然橡胶。为了实现更好的耐压性,软管可以用纤维或不锈钢丝增强。一些常用的增强方法包括编织、螺旋、针织和包裹。软管的变化可能是由于其尺寸、额定温度、重量、增强层的数量、增强层的类型、额定工作压力、柔韧性和经济性。
通常,液压软管可被描述为主要由橡胶和钢的交替层制备的复合结构。例如,软管可以主要由三层,即,管、增强件和覆盖件构成。
液压软管用于各种行业,如石油和天然气钻探、农业、建筑、采矿设备、重型机械、家用电器等。液压软管由于各种因素,如拖拉、磨损、由于多平面弯曲导致的金属丝层扭曲、操作条件等失效。软管的操作条件决定其使用寿命。例如,极端温度加速老化,频繁和极端的压力波动加速软管的疲劳寿命。
例如,运行时间/停机时间在采矿段起主要作用。在采矿中,典型的软管组件持续约从3000小时到8000小时,内管变脆并且不再起作用。这意味着1至2年的应用,但有很大的差异,意味着软管可能有时甚至更早失效,意味着露天矿挖掘机的停机时间。如果露天矿挖掘机停机,则整个矿井停工。
用于增加软管在上述应用领域中的最大使用时间的一种方法是制备长期暴露于热、油和化学品之后具有物理强度和性能保持两者的氢化丁腈橡胶(HNBR)内层。
但是,HNBR具有高的蠕变趋势。此外,HNBR非常昂贵。
因此,需要为液压软管应用提供改善的橡胶组合物。
已通过提供根据权利要求1的用于橡胶的固化组合物、根据权利要求2的未固化橡胶组合物、根据权利要求9的固化的橡胶组合物、根据权利要求10的包括由固化的橡胶组合物制备的管的液压软管和根据权利要求13的用于制备固化的橡胶组合物的方法实现上述目的。
根据本发明的第一方面,提供一种用于橡胶的固化组合物,其包含:
-选自二丙烯酸锌和甲基丙烯酸锌及其混合物的金属助剂
-有机过氧化物
-硫
-水滑石化合物。
上述固化组合物是包含上述金属助剂以及有机过氧化物和硫的混合体系。这种组合在橡胶基体中产生两种不同类型的键,导致固化的橡胶组合物的改善的物理特性。例如,这允许制备新的NBR(丙烯腈丁二烯橡胶)内管,其适合用于具有合理成本并且在冲击测试中在高压和高温条件下表现极好的液压软管。根据本发明的固化组合物中的这些固化剂的组合提供了苛刻应用中液压软管所需的最佳性能。
应注意的是,单独用有机过氧化物进行交联将导致形成共价键,如图1中所示。这种碳-碳键非常刚性和稳定,并且解释了与硫硫化橡胶相比过氧化物固化原料更低的拉伸强度和撕裂强度的原因。这种共价键的良好热稳定性也解释了过氧化物固化体系的优异热老化特性。相比之下,如图2中所示的在硫固化中形成的(多)硫化物交联是热弱性的,但在应力下是可移动的并且可以沿烃链滑动。这种可移动性已被用于解释硫固化材料优异的拉伸强度和撕裂强度。然而,当暴露于热时,硫固化橡胶易降解。
与之相比,不受具体理论的限制,据信金属助剂-过氧化物交联键是“离子的”,如图3中所示。该离子键表现出良好的热老化稳定性和沿烃链滑动和重整(reform)的能力两者。因此,该体系体现了过氧化物和硫交联体系两者的特性,提供高拉伸强度和撕裂强度以及优异的热老化性能。
通常用于橡胶或塑料工业的有机过氧化物可用作本发明的第一方面的固化组合物中的有机过氧化物。一般地,有机过氧化物选自过氧化二异丙苯、二叔丁基过氧化物、叔丁基枯基过氧化物、氢过氧化枯烯、过氧化苯甲酰、过氧化2,4-二氯苯甲酰、2,5-二甲基-2,5-二(叔丁基过氧基)己炔-3、1,1-二(叔丁基过氧基)-3,3,5-三甲基环己烷、过氧苯甲酸叔丁酯、2,5-二甲基-2,5-二(过氧化苯甲酰)己烷和1,3-二(叔丁基过氧异丙基)苯及其混合物。优选使用过氧化二异丙苯、过氧化苯甲酰或其混合物。由于其合理的价格和可得性,过氧化二异丙苯是最优选的。
金属助剂选自二丙烯酸锌和甲基丙烯酸锌及其混合物。这些金属助剂在各种橡胶和未处理的金属基板之间产生极强的粘附键(adhesive bond)。金属助剂容易复合到橡胶原料中,其中当用过氧化物固化时它们交联到橡胶中。因此,它们起到粘合促进剂以及交联剂的作用以增强固化橡胶的粘合性能和机械性能两者。二丙烯酸锌是最好的粘合助剂,但是除了粘合之外,需要进一步改善的耐磨性和撕裂强度时,甲基丙烯酸锌是好的替代品。
根据本发明的固化组合物另外包含硫。通过添加硫,提高固化橡胶的拉伸强度和撕裂强度。另外,改善与未处理的金属表面的粘合。金属丝粘合(wire adhesion)极其重要,因为其导致容易组装,并且许多理论也表明其有助于在施加脉冲时实现有效的负荷传递。对于涂覆黄铜的钢丝尤其如此。不受具体理论的限制,据信后面的技术效果是由于固化橡胶与在黄铜(CuZn)涂覆的钢的顶部上形成的CuS层的硫键的缠结。因此,可通过使用根据本发明的第一方面的固化组合物获得的固化橡胶非常适合用于制造液压软管,其中由通过根据本发明的第一方面的固化组合物固化的橡胶制成的最内层直接接触由涂覆黄铜的钢制成的增强层。结果,这种液压软管表现出很小的蠕变,并增强了寿命。
最后,根据本发明的第一方面的固化组合物还包含用于不可逆酸清除的水滑石化合物。在俄罗斯和挪威,以其天然存在的形式小量开采水滑石。以商业量制备的合成形式一般地可由式(I)描述:
Mg(1-x)Alx(OH)2(CO3)x/2·nH2O;0.25<x<0.33。(I)
因此,如式(I)所述的合成水滑石可以包括给定x范围的各种化合物的混合物。合成形式的水滑石可以从多种来源获得,包括来自Kyowa Chemical Industry Co.,Ltd.的和来自Sud-Chemie AG的911,来自Ciba SpecialtyChemicals的713和来自Huber的由于其增强的热稳定性,优选使用脱水的水滑石化合物,如来自Kyowa的
根据本发明的第二方面,提供了包含橡胶基体和本发明的第一方面的固化组合物中所描述的固化组合物的未固化橡胶组合物。
在本发明的优选实施方案中,橡胶基体选自丙烯腈丁二烯橡胶、氢化丁腈橡胶、氯磺化聚乙烯、苯乙烯-丁二烯橡胶或其混合物。优选地,基体包含丙烯腈丁二烯橡胶。丙烯腈丁二烯橡胶(NBR)是2-丙烯腈和各种丁二烯单体(1,2-丁二烯和1,3-丁二烯)的不饱和共聚物族。尽管其物理和化学性质根据聚合物的腈组成变化,但这种形式的合成橡胶在一般地耐油、燃料和其它化学品方面是不寻常的(聚合物中的腈越多,耐油性越高,但是材料的柔韧性越低)。更优选地,丙烯腈丁二烯橡胶与选自氯磺化聚乙烯、苯乙烯-丁二烯橡胶、氢化腈及其混合物的橡胶共混。
优选地,根据本发明的第二方面的未固化橡胶组合物包含每100份橡胶2至15份金属助剂。
优选地,根据本发明的第二方面的未固化橡胶组合物包含每100份橡胶2至15份有机过氧化物。
优选地,根据本发明的第二方面的未固化橡胶组合物包含每100份橡胶0.5至2.0份硫。
优选地,根据本发明的第二方面的未固化橡胶组合物包含每100份橡胶2至20份水滑石化合物。
优选地,根据本发明的第二方面的未固化橡胶组合物包含每100份橡胶5至20份氢化丁腈橡胶。
根据本发明的第二方面的未固化橡胶组合物优选包含抗臭氧剂。可以使用任何能够将其表面上的臭氧分解成氧的化合物作为抗臭氧剂。例如,氧化铝有效地用作用于聚合物如橡胶的抗臭氧剂。这被称为臭氧的催化分解,并且该反应通常在低于热分解温度的温度下发生。因此,通过使用抗臭氧剂,可以抑制臭氧劣化引起的裂纹的产生和增长以及橡胶碎裂(chipping)。
根据本发明的第二方面的未固化橡胶组合物优选包含抗氧化剂。抗氧化剂的实例包括但不限于胺衍生物如二苯胺抗氧化剂、对苯二胺抗氧化剂和萘胺抗氧化剂;喹啉衍生物;氢醌衍生物;酚类(单酚、双酚、三酚、受阻酚、多酚、硫代双酚);苯并咪唑;硫脲;亚磷酸酯;和有机硫醇酯(organic thioate)。
二苯胺抗氧化剂的实例包括对异丙氧基二苯胺、对(对甲苯磺酰胺)二苯胺、N,N-二苯基乙二胺和辛基化二苯胺。
对苯二胺抗氧化剂的实例包括:N-(1,3-二甲基丁基)-N'-苯基-对苯二胺、N-异丙基-N'-苯基-对苯二胺、N,N'-二苯基-对苯二胺、N,N'-二-2-萘基-对苯二胺、N-环己基-N'-苯基-对苯二胺、N,N'-双(1-甲基庚基)-对苯二胺、N,N'-双(1,4-二甲基戊基)-对苯二胺、N,N'-双(1-乙基-3-甲基戊基)-对苯二胺、N-4-甲基-2-戊基-N'-苯基-对苯二胺、N,N'-二芳基-对苯二胺、受阻二芳基-对苯二胺、苯基-己基-对苯二胺和苯基-辛基-对苯二胺。
萘胺抗氧化剂的实例包括苯基-α-萘胺、苯基-β-萘胺和醛醇-α-三甲基-1,2-萘胺。
喹啉抗氧化剂(喹啉衍生物)的实例包括2,2,4-三甲基-1,2-二氢喹啉聚合物和6-乙氧基-2,2,4-三甲基-1,2-二氢喹啉。
氢醌抗氧化剂(氢醌衍生物)的实例包括2,5-二-(叔戊基)氢醌和2,5-二叔丁基氢醌。
至于酚抗氧化剂(酚类),单酚抗氧化剂的实例包括2,6-二叔丁基-4-甲基苯酚、2,6-二叔丁基-4-乙基苯酚、2,6-二叔丁基苯酚、1-氧-3-甲基-4-异丙基苯、丁基化羟基茴香醚、2,4-二甲基-6-叔丁基苯酚、正十八烷基-3-(4'-羟基-3',5'-二叔丁基苯基)丙酸酯和苯乙烯化苯酚。双酚、三酚和多酚抗氧化剂的实例包括2,2'-亚甲基-双(4-甲基-6-叔丁基苯酚)、2,2'-亚甲基-双(4-乙基-6-叔丁基苯酚)、4,4'-亚丁基-双(3-甲基-6-叔丁基苯酚)、1,1'-双(4-羟基苯基)-环己烷和四[亚甲基-3-(3',5'-二叔丁基-4'-羟基苯基)丙酸酯]甲烷。硫代双酚抗氧化剂的实例包括4,4'-硫代双-(6-叔丁基-3-甲基苯酚)和2,2'-硫代双-(6-叔丁基-4-甲基苯酚)。
苯并咪唑抗氧化剂(苯并咪唑(benzimidazoles))的实例包括2-巯基甲基苯并咪唑。硫脲抗氧化剂(硫脲(thioureas))的实例包括三丁基硫脲。亚磷酸酯抗氧化剂(亚磷酸酯(phosphites))的实例包括亚磷酸三(壬基苯基)酯。有机硫醇酯抗氧化剂(有机硫醇酯(organic thioates))的实例包括硫代二丙酸二月桂酯。
其中,就显著提高耐臭氧性而言,优选对苯二胺抗氧化剂,并且更优选N-(1,3-二甲基丁基)-N'-苯基-对苯二胺。
在根据本发明的第二方面的未固化橡胶组合物中,每100质量份橡胶成分待添加的聚合物用抗臭氧剂和抗氧化剂的总合计量优选为1.5质量份或更多,且更优选为2.2质量份或更多。如果总合计量小于1.5质量份,则可能不能充分得到防止臭氧劣化的效果。另外,总合计量优选为25质量份或更少,且更优选为23质量份或更少。如果总合计量多于25质量份,则拉伸参数可能降低并且可能引起褐变。
根据本发明的第二方面的未固化橡胶组合物优选包含导致耐臭氧性改善的蜡。
蜡的实例包括石油蜡如石蜡,和植物蜡如巴西棕榈蜡、米蜡、小烛树蜡、日本蜡、漆蜡、甘蔗蜡和棕榈蜡。其中,石油蜡是优选的,并且石蜡是更优选的,因为它们提供优异的耐臭氧性。
每100质量份橡胶成分待添加的蜡的量优选为0.1质量份或更多,且更优选为0.5质量份或更多。如果该量小于0.1质量份,则可能不能由其形成有效的膜。该量优选为5质量份或更少,且更优选为3质量份或更少。如果该量大于5质量份,则可能不能充分抑制橡胶表面上的变色。
根据本发明的第二方面的未固化橡胶组合物优选包含氧化锌。氧化锌有效地用作抗臭氧剂的臭氧分解反应的促进剂。氧化锌没有特别限制,且可以是橡胶工业中常用的氧化锌。
每100质量份橡胶成分待添加的氧化锌的量优选为1质量份或更多,且更优选为2质量份或更多。如果该量小于1质量份,则氧化锌可能不能充分用作臭氧分解的促进剂。该量优选为10质量份或更少,且更优选为5质量份或更少。如果该量多于10质量份,则氧化锌不太可能分散,并且可能降低断裂能。
本发明的耐臭氧橡胶组合物优选包含填料如炭黑或二氧化钛(titane dioxide),导致橡胶强度提高。
每100质量份橡胶成分待添加的填料的量优选为10质量份或更多,且更优选为30质量份或更多。如果该量小于10质量份,则断裂能和抓地性能(grip performance)倾向于降低。填料的量优选为100质量份或更少,且更优选为70质量份或更少。如果该量大于100质量份,则分散性倾向于降低。
除了上述成分之外,根据本发明的第二方面的未固化橡胶组合物可以适当地还包含在制备橡胶组合物中通常使用的配混剂,如二氧化硅、硅烷偶联剂、油、硬脂酸和硫化促进剂。
根据本发明的第三方面,提供了可通过固化如本发明的第二方面所描述的未固化橡胶组合物获得的固化橡胶。一般地,未固化橡胶组合物通过施加热被固化。固化可以通过已知方法进行,而不受特别限制。例如,可以通过将未固化橡胶组合物、作为固化剂的氧化锌、作为增强剂的炭黑、固化促进剂等共混在一起,使所得组合物形成片或任何其他期望的形状,并且对其进行模压成型来进行固化。用于固化反应的加热条件没有特别限制,并且例如,固化可以在130至210℃的温度下进行约5至60分钟的时间。
根据本发明的第四方面,提供了一种液压软管,其包括由如本发明的第三方面所描述的固化橡胶制成的管。
一般地,液压软管包括三层:最内层或管、增强层和覆盖层。增强件使得软管能够处理流体压力和压力尖峰,并且在正确使用时防止过早的软管爆裂。其确定软管的工作压力。工作压力低的软管通常使用纺织纤维增强件,而处理较高压力的软管一般地使用高强度钢丝。
钢增强的软管又分为两类:编织软管和螺旋软管。金属丝编织软管根据尺寸处理至6000psi的工作压力,有一个或两个编织层。一般地以更大直径处理高压力的螺旋软管具有偏置绕管盘旋的金属丝,连续的层以相反的角度布置。通常有四层或六层钢增强件。在编织和螺旋软管中,橡胶层将钢包层分开,以确保整个软管壁的良好的粘合。
覆盖件保护管和增强件免受热、磨损和腐蚀,以及热、冷、UV光和臭氧造成的环境恶化。取决于应用,覆盖件由合成橡胶、纤维编织物或织物包层制成。
优选地,液压软管包括由固化橡胶制成的最内层和增强层。增强层优选包括金属,优选钢,或由金属,优选钢构成。更优选地,增强层包括螺旋或编织钢丝。特别优选使用涂覆黄铜的钢,以增强与最内橡胶层的粘合。
根据本发明的第五方面,提供了一种用于制备固化橡胶的方法,其包括:
-提供如本发明的第二方面所描述的未固化橡胶组合物
-热处理未固化橡胶组合物。
在附图中:
图1示出了橡胶中的用有机过氧化物固化引起的共价键。
图2示出了橡胶中的单或多硫化物键。
图3示出了由金属助剂与有机过氧化物的组合引起的橡胶中的离子键。
图4和5示出了在121℃下在空气中加热后,与不同市售组成的橡胶制成的两种管相比较的由本发明的橡胶组合物制成的管的拉伸强度和断裂伸长率测试。
图6和7示出了在121℃下在油中加热后,与不同市售组成的橡胶制成的两种管相比较的由本发明的橡胶组合物制成的管的拉伸强度和断裂伸长率测试。
图8示出了在100℃下在空气中加热后,与不同市售组成的橡胶制成的两种管相比较的由本发明的橡胶组合物制成的管的压缩永久变形。
以下,基于实施例和比较例对本发明进行说明。
实施例(样品31449)
如下制备橡胶组合物:
31449是新内管的样品代码,并且其组成主要基于NBR基体和如权利要求部分所描述的新型混合固化。
将31449与内部混合物混合,然后用于挤出机中以形成管。挤出是用于产生固定横截面轮廓的物体的过程。推动材料通过期望横截面的直径。为了在挤出过程中制造液压软管的管,挤出连续的圆柱形管。该管用于制造编织或螺旋软管。
比较例1(K4890)
将高效硫固化体系K4890作为比较例1。
比较例2(AS2831)
将常规硫固化体系AS2831作为比较例2。
比较例3(ML3792-1)
ML3792-1与31449相似,但不含硫。
拉伸测试和断裂伸长率测试
在121℃下、在热空气和IRM903油中对固化橡胶(1)31449、(2)K4890和(3)AS2831进行依赖于时间的拉伸和伸长率变化。对于热空气和IRM903两者,与K4890和AS2831相比,31449样品显示更少的拉伸和伸长率下降。根据ASTM D573(Standard Test Method forRubber—Deterioration in an Air Oven)和ASTM D471(Standard Test Method forRubber Property—Effect of Liquids)进行测试。请参看图4-7。图4和图5示出了在121℃下、在热空气中的固化橡胶化合物的拉伸和伸长率变化,而图6-7示出了在121℃下、在IRM903油中的固化橡胶化合物的拉伸和伸长率变化。
压缩永久变形测试
根据ASTM D 395(Standard Test Methods for Rubber Property—CompressionSet)在100℃下对固化橡胶(1)31449、(2)K4890和(3)AS2831进行依赖于时间的压缩永久变形。31449样品显示更少的永久变形。请参看图8。
金属丝粘合测试
根据ASTM D 1871(Standard Test Method for Adhesion Between Tire BeadWire and Rubber)对固化的橡胶(1)31449和(2)ML3792-1进行比较橡胶与涂覆黄铜的钢丝粘合。31449粘合以87磅力(lbf)表现出很高的粘合力,其中ML3792-1为7.9磅力。
Claims (13)
1.用于橡胶的固化组合物,其包含:
-选自二丙烯酸锌和甲基丙烯酸锌的金属助剂
-有机过氧化物
-硫
-水滑石化合物。
2.包含橡胶基体和权利要求1所述的固化组合物的未固化橡胶组合物。
3.根据权利要求2所述的未固化橡胶组合物,其中所述橡胶基体选自丙烯腈丁二烯橡胶、氢化丁腈橡胶、氯磺化聚乙烯、苯乙烯-丁二烯橡胶或其混合物。
4.根据权利要求2或3所述的未固化橡胶组合物,其中所述有机过氧化物以每100份橡胶2至15份的量存在。
5.根据权利要求2至4所述的未固化橡胶组合物,其中所述金属助剂以每100份橡胶2至15份的量存在。
6.根据权利要求2或5所述的未固化橡胶组合物,其中硫以每100份橡胶0.5至2.0份的量存在。
7.根据权利要求2或6所述的未固化橡胶组合物,其中,所述水滑石化合物以每100份橡胶2至20份的量存在。
8.根据权利要求2或7所述的未固化橡胶组合物,其中氢化丁腈橡胶以每100份橡胶5至20份的量存在。
9.可通过固化如权利要求2至8中任一项所述的未固化橡胶组合物获得的固化橡胶。
10.液压软管,其包括由如权利要求9所述的固化橡胶和增强层制成的管。
11.根据权利要求10所述的液压软管,其中所述增强层包含涂覆黄铜的钢并直接接触最内层。
12.根据权利要求10或11中任一项所述的液压软管,其中所述增强层由螺旋或编织金属丝增强件制成。
13.一种用于制备固化橡胶的方法,其包括:
-提供如权利要求2至8中任一项所述的未固化橡胶组合物
-热处理所述未固化橡胶组合物。
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
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IN3143/DEL/2015 | 2015-09-30 | ||
IN3143DE2015 | 2015-09-30 | ||
GBGB1519958.1A GB201519958D0 (en) | 2015-09-30 | 2015-11-12 | Rubber and hydraulic hose comprising a inner tube made of the rubber material |
GB1519958.1 | 2015-11-12 | ||
PCT/EP2016/072574 WO2017055168A1 (en) | 2015-09-30 | 2016-09-22 | Rubber and hydraulic hose comprising a inner tube made of the rubber material |
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CN108350228A true CN108350228A (zh) | 2018-07-31 |
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CN201680055632.5A Pending CN108350228A (zh) | 2015-09-30 | 2016-09-22 | 橡胶和包括由橡胶材料制备的内管的液压软管 |
Country Status (7)
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US (2) | US20180273721A1 (zh) |
EP (1) | EP3317344B1 (zh) |
JP (1) | JP6479263B2 (zh) |
CN (1) | CN108350228A (zh) |
ES (1) | ES2704958T3 (zh) |
GB (1) | GB201519958D0 (zh) |
TR (1) | TR201900032T4 (zh) |
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DE102017215964A1 (de) * | 2017-09-11 | 2019-03-14 | Contitech Schlauch Gmbh | Mehrschichtiger flexibler Schlauch |
CN114716743B (zh) * | 2022-03-25 | 2023-05-09 | 成都飞机工业(集团)有限责任公司 | 一种氢化丁腈橡胶补强剂及其制备方法、应用 |
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TR201900032T4 (tr) | 2019-02-21 |
GB201519958D0 (en) | 2015-12-30 |
EP3317344B1 (en) | 2018-11-14 |
JP2018531310A (ja) | 2018-10-25 |
US20210214521A1 (en) | 2021-07-15 |
JP6479263B2 (ja) | 2019-03-06 |
US20180273721A1 (en) | 2018-09-27 |
ES2704958T3 (es) | 2019-03-20 |
EP3317344A1 (en) | 2018-05-09 |
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