CN102300921A - 基于接枝聚乙烯的粘合剂组合物 - Google Patents
基于接枝聚乙烯的粘合剂组合物 Download PDFInfo
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- CN102300921A CN102300921A CN201080006006XA CN201080006006A CN102300921A CN 102300921 A CN102300921 A CN 102300921A CN 201080006006X A CN201080006006X A CN 201080006006XA CN 201080006006 A CN201080006006 A CN 201080006006A CN 102300921 A CN102300921 A CN 102300921A
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Images
Classifications
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Abstract
本发明涉及粘合剂组合物,它包括,相对于它的总重量:1-40%的接枝了官能化单体的聚乙烯(A)或聚乙烯(A1)与不同于(A1)的第二种聚合物(A2)的共混物,其中(A1)和(A2)的该共混物共接枝了不饱和官能化单体,相对于(A)而言不饱和官能化单体的重量含量是在30-100000ppm范围内;25-98%的具有在0.900-0.965范围的密度的非接枝聚乙烯(B);1-35%的弹性材料产品(C)。本发明还有涉及包括这些组合物的多层结构,该结构能够用于金属管的保护,该金属管用于输油管和输气管的制造。
Description
本发明的领域
本发明涉及包括接枝聚乙烯的粘合剂组合物。
该组合物使得有可能制造出能够用作管材的保护结构的多层结构,并且该管材能够用于例如输油管或输气管的制造。
现有技术
全世界能量需要的发展使得需要构造新的输油管和输气管,以便油和气能够从生产国家运送到消费国。这些输油管和输气管是从连接在一起的金属管制造的。这些金属管一般通过涂层加以保护以避免环境影响从而防止它们的腐蚀,例如用聚烯烃(一般聚丙烯或聚乙烯)的涂层。因为聚烯烃不粘附于金属上,所以一般使用中间层,这使得有可能施涂聚烯烃涂层。例如,有可能使用环氧树脂和聚烯烃-基粘合剂组合物的中间层,在本说明书中也称作“粘结剂”。
图1显示了用保护性的多层结构覆盖的空心金属管(1)的例子。在图1中,该保护结构是从管的金属表面开始,组成如下:环氧树脂的涂层(3),粘结剂的涂层(5)和聚烯烃的涂层(7)。
为了使这些结构能够用于输油管或输气管的构造,它们必须在使用它们的每一个国家中受到批准。一般,批准是在于测量在聚烯烃涂层和环氧树脂涂层之间的粘合性,该粘合性是因为在两层之间粘结剂的存在而提供的。这一批准的条件能够对于各国家而各不同。取决于国家,两层必须在室温下和/或在高温即80℃下粘合。因此需要制造在室温下和在高温下粘合的粘结剂,这样它们能够用于全部的国家,无论批准规程怎样。
现有技术早已描述粘结剂组合物。例如,文件WO2006125913描述了包括密度在0.94至0.98之间的聚乙烯(PE)与聚丙烯的共混物的一种粘结剂,该共混物共接枝了(co-grafté)不饱和官能化单体并且能够被稀释在密度在0.94至0.98之间的非接枝聚乙烯中。该粘结剂用于制造管材,后者用于构造输油管。
该粘结剂在直至高达80℃的环境温度下显示出良好的粘合性。
为了测量该粘合性,在第一阶段中,在管的形成之后,刀子或口凿裁切出舌状物(languette):这构成“涂底漆(amorçage)”阶段。在环氧树脂涂层和聚烯烃涂层之间,与粘结剂相适应地裁切出该舌状物。在第二阶段中,通过将狭口(mors)固定在第一阶段中形成的舌状物上来测量粘合力:通过在舌状物拔出来测量剥离强度。除良好的粘合性之外,因此需要使舌状物涂底漆阶段变得更容易。对于在室温下不可能涂底漆的粘结剂,它需要在加热该管之后进行。这一加热构成了附加的操控阶段。此外,在某些国家中的批准规程禁止该加热,因此阻止了在这些国家中使用这些粘结剂。现在,用描述在该文件中的粘结剂,涂底漆是不容易的或在室温下甚至不可能。
另一种粘结剂组合物已公开在文件EP1043375中,该粘结剂包括密度在0.935至0.980之间的聚乙烯与选自于弹性体、极低密度聚乙烯中的聚合物的共混物,该共混物共接枝了不饱和羧酸并且被稀释于密度在0.93至0.95之间的聚乙烯中。该粘结剂可用于例如在软包装或汽油罐中形成多层结构,并且不涉及用于输油管的制造的金属管。
还有以通过接枝的金属茂催化所获得的聚乙烯为基础的组合物。这些组合物相对于通过自由基聚合或通过齐格勒-纳塔型的催化所获得的接枝聚乙烯具有改进的粘合性能,该催化是按照名称“非金属茂”来分类的。通过金属茂催化获得的聚乙烯,一般是包括α-烯烃共聚用单体的乙烯聚合物,其具有比非金属茂聚乙烯更窄的分子量分布。此外,α-烯烃共聚用单体在金属茂聚乙烯链内的分布是比在各种非金属茂聚乙烯链中更均匀。最终,金属茂聚乙烯的各链包括比非金属茂聚乙烯链更少的支化长链。这些内在的性质会导致该金属茂聚乙烯的物理化学性能,例如熔融状态下的流动性,不同于非金属茂聚乙烯的那些性能。
在描述以接枝金属茂聚乙烯为基础的粘合剂组合物的文件中,可提到例如文件WO 97/27259,它描述粘合剂组合物,后者包括非金属茂聚乙烯,5-35 wt%的特殊接枝金属茂聚乙烯的组合物和任选的至多30
wt%的含烃弹性体。然而,该文件没有描述在高温下保持有效性并且允许在室温下容易涂底漆(如前面所述)的一种粘合剂组合物。另一种粘合剂组合物也描述在文件WO
99/37730中,该组合物包括乙烯和携带酯型的极性官能团的烯属单体的共聚物、5-35 wt%的特殊接枝金属茂聚乙烯的组合物和任选的至多30wt%的含烃弹性体。这些粘合剂配制剂因此包括至少65 wt%的乙烯和携带酯型的极性官能团的烯属单体的共聚物以及弹性体;它们在高温下显示出低的粘合性,这意味着当批准程序需求在高温下的粘合性时它们不能使用。
因此仍然需要寻找新的粘结剂组合物,这使得有可能制造出能够用于输油管或输气管的构造中的多层结构。更具体地说,这些粘结剂必须有可能对于在室温下以及在高温下直接粘结于其上的各层获得良好的粘合性,此外测量这一粘合性的涂底漆必须是在室温下容易的。
本发明的概述
本发明事实上涉及以通过金属茂催化获得的非接枝聚乙烯(B)为基础的新型组合物,这使得有可能克服如上所述的缺点。
该组合物包括,相对于它的总重量而言:
• 1-40%的接枝了不饱和官能化单体的聚乙烯(A)或聚乙烯(A1)与不同于(A1)的第二种聚合物(A2)的共混物,其中(A1)和(A2)的该共混物共接枝了不饱和官能化单体,相对于(A)而言官能化单体的重量含量是在30-100000 ppm范围内;
• 25-98%的具有在0.900-0.965范围的密度的通过金属茂催化获得的非接枝聚乙烯(B);
• 1-35%的弹性材料产品(C)。
该新型组合物在室温下或在高温下(例如80℃)对于许多基材(supports)显示出良好的粘合性,例如聚乙烯或环氧树脂的基材。一般认为,当根据标准NF A 49-710,剥离强度是至少大于250N/cm时,在室温下的粘合性是良好的。一般认为,当剥离强度是至少大于100N/cm(NF
A 49-710)时,在80℃下的粘合性是良好的。该组合物能够用于任何类型的多层结构中。该组合物的优选用途是在引入了(intégrant)包括聚乙烯涂层的结构的管材涂层中。本发明特别可用于涂有聚乙烯(PE)的金属表面。申请人发现,该粘结剂允许在不同层之间具有优异粘合性能的多层结构的形成,但是付出低的制造成本。该结构的涂底漆是容易的,尤其对于环氧树脂/粘结剂/PE涂层型的结构。
本发明的各种优选实施方案描述如下;需要指出,这些各种实施方案能够彼此结合。
有利地,根据本发明的组合物包括,相对于它的总重量,10-30 wt%的接枝聚乙烯或共接枝共混物(A),40-80%的非接枝聚乙烯(B)和10-30 wt%的弹性材料产品(C)。
聚乙烯(B)的密度能够有利地是大于或等于0.925,例如在0.930至0.960之间。
优选,聚乙烯(B)包括至少95 mol%的乙烯。
优选,接枝在聚乙烯上或在共接枝共混物(A)上的官能化单体是不饱和羧酸或该酸的不饱和酸酐。
当聚合物(A)是共接枝共混物,它优选包括90-20份的聚乙烯(A1)和10-80份的聚合物(A2)。
聚合物(A2)有利地是聚烯烃。该聚烯烃优选地选自于乙烯和/或丙烯的均聚物以及共聚物。相当优选,聚烯烃(A2)是不同于(A1)的乙烯和α-烯烃的均聚物或共聚物。
根据一个实施方案,聚合物(A)是金属茂聚乙烯(A1)和非金属茂线性低密度聚乙烯(A2)的共接枝共混物。
优选,(A1)的密度是在0.860-0.96g/cm3范围。优选,(A2)的密度是在0.9-0.94g/cm3范围。
优选,该弹性材料产品(C)具有低于100MPa的挠曲模量,该模量是根据标准ISO 178:2001测量的。
根据本发明的第一个方案,该弹性材料产品(C)是选自乙烯-(甲基)丙烯酸烷基酯共聚物或乙烯-(甲基)丙烯酸烷基酯-马来酸酐三元共聚物。
根据本发明的第二个方案,弹性材料产品(C)是密度在0.860-0.900范围的乙烯与α-烯烃的共聚物,如乙烯和丙烯的共聚物,例如包括二烯烃的乙烯-丙烯橡胶(EPDM),不包括二烯烃的乙烯-丙烯橡胶(EPR)或极低密度聚乙烯(PETBD)。
根据本发明的优选方案,组合物包括:
• 10-30 wt%的由通过金属茂催化(A1)获得的聚乙烯与通过齐格勒-纳塔催化(A2)获得的聚乙烯的共接枝共混物(A),(A1)和(A2)的共混物是用马来酸酐共接枝的,官能化单体相对于(A)的重量含量是在30-100000 ppm范围;
• 40-80%的密度在0.900-0.965范围的非接枝金属茂聚乙烯(B);
• 以及10-30 wt%的乙烯-(甲基)丙烯酸烷基酯共聚物(C)。
本发明的另一个目的是根据本发明的组合物的膜。
本发明还涉及多层结构,它包括在称作“基材层”的至少一个其它层上的本发明组合物的至少一个层。
根据根据本发明的结构的第一种变型,基材层包括聚烯烃,该聚烯烃优选是聚乙烯。
根据根据本发明的结构的第二种变型,基材层包括环氧树脂。
本发明的优选结构包括组合物的涂层,该涂层是在包括环氧树脂的第一基材层和包括聚乙烯的第二基材层之间。
本发明还涉及根据本发明的组合物或结构在管材中的用途,该管材尤其用于金属管的防腐蚀。
本发明还涉及覆盖了根据本发明的结构的管材。管优选是金属的。相当地优选,该管覆盖包括环氧树脂、本发明粘结剂层和聚烯烃涂层的保护用多层结构,这些层是按照从管的内部到外部的顺序布置的。
根据本发明的管能够有利地用于输送气体或液体,相当特别的是石油产品或气体。
在阅读下面给出的叙述之后,其它优点变得更清楚。
附图的叙述
下面的叙述仅仅为了举例说明而给出并且是非限制性的,参见附图,其中早已描述的图1是覆盖了保护结构的管(1)的例子,该保护结构是相继由环氧树脂层(3)、粘结剂层(5)和聚烯烃层(7)组成。
本发明的详细说明
根据本发明的组合物包括,相对于它的总重量:
• 1-40%的接枝了官能化单体的聚乙烯(A)或聚乙烯(A1)与不同于(A1)的第二种聚合物(A2)的共混物,其中(A1)和(A2)的该共混物共接枝了官能化单体,相对于(A)而言官能化单体的重量含量是在30-100000 ppm范围内;
• 25-98%的具有在0.900-0.965范围的密度的通过金属茂催化获得的非接枝聚乙烯(B);
• 1-35%的弹性材料产品(C)。
聚乙烯(PE)(A)或(A1)能够是乙烯的均聚物或包括至少50 mol.%的乙烯和第二种α-烯烃的共聚物。优选,乙烯的摩尔数是大于90%,相当地优选大于95%。
在本说明书中,共聚物是指通过至少两种不同的共聚单体的共聚合获得的聚合物。
1-丁烯,1-己烯,1-辛烯或1-癸烯能够有利地用作能够与乙烯共聚合的第二种α-烯烃。
根据标准ASTM D 1505测量的PE(A)或(A1)的密度能够是0.860-0.96,有利地0.900-0.940,例如0.910-0.935。
相当地优选,聚乙烯(A)或(A1)是线性低密度聚乙烯(PEBDL):该聚合物是具有少量的长链的基本上线性型。“长链”是指在乙烯的聚合过程中产生的链并且不是那些任选通过与乙烯共聚合的第二种α-烯烃所引入的链。根据本发明,长链的数量被认为是低的,当它的平均数是小于或等于0.01,优选小于或等于0.005(对于100个碳原子数)时。
碳链的数量能够根据Randall在Rev. Macromol.
Chem. Phys.,C29,第285-297页中描述的谱定量方法,用核磁共振测量的。
该PEBDL能够通过使用菲利普(Phillips),齐格勒-纳塔或金属茂型的催化剂,用催化方法获得。
根据一个实施方案,该PEBDL是金属茂聚乙烯。在本申请中,金属茂聚乙烯表示在一般由金属例如锆或钛的原子和键接于该金属上的两个环状烷基分子组成的单位点(mono-site)催化剂存在下所制造的PE。更具体地说,该金属茂催化剂通常是由键接于金属上的两个环戊二烯环组成。这些催化剂常常与作为助催化剂或活化剂的铝氧烷(aluminoxanes),优选甲基铝氧烷(MAO),一起使用。铪也能够用作有环戊二烯固定在其上的金属。其它金属茂能够包括IV A,V A,和VI A族的过渡金属。镧系元素的金属也能够使用。
根据本发明,该PE (A)或(A1)能够是通过金属茂催化获得的聚乙烯。通过金属茂催化获得的聚乙烯有利地通过它的
/比率<3和优选<2来表征,其中和分别表示重均分子量和数均分子量。另外地,它也能够具有低于6.53的MFR(熔体流动速率)或熔体流动指数(MFI)以及大于MFR减去4.63的Mw/Mn比率。MFR表示MFI10(在10 kg的负荷下在190℃下的MFI)与MFI2(在2.16 kg的负荷下在190℃下的MFI)的比率。其它金属茂聚乙烯是通过大于或等于6.13的MFR以及小于或等于MFR减去4.63的Mw/Mn比率来定义的。
根据本发明,重均分子量和数均分子量的比率能够例如在将聚合物溶解在四氢呋喃中之后由凝胶渗透色谱法(GPC)测量。
当使用聚乙烯(A1)与第二种聚合物(A2)的共混物时,(A2)不同于(A1)。有利地,聚合物(A2)是聚烯烃。聚烯烃优选地是选自乙烯的均聚物或乙烯与另一种烯烃例如1-丁烯,1-己烯,1-辛烯或1-癸烯的共聚物。优选,聚合物(A2)是聚乙烯和相当地优选是线性低密度聚乙烯。优选,该PEBDL是通过齐格勒-纳塔催化获得的。
“齐格勒-纳塔”催化剂一般是由4或5族的过渡金属例如钛或钒的卤代化合物以及2、12、13族的金属例如铍、镁、锌或铝的烷基化化合物组成。例如,可以提到TiCl4与Al(C2H5)3的结合物。
(A2)的密度能够是在0.9-0.94范围内,例如0.905-0.925范围内。
根据本发明的尤其优选的变型,(A)是通过金属茂催化获得的聚乙烯(A1)与非金属茂聚乙烯(A2)的共混物。根据这一变型,聚乙烯(A2)优选是PEBDL。聚乙烯(A2)能够通过齐格勒-纳塔催化来获得。
聚乙烯(A)或聚乙烯(A1)和聚合物(A2)的共混物(共)接枝了不饱和官能化单体。
优选,不饱和官能化单体是选自下列这些中的单体:
• 不饱和羧酸类和它的盐,优选具有2-30个碳原子的那些,例如丙烯酸或甲基丙烯酸和这些酸的盐;
• 羧酸酐,优选具有4-30个碳原子的那些:它们能够例如选自于马来酸,衣康酸,柠康酸,烯丙基琥珀酸,环己-4-烯-1,2-二羧酸,4-亚甲基环己-4-烯-1,2-二羧酸,双环(2,2,1)庚-5-烯-2,3-二羧酸,和x-甲基双环(2,2,1)庚-5-烯-2,2-二羧酸的酸酐。
优选,马来酸酐用作不饱和官能化单体。
(A)的量(重量)是相对于组合物的总重量的1-40%,有利地在5-40%之间,优选10-35%,或甚至10-30%。
接枝反应能够根据在溶液中的间歇方法,或优选,根据用熔体混合设备的连续方法来进行,这些是所属技术领域的专业人员公知的技术。对于连续接枝的方法,使用所属技术领域的专业人员已知的将塑料在熔化状态下挤出的设备。作为例子,可以提到密炼机(internal
mixers),辊式混合器(roller mixers),单螺杆挤出机(single-screw extruders),反转或顺转式双螺杆挤出机(counter-rotating
or co-rotating twin-screw extruders),连续共捏合机(continuous
co-kneaders)。接枝设备能够是以上所述的设备中的一种或它们的结合,例如与单螺杆挤出机相结合的共捏合机,与泵相结合的顺转式双螺杆挤出机。对于挤出,该设备优选包括聚合物熔化区段,在所存在的物质之间的混合和反应用的区段以及除去挥发性化合物的保持/脱气区段。该设备能够装有过滤系统和/或棒材切粒或水下造粒的系统。聚乙烯(A)或聚乙烯(A1)和聚合物(A2)的共混物,在自由基产生剂和官能化单体的存在下,被加入到该设备中,该设备的主体温度被控制,该温度被选择与自由基产生剂的分解的动力学相匹配。作为连续接枝用的自由基产生剂,优选使用各种类型的二烷基过氧化物,氢过氧化物或过氧酮缩醇(peroxycétals)。优选,使用在100-300℃,更优选180-250℃范围的温度。
聚乙烯,接枝用单体和自由基产生剂能够同时或单独地加入到挤出设备中。尤其,单体和/或自由基产生剂能够与作为主要原料的聚合物同时加入,或单独通过沿着该设备的液体注射来加入。
在注射阶段中,单体和/或自由基产生剂能够与一部分的聚合物的溶剂掺混。这一部分的溶剂具有促进反应性物质的混合以及在脱气阶段中挥发性化合物的除去的目的。
在保持/脱气阶段中,施加适合于挥发性化合物的脱挥发分的真空,并且真空的水平能够是几个毫巴-几百毫巴。
该接枝聚合物能够在挤出设备的出料端,利用造粒设备以粒料的形式被回收。
在接枝改性的聚合物中,接枝到聚合物(A)上的单体的量能够适当地选择,一般是在30-100000 ppm,优选600-50000 ppm范围,相对于接枝聚合物的总重量。接枝到聚合物(A)上的单体的量是利用傅里叶转换红外光谱分析法,由丁二酸官能团的测定来获得的。
非接枝聚乙烯(B)是具有在0.900-0.965范围的密度的聚乙烯,即它能够是低密度聚乙烯,PEBDL,中密度聚乙烯或高密度聚乙烯。该聚乙烯(B)能够选自乙烯的均聚物或乙烯与另一种烯烃例如1-丁烯,1-己烯,1-辛烯或1-癸烯的共聚物。PE(B)的密度有利地是在0.900-0.960范围。它能够是大于0.925,优选在0.925至0.960之间,例如在0.930至0.940之间。该PE(B)是通过金属茂催化获得的。金属茂聚乙烯能够有利地通过比率/<3和优选<2来表征,其中和分别表示重均分子量和数均分子量。“金属茂聚乙烯”也表示具有低于6.53的MFR(熔体流动速率或MFI熔体流动指数)以及大于MFR减去4.63的Mw/Mn比率的聚乙烯。MFR表示MFI10(在10 kg的负荷下在190℃下的MFI)与MFI2(在2.16
kg的负荷下在190℃下的MFI)的比率。其它金属茂聚乙烯是通过大于或等于6.13的MFR以及小于或等于MFR减去4.63的Mw/Mn比率来定义的。
相对于组合物的总重量,(B)的量(重量)是在25-98%,优选40-80%范围内。
有利地,非接枝聚乙烯(B)包括至少90 mol.%的乙烯,优选至少95 mol.%的乙烯。
该弹性材料产品(C)与(A)和(B)不同。
弹性材料产品(C)能够具有小于或等于100MPa,优选小于或等于80MPa,相当优选小于或等于40MPa的挠曲模量,该模量是根据标准ISO 178:2001测量的。该挠曲模量也能够大于1MPa。
作为弹性材料产品(C)的例子,可以提到选自下列这些中的聚合物:
• 密度在0.860-0.90范围的乙烯-α-烯烃共聚物,如选自EPR(乙烯-丙烯-橡胶的缩写)和EPDM(乙烯-丙烯-二烯烃的缩写)中的乙烯-丙烯共聚物,和极低密度聚乙烯(PETBD),它们一般是乙烯-丁烯-1,乙烯-己烯-1,乙烯-辛烯-1共聚物;
• 乙烯-(甲基)丙烯酸烷基酯共聚物或乙烯-(甲基)丙烯酸烷基酯-马来酸酐共聚物;
• 乙烯和羧酸乙烯基酯的共聚物,如乙烯-乙酸乙烯基酯共聚物;
• 苯乙烯/乙烯-丁烯/苯乙烯(SEBS),苯乙烯/丁二烯/苯乙烯(SBS),苯乙烯/异戌二烯/苯乙烯(SIS),苯乙烯/乙烯-丙烯/苯乙烯(SEPS)嵌段共聚物或苯乙烯-丁二烯无规(SBR)共聚物;
• 聚异戊二烯;
• 聚丁二烯。
相对于组合物的总重量,(C)的量(重量)是在1-35%,优选10-30%范围内。
根据一个实施方案,该组合物包括,相对于它的总重量,5-40wt%(上、下限被排除)的接枝聚乙烯或共接枝共混物(A),30-75wt%的非接枝聚乙烯(B)和10-30 wt%的产品(C)。
根据另一个实施方案,该组合物包括,相对于它的总重量,10-30wt%的接枝聚乙烯或共接枝共混物(A),40-80wt%的非接枝聚乙烯(B)和10-30 wt%的产品(C)。优选,组合物包括,相对于它的总重量,12-25 wt%的接枝聚乙烯或共接枝共混物(A),50-76%的非接枝聚乙烯(B)和12-25 wt%的产品(C)。
根据本发明的组合物能够通过热塑性塑料生产的已知技术,例如通过捏合(malaxage)或挤出,来制备。
本发明的粘结剂能够任选地包括各种添加剂如抗氧化剂,紫外线吸收剂,抗静电剂,成核剂,填料,润滑剂和阻燃产品。
紫外线吸收剂的例子是2,4-二羟基二苯甲酮,2-(2’-羟基-3’,5’-二-叔丁基苯基)-5-氯苯并三唑,2-(2-羟基-3-叔丁基-5-甲基苯基)-5-氯苯并三唑,和双(2,2’,6,6’)-四甲基-4-哌啶)癸二酸酯。
抗氧化剂的例子是2,6-二-叔丁基-对-甲酚,O-叔丁基-对-甲酚,四[亚甲基-3-(3,5-二叔丁基-4-羟苯基)丙酸酯]甲烷,对-萘基胺,和对-苯二胺。
抗静电剂的例子是月桂基二乙醇胺,棕榈酰基二乙醇胺,硬脂基二乙醇胺,油基二乙醇胺,二十二烷基二乙醇胺,聚氧化乙烯-烷基胺,硬脂基-甘油单酸酯,和2-羟基-4-正辛氧基二苯甲酮。
成核剂的例子是对-叔丁基苯甲酸铝,二亚苄基-山梨糖醇和羟基-二-对-叔丁基苯甲酸铝。
能够使用的填料是例如玻璃纤维,碳纤维,滑石,粘土,硅石,碳酸钙,硫酸钡,氢氧化镁,氢氧化钙和氧化钙。
润滑剂的功能是促进组合物的制造,尤其它的挤出。润滑剂的例子是硬脂酰胺,油酰胺,芥酰胺,硬脂酸钙,硬脂酸锌,硬脂酸铝,硬脂酸镁,和聚乙烯蜡。
阻燃产物的例子是金属氢氧化物,卤化试剂,氧化锑,十溴双苯基醚,和双(3,5-二溴-4-溴丙氧基苯基)砜。
这些其它添加剂的量能够选自对于本发明的粘结剂不具有有害影响的合适量。例如,相对于组合物的总重量,合适量是约0.01-5
wt%的抗氧化剂;约0.01-5 wt%的紫外线吸收剂;约0.01-1
wt%的抗静电剂;约0.01-5 wt%的成核剂;约0.1-60
wt%的填料;约0.01-1 wt%的润滑剂;和约0.1-50
wt%的阻燃产品。
根据本发明的组合物能够通过使用用于混合热塑性材料的已知技术,例如挤出或捏合,将各种聚烯烃与任选的添加剂混合来获得。能够使用具有桨叶或转子的密炼机,外部混合器,单螺杆挤出机,或顺转式或反转式双螺杆挤出机。优选,所使用的设备的温度是在90-250℃范围,相当优选是在120℃至200℃之间。
有利地,最终组合物具有在1-10 g/10min范围的MFI(190℃,2.16 kg)。
通过用于膜的制造中的已知技术,例如扁平模头挤塑(也称作“挤塑”)或吹气-鼓泡挤出,从粘结剂组合物制造膜。优选,膜具有在0.05
mm-2 mm范围的厚度。
本发明涉及多层结构,它包括在至少一个基材层上的根据本发明的组合物的层;与根据本发明的组合物的层直接接触的层被称作“基材层”。
组合物的层优选具有在0.05 mm-2 mm范围的厚度。
根据一个实施方案,根据本发明的组合物的层与包括环氧树脂的基材层接触。在施涂之前,该环氧树脂能够呈现粉末的形式。优选该层具有在0.1-10
mm范围的厚度。
根据另一个实施方案,根据本发明的组合物的层与包括聚烯烃的基材层接触。有利地,该聚烯烃是聚乙烯。优选,聚乙烯具有大于或等于0.92,优选在0.92-0.97范围,相当地优选0.94-0.97的密度。
特别优选的结构结合了这最后两个实施方案;即它是这样一种结构,该结构相继包括:包括环氧树脂的第一基材层,根据本发明的组合物的层以及包括聚烯烃(优选聚乙烯)的层。优选这一层具有在1-50 mm范围内的厚度。
这些结构能够用于金属管的防腐或用于输气管或输油管的制造。
本发明的另一个目的是包括根据本发明的结构的管。该管优选是由金属制成。相当优选,根据本发明的管包括下列相继各层:金属的层/包括环氧树脂的层/根据本发明的粘结剂的层/包括聚乙烯的保护层,这些层是按照从管的内部到外部的顺序布置的。
所属技术领域的专业人员已知的技术能够用于制造根据本发明的管。例如,能够使用共挤塑的技术。当管的中心是金属时,能够例如使用这一种优选的管制造方法:
• 加热该金属管,例如在150-250℃范围;
• 将粉末形式的包括环氧树脂的组合物施涂在该管上;环氧树脂然后被转化成熔化状态;
• 其次,将粘结剂组合物的膜施涂于熔化状态的环氧树脂上;
• 第三,用熔化状态的包括聚乙烯的组合物覆盖粘结剂组合物的熔化膜。
根据本发明的管能够有利地用于输送气体或液体,相当特别的是石油产品或气体。
本发明现在用如下所述的实施方案的具体例子来举例说明。需要指出的是,这些实施例无论如何不希望限制本发明的范围。
实施例
下列产物用于制备根据本发明的组合物的例子并且评价与现有技术的组合物相比的本发明优点。
共接枝共混物
(A)
:制备
包含在(A)中的聚合物是具有0.934的密度的通过金属茂催化(A1)获得的PEBDL与具有0.920的密度的通过齐格勒-纳塔催化(A2)获得的PEBDL分别按照70/30的重量比的共混物。下面的规程用来生产共接枝聚合物的共混物:
首先,(A1)和(A2)在袋中被混合。该混合物然后被加入到包括8个加热区段并具有下列温度分布图(从进料斗到挤出机机头)的顺转式挤出机中:190℃/190℃/210℃/240℃/250℃/250℃/230℃/230℃。马来酸酐(1.5
wt%,相对于所引入聚合物的重量)和以2,5-二(叔丁基过氧基)-2,5-二甲基己烷(Luperox® 101)为基础的自由基引发剂被加入到第二区段中。用马来酸酐共接枝的共混物是在挤出机排放口时获得的。
非接枝聚乙烯
(B)
mPE M 3427 是具有0.934的密度和2.7 g/10min的MFI的通过金属茂催化获得的由Total
Petrochemicals生产的聚乙烯(ASTM D 1238,2.16 kg,190℃)。
弹性体化合物
(C)
ENGAGE® EG 8200G 是具有28 MPa的挠曲模量(ISO 178:2001)和0.882的密度的由DOW生产的极低密度聚乙烯。
LOTRYL®
30BA02 是具有9 MPa的挠曲模量(ISO 178:2001)的由Arkema生产的乙烯-丙烯酸丁酯共聚物。
根据本发明的组合物(EX1,EX2和EX3)和对比组合物(CP1和CP2)与它们的重量比一起示于表1中:
表1
EX1 | EX2 | CP1 | CP2 | |
CO-GRAFT (A) | 25 | 25 | 25 | 80 |
mPE M 3427 | 55 | 55 | 75 | |
ENGAGE® EG 8200G | 20 | |||
LOTRYL® 30BA02 | 20 | 20 |
也通过在与共接枝共混物(A)的制造中相同的条件下由80%的mPE M 3427和20% LOTRYL® 30BA02的混合物共接枝,来进行对比实施例3(CP3)。
为了从根据本发明的配方和对比配方制造膜,首先该配方的各成分(A)、(B)和/或(C)在袋中被混合。这些成分的这一混合物然后被加入到包括8个加热区段并具有下列温度分布图(从进料斗到挤出机机头)的顺转式挤出机中:190℃/190℃/210℃/240℃/250℃/250℃/230℃/230℃。对于20 kg/h的流速,螺杆的转速设定在250转/分。在挤出机出口有允许组合物形成膜的平模(filière plate)。
钢管被加热至195℃。环氧树脂(Eurocote 714.4)通过喷涂被施涂于该管上。该树脂,它被认为是凝胶的形式,是在25秒之后通过辊压先前获得的粘合剂组合物的挤出薄膜而被覆盖。高密度聚乙烯4206B(Total
Petrochemicals)的3 mm厚度层立即通过辊压在仍然处于熔化状态的该粘结剂上来施涂。
该管然后用水冷到室温。
与粘合性相关的结果列于表2中。为了测量环氧树脂和PE层的粘合性,在第一阶段中通过在室温下使用刀分离舌状物来进行涂底漆;当在室温下的涂底漆是可能的时,术语“OK”示于表2的“RT涂底漆”行中。如果在室温下涂底漆是不可能的,在分离该舌状物之前该管首先被加热;当在室温下涂底漆是不可能的时,术语“失败(fail)”示于表2的“RT涂底漆”行中。
一旦该舌状物被分离,试样被放入到控制的加热室中并且标准NF A 49-710的规程用于测量该剥离强度。在23℃和80℃下进行试验;获得的结果也示于表2中。
表2
EX1 | EX2 | CP1 | CP2 | CP3 | |
RT涂底漆 | OK | OK | Fail | OK | OK |
剥离强度,23℃ | 371 | 295 | 271 | 159 | 180 |
剥离强度,80℃ | 169 | 124 | 160 | 未测量 | 70 |
根据本发明的粘结剂在室温下和在高温下都具有优异的的粘合性。EX1和CP2表明,当按照根据本发明的组合物的比例,部分的接枝聚合物(A)被非接枝聚乙烯(B)替代时,在室温下改进粘合性。
Claims (15)
1.组合物,它包括,相对于它的总重量:
• 1-40%的接枝了官能化单体的聚乙烯(A)或聚乙烯(A1)与不同于(A1)的第二种聚合物(A2)的共混物,其中(A1)和(A2)的该共混物共接枝了不饱和官能化单体,相对于(A)而言不饱和官能化单体的重量含量是在30-100000 ppm范围内;
• 25-98%的具有在0.900-0.965范围的密度的通过金属茂催化获得的非接枝聚乙烯(B);
• 1-35%的弹性材料产品(C)。
2.根据权利要求1的组合物,特征在于组合物包括,相对于它的总重量,10-30 wt%的接枝聚乙烯或共接枝共混物(A),40-80%的非接枝聚乙烯(B)和10-30 wt%的弹性材料产品(C)。
3.根据权利要求1-2中一项的组合物,其中聚乙烯(B)的密度大于或等于0.925。
4.根据权利要求1-3中一项的组合物,其中聚乙烯(B)的密度是在0.930至0.960之间。
5.根据权利要求1-4中一项的组合物,其中接枝在聚乙烯上或在混合物(A)上的官能化单体是不饱和羧酸或该酸的不饱和酸酐。
6.根据权利要求1-5中一项的组合物,其中(A2)是聚烯烃。
7.根据权利要求6的组合物,其中聚烯烃(A2)是不同于(A1)的聚乙烯。
8.根据权利要求7的组合物,特征在于(A)是(A1)和(A2)的共接枝共混物和该共混物包括80-20份的密度在0.865-0.950范围内的由金属茂催化(A1)获得的聚乙烯和20-80份的密度在0.900-0.940 g/cm3范围内的由齐格勒-纳塔催化获得的线性低密度聚乙烯(A2)。
9.根据权利要求1-8中一项的组合物,其中(C)具有低于100MPa的挠曲模量,该模量是根据标准ISO 178:2001来测量的。
10.根据权利要求1-9中一项的组合物,其中(C)选自乙烯-(甲基)丙烯酸烷基酯共聚物或乙烯-(甲基)丙烯酸烷基酯-马来酸酐三元共聚物。
11.根据权利要求1-9中一项的组合物,其中(C)是密度在0.860-0.90范围的乙烯与α-烯烃的共聚物。
12.多层结构,它包括在称作“基材层”(3,7)的至少一个其它层上的根据权利要求1-11中一项的组合物(5)的至少一个层。
13.根据权利要求12的结构,其中组合物(5)的层被插入在包括环氧树脂(3)的第一基材层与包括聚乙烯(7)的第二基材层之间。
14.根据权利要求1-11中一项的组合物或根据权利要求12或13的结构在管中的用途。
15.根据权利要求12或13的结构在金属管的防腐中的用途。
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CN104531005A (zh) * | 2014-12-19 | 2015-04-22 | 上海邦中新材料有限公司 | 一种埋地排水用钢带增强聚乙烯管用粘结树脂 |
CN110821046A (zh) * | 2019-11-20 | 2020-02-21 | 北京市建筑工程研究院有限责任公司 | 一种缓粘结预应力筋及其制备方法 |
CN112111097A (zh) * | 2020-09-23 | 2020-12-22 | 上海长园电子材料有限公司 | 一种热缩套管的配方及制备方法和应用 |
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RU2505574C1 (ru) * | 2012-12-07 | 2014-01-27 | Закрытое акционерное общество "МЕТАКЛЭЙ" (ЗАО "МЕТАКЛЭЙ") | Термопластичный адгезив |
CN103289599B (zh) * | 2013-05-07 | 2016-05-04 | 安徽金门工贸有限公司 | 一种耐低温封边热熔胶及其制备方法 |
FR3009516B1 (fr) | 2013-08-09 | 2021-01-29 | Arkema France | Structure multicouche pour un tube |
CN103709974B (zh) * | 2013-12-31 | 2015-10-07 | 广州市合诚化学有限公司 | 一种低加工温度粘接树脂及其制备方法与应用 |
WO2015181333A1 (en) * | 2014-05-28 | 2015-12-03 | Cryovac, Inc. | Multilayer heat shrinkable films |
US9650548B2 (en) * | 2014-08-06 | 2017-05-16 | Equistar Chemicals, Lp | Polyolefin-based compositions, adhesives, and related multi-layered structures prepared therefrom |
CN104497931B (zh) * | 2014-12-10 | 2016-08-24 | 上海邦中新材料有限公司 | 一种用于铜塑复合板的粘结树脂 |
WO2016091543A1 (en) * | 2014-12-11 | 2016-06-16 | Sabic Global Technologies B.V. | Polymer compositions for thermal spray coating |
RU2600167C2 (ru) * | 2014-12-30 | 2016-10-20 | Публичное акционерное общество "СИБУР Холдинг" | Адгезионная композиция на основе полиэтилена |
US10633524B2 (en) | 2016-12-01 | 2020-04-28 | Cryovac, Llc | Multilayer heat shrinkable films |
CN107559539A (zh) * | 2017-09-29 | 2018-01-09 | 江苏天时新材料科技有限公司 | 三层pe结构防腐层 |
RU2768173C1 (ru) * | 2018-11-06 | 2022-03-23 | Публичное акционерное общество "СИБУР Холдинг" | Адгезионная композиция на основе полиэтилена с улучшенной долговременной стабильностью, способ ее получения и применение |
WO2020096475A1 (en) * | 2018-11-06 | 2020-05-14 | Public Joint Stock Company "Sibur Holding" | Adhesive polyethylene composition, process for manufacturing and use of the same |
RU2705584C1 (ru) * | 2018-11-07 | 2019-11-08 | Публичное Акционерное Общество "Нижнекамскнефтехим" | Адгезионная полиэтиленовая композиция для изоляционного покрытия стальных труб |
CN115612424B (zh) * | 2022-12-21 | 2023-03-21 | 广州鹿山新材料股份有限公司 | 耐高温胶粘剂及其制备方法和应用 |
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US4452942A (en) * | 1982-02-19 | 1984-06-05 | Chemplex Company | Adhesive blends containing anacid or anhydride grafted LLDPE |
US4684576A (en) * | 1984-08-15 | 1987-08-04 | The Dow Chemical Company | Maleic anhydride grafts of olefin polymers |
US5352739A (en) * | 1992-11-06 | 1994-10-04 | Exxon Chemical Patents Inc. | Compatibilization of elastomer blends |
US6545091B1 (en) | 1996-01-25 | 2003-04-08 | E. I. Du Pont De Nemours & Co. | Adhesive compositions based on blends of grafted metallocene catalyzed and non-grafted conventional polyethylenes |
US6166142A (en) | 1998-01-27 | 2000-12-26 | E. I. Du Pont De Nemours And Company | Adhesive compositions based on blends of grafted metallocene catalyzed and polar ethylene copolymers |
DE60028113T2 (de) | 1999-04-06 | 2006-12-28 | Arkema France | Koextrusionbindung, seine Verwendung für eine Multischichtstruktur und die Struktur hergestellt davon |
FR2886307B1 (fr) | 2005-05-26 | 2007-07-13 | Arkema Sa | Liant de coextrusion de pe et pp cogreffes dilues dans un pe non greffe. |
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CN104531005A (zh) * | 2014-12-19 | 2015-04-22 | 上海邦中新材料有限公司 | 一种埋地排水用钢带增强聚乙烯管用粘结树脂 |
CN110821046A (zh) * | 2019-11-20 | 2020-02-21 | 北京市建筑工程研究院有限责任公司 | 一种缓粘结预应力筋及其制备方法 |
CN112111097A (zh) * | 2020-09-23 | 2020-12-22 | 上海长园电子材料有限公司 | 一种热缩套管的配方及制备方法和应用 |
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BRPI1006977A2 (pt) | 2016-04-12 |
IL213849A0 (en) | 2011-07-31 |
DK2384352T3 (da) | 2013-02-18 |
CN102300921B (zh) | 2015-09-02 |
EA018678B1 (ru) | 2013-09-30 |
PL2384352T3 (pl) | 2013-04-30 |
BRPI1006977B1 (pt) | 2019-06-04 |
US8247053B2 (en) | 2012-08-21 |
CO6410239A2 (es) | 2012-03-30 |
FR2941701B1 (fr) | 2012-04-06 |
FR2941701A1 (fr) | 2010-08-06 |
MX2011007855A (es) | 2011-08-15 |
WO2010086559A1 (fr) | 2010-08-05 |
US20110318517A1 (en) | 2011-12-29 |
AR075178A1 (es) | 2011-03-16 |
EP2384352A1 (fr) | 2011-11-09 |
BRPI1006977B8 (pt) | 2022-11-08 |
EA201101143A1 (ru) | 2011-12-30 |
ES2399815T3 (es) | 2013-04-03 |
IL213849A (en) | 2015-01-29 |
EP2384352B1 (fr) | 2012-11-14 |
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