CN1623764A - 辐照接枝含氟聚合物基的管道在加油站输送汽油中的应用 - Google Patents
辐照接枝含氟聚合物基的管道在加油站输送汽油中的应用 Download PDFInfo
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- CN1623764A CN1623764A CNA2004100979988A CN200410097998A CN1623764A CN 1623764 A CN1623764 A CN 1623764A CN A2004100979988 A CNA2004100979988 A CN A2004100979988A CN 200410097998 A CN200410097998 A CN 200410097998A CN 1623764 A CN1623764 A CN 1623764A
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- fluoropolymer
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- polyolefin
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Abstract
按第一方式,本发明是一种管道在加油站输送汽油中的应用,该管包括:与输送流体接触的以辐照接枝不饱和单体的氟聚合物的内层,和直接与它连接的聚烯烃外层。另一方案,包括在辐照接枝的氟聚合物一侧有氟聚合物层,优选PVDF层。第二方式,包括:以辐照接枝的氟聚合物的中心层,直接与它连接的聚烯烃外层和与汽油接触的聚烯烃内层。按方案,可用辐照接枝的氟聚合物与氟聚合物的混合物层代替辐照接枝的氟聚合物层。第三方式,包括:聚烯烃的中心层,直接与它连接的辐照接枝的氟聚合物外层和辐照接枝的氟聚合物内层。按方案,至少一层辐照接枝的氟聚合物层被氟聚合物层覆盖。辐照接枝的氟聚合物层是在PVDF层与聚烯烃层之间的粘合剂层。与汽油接触的内层是辐照接枝的氟聚合物层,或氟聚合物层,或辐照接枝的氟聚合物与氟聚合物的混合物层。
Description
本发明的技术领域
本发明涉及一种基于以辐照接枝不饱和单体的含氟聚合物的管道,以用于加油站输送汽油。更确切地,这种管道包括至少一层以辐照接枝不饱和单体的含氟聚合物和至少一层聚烯烃。这些管道用于加油站输送汽油,以把这种流体从储油罐送到汽油分配器,再从汽油分配器送至用户车上。
现有技术与技术问题
人们知道这些含氟聚合物,例如偏氟乙烯CF2=CH2(VDF)基的含氟聚合物,如PVDF(聚偏氟乙烯)具有极佳的机械稳定性、非常高的化学惰性以及良好的耐老化性。然而,含氟聚合物的这种化学惰性使其难以将它们粘结起来,或将它们与其它材料结合。
专利EP 558 373描述了一种输油管,它分别包括用聚酰胺制成的外层、粘合剂层和与汽油接触的由含氟聚合物(有利的是PVDF,聚偏氟乙烯的缩写)所构成的内层。其汽油渗透率很理想,但冲击强度不够。
专利EP 696 301、EP 740 754和EP 726 926描述了许多输油管,它们分别包括聚酰胺的外层、粘合剂层、PVDF(聚偏氟乙烯)层、粘合剂层和与石油接触的聚酰胺的内层。它们的渗透性和冲击强度都非常好,然而,根据聚酰胺的性质和生产这种管道所使用的共挤出设备,可能需要在聚酰胺内层中添加增塑剂。由此导致这种增塑剂可能挤出,并且被汽油带走,于是可能引起管道或发动机的加油设备的堵塞。
专利EP 1 243 832描述了一种管道,它包括聚酰胺外层、由氟聚合物和链上有反应性官能基的甲基丙烯酸烷基酯的混合物构成的层,和由聚酰胺基体和聚烯烃分散相的混合物构成的与汽油接触的内层。
专利US 4 749 607描述了一种多层系统,它包括改性的含卤素的热塑性聚合物层和改性的聚烯烃层。改性的含卤素的热塑性聚合物可以是含氟聚合物,其中采用直接共聚合方法,或者借助于自由基引发剂采用化学接枝方法而加入了极性官能团。
在现有技术的这些文件中,还没有描述过以辐照方法在其上接枝不饱和单体的含氟聚合物层。此外,描述的这些管道外径通常是8mm,这些管道包括聚酰胺层,它们尤其用于汽车,以把汽油从储油罐送至发动机的加油设备。在这些加油站中,这些管道的直径应该比较大,并且如果使用在前面现有技术中描述的这些管道,这些管道的成本会太高。
另外,现在人们知道生产以辐照在其上接枝不饱和单体的含氟聚合物,并使这些改性的含氟聚合物在聚烯烃与含氟聚合物之间是良好的粘合剂。下面,将采用辐照在其上接枝不饱和单体的含氟聚合物简化表达为以辐照接枝的含氟聚合物。
这些以辐照接枝的含氟聚合物还可以构成在聚烯烃上的粘合层,而不用添加其它的含氟聚合物层,便可得到具有抗化学腐蚀层和阻挡层的结构。在现有技术中没有描述使用这种结构以用于加油站输送汽油,把储油罐中的流体送到汽油分配器,再从汽油分配器送至用户车辆上。
本发明的简要描述
根据第一种方式,本发明涉及一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管包括:
与待输送流体接触的内层,该内层由以辐照接枝的含氟聚合物构成,和直接与它连接的聚烯烃外层。
根据一种方案,以辐照接枝的含氟聚合物和含氟聚合物,优选地PVDF的混合物层代替以辐照接枝的含氟聚合物层。
根据另一种方案,该管道包括在以辐照接枝的含氟聚合物一侧配置有含氟聚合物层,优选地PVDF层。这就是说该管道相继地包括含氟聚合物层,优选地PVDF层、以辐照接枝的含氟聚合物(任选地与含氟聚合物混合)构成的层,并直接连接到其聚烯烃外层。这个以辐照接枝的含氟聚合物层是在PVDF层与聚烯烃层之间的粘合剂层。与汽油接触的内层因此可以是采用辐照接枝的含氟聚合物层,或者是含氟聚合物层(优选地PVDF层),或者是采用辐照接枝的含氟聚合物与含氟聚合物(优选地PVDF)的混合物层。
根据第二种方式,本发明涉及一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管道包括:
由以辐照接枝的含氟聚合物构成的中心层,直接与它连接的聚烯烃外层和聚烯烃内层。这种聚烯烃内层是与汽油接触的层。
根据一种方案,可用以辐照接枝的含氟聚合物与含氟聚合物(优选地PVDF)的混合物层代替采用辐照接枝的含氟聚合物层。
根据第三种方式,本发明涉及一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管道包括:
由聚烯烃构成的中心层,直接与它连接的以辐照接枝的含氟聚合物外层和以辐照接枝的含氟聚合物内层。
根据一种方案,可用以辐照接枝的含氟聚合物与含氟聚合物(优选地PVDF)的混合物层代替至少一层以辐照接枝的含氟聚合物层。
根据另一种方案,至少一层以辐照接枝的含氟聚合物(任选地与含氟聚合物混合)层被含氟聚合物层(优选地PVDF层)所覆盖。以辐照接枝的含氟聚合物层是在PVDF层与聚烯烃层之间的粘合剂层。与汽油接触的内层因此是采用辐照接枝的含氟聚合物层,或者是含氟聚合物层(优选地PVDF层),或者是采用辐照接枝的含氟聚合物与含氟聚合物(优选地PVDF)的混合物层。
在上述管道中,在以辐照接枝的含氟聚合物层(或含有以辐照接枝的含氟聚合物的层)与一层或多层聚烯烃之间可设置官能化聚烯烃层,它的官能基能与采用辐照在含氟聚合物上接枝的官能基进行反应。例如,如果采用辐照在含氟聚合物上接枝马来酸酐,则该官能化聚烯烃层是由乙烯、甲基丙烯酸缩水甘油酯和任选地丙烯酸烷基酯的共聚物构成的,任选地是与聚乙烯的混合物。
在上述结构中,与待输送流体接触的内层可以含有炭黑、炭的纳米管和任何其它能使其变成导电体,以避免静电积累的添加剂。
可以采用共挤塑方法生产这些管道,这种技术本身是已知的。
本发明还涉及在本发明第三种方式中使用的管道作为新主题。
本发明的详细描述
关于含氟聚合物,应理解是在其链中有至少一种单体的任何聚合物,该单体选自含有能打开而被聚合的乙烯基团的化合物,并且这些化合物含有直接与这种乙烯基团连接的至少一个氟原子、氟代烷基或氟代烷氧基。
作为单体实例,可以列举氟乙烯、偏氟乙烯(VDF)、三氟乙烯(VF3)、氯三氟乙烯(CTFE)、1,2-二氟乙烯、四氟乙烯(TFE)、六氟丙烯(HFP);全氟(烷基乙烯基)醚,例如全氟(甲基乙烯基)醚(PMVE)、全氟(乙基乙烯基)醚(PEVE)和全氟(丙基乙烯基)醚(PPVE)、全氟(1,3-间二氧杂环戊烯)、全氟(2,2-二甲基-1,3-间二氧杂环戊烯)(PDD);式CF2=CFOCF2CF(CF3)OCF2CF2X产品,式中X是SO2F、CO2H、CH2OH、CH2OCN或CH2OPO3H、式CF2=CFOCF2CF2SO2F产品、式F(CF2)nCH2OCF=CF2产品,式中n是1、2、3、4或5、式R1CH2OCF=CF2产品,式中R1是氢或F(CF2)z,z是1、2、3或4、式R3OCF=CH2产品,式中R3是F(CF2)z-,z是1、2、3或4、全氟丁基乙烯(PFBE)、3,3,3-三氟丙烯和2-三氟甲基-3,3,3-三氟-1-丙烯。
该含氟聚合物可以是均聚物或共聚物。它还可以有不含氟的单体,例如乙烯。
作为实例,该含氟聚合物选自:
-偏氟乙烯(VDF)的均聚物或共聚物,它们优选含有至少50重量%VDF,该共聚物选自氯三氟乙烯(CTFE)、六氟丙烯(HFP)、三氟乙烯(VF3)和四氟乙烯(TFE)。
-三氟乙烯(VF3)的均聚物或共聚物,
-结合氯三氟乙烯(CTFE)、四氟乙烯(TFE)、六氟丙烯(HFP)和/或乙烯结构单元残基和任选地VDF和/或VF3结构单元的共聚物,特别是三聚物。
有利地,该含氟聚合物是聚(偏氟乙烯)(PVDF)的均聚物或共聚物。优选地,PVDF含有至少50重量%VDF,更优选地至少75重量%,更好地至少85重量%。该共聚单体优选为HFP。
有利地,PVDF的粘度是100-2000Pa.s,该粘度是使用毛细管式流变计,在剪切梯度100s-1与230℃条件下测量的。事实上,这些PVDF是非常适合于挤塑和注塑。优选地,PVDF的粘度是300-1200Pa.s,该粘度是使用毛细管式流变计,在剪切梯度100s-1与230℃条件下测量的。
因此,以商标KYNAR710或720销售的PVDF非常适合于这种配方。
关于采用辐照接枝的含氟聚合物,它是采用辐照将不饱和单体接枝在含氟聚合物上的方法得到的。
在现有技术已知的熔化介质中,采用任何的混合技术,使含氟聚合物预先与不饱和单体进行混合。这个混合步骤可在任何的混合设备中进行,这种混合设备例如是在热塑性塑料工业中使用的挤塑机或捏和机。优选地,使用挤塑机将该混合物制成颗粒形式。
然后,使用电子源和光子源,以辐照剂量10-200kGray,优选地10-150kGray辐照含氟聚合物和不饱和单体的固体混合物。特别优选的是使用钴60源进行辐照。
由此可达到不饱和单体的接枝高达0.1-5重量%(即接枝的不饱和单体相应于每99.9-95份含氟聚合物为0.1-5份),有利地0.5-5重量%,优选地1-5重量%。接枝不饱和单体的含量取决于在待辐照的含氟聚合物/不饱和单体混合物中不饱和单体的起始含量。该含量还取决于接枝效率,因此也取决于辐照的时间和能量。
然后,除去未接枝的不饱和单体以及接枝所释放的残余物,特别是HF。可以按照本技术领域的技术人员已知的技术进行这种操作。可以采用真空下的脱气,任选地同时加热的方法。也可能把改性的含氟聚合物溶于适当的溶剂(例如N-甲基吡咯烷酮)中,然后在非-溶剂中沉淀该聚合物,例如在水或在醇中沉淀该聚合物。
这里,这种采用辐照接枝方法的优点之一是可得到高含量的接枝不饱和单体,而采用自由基引发剂的经典接枝方法的接枝不饱和单体含量低。因此,通常,采用辐照接枝的方法,其含量有可高于1%(即每99份含氟聚合物为1份不饱和单体),甚至高于1.5%,而采用通常在挤出机中进行的传统的接枝方法,该含量约0.1-0.4%。
另一方面,在《冷》的条件下,典型地在低于100℃,甚至70℃的温度下进行辐照接枝,其结果是含氟聚合物和不饱和单体的混合物没有达到熔化状态,如通常在挤出机中进行的接枝方法。因此,一个基本不同是在半-结晶的含氟聚合物的情况下(例如使用PVDF的便是这种情况),这种接枝是在无定形相中不是在结晶相中进行的,而在挤出机中以熔融态接枝的情况下产生均匀的接枝。在采用辐照接枝的情况下与在挤出机中进行接枝的情况下,不饱和单体在含氟聚合物链上的分布是不相同的。因此,与采用在挤出机中接枝得到的产物相比,这种改性的含氟产物中不饱和单体在含氟聚合物链上的分布是不同的。
在这个接枝步骤中,优选的是要避免氧的存在。因此有可能用氮气或氩气吹扫以除去含氟聚合物/不饱和单体混合物中的氧。
这样得到的以辐照接枝的含氟聚合物可以原样使用,或者与未以辐照接枝的同样含氟聚合物混合使用,或者与其它含氟聚合物或者与其它聚合物(例如丙烯酸聚合物)混合使用。作为丙烯酸聚合物实例,可以列举PMMA和芯壳型冲击改性剂。
以辐照接枝的含氟聚合物在改性前具有含氟聚合物的所有特征,特别是非常好的抗化学性与非常好的抗氧化性,以及热机械强度。此外,与未改性的含氟聚合物相比,根据本发明方法改性的这些聚合物其粘合性大大增加。
关于不饱和单体,它具有至少一个C=C双键以及至少一个极性官能基,这个官能基可以是下述官能基中之一:
-羧酸,
-羧酸盐,
-羧酸酐,
-环氧化物,
-羧酸酯,
-甲硅烷基,
-羧酸酰胺,
-羟基
-异氰酸酯。
也可考虑多种不饱和单体的混合物。
有4-10个碳原子的不饱和二羧酸及其官能衍生物,特别是它们的酸酐,是特别优选的接枝单体。
作为不饱和单体实例,可以列举甲基丙烯酸、丙烯酸、富马酸、衣康酸、十一碳烯酸、十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠、马来酸酐、二氯马来酸酐、二氟马来酸酐、衣康酸酐、巴豆酸酐、丙烯酸缩水甘油酯或甲基丙烯酸缩水甘油酯、烯丙基缩水甘油醚;乙烯基硅烷,例如乙烯基三甲氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三乙酸基硅烷、γ-甲基丙烯氧基丙基三甲氧基硅烷。
优选地,为了达到良好的粘合性,应选择马来酸酐或十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠。这些不饱和单体还具有其固态的优点,易于将它们加到挤塑机中。非常特别优选的是马来酸酐,因为它能够得到良好的粘合性。
其它可使用的接枝单体例如是不饱和羧酸的C1-C8烷基酯或不饱和羧酸的缩水甘油酯衍生物,例如丙烯酸甲酯、甲基丙烯酸甲酯、丙烯酸乙酯、甲基丙烯酸乙酯、丙烯酸丁酯、甲基丙烯酸丁酯、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、马来酸单乙酯、马来酸二乙酯、富马酸单甲酯、富马酸二甲酯、衣康酸单甲酯、衣康酸二乙酯;不饱和羧酸酰胺衍生物,例如丙烯酰胺、甲基丙烯酰胺、马来酸单酰胺、马来酸二酰胺、马来酸N-单乙基酰胺、马来酸N,N-二乙基酰胺、马来酸N-单丁基酰胺、马来酸N,N-二丁基酰胺、富马酸单酰胺、富马酸二酰胺、富马酸N-单乙基酰胺、富马酸N,N-二乙基酰胺、富马酸N-单丁基酰胺、富马酸N,N-二丁基酰胺;不饱和羧酸酰亚胺衍生物,例如马来酰亚胺、N-丁基马来酰亚胺和N-苯基马来酰亚胺;不饱和羧酸金属盐,例如丙烯酸钠、甲基丙烯酸钠、丙烯酸钾和甲基丙烯酸钾。
由于不饱和单体上有C=C双键,因此不排除不饱和单体的聚合以得到在含氟聚合物上接枝的聚合物链,或者游离的(即没有与含氟聚合物连接的)聚合物链。聚合物链应该理解是有10个以上不饱和单体单元的链。在本发明的范围内,为了有利于含氟聚合物的粘合性,优选的是限制接枝或游离的聚合物链的存在,因此寻求获得10个以下不饱和单体单元的链。优选地,限制于5个以下不饱和单体单元的链,还更优选地2个以下不饱和单体单元的链。
同样地,不排除不饱和单体具有一个以上的C=C双键。因此例如可以使用如甲基丙烯酸烯丙酯、三甲基丙烯酸三羟甲基丙烷酯或二甲基丙烯酸乙二醇酯之类的不饱和单体。但是,在这些化合物中有一个以上的双键可能导致含氟聚合物的交联,因此导致流变性能的改变,甚至导致生成凝胶,这是人们所不希望的。这时,在限制交联的同时也难以获得良好的接枝产率。因此,只含有一个C=C双键的不饱和单体是优选的。优选的不饱和单体因此是只具有一个C=C双键和至少一个极性官能基的那些不饱和单体。
从这个观点出发,马来酸酐,和十一碳烯酸、十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠完全一样构成了良好的可接枝化合物,因为它们在聚合时不同时进行交联。马来酸酐是特别优选的。
关于含氟聚合物与不饱和单体的比例,有利地,含氟聚合物的比例是90-99.9重量%,而不饱和单体分别为0.1-10重量%。优选地,含氟聚合物的比例是95-99.9重量%,而不饱和单体分别为0.1-5重量%。
混合步骤后,观察到含氟聚合物与不饱和单体混合物损失在混合步骤开始时加入的不饱和单体的约10-50%。这个比例取决于不饱和单体的挥发性和性质。事实上,该单体已在挤塑机或混合器中脱气,且在通风回路中加以回收。
关于所述特有的接枝步骤,混合步骤后回收的产物的有利条件是用聚乙烯袋包装,除去空气后封闭。关于辐照方法,可以毫无区别地使用人们更多已知称为β辐照的电子辐照,和人们更多已知称为γ辐照的光子辐照。有利地,其剂量是2-6Mrad,优选地3-5Mrad。
关于除去未接枝不饱和单体和接枝释放残余物的步骤,有可能采用本技术领域的技术人员已知的任何技术。与混合步骤开始时存在的单体相比,以辐照接枝的单体比例是50-100%。可以使用对含氟聚合物和对以辐照接枝的官能基为惰性的溶剂洗涤。例如,在接枝马来酸酐时,可以使用氯代苯洗涤。也可以更简单地将在接枝步骤后回收的产物置于真空下,任选地同时加热以进行脱气。
现在描述在本发明第三种方式中使用的管道。这些管道可以是任何尺寸的,有利地,外径10-100mm,厚度1-5mm。有利地,可以与以辐照接枝的含氟聚合物混合的含氟聚合物有利地是PVDF均聚物或共聚物。其重量比可以是1-90%PVDF,优选地20-60%。对着在第一个和第三个方式中以辐照接枝的含氟聚合物层可以添加的含氟聚合物层有利地是PVDF均聚物或共聚物。聚烯烃层可以是用聚乙烯或用聚丙烯制成的。有利地,这是PEHD。作为实例,可以列举ATOFINA公司的FINATHENE 3802,它的密度是0.938,MVI(熔体体积指数)是0.2cm3/10min(190℃-2.16kg)。关于可以在采用辐照接枝的含氟聚合物层与聚烯烃层之间插入的官能聚烯烃层,有利的是含有环氧化物的聚烯烃,因为采用辐照接枝的含氟聚合物用酸酐进行接枝很有利。
这种官能的聚烯烃是乙烯与不饱和环氧化物的共聚物,或者是用不饱和环氧化物接枝的聚烯烃。
关于用不饱和环氧化物接枝的聚烯烃,聚烯烃应理解是含有烯烃结构单元的聚合物,例如如含有乙烯、丙烯、1-丁烯或任何其它α烯烃结构单元的聚合物。作为实例,可以列举:
-聚乙烯,例如LDPE、HDPE、LLDPE或VLDPE;聚丙烯;乙烯/丙烯共聚物;EPR(乙烯/丙烯橡胶)或PE金属茂(采用单位点催化而得到的共聚物),
-乙烯与至少一种选自不饱和羧酸盐或酯,或饱和的羧酸乙烯酯中的产品的共聚物。
还可能涉及苯乙烯/乙烯-丁烯/苯乙烯嵌段共聚物(SEBS)、苯乙烯/丁二烯/苯乙烯嵌段共聚物(SBS)、苯乙烯/异戊二烯/苯乙烯嵌段共聚物(SIS)、苯乙烯/乙烯-丙烯/苯乙烯嵌段共聚物、乙烯/丙烯/二烯嵌段共聚物(EPDM)。
有利地,该聚烯烃选自LLDPE、VLDPE、聚丙烯、乙烯/乙酸乙烯共聚物或乙烯/(甲基)丙烯酸烷基酯共聚物。该密度有利地是0.86-0.965,流动指数(MFI)可以是0.3-40(以g/10min表示,在190℃,在负载2.16kg下)。
关于乙烯与不饱和环氧化物的共聚物,例如可以列举乙烯、(甲基)丙烯酸烷基酯和不饱和环氧化物的共聚物,或乙烯、饱和羧酸乙烯酯和不饱和环氧化物的共聚物。环氧化物的量可以至多为该共聚物重量的15%,乙烯的量可以是至少50重量%。有利地,环氧化物的比例是2-10重量%。有利地,(甲基)丙烯酸烷基酯的比例是0-40重量%,优选地5-35重量%。
有利的是乙烯、(甲基)丙烯酸烷基酯和不饱和环氧化物的共聚物。
优选的(甲基)丙烯酸烷基酯烷基具有2-10个碳原子。
MFI(熔体流动指数)例如可以是0.1-50(以g/10min表示,在190℃,在负载2.16kg下)。
可使用的丙烯酸烷基酯或甲基丙烯酸烷基酯的实例特别是甲基丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丁酯、丙烯酸异丁酯、丙烯酸-2-乙基己基酯。可使用的不饱和环氧化物实例特别是:
-脂族缩水甘油的酯和醚,例如烯丙基缩水甘油醚、乙烯基缩水甘油醚、马来酸缩水甘油酯和衣康酸缩水甘油酯、丙烯酸缩水甘油酯和甲基丙烯酸缩水甘油酯,和
-脂环族缩水甘油的酯和醚,例如2-环己烯-1-缩水甘油醚、环己烯-4,5-二缩水甘油基羧酸酯、环己烯-4-缩水甘油基羧酸酯、5-降冰片烯-2-甲基-2-缩水甘油基羧酸酯和内顺式-双环(2,2,1)-5-庚烯-2,3-二缩水甘油基二羧酸酯。
实施例
使用下述含氟聚合物:
Kynar720:ATOFINA公司的PVDF均聚物,MVI(熔体体积指数)为10cm3/10min(230℃,5kg)。
KynarADX 120:ATOFINA公司销售的采用马来酸酐辐射接枝的PVDF均聚物,MVI(熔体体积指数)为7cm3/10min(230℃,5kg)。
ADX 120的制备
制备ARKEMA公司的Kynar720的PVDF与1.2质量%马来酸酐的混合物。使用双螺杆挤塑机制备这种混合物,该挤塑机运行条件是230℃、150转/分与流量10kg/h。如此制备的颗粒产品装入铝制密封袋中,然后用氩气流吹扫以除去氧气。这些袋再用γ射线(钴60源)以3Mrad(10Mev加速)辐照17小时。测定接枝率为50%,在N-甲基吡咯烷酮中溶解,然后在水/THF混合物(以重量计,50/50)中沉淀步骤后证实这个比。这时,在接枝操作后得到的产物置于130℃真空下过夜,以便除去残留的马来酸酐和辐照时释放的氢氟酸。
接枝马来酸酐的最后含量是0.6%(根据在1870cm-1的C=O带,采用红外光谱分析得到的)。
使用下述的官能的聚烯烃:
Lotader8840:ATOFINA公司的乙烯与甲基丙烯酸缩水甘油酯的共聚物,其MVI(熔体体积指数)为5cm3/10min(在190℃,在负载2.16kg下)。它含有92重量%乙烯和8重量%甲基丙烯酸缩水甘油酯。
使用下述的聚乙烯:
PEHD 2040ML55:表示ATOFINA公司的高密度聚乙烯,MFI为4g/10min(在190℃,在负载2.16kg下)。它的密度是0.955。
实施例1(根据本发明)
在Mc Neil共挤塑生产线上,共挤塑出一种三层结构,该结构从外到里是由PEHD 2040ML55(2.6mm)与LOTADER 8840(100μm)共挤塑的一层和KynarADX 120(300μm)层构成的。制得管的直径32mm,厚度3mm,这种管在LOTADER与PEHD之间的界面不可剥离,在LOTADER与KynarADX 120之间的粘合力为60N/cm。这种三层结构不存在任何共挤塑问题。在M15汽油中在60℃老化1个月后,没有观察到任何的剥落,可以测量出剥离力为25N/cm。
实施例2(对比)
在Mc Neil共挤塑生产线上,共挤塑出一种三层结构,该结构从外到里是由PEHD 2040ML55(2.6mm)与LOTADER 8840(100μm)共挤塑的一层和Kynar 720(300μm)层构成的。制得管的直径32mm,厚度3mm,这种管在LOTADER与PEHD之间的界面不可剥离,在LOTADER与Kynar 720之间的粘合力为1N/cm。这种三层结构不存在任何共挤塑问题。在室温下储存30分钟后,在PVDF与LOTADER之间出现自发分层。
实施例3(根据本发明)
在Mc Neil共挤塑生产线上,共挤塑出一种4层结构,该结构从外到里是由PEHD 2040ML55(2.6mm)与LOTADER 8840(100μm)共挤塑的一层、Kynar ADX 120(100μm)层和Kynar 720(200μm)层构成的。制得管的直径32mm,厚度3mm,这种管在LOTADER与PEHD之间的界面不可剥离,在LOTADER与Kynar ADX 120之间的粘合力为60N/cm,在Kynar ADX 120与Kynar 720之间的界面不可剥离。这种4层结构不存在任何共挤塑问题。在M15汽油中在60℃老化1个月后,没有观察到任何的剥离,可以测量出在LOTADER/Kynar ADX 120界面的剥离力为25N/cm。
实施例4(根据本发明)
在Mc Neil共挤塑生产线上,共挤塑出一种5层结构,该结构从外到里是由Kynar ADX 120(200μm)、LOTADER 8840(100μm)、PEHD 2040ML55(2.4mm)与LOTADER 8840(100μm)共挤塑的一层和Kynar ADX 120(200μm)层构成的。制得管的直径32mm,厚度3mm,这种管在LOTADER与PEHD之间的界面不可剥离,在LOTADER与外Kynar ADX 120之间的粘合力为40N/cm,在LOTADER与内Kynar ADX 120之间的剥离力为55N/cm。这种5层结构不存在任何共挤塑问题。在M15汽油中在60℃老化1个月后,没有观察到任何的剥离,可以测量出在LOTADER/外Kynar ADX 120界面的剥离力为15N/cm,还可以测量出在LOTADER/内Kynar ADX 120界面的粘合力为24N/cm。
实施例5(根据本发明)
在Mc Neil共挤塑生产线上,共挤塑出一种三层结构,该结构从外到里是由Kynar ADX 120(150μm)、PE Stamylex 1016 LF(LLDPE,MFI为1.1g/10min,在190℃,在负载2.16kg下)/LOTADER 8840以重量比50/50的混合物,(厚度2.7mm),和新的Kynar ADX 120层(150μm)构成的。制得管的直径32mm,厚度3mm,这种管在外Kynar ADX 120与PE/LOTADER混合物之间的粘合力为35N/cm,在内Kynar ADX 120与PE/LOTADER混合物之间的粘合力为45N/cm。这种三层结构不存在任何共挤塑问题。在M15汽油中在60℃老化表明,没有观察到任何的剥离,这种结构在低于1%汽油中在1个月后还凝成块状。
Claims (19)
1.一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管道包括:
与待输送流体接触的内层,该内层由以辐照在其上面而接枝不饱和单体的含氟聚合物构成,和直接与它连接的聚烯烃外层。
2.根据权利要求1所述的应用,其中用以辐照接枝的含氟聚合物和含氟聚合物,优选PVDF的混合物层代替以辐照接枝的含氟聚合物层。
3.根据权利要求1或2所述的应用,其中该管道包括在以辐照接枝的含氟聚合物一侧配置的含氟聚合物层。
4.一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管道包括:
由以辐照接枝的含氟聚合物构成的中心层,直接与它连接的聚烯烃外层和聚烯烃内层。
5.根据权利要求4所述的应用,其中用以辐照接枝的含氟聚合物和含氟聚合物的混合物层代替采用辐照接枝的含氟聚合物层。
6.一种管道在加油站输送汽油中的应用,把储油罐的流体送到汽油分配器,再从汽油分配器送至用户车辆上,该管道包括:
由聚烯烃构成的中心层,直接与它连接的以辐照接枝的含氟聚合物外层和以辐照接枝的含氟聚合物内层。
7.根据权利要求6所述的应用,其中可用以辐照接杖的含氟聚合物与含氟聚合物的混合物层代替至少一层以辐照接枝的含氟聚合物层。
8.根据权利要求6或7所述的应用,其中至少一层以辐照接枝的含氟聚合物(任选地与含氟聚合物混合)层被含氟聚合物层覆盖。
9.根据上述权利要求中任一权利要求所述的应用,其中在以辐照接枝的含氟聚合物层(或含有以辐照接枝的含氟聚合物的层)与一层或多层聚烯烃之间可配置官能化聚烯烃层,它的官能基能与采用辐照在含氟聚合物上接枝的官能团进行反应。
10.根据上述权利要求中任一权利要求所述的应用,其中不饱和单体具有至少一个C=C双键以及至少一个极性官能基,这种官能基可以是羧酸、羧酸盐、羧酸酐、环氧化物、羧酸酯、甲硅烷基、羧酸酰胺、羟基和异氰酸酯的官能基。
11.根据权利要求10所述的应用,其中不饱和单体只有一个C=C双键。
12.根据权利要求11所述的应用,其中不饱和单体是不饱和羧酸酐。
13.根据权利要求12所述的应用,其中不饱和单体是马来酸酐。
14.根据权利要求11所述的应用,其中不饱和单体是十一碳烯酸、十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠。
15.根据权利要求9和10所述的应用,其中官能的聚烯烃是乙烯与不饱和环氧化物的共聚物,或者是用不饱和环氧化物接枝的聚烯烃。
16.根据上述权利要求中任一权利要求所述的应用,其中与待输送流体接触的内层可以含有炭黑、炭纳米管和任何其它能使其变成导电体,以避免静电积累的添加剂。
17.管道,它包括由聚烯烃构成的中心层,直接与它连接的以辐照接枝的含氟聚合物外层,和以辐照接枝的含氟聚合物内层。
18.根据权利要求17所述的管道,其中至少一层以辐照接枝的含氟聚合物层可用一层采用辐照接枝的含氟聚合物和含氟聚合物的混合物层代替。
19.根据权利要求17或18所述的管道,其中至少一层以辐照接枝的含氟聚合物层(任选地与含氟聚合物混合的层)被一层含氟聚合物覆盖。
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US (1) | US20050170121A1 (zh) |
EP (2) | EP1537989B1 (zh) |
JP (1) | JP4224857B2 (zh) |
KR (2) | KR20050053026A (zh) |
CN (1) | CN100500433C (zh) |
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- 2004-11-24 EP EP04292760.8A patent/EP1537989B1/fr active Active
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- 2004-11-24 ES ES06075800T patent/ES2299136T3/es active Active
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- 2004-11-30 US US11/000,163 patent/US20050170121A1/en not_active Abandoned
- 2004-12-01 JP JP2004347996A patent/JP4224857B2/ja not_active Expired - Fee Related
- 2004-12-01 KR KR1020040099861A patent/KR20050053026A/ko not_active Application Discontinuation
- 2004-12-01 CN CNB2004100979988A patent/CN100500433C/zh not_active Expired - Fee Related
- 2004-12-01 CA CA002487080A patent/CA2487080C/fr not_active Expired - Fee Related
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CN108472924A (zh) * | 2015-12-08 | 2018-08-31 | 阿科玛法国公司 | 包括含有含氟聚合物和丙烯酸类共聚物的层的多层结构体-相关的生产方法和管 |
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KR20050053026A (ko) | 2005-06-07 |
TWI273087B (en) | 2007-02-11 |
ATE382469T1 (de) | 2008-01-15 |
ES2529672T3 (es) | 2015-02-24 |
EP1537989A1 (fr) | 2005-06-08 |
JP2005207582A (ja) | 2005-08-04 |
ES2299136T3 (es) | 2008-05-16 |
EP1690673A2 (fr) | 2006-08-16 |
CA2487080A1 (fr) | 2005-06-01 |
CN100500433C (zh) | 2009-06-17 |
MY139176A (en) | 2009-08-28 |
JP4224857B2 (ja) | 2009-02-18 |
TW200530114A (en) | 2005-09-16 |
DE602004011101D1 (de) | 2008-02-14 |
DE602004011101T2 (de) | 2009-01-02 |
EP1537989B1 (fr) | 2014-12-24 |
KR20070032970A (ko) | 2007-03-23 |
MY170933A (en) | 2019-09-19 |
US20050170121A1 (en) | 2005-08-04 |
EP1690673B1 (fr) | 2008-01-02 |
CA2487080C (fr) | 2009-09-08 |
EP1690673A3 (fr) | 2006-08-23 |
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