CN101522735A - 通过不饱和极性单体的辐射接枝而官能化的偏二氟乙烯共聚物 - Google Patents
通过不饱和极性单体的辐射接枝而官能化的偏二氟乙烯共聚物 Download PDFInfo
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- CN101522735A CN101522735A CNA2007800369847A CN200780036984A CN101522735A CN 101522735 A CN101522735 A CN 101522735A CN A2007800369847 A CNA2007800369847 A CN A2007800369847A CN 200780036984 A CN200780036984 A CN 200780036984A CN 101522735 A CN101522735 A CN 101522735A
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Abstract
本发明涉及VDF和能与VDF共聚的至少一种单体的共聚物,其中,该VDF共聚物具有至少50重量%、优选至少75重量%的VDF,在该VDF共聚物上辐射接枝有至少一种不饱和极性单体,特征在于,所述VDF共聚物在接枝前具有如下特性:结晶温度Tc(根据ISO标准11357-3通过DSC测量)为50~120℃、优选为85~110℃;σY的限定阈值为10~40MPa、优选为10~30MPa;熔融态下的粘度ν(在100s-1和230℃下用毛细管流变仪测量)为100~1500Pa·s、优选为 400~1200Pa·s。本发明进一步涉及包含所述改性共聚物和PVDF的混合物。所述改性共聚物或所述混合物还可与热塑性聚合物、弹性体或无机材料组合。
Description
技术领域
本发明涉及通过在PVDF上辐射接枝至少一种不饱和极性单体而获得的官能化PVDF,并且还涉及包含该官能化PVDF和未改性PVDF的共混物。该官能化PVDF或该共混物具有与许多材料(如热塑性聚合物或无机材料)粘合的特性,从而可获得多层结构。本发明还涉及这些多层结构并且还涉及其中共挤出该官能化PVDF的层或该共混物的层的共挤出方法。
所要解决的技术问题
已知PVDF提供优异的机械稳定性、非常高的化学惰性以及良好的抗老化性。这些性质用在各种应用领域中。例如可提及用于化学工程工业或微电子的挤出或注射模塑部件的制造、PVDF以不可渗透的导管的形式用于气体或烃的输送、建筑领域中保护膜或涂层的形成、以及用于电气工程用途的保护部件的生产。然而,也已知难以使PVDF与其它材料粘合。
欧洲申请EP1484346、EP1537989、EP1541343或国际申请WO2006/045630或WO2006/042764描述了用于改性含氟聚合物(尤其是PVDF)的方法,使含氟聚合物可以粘着到热塑性聚合物上或无机材料上。该方法在于辐射接枝不饱和极性单体。本申请人已经观察到:如果通过该方法改性的含氟聚合物是具有某些热特性和机械特性的特殊PVDF共聚物,则可极大地提高粘附力。本申请人还观察到:在该官能化PVDF的存在下可获得更高的共挤出线速度。
背景技术
欧洲申请EP1101994描述了包含官能化含氟聚合物层的燃料软管。该官能化含氟聚合物可为通过辐射接枝而官能化的含氟聚合物。
欧洲申请EP1484346、EP1537989、EP1541343、EP1637319描述了用于改性含氟聚合物(尤其是PVDF)的方法,该方法在于辐射接枝不饱和极性单体。该PVDF可为均聚物或共聚物。
国际申请WO2006/045630描述了官能化PVDF与粘度η为100~1500Pa·s且结晶温度Tc为50~120℃的柔性含氟聚合物的共混物。该官能化PVDF优选通过辐射接枝获得并优选包含超过80摩尔%的VDF,甚至更优选其为均聚物。
申请EP1508927描述了单独使用的官能化PVDF或在共混物中使用的官能化PVDF的实施例。在所述实施例中,使用级别 2801或 761。改性的 2801是VDF-HFP共聚物且具有如下特性:11%的HFP、20~34MPa的σY、116.8℃的Tc和约2500Pa·s的粘度η(230℃、100s-1)。 761是PVDF均聚物。级别2801比根据本发明改性的PVDF更粘。在辐射步骤之后,PVDF具有一定的交联度,所述交联度与在PVDF链之间产生交联点的事实相关:该事实具有进一步提高熔体粘度的效果,从而使官能化PVDF不论在熔融态或者在溶剂溶液中都更加难以转化和使用。
上述文献均未涉及具有本发明热特性和机械特性的PVDF。
发明内容
本发明涉及VDF和能与VDF共聚的至少一种单体的共聚物,该共聚物具有至少50%、优选至少75%的VDF重量含量,在该共聚物上辐射接枝有至少一种不饱和极性单体,特征在于,所述VDF共聚物在接枝前具有如下特性:
·结晶温度Tc(根据标准ISO11357-3通过DSC测量)为50~120℃、优选为85~110℃;
·屈服强度σY为10~40MPa、优选为10~30MPa;和
·熔体粘度η(在100s-1和230℃下用毛细管流变仪测量)为100~1500Pa·s、优选为400~1200Pa·s。
优选地,该VDF共聚物在接枝前具有200~1000MPa、优选200~600MPa的杨氏(拉伸)模量。
本发明还涉及包含该改性共聚物和PVDF的共混物。该改性共聚物或该共混物可与热塑性聚合物、弹性体或无机材料组合。
具体实施方式
对于在其上进行接枝的PVDF,其为VDF(偏二氟乙烯,CH2=CF2)和能与VDF共聚的至少一种单体的共聚物,其中VDF的重量含量为至少50%、优选至少75%。该共聚单体可为,例如,氟乙烯(VF)、三氟乙烯、三氟氯乙烯(CTFE)、1,2-二氟乙烯、四氟乙烯(TFE)、六氟丙烯(HFP)、3,3,3-三氟丙烯和2-三氟甲基-3,3,3-三氟-1-丙烯。为了易于挤出,其优选为热塑性PVDF。
优选VDF-HFP共聚物,其中HFP的重量含量为4~22%、优选为10~20%(在接枝不饱和极性单体前计算的含量)。
另外,PVDF具有如下特性(在经历接枝前):
·结晶温度Tc(根据标准ISO11357-3通过DSC测量)为50~120℃、优选为85~110℃;
·屈服强度σY(在20℃下测量)为10~40MPa、优选为10~30MPa;和
·熔体粘度η(在100s-1和230℃下用毛细管流变仪测量)为100~1500Pa·s、优选为400~1200Pa·s。
而且,其在接枝前具有200~1000MPa、优选200~600MPa的杨氏(拉伸)模量(ASTM D-638)。
关于EP1508927中所述的级别 2801,改性的PVDF最初具有较低的粘度η,这意味着:在改性后,官能化PVDF的粘度也低于改性的 2801。这有助于官能化PVDF的使用,不论其为熔融态或者在溶剂溶液中。
相对于现有技术的官能化PVDF,该官能化PVDF或该共混物具有如下优点:
·对聚合物和无机材料的更强的粘附力;
·更易于使用,不论其为熔融态或者在溶剂溶液中;以及
·它们允许更高的共挤出速度。
具有19%HFP的VDF-HFP共聚物;
Tc:87.4℃
σY:15MPa
η:1000Pa·s,以及
杨氏(拉伸)模量:220MPa。
具有16%HFP的VDF-HFP共聚物
Tc:103℃
σY:18MPa
η:900Pa·s
杨氏(拉伸)模量:360MPa。
关于官能化PVDF,其通过在如上所述的PVDF上辐射接枝至少一种不饱和极性单体而获得。这随后被称作官能化PVDF。
该方法包括如下步骤:
a)首先将PVDF和至少一种不饱和极性单体通过现有技术中已知的任何熔融共混技术共混。该共混步骤在例如热塑性材料工业中所使用的挤出机或捏合机的任意混合装置中进行。优选地,使用挤出机把共混物转化成粒料。因此,对共混物(在本体中)进行接枝,而不是如诸如文献US5576106中所述的在粉末表面处进行接枝。相对于0.1~20重量%、优选1~10重量%的不饱和极性单体,PVDF的比例分别为80~99.9重量%、优选为90~99重量%。
b)接下来,使用辐射剂量为10~200kGray、优选为10~150kGray的电子或光子源对该固态共混物进行辐照(β或者γ辐射)。该共混物可例如包装在聚乙烯袋中,排出空气并然后密封该袋。有利地,剂量为2~6Mrad且优选为3~5Mrad。特别优选使用钴-60弹的辐照。
接枝的不饱和极性单体的量为0.1~5重量%(也就是说,相对于99.9~95重量份的PVDF,接枝的不饱和极性单体相应地为0.1~5重量份),有利地为0.5~5重量%、优选为0.9~5重量%。该量取决于待辐照的共混物中的不饱和极性单体的初始量。其还取决于接枝的效率,从而取决于辐照的持续时间和能量。
c)然后可任选地除去未接枝的不饱和极性单体以及由该接枝放出的残余物(特别是HF)。如果未接枝的不饱和极性单体可能破坏粘附力、或者引起毒性问题,则该最终步骤可为必须的。该操作可根据本领域技术人员已知的技术进行。可应用真空脱气,任选地在加热的同时应用真空脱气。还可将官能化PVDF溶解在合适的溶剂(例如N-甲基吡咯烷酮)中,然后使其在非溶剂(例如水或醇)中沉淀,或者使用对含氟聚合物以及接枝的官能团具有惰性的溶剂洗涤该官能化PVDF。例如,当接枝马来酸酐时,其可用氯苯洗涤。
该辐射接枝方法的优点之一是能够获得比使用自由基引发剂的常规接枝方法高的接枝不饱和极性单体含量。因此,一般地说使用该辐射接枝方法可获得大于1%的含量(1份不饱和单体/99份PVDF),甚至大于1.5%的含量,而该结果无法用在挤出机中进行的常规接枝方法获得。
另一方面,在“低温”(通常低于100℃、甚至低于50℃的温度)下进行该辐射接枝,使待辐照的共混物不像在挤出机中进行的常规接枝方法一样处于熔融态。一个本质的差别是:接枝在无定形相中进行而不是在结晶相中进行,然而,在挤出机中以熔融态进行接枝的情况中产生均匀接枝。因此,在辐射接枝的情况下,不饱和极性单体不以与在挤出机中接枝的情况下相同的方式分布在整个PVDF链中。因此,相对于通过在挤出机中接枝获得的产品,官能化PVDF在整个PVDF链中具有不同的不饱和极性单体分布。
在该接枝步骤期间,优选避免氧气的存在。因此,可使用氮气或氩气冲洗该待辐照的共混物以除去氧气。该官能化PVDF具有非常良好的耐化学性和抗氧化性,而且,在该PVDF改性前具有良好的热机械性能。
关于该不饱和极性单体,其具有C=C双键并且还具有可选自如下官能团的至少一种极性基团:
-羧酸;
-羧酸盐;
-羧酸酐;
-环氧化物;
-羧酸酯;
-甲硅烷基;
-烷氧基硅烷;
-羧酸酰胺;
-羟基;或
-异氰酸酯。
此外,还可想到几种不饱和单体的混合物。
具有4~10个碳原子的不饱和羧酸和它们的官能化衍生物、特别是它们的酸酐是特别优选的不饱和单体。作为不饱和单体的实例,可提及甲基丙烯酸、丙烯酸、马来酸、富马酸、衣康酸、柠康酸、十一碳烯酸、烯丙基琥珀酸、4-环己烯-1,2-二羧酸、4-甲基-4-环己烯-1,2-二羧酸、二环[2.2.1]庚-5-烯-2,3-二羧酸、x-甲基二环[2.2.1]庚-5-烯-2,3-二羧酸、十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠、马来酸酐、衣康酸酐、柠康酸酐、二氯马来酸酐、二氟马来酸酐、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、乙烯基三乙酰氧基硅烷和γ-甲基丙烯酰氧丙基三甲氧基硅烷。
不饱和单体的其它实例包括:不饱和羧酸的C1~C8烷基酯或缩水甘油酯衍生物,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、衣康酸单甲酯和衣康酸二乙酯;不饱和羧酸的酰胺衍生物,例如丙烯酰胺、甲基丙烯酰胺、马来酰胺、马来二酰胺、N-乙基马来酰胺、N,N-二乙基马来酰胺、N-丁基马来酰胺、N,N-二丁基马来酰胺、富马酰胺、富马二酰胺、N-乙基富马酰胺、N,N-二乙基富马酰胺、N-丁基富马酰胺和N,N-二丁基富马酰胺;不饱和羧酸的酰亚胺衍生物,例如马来酰亚胺、N-丁基马来酰亚胺和N-苯基马来酰亚胺;以及不饱和羧酸的金属盐,例如丙烯酸钠、甲基丙烯酸钠、丙烯酸钾、甲基丙烯酸钾和十一碳烯酸锌、十一碳烯酸钙或十一碳烯酸钠。
优选地,该不饱和单体不具有超过1个的C=C双键,因为这将导致共聚物的交联。二丙烯酸酯或三丙烯酸酯是具有超过1个C=C双键的不饱和单体的实例。从该观点看,马来酸酐与十一碳烯酸锌、十一碳烯酸钙和十一碳烯酸钠形成良好的可接枝配混物,因为它们对于均聚或甚至产生交联具有低的倾向。
优选使用马来酸酐。这是因为该单体提供如下优点:
-其是固体并且在熔融共混之前可容易地和含氟聚合物粒料一起引入;
-其为固态,而且易于处理(特别是其挥发性不是非常高);
-其能够获得良好的粘着性质;
-其对许多化学官能团是特别有活性的;和
-与其它不饱和单体如(甲基)丙烯酸或丙烯酸酯不同,其不均聚且无需稳定化。
该官能化PVDF可单独使用或者作为与另一PVDF(其可为PVDF均聚物或共聚物)的共混物使用。优选地,对所述另一PVDF进行选择使得这两种PVDF是相容的并且该共混物仅有一个DSC熔融峰。优选地,所述另一PVDF是VDF和能与VDF共聚的至少一种单体的共聚物,该共聚物具有至少50%、优选至少75%的VDF重量含量,并且其具有相同的上述热和机械特性。该共混物分别包含1~99重量%、优选50~99重量%的官能化PVDF以及相应的99~1重量%、优选50~1重量%的另一PVDF。该共混物可在熔融介质中使用适合于热塑性材料的共混工具(例如使用挤出机)进行制备。
官能化PVDF或共混物的用途
官能化PVDF或共混物可与热塑性聚合物、弹性体或无机材料组合。本发明还涉及包括以下层的多层结构:
·至少一个由至少一种官能化PVDF或共混物组成的层,以及
·至少一个由至少一种热塑性聚合物和/或至少一种弹性体组成的层;
和
·至少一个无机材料层。
对于本发明的各个多层结构,各层通过表述“由聚合物X组成的层”以可能的最宽泛的方式来限定。相应地,该多层结构通过“聚合物X的层”来限定。
具有热塑性聚合物的层的多层结构
该结构可通过例如共挤出、滚塑或挤出-吹塑的技术来制备。其可采用膜、管、容器或空心体的形式。
作为热塑性聚合物的实例,可提及:
·聚酰胺(例如PA-6、PA-11、PA-12、PA-6,6等);
·包含乙烯或丙烯作为主要成分(>50重量%)的聚合物。可提及,例如,聚烯烃(PE、PP)以及乙烯与选自如下的至少一种乙烯共聚单体的共聚物:α-烯烃,优选丁烯或辛烯;饱和羧酸的乙烯基酯,优选醋酸乙烯酯或丙酸乙烯酯;(甲基)丙烯酸烷基酯,优选丙烯酸甲酯、丙烯酸丁酯或丙烯酸乙酯;
·基于氯乙烯的聚合物,例如PVC(柔性或刚性)、氯化PVC(CPVC)或者基于偏二氯乙烯的聚合物(例如PVDC);
·ABS(丙烯腈-丁二烯-苯乙烯共聚物)或SAN(苯乙烯-丙烯腈共聚物);
·丙烯酸类聚合物,尤其是PMMA均聚物或共聚物;
·饱和聚酯(PET、PBT、PBN);
·聚碳酸酯;
·聚苯硫醚(PPS);
·聚苯醚(PPO);
·EVOH(乙烯-乙烯醇共聚物);
·聚醚醚酮(PEEK);
·聚氧亚甲基(聚甲醛)(polyoxymethylene(acetal));
·聚醚砜;
·聚氨酯;
·基于苯乙烯的聚合物和共聚物,尤其是高抗冲聚苯乙烯或结晶聚苯乙烯以及SBS型的苯乙烯-二烯嵌段共聚物;
·含氟聚合物,例如PVDF、PTFE、TFE/HFP共聚物、乙烯/TFE共聚物、乙烯/三氟氯乙烯共聚物和聚氟乙烯。
该聚烯烃可以是如下类型的聚乙烯:MDPE(中密度)、HDPE(高密度)、LDPE(低密度)、LLDPE(线性低密度)、由茂金属型催化或更通常的单点型催化制备的聚乙烯、或者交联聚乙烯(PEX)。其可为均聚物或共聚物。该共聚物可特别地为共聚单体含量大于5重量%的共聚物,例如型乙烯-辛烯共聚物。还可提及最近由Dow开发的商标为的包含硬嵌段和软嵌段的烯烃嵌段共聚物(OBC),其根据申请WO2005/090425、WO2005/090426和WO2005/090427的教导制备。
术语热塑性树脂包括符合IUPAC在2002年所提出的定义的热塑性弹性体,其为具有通过玻璃状区域或结晶状区域的分散而增强的连续弹性体相的可熔融加工共聚物,其中,所述玻璃状区域或结晶状区域在有限的温度范围内起到连接点的作用。在热塑性弹性体中,最具体地可提及TPO。
作为弹性体的实例,可提及:
·聚氯丁二烯;
·丁腈橡胶(例如丙烯腈-丁二烯共聚物);
·丙烯酸类弹性体;
·含氟弹性体;
·EPM和EPDM;
·聚氨酯弹性体;和
·共聚醚酰胺和共聚酯酰胺(例如由Arkema出售的PEBAX级别)。
关于弹性体的更多细节,可参考Ullmann’s Encyclopaedia of IndustrialChemistry,Vol.A23,1993版,ISBN 3-527-20123-8,第239-334页。
当官能化PVDF或共混物层与热塑性聚合物或弹性体层之间的粘附力不足时,可将至少一个粘合连接物层(adhesion tie layer)置于这两层之间。该粘合连接物有利地具有与官能化PVDF上所存在的那些官能团反应的化学官能团。例如,如果已经把酸酐官能团接枝到PVDF上,该粘合连接物有利地包含环氧或羟基官能团。可将该粘合连接物层分成两层。也就是说,可将第一粘结层和与其不同的第二粘结层置于热塑性聚合物层和官能化PVDF或共混物的层之间,其中这两个粘结层彼此倚靠设置。
作为多层结构的实例,可提及包含彼此依次倚靠设置的下列各层的多层结构:
·一个包含至少一种热塑性聚合物和/或至少一种弹性体的层;
·任选的至少一个粘合连接物层;
·包含官能化PVDF或共混物的层;和
·任选的一个包含含氟聚合物、优选PVDF均聚物或共聚物的层。
在管或导管、容器或空心体的情况下,热塑性聚合物层为外层或内层。这种结构的实例如下:其中热塑性聚合物是聚乙烯,其为导管或容器的形式且其用于输送或储存能够破坏聚烯烃的化学品,且聚乙烯层为外层。该化学品可例如为烃(石油、燃料等)或腐蚀性产品(酸、碱、过氧化氢等)。官能化PVDF或共混物的层和/或含氟聚合物层可保护聚烯烃层。在烃的情况下,其防止聚烯烃溶胀。
多层结构的其它实例包含彼此依次倚靠设置的下列各层:
·任选的一个包含含氟聚合物、优选PVDF均聚物或共聚物的层;
·包含官能化PVDF或共混物的层;
·任选的至少一个粘合连接物层;
·一个包含至少一种热塑性聚合物和/或至少一种弹性体的层;
·任选的至少一个粘合连接物层;
·包含官能化PVDF或共混物的层;
·任选的一个包含含氟聚合物、优选PVDF均聚物或共聚物的层。
这种结构的实例如下:其中热塑性聚合物是聚乙烯,其为导管或容器的形式且其用于输送或储存能够破坏聚烯烃的化学品。该化学品可例如为烃(石油、燃料等)或腐蚀性产品(酸、碱、过氧化氢等)。官能化PVDF或共混物的层和/或任选的含氟聚合物层具有保护内部聚乙烯层的作用。在烃的情况下,它们还防止聚乙烯溶胀。
具有无机材料层的多层结构
术语“无机材料”理解为表示:
·金属;
·玻璃;
·混凝土;
·硅;或
·石英。
因此,包含官能化PVDF或共混物的层形成用于无机材料的保护涂层。换句话说,该无机材料被包含根据本发明的至少一种官能化PVDF或共混物的组合物所涂覆。例如,该组合物使其在所有形式中均避免腐蚀。其还可任选地包含至少一种丙烯酸类聚合物,例如PMMA。其还可任选地包含选自如下的一种或多种添加剂:UV稳定剂、无机填料、颜料和/或染料、导电填料(如炭黑或碳纳米管)等。
该金属可例如为铁、铜、铝、钛、铅、锡、钴、银、钨、镍、锌或合金(例如钢、或者碳钢、镍钢、铬钢、镍-铬钢、铬-钼钢或硅钢、不锈钢、铸铁、坡莫合金、铝-镁合金、铝-硅合金、铝-铜-镍-镁合金、或铝-硅-铜-镍-镁合金、黄铜、青铜、硅青铜、硅黄铜、或镍青铜)。
该金属首先可经历物理和/或化学预处理,其目的是清洗金属表面以促进官能化PVDF或共混物的层的粘合。可能的预处理如下:碱洗、用溶剂(如三氯乙烯)清洗、刷光、喷丸硬化、磷化处理、铬酸盐处理、阳极化(例如用于铝和其合金)、铬阳极化、硅烷化、研磨、酸洗且特别是磺基铬酸洗。一种可能的预处理可在于采用粘合增进剂。粘合增进剂已经由P.E.Cassidy在综述Ind.Eng.Chem.Prod.Res.Development,1972,第11卷,N02,第170~177页或由A.J.Kinlock在J.Mat.Sci.,1980,15,p.2141-66所述。作为可能的化学预处理的实例,可提及Alodine NR1453、Alodine NR2010、Accomet C或Safeguard 6000。预处理还可由这些不同预处理的组合、特别是物理和化学预处理的组合组成。
该金属可为各种形状和几何形状,例如如下的形状:
·展开面,例如片材、板材或箔;
·空心体,例如贮器、容器、瓶、圆筒或化学反应器;
·管或导管、弯管、阀、针阀或泵;
·线材、股绳、缆索或牵索;或
·电极。
涂层可以熔融态、溶剂溶液或粉末形式进行施加。在粉末的情况下,可使用在于将加热的金属部件浸渍到粉末流化床中的流化床技术,或者可使用静电粉末涂覆技术。将粉末引入喷枪中,在该喷枪中,粉末由压缩空气输送并穿过提升到高电位(通常为约10~约100kV)的喷嘴。所施加的电压可以是正极性或负极性的。粉末通过喷枪的流速一般为10~200g/min、优选为50~120g/min。在粉末通过喷嘴期间,粉末变得带有一定的电量,并且将由压缩空气输送的粉末粒子施加到接地(即处于零静电位)的金属部件上。粉末粒子通过它们的静电荷保留在该表面上,并且该静电吸引力足以使涂覆有该粉末的物体移动并在烘箱中加热。
在电极领域中的用途
官能化PVDF或共混物可用于制造正极或负极,特别是用于锂离子电池的正极或负极。一般通过在含氟聚合物粘合剂的存在下将填料分散在溶剂中来生产电活性层,该电活性层含有混合的氧化物填料或者碳和/或石墨填料、以及其它成分以控制电性能。然后,将分散体通过流延方法沉淀在金属集电体上,然后蒸发溶剂以获得负极或正极(取决于所使用的填料的类型)。电池的性能强烈地取决于粘合剂的特性。良好的粘合剂可产生充分填充有电活性成分的层,从而可具有高的比容量。对于充电/放电循环期间的氧化-还原反应,该粘合剂还必须是稳定的并且还必须不受电池中所存在的电解质的影响。该电解质通常含有碳酸酯型溶剂(碳酸乙酯或碳酸丙烯酯)和锂盐(LiPF6、LiBF4)。有关含氟聚合物粘合剂的进一步细节可参考EP1508927、US2003/0072999、US2003/0232244和US5460904。在EP1508927A2的实施例2和3中,官能化PVDF可特别地用本发明的官能化PVDF或共混物代替。
本发明还涉及使用根据本发明的官能化PVDF或共混物来制造电池、优选锂离子电池的正极或负极。
本发明还涉及用于锂离子电池的正极或负极,其包含由下列各层组成的结构:
·一个金属层L1;和
·一个层L2,所述层L2包含本发明的官能化PVDF或共混物。
对于正极,金属优选为铝,且对于负极,金属优选为铜。
共挤出方法
本申请人已经观察到,可利用共挤出技术来提高共挤出线速度(即,共挤出的多层结构的速度,单位为m/min)而不损害官能化PVDF(或共混物)的层和与其接触的层之间的粘着质量,在共挤出技术中,共挤出至少一个包含官能化PVDF或共混物的层和至少一个热塑性聚合物的层。
本发明还涉及使用官能化PVDF或共混物的共挤出方法,该方法在于共挤出至少一个官能化PVDF或共混物的层和至少一个热塑性聚合物或弹性体的层。
实施例
所使用的产品:
Tc:135℃
σY:55MPa
η:900Pa·s(230℃,100s-1);和
杨氏模量:2200MPa。
PVDF-1:具有16重量%HFP的VDF-HFP共聚物,其具有如下性质:
Tc:103℃;
σY:18MPa;
η:900Pa·s;和
杨氏(拉伸)模量:360MPa。
实施例1:官能化PVDF的制备
在Werner40型挤出机中,在190℃下将PVDF-1与2重量%的马来酸酐共混。该共混在如下条件下进行:所有的挤出机出口关闭,螺杆速度为200rpm且通过量为60kg/h。
将造粒为棒状的产物引入到具有不可渗透的铝层的袋子中。用20kGray对该袋子进行辐照。在辐照后,使产物在245℃、最高真空度和200rpm下再次进入挤出机中。通过量为25kg/h。在该脱挥发分步骤后进行产物的红外分析,该分析显示:0.31%的接枝度和300ppm的游离马来酸酐量。该产物称作官能化PVDF 1。
实施例2:官能化PVDF的制备
实施例3(对比)
使用McNeil挤出机制造具有如下结构的多层管(外径:14mm):
PEX层为外层。所有层彼此粘附。在如下条件下以40m/min进行挤出:
·PE层:230℃
·官能化PVDF:250℃,和
· 720:250℃。
实施例4(对比)
在与实施例3中相同的条件下,制造具有如下结构的管:
720(130μm)/在含有16%HFP和在230℃、100s-1下具有900Pa·s粘度的VDF-HFP共聚物中稀释至50%的官能化PVDF2(50μm)/AX8840(50μm)/PEX(780μm)。
实施例5(根据本发明)
在与实施例3中相同的条件下,制造具有如下结构的管:
720(130μm)/官能化PVDF1(50μm)/AX8840(50μm)/PEX(780μm)。
表1
实施例6(根据本发明)
在Collin bubble挤出机上制造具有如下结构的膜:
在230℃下,对总厚度250μm的膜进行挤出。测得官能化PVDF 1和EVOH之间的粘附力为18N/cm。
实施例7(对比)
在Collin bubble挤出机上制造具有如下结构的膜:
在230℃下,对总厚度250μm的膜进行挤出。测得官能化PVDF 1和EVOH之间的粘附力为0.5N/cm。
表2
Claims (21)
1.VDF和能与VDF共聚的至少一种单体的共聚物,所述共聚物具有至少50%、优选至少75%的VDF重量含量,在该共聚物上辐射接枝有至少一种不饱和极性单体,特征在于,所述VDF共聚物在接枝前具有如下特性:
·结晶温度Tc(根据标准ISO11357-3通过DSC测量)为50~120℃、优选为85~110℃;
·屈服强度σY为10~40MPa、优选为10~30MPa;和
·熔体粘度η(在100s-1和230℃下用毛细管流变仪测量)为100~1500Pa·s、优选为400~1200Pa·s。
2.权利要求1的共聚物,特征在于,所述VDF共聚物在接枝前具有200~1000MPa、优选200~600MPa的杨氏(拉伸)模量。
3.权利要求1或2的共聚物,特征在于,所述VDF共聚单体选自氟乙烯(VF)、三氟乙烯、三氟氯乙烯(CTFE)、1,2-二氟乙烯、四氟乙烯(TFE)、六氟丙烯(HFP)、3,3,3-三氟丙烯和2-三氟甲基-3,3,3-三氟-1-丙烯。
4.权利要求1-3中任一项的共聚物,特征在于,所述VDF共聚物为在接枝前具有4~20%、优选10~20%的HFP重量含量的VDF-HFP共聚物。
5.权利要求1-4中任一项的共聚物,特征在于,所述用于辐射接枝该不饱和极性单体的方法包括如下步骤:
a)将所述VDF共聚物和至少一种不饱和极性单体熔融共混;
b)使用辐射剂量为10~200kGray、优选10~150kGray的电子或光子辐射来对所述固态共混物进行辐照;和
c)任选地,除去未接枝的不饱和极性单体以及由该接枝放出的残余物。
6.至少一种权利要求1-5中任一项所限定的其上已接枝有所述不饱和极性单体的共聚物与至少一种PVDF均聚物或共聚物的共混物。
7.权利要求6的共混物,特征在于,相对于99~1%、优选1~50%的PVDF均聚物或共聚物,其上已接枝有所述不饱和极性单体的所述共聚物的重量比例分别为1~99%、优选为50~99%。
8.权利要求6的共混物,特征在于,所述PVDF与其上已接枝有所述不饱和极性单体的所述共聚物相容并且仅具有一个DSC熔融峰。
9.权利要求6-8中任一项的共混物,特征在于,与其上已接枝有所述不饱和极性单体的所述共聚物共混的所述PVDF是VDF和能与VDF共聚的至少一种单体的共聚物,所述共聚物具有至少50%、优选至少75%的VDF重量含量并具有如下特性:
·结晶温度Tc(根据标准ISO11357-3通过DSC测量)为50~120℃、优选为85~110℃;
·屈服强度σY为10~40MPa、优选为10~30MPa;和
·熔体粘度η(在100s-1和230℃下用毛细管流变仪测量)为100~1500Pa·s、优选为400~1200Pa·s。
10.权利要求9的共混物,特征在于,与其上已接枝有所述不饱和极性单体的所述共聚物共混的所述PVDF具有200~1000MPa、优选200~600MPa的杨氏模量。
11.多层结构,其包括由权利要求1-5中任一项所述共聚物或权利要求6-10中任一项所述共混物组成的至少一个层,以及:
·由至少一种热塑性聚合物和/或至少一种弹性体组成的至少一个层;和
·至少一个无机材料层。
12.多层结构,其包括彼此依次倚靠设置的如下层:
·包含至少一种热塑性聚合物和/或至少一种弹性体的一个层;
·任选的至少一个粘合连接物层;
·包含权利要求1-5中任一项所述共聚物或权利要求6-10中任一项所述共混物的一个层;和
·任选的一个包含含氟聚合物的层,所述含氟聚合物优选为PVDF均聚物或共聚物。
13.多层结构,其包括彼此依次倚靠设置的如下层:
·任选的一个包含含氟聚合物的层,所述含氟聚合物优选为PVDF均聚物或共聚物;
·包含权利要求1-5中任一项所述共聚物或权利要求6-10中任一项所述共混物的一个层;
·任选的至少一个粘合连接物层;
·包含至少一种热塑性聚合物和/或至少一种弹性体的一个层;
·任选的至少一个粘合连接物层;
·包含权利要求1-5中任一项所述共聚物或权利要求6-10中任一项所述共混物的一个层;和
·任选的一个包含含氟聚合物的层,所述含氟聚合物优选为PVDF均聚物或共聚物。
14.根据权利要求11-13中任一项的多层结构,特征在于,所述热塑性聚合物选自:
·聚酰胺,优选PA-6、PA-11、PA-12和PA-6,6;
·包含超过50重量%的乙烯和/或丙烯的聚合物;
·包含超过50重量%的氯乙烯的聚合物;
·ABS(丙烯腈-丁二烯-苯乙烯共聚物)或SAN(苯乙烯-丙烯腈共聚物);
·丙烯酸类聚合物;
·饱和聚酯(PET、PBT、PBN);
·聚碳酸酯;
·聚苯硫醚(PPS);
·聚苯醚(PPO);
·EVOH(乙烯-乙烯醇共聚物);
·聚醚醚酮(PEEK);
·聚氧亚甲基(聚甲醛);
·聚醚砜;
·聚氨酯;
·包含超过50重量%苯乙烯的聚合物和共聚物;以及
·含氟聚合物,例如PVDF、PTFE、TFE/HFP共聚物、乙烯/TFE共聚物、乙烯/三氟氯乙烯共聚物和聚氟乙烯。
15.权利要求14的多层结构,特征在于,所述热塑性聚合物是聚烯烃或者乙烯与至少一种选自如下乙烯共聚单体的共聚物:α-烯烃,优选丁烯或辛烯;饱和羧酸的乙烯基酯,优选醋酸乙烯酯或丙酸乙烯酯;(甲基)丙烯酸烷基酯,优选丙烯酸甲酯、丙烯酸丁酯或丙烯酸乙酯。
16.权利要求15的多层结构,特征在于,所述聚烯烃为MDPE(中密度)型、HDPE(高密度)、LDPE(低密度)、LLDPE(线性低密度)、由茂金属型催化或更通常的单点型催化制备的聚乙烯、或者交联聚乙烯(PEX)的聚乙烯均聚物或共聚物。
17.权利要求11-16中任一项的多层结构,其为膜、管或导管、容器或空心体的形式。
18.用于无机材料的保护涂层,其包含:
·权利要求1-5中任一项所述VDF共聚物或权利要求6-10中任一项所述共混物;和
·任选的至少一种丙烯酸类聚合物。
19.权利要求18的涂层,特征在于,所述无机材料为:
·金属;
·玻璃;
·混凝土;
·硅;或者
·石英。
20.权利要求1-5中任一项的改性共聚物或权利要求6-10中任一项所述的共混物在制造电池、优选锂离子电池的正极或负极中的应用。
21.锂离子电池的正极或负极,包括由如下层组成的结构:
·一个金属层L1;和
·一个层L2,所述层L2包含权利要求1-5中任一项的改性共聚物或权利要求6-10中任一项所述的共混物。
22.权利要求21的电极,特征在于,所述金属为铝或铜。
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CN110892018A (zh) * | 2017-07-14 | 2020-03-17 | 阿科玛股份有限公司 | 高强度聚偏二氟乙烯复合材料 |
CN110997799A (zh) * | 2017-07-14 | 2020-04-10 | 阿科玛股份有限公司 | 基于高强度聚偏二氟乙烯的上胶增强纤维 |
CN110997799B (zh) * | 2017-07-14 | 2023-08-04 | 阿科玛股份有限公司 | 基于高强度聚偏二氟乙烯的上胶增强纤维 |
CN110892018B (zh) * | 2017-07-14 | 2023-10-27 | 阿科玛股份有限公司 | 高强度聚偏二氟乙烯复合材料 |
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Also Published As
Publication number | Publication date |
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NO20090985L (no) | 2009-05-05 |
WO2008017789A3 (fr) | 2008-03-27 |
JP2010500440A (ja) | 2010-01-07 |
EP2052002A2 (fr) | 2009-04-29 |
US20100255378A1 (en) | 2010-10-07 |
FR2904828B1 (fr) | 2008-09-19 |
WO2008017789A2 (fr) | 2008-02-14 |
FR2904828A1 (fr) | 2008-02-15 |
JP5457180B2 (ja) | 2014-04-02 |
CA2660341A1 (fr) | 2008-02-14 |
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