CN1409745A - 树脂结构体及其用途 - Google Patents
树脂结构体及其用途 Download PDFInfo
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- CN1409745A CN1409745A CN00817028A CN00817028A CN1409745A CN 1409745 A CN1409745 A CN 1409745A CN 00817028 A CN00817028 A CN 00817028A CN 00817028 A CN00817028 A CN 00817028A CN 1409745 A CN1409745 A CN 1409745A
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Abstract
一种热塑性树脂结构体,其特征是,实质上是采用由(a)聚酰胺树脂5~80体积%及(b)聚亚苯基硫醚树脂95~20体积%组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成(b)聚亚苯基硫醚树脂成为基体相(连续相)、(a)聚酰胺树脂成为分散相的相结构,该结构体可用于制成阻挡性、强度、耐久性、成型加工性优良的塑料容器、管状体及其附属部件。
Description
技术领域
本发明涉及气体和/或液体的耐透过性优良的热塑性树脂结构体及其用途。特别是涉及,通过使聚酰胺树脂和聚亚苯基硫醚树脂形成特定的相结构,从而得到具有优异的耐透过性、低吸水性、吸湿时的尺寸稳定性和成型加工性,适于制作气体和/或液体的阻挡部件的树脂成型品以及适于制作油、汽油等化学剂液贮存及输送用容器、配管类、食品用、医用包装材料及容器等的叠层结构体及其用途。
背景技术
聚酰胺树脂,由于其平衡性好地具备机械特性、耐热性、耐药品性及成型性,因此,广泛用于电气电子部件及汽车部件等。另外,近几年来,为了确保安全性、保存稳定性,尤其是环境污染防止性,在防止内容物的泄漏及外部气体的混入等目的方面,要求对气体有阻挡性(耐透过性)的树脂成型品在增加,其中,聚酰胺树脂,因具有优良的气体阻挡性,从而作为各种成型品而在使用。然而,聚酰胺树脂,通过吸湿使强韧性更加提高的另一面,是尺寸变化及刚性等下降,以及在高湿度下使用时,化学剂液及气体的耐透过性下降,很多情况下,其使用范围受到限制,所以,希望加以改善。
为了改善这种聚酰胺树脂的物理性质,此前,有方案提出一种与耐水性、耐透过性优良而韧性及成型加工性等有问题的聚亚苯基硫醚(以下简称为PPS树脂)组合的树脂组合物及成型体。
然而,与聚酰胺树脂单体相比,这些方法的确使吸水时的尺寸稳定性及刚性得到提高,但未必能满足要求。另外,在用于要求耐透过性及刚性的场合,还不能说是充分的。因此,进一步要求兼备聚酰胺树脂具有的特性和PPS树脂具有的特性、高度地特性平衡优良的成型材料。
另外,在把阻挡性高的树脂构成的阻挡层加以层压得到的叠层结构体中,作为形成阻挡层的树脂,其代表例可以举出聚酰胺树脂(例如,特开昭58-220738号公报)。然而,最近,作为汽车燃料的汽油和醇类的混合物、所谓的气醇的使用机会也在增加,在这种情况下,采用现有技术制得的塑料容器,其阻挡性不充分,所以,希望有一种把阻挡性更加提高的技术。
另一方面,人们已知PPS树脂对汽油和汽车油等化学剂液及水、二氧化碳气体显示出极高的阻挡性,提出了使用它的吹塑成型中空容器及管状体等(例如,特开昭62-90216号公报、特开昭61-255832号公报、特开平3-32816号公报等)。然而,由于PPS树脂和其他树脂的层间粘合性不充分,所以难以与以聚乙烯、聚丙烯等聚烯烃系材料为首的其他树脂材料共挤出或层压加工等。
本发明以实现聚酰胺树脂具有的机械强度及韧性、和PPS树脂具有的低吸水性及耐透过性的高度的平衡作为课题,目的是要提供一种尽可能抑制作为聚酰胺树脂本质特征的由吸湿所引起的尺寸变化及刚性等机械性质下降和化学剂液、气体的耐透过性降低的热塑性树脂结构体,特别是适用于气体和/或液体阻挡部件的聚酰胺-PPS系树脂成型体,以及适于制作阻挡性、成型加工性、层间粘合性、强韧性优良、可提高制造稳定性和经济性的优良的塑料容器的理想的叠层结构体。
发明的公开
本发明人为了解决上述课题而进行探讨的结果发现,把聚酰胺树脂和PPS树脂配合特定量,再根据需要配合无机填料,在所得到的树脂组合物中,其树脂相分离结构通过控制分散结构,使PPS树脂相在结构体中形成连续的相,可以解决上述课题,从而完成本发明。
即,本发明提供:
1.一种热塑性树脂结构体,其特征是,实质上是采用由(a)聚酰胺树脂5~80体积%及(b)聚亚苯基硫醚树脂95~20体积%组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成(b)聚亚苯基硫醚树脂成为基体相(连续相)、(a)聚酰胺树脂成为分散相的相结构。
2.上述(1)中所述的热塑性树脂结构体,其特征是,(a)聚酰胺树脂和(b)聚亚苯基硫醚的混合比率分别为55~80体积%及45~20体积%。
3.上述(1)中所述的热塑性树脂结构体,其特征是,(a)聚酰胺树脂和(b)聚亚苯基硫醚的混合比率分别为60~75体积%及40~25体积%。
4.一种热塑性树脂结构体,其特征是,是采用相对于由(a)聚酰胺树脂15~85体积%及(b)聚亚苯基硫醚85~15体积%构成的树脂组合物100重量份,含有(c)无机填料0~200重量份的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成由(b)聚亚苯基硫醚树脂构成的相和由(a)聚酰胺树脂构成的相都是实质的连续相的相结构。
5.一种热塑性树脂结构体,其特征是,是采用由(a)聚酰胺树脂55~95体积%及(b)聚亚苯基硫醚树脂45~5体积%所组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成由由(a)聚酰胺树脂构成的连续相和由(b)聚亚苯基硫醚树脂构成的带状分散相构成的相结构。
6.权利要求1~5中的任何1项所述的热塑性树脂结构体,其特征是,相对于(a)成分的聚酰胺树脂及(b)成分的聚亚苯基硫醚的合计量100重量份,含有(c)无机填料0.5~200重量份。
7.一种成型品,其特征是,是(1)~(6)中的任何1项所述的热塑性树脂结构体的成型品,是采用从注射成型、注射压缩成型、压缩成型中选择的至少一种方法成型的。
8.一种化学剂液或气体的输送或贮存用容器,其特征是,是加工上述(1)~(7)中任何1项所述的热塑性树脂结构体而得到的。
9.一种化学剂液或气体的输送或贮存用容器的附属部件,其特征是,是加工上述(1)~(7)中任何1项所述的热塑性树脂结构体而得到的。
10.一种叠层结构体,其特征是,上述(1)~(6)中的任何1项所述的热塑性树脂结构体构成阻挡层。
11.上述(10)所述的叠层结构体,其特征是,在阻挡层的一个面或两个面上形成相邻层,构成该相邻层的树脂层,是与构成阻挡层的热塑性树脂结构体不同的热塑性树脂层构成的。
12.上述(11)所述的叠层结构体,其特征是,构成相邻层的热塑性树脂是从聚烯烃树脂、热塑性聚酯树脂、聚酰胺树脂、聚碳酸酯树脂、ABS树脂中选择的至少1种树脂。
13.上述(11)所述的叠层结构体,其特征是,构成相邻层的热塑性树脂是高密度聚乙烯。
14.上述(11)所述的叠层结构体,其特征是,在阻挡层和相邻层之间构成粘合层。
15.上述(10)~(14)中的任何1项所述的叠层结构体,其特征是,是采用共挤出成型法成型的。
16.上述(10)~(15)中的任何1项所述的叠层结构体,其特征是,使用共挤出成型法,成型为多层管或多层吹塑中空成型体。
附图的简单说明
图1是PPS树脂成分(PPS)形成连续相、聚酰胺树脂成分(PA)形成分散相的相结构模型图。
图2是PPS树脂成分和聚酰胺树脂成分都形成实质的连续相的相结构例模型图。
图3是聚酰胺树脂成分形成连续相,PPS树脂成分以多个薄的2维重叠的带(层)状形式形成分散相的相结构模型图。
图4是显示实施例13中得到的树脂结构体的相分离结构的电子显微镜照片,黑色部分为PPS树脂成分。
图5是显示实施例14中得到的树脂结构体的相分离结构的电子显微镜照片,黑色部分为PPS树脂成分。
图6是显示实施例15中得到的树脂结构体的相分离结构的电子显微镜照片,黑色部分为PPS树脂成分。
图7是显示比较例5中得到的树脂结构体的相分离结构的电子显微镜照片,黑色部分为PPS树脂成分。
实施发明的最佳方案
下面说明本发明的实施方案。在本发明中,所谓“重量”,意指“质量”。
本发明中使用的(a)聚酰胺树脂,是以氨基酸、内酰胺或二胺和二羧酸作为主要构成成分的聚酰胺。作为其主要构成成分的代表例,可以举出6-氨基己酸、11-氨基十一烷酸、12-氨基十二烷酸、对氨基甲基安息香酸等氨基酸;ε-己内酰胺、ω-月桂内酰胺等内酰胺;四亚甲基二胺、六亚甲基二胺、2-甲基五亚甲基二胺、九亚甲基二胺、十一亚甲基二胺、十二亚甲基二胺、2,2,4-/2,4,4-三甲基六亚甲基二胺、5-甲基九亚甲基二胺、间苯二甲基二胺、对苯二甲基二胺、1,3-双(氨基甲基)环己烷、1,4-双(氨基甲基)环己烷、1-氨基-3-氨基甲基-3,5,5-三甲基环己烷、双(4-氨基环己基)甲烷、双(3-甲基-4-氨基环己基)甲烷、2,2-双(4-氨基环己基)丙烷、双(氨基丙基)哌嗪、氨基乙基哌嗪等脂肪族、脂环族、芳香族二胺以及己二酸、辛二酸、壬二酸、癸二酸、十二烷二酸、对苯二甲酸、间苯二甲酸、2-氯对苯二甲酸、2-甲基对苯二甲酸、5-甲基间苯二甲酸、5-钠磺间苯二甲酸、2,6-萘二羧酸、六羟基对苯二甲酸、六羟基间苯二甲酸等脂肪族、脂环族、芳香族二羧酸等,在本发明中,从这些原料衍生出来的尼龙均聚物或共聚物,可分别单独使用或以混合物的形式使用。
在本发明中,特别有用的聚酰胺树脂是熔点150℃以上、耐热性和强度优良的聚酰胺树脂,作为具体的例子可以举出聚己酰胺(尼龙6)、聚己二酸己二胺(尼龙66)、聚己二酰丁二胺(尼龙46)、聚癸二酰己二胺(尼龙610)、聚十二烷二酰己二胺(尼龙612)、聚十一酰胺(尼龙11)、聚十二酰胺(尼龙12)、聚己酰胺/聚己二酰己二胺共聚物(尼龙6/66)、聚己酰胺/聚对苯二甲酰己二胺共聚物(尼龙6/6T)、聚己二酰己二胺/聚对苯二甲酰己二胺共聚物(尼龙66/6T)、聚己二酰己二胺/聚间苯二甲酰己二胺共聚物(尼龙66/6I)、聚对苯二甲酰己二胺/聚间苯二甲酰己二胺共聚物(尼龙6T/6I)、聚对苯二甲酰己二胺/聚十二酰胺共聚物(尼龙6T/12)、聚己二酰己二胺/聚对苯二甲酰己二胺/聚间苯二甲酰己二胺共聚物(尼龙66/6T/6I)、聚亚二甲苯基己二酰胺(尼龙XD6)、聚对苯二甲酰己二胺/聚-2-甲基五亚甲基对苯二甲酰胺共聚物(尼龙6T/M 5T)、聚对苯二甲酰壬二胺(尼龙9T)及它们的混合物等。
作为特别理想的聚酰胺树脂,可以举出尼龙6、尼龙66、尼龙610、尼龙6/66共聚物,另外,尼龙6T/66共聚物、尼龙6T/6I共聚物、尼龙6T/12以及尼龙6T/6共聚物等具有对苯二甲酰己二胺单元的共聚物,而且,根据耐冲击性、成型加工性、相溶性等必要特性,这些聚酰胺树脂作为混合物使用是合适的。
对这些聚酰胺树脂的聚合度未作特别限定,在样品浓度0.01g/ml的98%浓硫酸溶液中,于25℃测得的相对粘度在1.5~7.0的范围是优选的,2.0~6.0的范围的聚酰胺树脂是特别优选的。
另外,在本发明的聚酰胺树脂中,为了提高长期耐热性,最好使用铜化合物。作为铜化合物的具体例子,可以举出氯化亚铜、氯化铜、溴化亚铜、溴化铜、碘化亚铜、碘化铜、硫酸铜、硝酸铜、磷酸铜、醋酸亚铜、醋酸铜、水杨酸铜、硬脂酸铜、安息香酸铜以及上述无机卤化铜与苯二甲基二胺、2-巯基苯并咪唑、苯并咪唑等的络合物等。其中,1价的铜化合物,特别是1价的卤化铜化合物是优选的,醋酸亚铜、碘化亚铜等是特别合适的铜化合物。铜化合物的添加量,通常相对于聚酰胺树脂100重量份为0.01~2重量份是优选的,在0.015~1重量份的范围是更优选的。当添加量过多时,在熔融成型时金属铜产生游离,引起着色,使制品的价值降低。在本发明中,也可以以与铜化合物并用的方式添加卤化碱金属化合物。作为这些卤化碱金属化合物的例子,可以举出氯化锂、溴化锂、碘化锂、氯化钾、溴化钾、碘化钾、溴化钠以及碘化钠,而碘化钾和碘化钠是特别优选的。
本发明使用的(b)PPS树脂是具有用下述结构式表示的重复单元的聚合物,从耐热性的观点考虑,含有70摩尔%以上、进一步为90摩尔%以上的用上述结构式表示的重复单元的聚合物的聚合物是优选的。另外,PPS树脂的该重复单元的不足30摩尔%也可以采用具有下述结构的重复单元等构成。
部分具有这种结构的PPS聚合物,由于熔点变低,故在本发明的叠层结构体中,在阻挡层以外使用的热塑性树脂的熔点低时,在成型性上是有利的。
本发明中使用的PPS树脂的熔融粘度,只要能熔融混炼则不作特别限制,通常50~20000泊(320℃,剪断速度1000秒-1)是优选使用的,100~5000泊的范围是更优选的。
这种PPS树脂,可用通常公知的方法即特公昭45-3368号公报记载的制造分子量较小的聚合物的方法,或者特公昭52-12240号公报及特开昭61-7332号公报记载的制造分子量较大的聚合物的方法来制造。在本发明中,把上述那样得到的PPS树脂施行以下各种处理后使用当然也是可以的:通过空气中加热进行的交联/高分子量化;在氮等惰性气氛下或减压下的热处理;采用有机溶剂、热水、酸性水溶液等进行的洗涤;采用酸酐、胺、异氰酸酯、含官能团的二硫醚化合物等含有官能团的化合物进行的活性化等。
作为PPS树脂的通过加热进行交联/高分子量化的具体方法,可以举出在空气、氧气等氧化性气体气氛下或上述氧化性气体和氮气、氩气等惰性气体的混合气体气氛下,在加热容器中进行加热,直至得到规定温度下所希望的熔融粘度的方法。加热处理温度,通常选择170~280℃,优选的是200~270℃。另外,加热处理时间,通常选择0.5~100小时,优选的是2~50小时,通过控制这两者,可以得到作为目标的粘度水平。加热处理装置,可以是通常的热风干燥机,也可以是旋转式或带搅拌叶片的加热装置,为了更有效更均匀地进行处理,采用旋转式或带搅拌叶片的加热装置是更优选的。
作为PPS树脂在氮等惰性气氛下或减压下进行处理时的具体的方法,可以举出,在氮等惰性气氛下或减压下,加热处理温度为150~280℃,优选200~270℃,加热时间为0.5~100小时,优选2~50小时的加热处理方法。加热处理装置,可以是通常的热风干燥机,也可以是旋转式或带搅拌叶片的加热装置,为了更有效更均匀的进行处理,采用旋转式或带搅拌叶片的加热装置是更优选的。
本发明所用的PPS树脂,最好是经过脱离子处理的PPS树脂。作为这种脱离子处理的具体方法,可以举出酸性水溶液洗涤处理、热水洗涤处理及有机溶剂洗涤处理等,这些处理也可以将2种以上方法组合起来使用。
作为用有机溶剂洗涤PPS树脂的具体方法,可以举出以下方法。即,作为用于洗涤的有机溶剂,只要没有分解PPS树脂的作用就不作特别限定,例如,可以举出N-甲基吡咯烷酮、二甲基甲酰胺、二甲基乙酰胺等含氮极性溶剂;二甲基亚砜、二甲基砜等亚砜、砜类溶剂;丙酮、甲乙酮、二乙酮、苯乙酮等酮类溶剂;二甲醚、二丙醚、四氢呋喃等醚类溶剂;氯仿、二氯甲烷、三氯乙烯、二氯乙烯、二氯乙烷、四氯乙烷、氯苯等卤类溶剂;甲醇、乙醇、丙醇、丁醇、戊醇、乙二醇、丙二醇、苯酚、二甲酚、聚乙二醇等醇类、酚类溶剂;苯、甲苯、二甲苯等芳香烃类溶剂等。在这些有机溶剂中,使用N-甲基吡咯烷酮、丙酮、二甲基甲酰胺、氯仿等是优选的。另外,这些有机溶剂,可以使用1种或将2种以上混合使用。作为采用有机溶剂的洗涤方法,有使PPS树脂浸渍在有机溶剂中等方法,根据需要,还可以进行适当的搅拌或加热。对在有机溶剂中洗涤时的洗涤温度未作特别限定,可选择常温~300℃左右的任意温度。洗涤温度愈高,洗涤效率愈好,通常在常温~150℃的洗涤温度下可以得到充分的效果。经过有机溶剂洗涤的PPS树脂,为了除去残留的有机溶剂,最好用水或温水洗涤数次。
作为用热水洗涤处理PPS树脂的具体方法,可以举出以下方法。即,为了体现使用热水洗涤的PPS树脂的理想的化学改性效果,使用的水最好是蒸馏水或脱离子水。热水处理操作,通常是把规定量的PPS树脂投入到规定量的水中,在常压下或在压力容器内通过加热、搅拌进行。PPS树脂和水的比例,水多为好,通常,可选择相对于水1升,PPS树脂为不大于200g的浴比。
作为酸处理PPS树脂的具体方法,可列举以下方法,即,有把PPS树脂浸渍在酸或酸性水溶液中等方法,根据需要,也可以加以适当搅拌或加热。所用的酸只要是不具有分解PPS树脂的作用的就不作特别限定,甲酸、乙酸、丙酸、丁酸等脂肪族饱和单羧酸;氯乙酸、二氯乙酸等卤代的脂肪族饱和羧酸;丙烯酸、巴豆酸等脂肪族不饱和单羧酸;安息香酸、水杨酸等芳香族羧酸;草酸、丙二酸、琥珀酸、苯二甲酸、富马酸等二羧酸;硫酸、磷酸、盐酸、碳酸、硅酸等的无机酸性化合物等。其中,使用醋酸、盐酸是更优选的。经过酸处理的PPS树脂为了除去残留的酸或盐等,最好用水或温水洗涤几次。而用于洗涤的水,从不损害经酸处理的PPS树脂的理想的化学改性效果的的观点看,蒸馏水或脱离子水是优选的。
在本发明中,为了提高(a)成分的聚酰胺树脂和(b)成分的PPS树脂的相溶性,也可以配合以前公知的相溶化剂。作为这些相溶化剂的具体例子,可以举出,具有选自环氧基、氨基、异氰酸酯基、羟基、巯基、脲基中的至少1种官能团的烷氧基硅烷等有机硅烷化合物;乙烯、丙烯等α-烯烃和从丙烯酸、甲基丙烯酸、马来酸、巴豆酸等α,β-不饱和羧酸、这些酸的酯、酸酐、卤化物、与钠、钾、镁、锌等的盐等衍生物中选择的至少1种化合物的无规、嵌段、接枝共聚物等改性的聚烯烃类;α-烯烃及α,β-不饱和酸的缩水甘油酯为主要构成成分的烯烃系共聚物等含环氧基的烯烃系共聚物以及多官能环氧化合物;它们也可以同时使用2种以上。
所谓本发明中所说的热塑性树脂结构体,是部分或全部地具有以下相结构的结构体:(1)PPS树脂成分形成连续相(基体相),聚酰胺树脂成分形成分散相的相结构(例如海岛结构);(2)PPS树脂成分和聚酰胺树脂成分都形成实质的连续相的相结构(例如海海结构);或者(3)聚酰胺树脂成分形成连续相,PPS树脂成分以多个薄的二维重叠的带(层)状形式形成分散相的相结构(层叠结构)。对结构体的形状未作特别限定。另外,在结构体的各种场所,上述相结构(1)、(2)或(3)共存,或出现几次的场合也有。该相结构(1)、(2)或(3)用扫描型及透射型电子显微镜进行观察、确认。
在本发明的热塑性树脂结构体中,(a)成分的聚酰胺树脂及(b)成分的PPS树脂的配合比例,在PPS树脂成分形成连续相(基体相)、聚酰胺树脂成分形成分散相的相结构(例如海岛结构,图1)的场合,聚酰胺树脂为5~80体积%、PPS树脂为95~20体积%。优选的是,聚酰胺树脂为55~80体积%、PPS树脂为45~20体积%。在这种PPS树脂成分为少量成分时,例如,通过适当控制聚酰胺树脂/PPS树脂的熔融粘度比,可以形成PPS树脂保持连续相的相结构。这种相结构的成型体,具有优良的吸水时特性和耐透过性的平衡,在叠层结构体的阻挡层中,强韧性、层间粘合性、阻挡性及经济性达到优良平衡,所以,是特别优选的。而且,两成分的配合比,聚酰胺树脂为60~75体积%、PPS树脂为40~25体积%是优选的。当(a)成分的聚酰胺树脂大于80体积%时,作为本发明的树脂成型体的特征的PPS树脂成分,难以形成连续相,无法达到本发明的目的。另外,当(a)成分的聚酰胺树脂小于5体积%时,引起树脂成型体韧性下降及叠层结构体的层间粘合性降低,是不理想的。
在得到PPS树脂成分和聚酰胺树脂成分都形成实质的连续相(基体相)的相结构(例如海海结构,图2)时,在聚酰胺树脂15~85体积%和PPS树脂85~15体积%的组成范围中,控制聚酰胺树脂以及PPS树脂的熔融粘度及相溶性是重要的。在具体实现该相分离结构时,聚酰胺树脂30~70体积%、PPS树脂70~30体积%的组成是优选的,而聚酰胺树脂35~65体积%、PPS树脂65~35体积%是更优选的,当(a)成分的聚酰胺树脂大于85体积%时,PPS树脂成分难以形成实质的连续相,无法得到达到本发明目的的结构体。
其次,在得到聚酰胺树脂成分形成连续相(基体相)、PPS树脂成分以多个薄的二维重叠的带(层)状形式形成分散相(层压结构,图3)的相结构的场合,聚酰胺树脂为55~95体积%、PPS树脂为45~5体积%。优选的是,聚酰胺树脂为60~95体积%、PPS树脂为40~5体积%,更优选的是聚酰胺树脂65~95体积%、PPS树脂35~5体积%。当(a)成分的聚酰胺树脂大于95体积%时,使PPS树脂成分的带状分散达到充分的长度和量变得困难,无法达到本发明的目的。另外,当(a)成分的聚酰胺树脂小于55体积%时,则PPS树脂成分难以形成带状分散相。
形成带状分散相的PPS树脂成分的L/T(长/厚)最好为30以上,更优选的是L/T为100以上,特别优选的是L/T为150以上。L/T为30以下时,无法得到达到目的阻挡性的结构体。另外,对L/T的上限未作特别限定,但工业上1×106以下是实用的。
作为可用于本发明的(c)无机填料,未作特别限定,可以使用纤维状、板状、粉末状和粒状等填料。具体的可以举出玻璃纤维、PAN类及沥青类碳纤维;不锈钢纤维、铝纤维及黄铜纤维等金属纤维;芳香族聚酰胺纤维等有机纤维;石膏纤维、陶瓷纤维、石棉纤维、锆纤维、氧化铝纤维、氧化硅纤维、氧化钛纤维、碳化硅纤维、玻璃质纤维、钛酸钾晶须、钛酸钡晶须、硼酸铝晶须、氮化硅晶须等纤维状、晶须状填料;硅灰石、绢云母、高岭土、云母、粘土、膨润土、石棉、滑石、铝硅酸盐等硅酸盐;蒙脱石、合成云母等膨润性层状硅酸盐;氧化铝、氧化硅、氧化镁、氧化锆、氧化钛、氧化铁等金属氧化物;碳酸钙、碳酸镁、白云石等碳酸盐;硫酸钙、硫酸钡等硫酸盐;玻璃珠、陶瓷珠、氮化硼、碳化硅、磷酸钙及硅石等非纤维状填料。上述填料中,玻璃纤维以及在必须有导电性的场合,PAN系碳纤维是优选使用的。玻璃纤维的种类,只要是一般用于树脂强化的则不作特别限定,例如,可从长纤维型或短纤维型的短单纱、精纺纤维等中选择使用。另外,上述填料也可以将2种以上同时使用。本发明中使用的上述填料,也可以将其表面用公知的偶合剂(例如,硅烷系偶合剂、钛酸酯系偶合剂等)、其他的表面处理剂进行预处理以及对膨润性层状硅酸盐,用有机 离子进行预处理而使用,从得到更优良的机械强度、阻挡性的意义上看是优选的。
另外,玻璃纤维,可用乙烯/乙酸乙烯共聚物等热塑性树脂、环氧树脂等热固性树脂被覆或集束。
上述(c)无机填料的添加量,相对于(a)聚酰胺树脂及(b)PPS树脂的合计量100重量份,为0.5~200重量份是优选的,更优选的是5~200重量份,特别优选的是10~150重量份。
本发明所述的叠层结构体是层压几种树脂的结构体,也是上述具有特定相结构的热塑性树脂结构体至少构成为1层(下面称作(1)阻挡层),另外,具有别的组成或相结构的本发明热塑性树脂结构体(该层也是阻挡层),或在该阻挡层的至少一面上构成与该阻挡层不同的树脂层(下面称作(2)相邻层)的结构体。另外,在本发明叠层结构体的优选的方案中,为了提高(1)阻挡层和(2)相邻层的粘合力,在该两层之间,适当构成对该两层有粘合性、并且具有共挤出性的树脂层(下面称作(3)粘合层)的层压体。具体地说,例如可以举出,(1)层/(2)层的2种2层结构、(2)层/(1)层/(2)层的2种3层结构、(2)层/(3)层/(1)层的3种3层结构、(2)层/(3)层/(1)层/(2)层的3种4层结构、(2)层/(3)层/(1)层/(3)层/(2)层的3种5层结构的层压结构,但并不限定于这些。
在本发明中,构成(2)相邻层的树脂,是用具有与本发明重要条件不同的相结构或组成的热塑性树脂构成的。对该热塑性树脂的种类未作特别限定,可根据叠层结构体的使用目的适当选择。作为具体例子,可以举出饱和聚酯树脂、聚砜树脂、聚四氟乙烯树脂、聚醚酰亚胺树脂、聚酰胺酰亚胺树脂、聚酰胺树脂、聚酰亚胺树脂、聚碳酸酯树脂、聚醚砜树脂、聚醚酮树脂、聚硫醚酮树脂、聚醚醚酮树脂、热塑性聚氨酯树脂、聚烯烃树脂、ABS树脂、聚酰胺弹性体、聚酯弹性体等,这些也可以以2种以上的混合物形式使用。其中,聚烯烃树脂、热塑性聚酯树脂、聚酰胺树脂、聚碳酸酯树脂以及ABS树脂是更优选的。
这里,作为优选的聚烯烃树脂的例子,可以举出低、中及高密度聚乙烯、聚丙烯、乙烯/丙烯共聚物、聚1-丁烯、聚-4-甲基戊烯-1、聚氯乙烯、聚氯丙烯以及聚甲基戊烯等。其中,低、中及高密度聚乙烯、聚丙烯、乙烯/丙烯共聚物是更优选使用的。
另外,作为优选的热塑性聚酯,例如,是指用对苯二甲酸等二羧酸和脂肪族二元醇制得的聚酯。作为对苯二甲酸以外的二羧酸,可以举出壬二酸、癸二酸、己二酸、癸烷二羧酸等碳原子数为2~20的脂肪族二羧酸、间苯二甲酸、萘二羧酸等芳香族二羧酸,或环己烷二羧酸等脂环式二羧酸等,这些既可单独使用,也可以混合物的形式使用。作为脂肪族二元醇,可以举出乙二醇、1,2-丙二醇、1,3-丙二醇、1,4-丁二醇、三亚甲基二醇、1,4-环己烷二甲醇及六亚甲基二醇等。具体的可以举出聚对苯二甲酸乙二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸丁二醇酯、聚对苯二甲酸六亚甲基酯、聚环亚己基二亚甲基对苯二甲酸酯、聚萘二甲酸乙二醇酯,其中,具有适度机械强度的聚对苯二甲酸丁二醇酯、或者由含有对苯二甲酸60摩尔%以上、优选的是70摩尔%以上和十二烷二羧酸和/或间苯二甲酸的二羧酸成分与1,4-丁二醇成分构成的共聚合聚酯是特别优选的。
对这些热塑性聚酯树脂的聚合度未作特别限定,在为优选使用的聚对苯二甲酸丁二醇酯、共聚合的聚对苯二甲酸丁二醇酯的场合,于25℃测得0.5%邻氯苯酚溶液的固有粘度,在0.5~2.5的范围是优选的,在0.8~2.0的范围是特别优选的。另外,在为聚对苯二甲酸乙二醇酯的场合,于25℃测得0.5%邻氯苯酚溶液的固有粘度,在0.54~1.5的范围是优选的,在0.6~1.2的范围是特别优选的。
作为优选的聚酰胺树脂的例子,与作为上述(a)成分而说明的聚酰胺树脂一样,然而,其中,由每个酰胺基的碳原子数为8~15的范围的结构单元所构成的聚酰胺树脂是合适的,而且,以氨基羧酸或其衍生物作为单体的聚酰胺树脂,从得到更优良的低温韧性来说是特别优选的。作为这种聚酰胺,可以举出聚十二酰胺(尼龙12)、聚十一酰胺(尼龙11)等,或者,在间甲酚中(聚合物浓度为0.5重量%),于25℃测得的相对粘度在1.0~7.0的范围,特别是可举出在1.5~5.0的范围的聚酰胺树脂。
对这些聚酰胺树脂的聚合度未作特别限定,在样品浓度0.01g/ml的98%浓硫酸溶液中,于25℃测得的相对粘度,在1.5~7.0的范围是优选的,在2.0~6.5的范围是更优选的,在2.5~5.5的范围是特别优选的。
构成这种(2)相邻层的热塑性树脂,还可以含有适于各树脂的增塑剂、抗氧化剂、成核剂和着色剂等添加剂。
在本发明中,采用保持特定相分离结构的热塑性树脂结构体构成的(1)阻挡层、在其一面或者两面上构成(2)相邻相的叠层结构体,也可以采用双色注射成型法等制得,然而,以膜状或片状的形式得到时,把形成各个层的组合物用分别的挤出机熔融后,供给到多层结构的模具,用共挤出成型法,预先使相邻层成型后,熔融挤出上述阻挡层,可采用这种所谓层压成型法等进行制造。另外,叠层结构体的形状为瓶、桶、罐等中空容器以及导管、软管等管状体的场合,可以采用通常的共挤出成型法,例如,内层为具有特定的相分离结构的阻挡层,而以相邻层形成外层的双层中空成型体的场合,把上述阻挡层用树脂组合物和相邻层用树脂组合物分别供给到2台挤出机,把这2种熔融树脂用压力供给到共同的模具内,分别形成环状流体后,加以合流,使阻挡层成为内层,而相邻层成为外层,然后,共挤出至模具外,通过通常公知的管成型法、吹塑成型法等进行成型,可以得到双层中空成型体。另外,对于3层中空成型体来说,用3台挤出机,用与上述一样的方法制成3层结构,或者,用2台挤出机,也可以得到2种3层结构的中空成型体。在这些方法中,从层间粘合力考虑,采用共挤出成型法成型是优选的。
在本发明的叠层结构体中,为了更加提高成型体的耐冲击性及成型性、各层间的粘合力,在(1)阻挡层和(2)相邻层之间适当构成(3)粘合层是优选的。作为构成粘合层的树脂,只要是对(1)阻挡层及(2)相邻层显示粘合性、并可以与它们共挤出则不特别限定结构。具体的例子可以举出,乙烯、丙烯等α-烯烃和丙烯酸和人甲基丙烯酸、马来酸、巴豆酸等α,β-不饱和羧酸、它们的酯、酸酐、卤化物、与钠、钾、镁、锌等的盐等的衍生物中选择的至少1种化合物所形成的无规、嵌段、接枝共聚物等改性的聚烯烃类;乙烯、丙烯等α-烯烃和从乙酸乙烯基酯、乙烯基醇、苯乙烯类中选择的至少1种化合物的无规、嵌段、接枝共聚物;共聚合聚酰胺类粘合剂;共聚合聚酯类粘合剂等。采用这些粘合剂的使用方法,可以取得2种2层、2种3层、3种3层、3种4层、3种5层等几种形态。
为了赋予本发明的热塑性树脂结构体导电性,可以使用导电性填料和/或导电性聚合物,对这些材料未作特别限定,然而,作为导电性填料,只要是通常用于树脂的导电的填料则不作特别限定,作为其具体例子,可以举出金属粉、金属片、金属条、金属纤维、金属氧化物、用导电性物质被覆的无机填料、碳粉、石墨、碳纤维、碳片、鳞片状碳等。
作为这种金属粉、金属片、金属条的金属品种的具体例子,可以举出银、镍、铜、锌、铝、不锈钢、铁、黄铜、铬、锡等。
作为金属纤维的金属品种的具体例子,可以举出铁、铜、不锈钢、铝、黄铜等。
这种金属粉、金属片、金属条、金属纤维,可以用钛酸酯系、铝系、硅烷系等表面处理剂进行表面处理。
作为金属氧化物的具体例子,可以举出SnO2(掺杂锑)、In2O3(掺杂锑)、ZnO(掺杂铝)等,这些也可用钛酸酯系、铝系、硅烷系偶合剂等表面处理剂进行表面处理。
作为在用导电性物质被覆的无机填料中的导电性物质的具体例子,可以举出铝、镍、银、碳、SnO2(掺杂锑)、In2O3(掺杂锑)等。作为被覆的无机填料,可以举出云母、玻璃珠、玻璃纤维、碳纤维、钛酸钾晶须、硫酸钡、氧化锌、氧化钛、硼酸铝晶须、氧化锌系晶须、氧化钛酸系晶须、碳化硅晶须等。作为被覆方法,可以举出真空蒸镀法、溅射法、无电解的镀敷法、烧结法等。另外,这些填料也可以用钛酸酯系、铝系、硅烷系偶合剂等表面处理剂进行表面处理。
碳粉,按其原料和制造方法可以分成乙炔碳黑、天然气碳黑、油碳黑、萘碳黑、热解碳黑、炉法碳黑、灯黑、槽法碳黑、辊法碳黑、盘法碳黑等。可在本发明中使用的碳粉,对其原料和制造方法未作特别限定,但乙炔碳黑和炉法碳黑是特别合适的。另外,碳粉,可以制成其粒径、表面积、DBP吸油量、灰分等特性不同的各种碳粉。本发明可用的碳粉,对其特性未作特别限定,但从强度和导电率的平衡考虑,平均粒径在500nm以下,特别是5~100nm,进一步是10~70nm是优选的。比表面积(BET法)在10m2/g以上,进一步在30m2/g以上是优选的。DBP给油量为50ml/100g以上,特别是为100ml/100g以上是优选的。灰分为0.5重量%以下,特别是0.3重量%以下是优选的。
这种碳粉也可以用钛酸酯系、铝系、硅烷系等表面处理剂进行表面处理。为了提高熔融混炼作业性,也可将其造粒后使用。
根据用途不同,要求表面的平滑性。从该观点出发,本发明所用的导电性填料,与本发明所用的(c)无机填料同样,与具有高的形状比的纤维状填料相比,粉状、粒状、板状、鳞片状或树脂组合物中的长度/直径比为200以下的纤维状的任何1种形态是优选的。
作为导电性聚合物的具体例子,可以举出聚苯胺、聚吡咯、聚乙炔、聚(对亚苯基)、聚噻吩、聚亚苯基亚乙烯基等。
上述导电性填料和/或导电性聚合物,也可以将2种以上同时使用。在这种导电性填料、导电性聚合物中,从强度和经济性的观点考虑,碳黑是特别适用的。
本发明所用的导电性填料和/或导电性聚合物的含量,因所用的导电性填料和/或导电性聚合物种类的不同而不同,所以,不能一概地规定,然而,从导电性、流动性和机械强度等的平衡的观点考虑,相对于(a)及(b)成分和(c)成分的合计量100重量份,用量为1~25重量份,优选的是3~100重量份。另外,更优选的是,相对于(a)成分和(b)成分的合计量100重量份,为了赋予导电性能,选择3~100重量份是优选的。
另外,在赋予导电性的场合,从得到充分的抗静电性能考虑,其体积固有电阻在1010Ω·cm以下是优选的。但是,上述导电性填料、导电性聚合物的配合,一般易引起强度和流动性的恶化。因此,如果得到作为目标的导电水平,则希望上述导电性填料和导电性聚合物的配合量尽可能少。作为目标的导电水平,因用途的不同而异,通常,体积固有电阻为大于1000Ω·cm~1010Ω·cm的范围。
在本发明的组合物中,在不损害本发明效果的范围内,可以添加其他成分,例如,抗氧化剂和耐热稳定剂(受阻酚类、对苯二酚类、磷酸酯类及它们的取代体)、耐候剂(间苯二酚系、水杨酸系、苯并***、二苯甲酮系、受阻胺系等)、脱模剂及润滑剂(褐煤酸及其金属盐、其酯、其半酯、硬脂醇、硬脂酰胺、各种双酰胺、双尿素及聚乙烯醋等)、颜料(硫化镉、酞菁、碳黑等)、染料(苯胺黑)、结晶成核剂(滑石、硅石、高岭土、粘土等)、增塑剂(对羟基安息香酸辛酯、N-丁基苯磺酰胺等)、抗静电剂(烷基硫酸盐型阴离子系抗静电剂、季铵盐型阳离子系抗静电剂、聚氧乙烯山梨糖醇酐单硬脂酸酯之类的非离子系抗静电剂、甜菜碱系两性抗静电剂等)、阻燃剂(例如,红磷、三聚氰胺氰尿酸酯、氢氧化镁、氢氧化铝等氢氧化物、聚磷酸铵、溴化聚苯乙烯、溴化聚亚苯基醚、溴化聚碳酸酯、溴化环氧树脂或它们的溴系阻燃剂和三氧化锑的组合等)、其他聚合物。
作为制造本发明树脂结构体的方法,只要是能制得作为本发明重要条件的相结构,则不作特别限定,在熔融混炼中,例如可以举出用双螺杆挤出机进行熔融混炼的场合,从主进料器供给聚酰胺树脂和PPS树脂,而从挤出机头部的侧进料器供给无机填料的方法,以及,事前把聚酰胺树脂和PPS树脂进行熔融混炼后,与无机填料进行熔融混炼的方法等。
本发明的热塑性树脂结构体及叠层结构体可用公知的方法赋形,对其成型方法未作限定,可以使用注射成型、挤出成型、吹塑成型、加压成型等。其中,采用从注射成型、注射压缩成型、压缩成型中选择的一种方法,从生产性优良、在工业上实施本发明的观点看,是优选的。另外,关于成型温度,通常可从高于PPS树脂熔点5~50℃的温度范围选择,一般为单层,而用双色成型法成型为多层也可以。
对本发明的树脂结构体中的各层的配置未作特别限定,既可以用本发明的热塑性树脂结构体构成所有的层,也可在其他层中用其他的热塑性树脂构成。由本发明的热塑性树脂结构体构成的层,为了充分发挥其耐透过性效果,当为2层以上时,最好用在最内面。另外,也可以使所得到的成型品彼此之间,或与其他成型品粘合或熔合,对其方法未作特别限定,可采用公知的技术。
本发明的热塑性树脂结构体及叠层结构体,充分利用其优良的气体阻挡性、耐久性、加工性,可很好地用作化学剂液或气体输送和/或贮存用容器及其附属部件以及采用共挤出成型法成型的多层管或多层吹塑中空成型体。作为化学剂液和气体,例如,氟隆-11、氟隆-12、氟隆-21、氟隆-22、氟隆113、氟隆-114、氟隆-115、氟隆134a、氟隆-32、氟隆-123、氟隆-124、氟隆-125、氟隆-143a、氟隆-141b、氟隆-142b、氟隆-225、氟隆-C318、R-502、1,1,1-三氯乙烷、一氯甲烷、二氯甲烷、氯乙烷、甲基氯仿、丙烷、异丁烷、正丁烷、二甲醚、蓖麻油基刹车液、二醇醚系刹车液、硼酸酯系刹车液、极冷地区用刹车液、硅酮油系刹车液、矿物油系刹车液、动力转向装置油、窗清洗液、汽油、甲醇、乙醇、异丁醇、丁醇、氮、氧、氢、二氧化碳、甲烷、丙烷、天然气、氩、氦、氙、医药剂等气体和/或液体,或者气化气体等的耐透过性优良,所以,例如以上述气体和/或液体的耐透过性膜为首,还可以举出下列各种主要用途,气囊、香波、柔发剂、液体肥皂、洗涤剂等各种药剂用瓶、化学剂液保存用容器、气体保存用容器、冷冻液容器、油移动液容器、清毒液用罐、输血泵用罐、燃料箱、洗涤液箱、贮油箱、罐等汽车部件、医疗器具用部件、以及作为一般生活器具部件的容器、瓶状成型体或附属于这些容器、瓶子的截止阀等阀门或接头类、附属泵的壳体、机身类等部件、导管下的燃料注油器、ORVR管、容器软管、排放软管等各种燃料管及连接部件(连接器等)、油管及连接部件、制动器软管及连接部件、窗清洗液用喷嘴及软管、冷却水、冷冻剂等用的冷却器软管及连接用部件、空调机冷冻剂用导管及连接用部件、地板供暖导管及连接部件、灭火器及灭火设备用软管、医用冷却机用管及连接用部件或阀门类、其他化学剂液及气体输送用管、药品保存用容器等要求具有对化学剂液及气体的耐透过性的用途、汽车部件、内燃机相关用途、电动工具罩类等机械部件;电气·电子部件、医疗、食品、家庭·办公用品、建材有关的部件、家具用部件等各种用途。
实施例
下面列举实施例来详细说明本发明,然而,本发明的要点并不只限于下列实施例。
(1)醇汽油透过性
使用由在直径40mm的挤出机头部成型为管状的阴模、冷却管子控制尺寸的精压模具以及拉伸机构成的装置,成型外径8mm、内径6mm的管子。再将其切成20cm长,在管子的一端加塞,把从市场购得的标准汽油和乙醇以75比25的重量比加以混合,制成醇汽油混合物,精确称取该醇汽油混合物6g放入其内部,把另一端也加塞。然后,测定总重,把试验的管子放入60℃的防爆型烘箱内,处理500小时,测定减少的重量。
(2)吸湿时的醇汽油透过性
与上述(1)同样,把填充醇汽油混合物的试验管,在温度40℃、相对湿度65%的恒温恒湿器中处理500小时,测定减少的重量。
(3)氧透过性
按照JIS K 7126 A法(差压法),用GTR-10(ヤナコ分析工业制造)进行测定。
(4)材料强度
按照下列标准方法测定。
拉伸强度:ASTM D 638
弯曲弹性模量:ASTM D 790
Izod(悬臂梁式)冲击强度:ASTM D 256
(5)吸水率
用ASTM 1号试验片(厚度1/8英寸),在温度60℃、相对湿度95%的恒温恒湿器中静置24小时,作为吸水时重量增加率,从刚刚成型的绝对干燥时(绝干时)和吸水后的重量求出。
吸水率(%)={(吸水后重量-绝干时重量)/绝干时重量}×100
(6)吸水时的尺寸稳定性
与上述吸水率一样,作为吸水时的尺寸增加率,在吸水处理了的试验片中,从刚刚成型的绝对干燥时(绝干时)和吸水后的试验片长度(长尺寸方向)求出。
吸水时的尺寸稳定性(%)={(吸水后的试验片长度-绝干时的试验片长度)/绝干时的试验片长度}×100
(7)吸水时的弹性模量
按照ASTM D 790测定与上述吸水率一样地吸水处理了的试验片的弯曲弹性模量。
(8)相分离结构的观察
把管成型体的断面部分(阻挡层),用电子显微镜(TEM、SEM)进行观察。
(9)熔融粘度比
采用柱塞式毛细管流变计,测定在熔融混炼温度下的剪断速度10秒-1的熔融粘度(泊;poise),求出粘度比。
熔融粘度比=(聚酰胺树脂的熔融粘度)/(PPS树脂的熔融粘度)
(10)叠层结构体的物理性质
(A)气醇阻挡性:
把管切成30cm长,管子的一端加塞,把从市场购得的标准汽油和甲醇以85比15(重量比)加以混合,把得到的醇汽油混合物装入管子内部,另一端加塞。然后,测定总重,把试验管放入40℃的防爆型烘箱内,根据重量变化,评价醇汽油透过性。
(B)成型体层间粘合强度
把管切削成宽10mm的长方形状,把夹着粘合层的内外层(粘合层附着在由热塑性树脂组合物构成的(2)相邻层侧)在互相成180度方向上拉伸,测定平均单位长度的粘合强度。参考例1(共聚合PPS的制造)
往带搅拌机的高压釜内装入硫化钠3.26kg(25摩尔,含40%结晶水)、氢氧化钠4g、醋酸钠三水合物1.36kg(约10摩尔)以及N-甲基吡咯烷酮7.9kg,一边搅拌一边缓慢升温至205℃,除去含水1.36kg的馏出水约1.5升。往残留的混合物中添加1,4-二氯苯3.38kg(23.0摩尔)、1,3-二氯苯0.37kg(2.5摩尔)以及NMP 2kg,于265℃加热5小时。将反应生成物用70℃温水洗3次,接着,用pH=4的60℃醋酸水溶液洗涤,再用70℃温水洗4次后,于80℃减压干燥24小时,得到熔点255℃、熔体流动速率(MFR)800g/10分(315℃,荷载5000g)的共聚合PPS树脂约2kg。参考例2(有机化层状硅酸盐的制造)
把Na型蒙脱石(クニミネ工业:クニピアF,阳离子交换容量120毫当量/100g)100g,搅拌分散在温水10升中,向其中添加溶解了三辛基甲基氯化铵48g(相对于阳离子交换容量为1当量)的温水2升,搅拌1小时。滤出生成的沉淀后,用温水洗涤。该洗涤和过滤操作进行3次,所得到的固体于80℃真空干燥,得到干燥的有机化层状硅酸盐。测定所得到的有机化层状硅酸盐的无机灰分量的结果是67重量%。再者,无机灰分量的测定,是从将有机化层状硅酸盐0.1g用500℃电炉灰化3小时前后的重量求出的。
实施例及比较例中使用的聚酰胺树脂及PPS如下。只要不特别声明,都是按照常规方法进行聚合、制造。<聚酰胺树脂>
(N6-1):熔点225℃,相对粘度2.80的尼龙6树脂。
(N6-2):熔点225℃,相对粘度3.30的尼龙6树脂。
(N6-3):熔点225℃,相对粘度3.40的尼龙6树脂。
(N6-4):熔点225℃,相对粘度4.30的尼龙6树脂。
(N6-5):把熔点225℃,相对粘度3.40的尼龙6树脂100重量份和在上述参考例2中得到的有机化层状硅酸盐5重量份进行混合,用双螺杆挤出机,于料筒温度250℃熔融挤出而得到的含层状硅酸盐的尼龙6树脂。
(N66):熔点265℃,相对粘度3.20的尼龙66树脂。
(N6/66):熔点217℃,相对粘度2.85的尼龙6/66共聚物。
(6T/12):熔点300℃,相对粘度2.50的尼龙6T/12共聚物。<PPS树脂>
(PPS-1):熔点280℃,熔体流动速率(MFR)为1000g/10分(315℃,荷载5000g)、重均分子量(Mw)为30000的PPS树脂。
(PPS-2):熔点280℃,MFR为300g/10分,Mw 49000,700泊的PPS树脂。
(PPS-3):熔点280℃,MFR为100g/10分,Mw 70000,1700泊的PPS树脂。
(PPS-4):熔点280℃,MFR为600g/10分,Mw 38000,450泊的PPS树脂。
(PPS-5):在上述参考例1中得到的熔点255℃、MFR 800g/10分的共聚合PPS树脂。<形成阻挡层的树脂组合物以外的热塑性树脂层(相邻层)>
(2-1):MFR 0.3g/10分、密度0.945的高密度聚乙烯。
(2-2):聚对苯二甲酸丁二醇酯(东丽公司制造,“ルミコン”5201X11)。
(2-3):尼龙11(东丽公司制造,“リルサン”BESN O P40TL)。<粘合层>
(3-1):乙烯/甲基丙烯酸缩水甘油酯=94/6(重量%)共聚物。
(3-2):乙烯/丙烯酸甲酯/甲基丙烯酸缩水甘油酯=64/30/6(重量%)共聚物。实施例1~12,比较例1-4
把表1、2中所示的聚酰胺树脂、PPS树脂混合,从日本制钢所制造的TEX 30型双螺杆挤出机的主进料器供给,在供给无机填料的场合,采用中间的侧进料器供料的方法,于混炼温度300℃、螺杆转速200rpm下进行熔融混炼。把得到的粒料干燥后,用注射成型(东芝机械公司制,IS 100 FA,金属模具温度80℃)制成试验片。另外,用上述方法制成醇汽油透过性评价用管。测定各样品的耐透过性、材料强度及吸水时特性等的结果示于表1、2。
又,这里表中GF表示玻璃纤维(纤维直径10μm、3mm的短单纱,日本电气玻璃公司制)、MF表示精纺纤维(平均纤维长140μm,平均纤维直径9μm,日本电气玻璃公司制)、PA表示聚酰胺树脂。
表1
(N6-1):熔点225℃、相对粘度2.80的尼龙6树脂(N6-2):熔点225℃、相对粘度3.30的尼龙6树脂(N66):熔点265℃、相对粘度3.20的尼龙66树脂(N6/66):熔点217℃、相对粘度2.85的尼龙6/66共聚物(PPS-1):熔点280℃、MFR1000g/10分、Mw=30000的PPS树脂(PPS-2):熔点280℃、MFR300g/10分、Mw=49000的PPS树脂
项目 | 单位 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 | 比较例1 | 比较例2 | |
配合组成 | 聚酰胺树脂种类配合量 | -体积% | N6-270 | N6-260 | N6-290 | N6670 | N6/6670 | N6-235 | N6-1100 | N6-170 |
PPS树脂种类配合量 | -体积% | PPS-130 | PPS-240 | PPS-110 | PPS-130 | PPS-130 | PPS-265 | - | PPS-230 | |
聚酰胺/PPS熔融粘度比(混炼温度:℃) | 5.5(300) | 3.6(300) | 5.5(300) | 4.7(300) | 1.8(300) | 3.6(300) | - | 0.6(300) | ||
相分离结构 | 连续层 | PPS | PPS和PA | PA | PPS | PPS和PA | PPS和PA | PA | PA | |
分散相 | PA | - | PPS带状分散 | PA | - | - | - | PPS球状分散 | ||
耐透过性 | 醇汽油透过性 | g | 0.2 | 0.4 | 0.6 | 0.3 | 0.4 | 0.1 | 1.7 | 1.5 |
吸湿时的醇汽油透过性 | g | 0.4 | 0.8 | 1.1 | 0.7 | 0.6 | 0.3 | 1.9 | 1.6 | |
氧透过性 | 注1 | 10 | 10 | 25 | 10 | 20 | 5 | 50 | 45 | |
材料强度 | 拉伸强度 | MPa | 70 | 75 | 82 | 84 | 73 | 71 | 72 | 66 |
弯曲弹性模量 | GPa | 2.9 | 3.0 | 3.3 | 2.9 | 2.8 | 3.1 | 2.9 | 2.8 | |
Izod冲击强度 | J/m | 49 | 45 | 55 | 51 | 52 | 43 | 54 | 28 |
吸水时特性 | 吸水率 | % | 1.3 | 0.9 | 3.0 | 1.2 | 1.4 | 0.3 | 3.9 | 2.1 |
尺寸安定性 | % | 0.04 | 0.06 | 0.65 | 0.05 | 0.06 | 0.01 | 0.58 | 0.19 | |
弯曲弹性模量 | GPa | 1.7 | 2.0 | 1.1 | 1.8 | 1.6 | 2.2 | 0.6 | 1.1 |
表2
(N6-1):熔点225℃、相对粘度2.80的尼龙6树脂(N6-2):熔点225℃、相对粘度3.30的尼龙6树脂(N66):熔点265℃、相对粘度3.20的尼龙66树脂(N6/66):熔点217℃、相对粘度2.85的尼龙6/66共聚物(PPS-1):熔点280℃、MFR1000g/10分、Mw=30000的PPS树脂(PPS-2):熔点280℃、MFR 300g/10分、Mw=49000的PPS树脂
项目 | 单位 | 实施例7 | 实施例8 | 实施例9 | 实施例10 | 实施例11 | 实施例12 | 比较例3 | 比较例4 | |
配合组成 | 聚酰胺树脂种类配合量 | -体积% | N6-270 | N6-260 | N6-175 | N6670 | N6/6670 | N6-235 | N6-1100 | N6-170 |
PPS树脂种类配合量 | -体积% | PPS-130 | PPS-240 | PPS-125 | PPS-130 | PPS-130 | PPS-265 | - | PPS-230 | |
无机充填材的种类配合量 | -重量% | GF40 | GF40 | GF40 | GF//滑石35//5 | GF//MF30//10 | GF40 | GF40 | GF40 | |
聚酰胺/PPS溶融粘度比(混炼温度:℃) | 5.5(300) | 3.6(300) | 1.6(300) | 4.7(300) | 1.8(300) | 3.6(300) | - | 0.6(300) | ||
相分离结构 | 连续层 | PPS | PPS和PA | PA | PPS | PPS和PA | PPS和PA | PA | PA | |
分散相 | PA | - | PPS带状分散 | PA | - | - | - | PPS球状分散 | ||
耐透过性 | 醇汽油透过性 | g | 0.2 | 0.3 | 0.3 | 0.3 | 0.3 | 0.1 | 1.5 | 1.4 |
吸湿时的醇汽油透过性 | g | 0.5 | 0.7 | 0.7 | 0.6 | 0.6 | 0.3 | 1.7 | 1.6 | |
氧透过性 | 注1 | 10 | 10 | 15 | 10 | 20 | 5 | 50 | 45 |
材料强度 | 拉伸强度 | MPa | 165 | 150 | 175 | 170 | 165 | 135 | 185 | 160 |
弯曲弹性模量 | GPa | 9.2 | 9.5 | 9.0 | 9.3 | 9.0 | 9.5 | 8.5 | 9.0 | |
Izod冲击强度 | J/m | 100 | 90 | 110 | 100 | 105 | 90 | 110 | 85 | |
吸水时特性 | 吸水率 | % | 0.7 | 0.6 | 0.9 | 0.6 | 0.7 | 0.3 | 3.0 | 1.5 |
尺寸安定性 | % | 0.03 | 0.02 | 0.03 | 0.03 | 0.03 | 0.01 | 0.13 | 0.05 | |
弯曲弹性模量 | GPa | 7.0 | 7.4 | 6.5 | 7.3 | 6.9 | 8.6 | 4.0 | 5.5 |
由实施例1~12及比较例1~4可知,规定了特定相分离结构的本发明树脂结构体,可得到耐透过性良好,吸水时的耐透过性、尺寸稳定性和吸水时的刚性的平衡特别优良的特性,有很高的实用价值。另外,用注射成型制成的试验片也具有优良的耐透过性,实用价值高。实施例13~21,比较例5~7
按表3、4所示的阻挡层配合组成,把聚酰胺树脂、PPS树脂及有机硅烷化合物(γ-环氧丙氧基丙基三甲氧基硅烷)混合,用日本制钢所制的TEX 30型双螺杆挤出机,在混炼温度270~320℃、螺杆转速200rpm下熔融混炼,得到粒料。把得到的粒料干燥后,用于管成型。
进行由由所得到的组合物构成的(1)阻挡层1层、由热塑性树脂构成的(2)相邻层1层以及介于阻挡层和相邻层之间的(3)粘合层1层构成的3种3层管子的成型。作为成型装置,可以使用由具有3台挤出机、把从该3台挤出机喷出的树脂通过转接器加以收集成型为管状的阴模、冷却管子控制尺寸的精压模具以及拉伸机构成的装置。
所得到的3层管,其外径8mm、内径6mm,外层(热塑性树脂层)厚0.70mm,粘合层厚0.10mm,内层(阻挡层)厚0.20mm。该多层管的评价结果示于表3、4。另外,评价相分离结构的电子显微镜照片分别示于图4~图7。
表3
(N6-3):熔点225℃、相对粘度3.40的尼龙6树脂(N6-4):熔点225℃、相对粘度4.30的尼龙6树脂(PPS-3):熔点280℃、MFR100g/10分、Mw=70000的PPS树脂(PPS-4):熔点280℃、MFR600g/10分、Mw=38000的PPS树脂(2-1):MFR 0.3g/10分、密度0.945的高密度聚乙烯(3-1):乙烯/甲基丙烯酸缩水甘油酯共聚物
项目 | 单位 | 实施例13 | 实施例14 | 实施例15 | 比较例5 | 比较例6 | 比较例7 | |
阻挡层(1)层配合组成 | 聚酰胺树脂(a)种类聚酰胺树脂配合量 | -体积% | N6-465 | N6-370 | N6-475 | - | N6-365 | N6-4100 |
PPS树脂(b)种类PPS树脂配合量 | -体积% | PPS-435 | PPS-430 | PPS-325 | PPS-3100 | PPS-335 | - | |
有机硅烷化合物 | 重量份数 | 0.8 | 0.6 | 0.4 | - | 0.8 | - | |
聚酰胺树脂/PPS树脂的熔融粘度比(混炼温度:℃) | 7.0(300) | 2.5(300) | 1.1(300) | - | 0.4(300) | - | ||
(2)层 | 热塑性树脂层(相邻层) | 2-1 | 2-1 | 3-1 | 2-1 | 2-1 | 2-1 | |
(3)层 | 粘合层 | 3-1 | 3-1 | 3-1 | 3-1 | 3-1 | 3-1 | |
阻挡层的相分离结构 | 连续层 | PPS | PPS和PA | PA | PPS | PA | PA | |
分散相 | PA | - | PPS带状分散 | - | PPS球状分散 | - | ||
气醇阻挡性 | 气醇透过率(g·mm/m2·24h·atm) | 0.38 | 0.41 | 0.48 | 0.24 | 4.12 | 5.70 | |
成型品层间粘合强度(kg/10mm) | 2.4 | 2.8 | 3.4 | 0.5以下 | 4.2 | 5.6 |
表4
(N6-3):熔点225℃、相对粘度3.40的尼龙6树脂(N6-4):熔点225℃、相对粘度4.30的尼龙6树脂(N6-5):含层状硅酸盐的尼龙6树脂(6T/12):熔点300℃、相对粘度2.50的尼龙6T/12共聚物(PPS-3):熔点280℃、MFR100g/10分、Mw=70000的PPS树脂(PPS-4):熔点280℃、MFR600g/10分、Mw=38000的PPS树脂(PPS-5):熔点255℃、MFR800g/10分的共聚合PPS树脂(2-1):MFR 0.3g/10分、密度0.945的高密度聚乙烯(2-2):聚对苯二甲酸丁二醇酯(2-3):尼龙11(3-1):乙烯/甲基丙烯酸缩水甘油酯共聚物(3-2):乙烯/丙烯酸甲酯/甲基丙烯酸缩水甘油酯共聚物
项目 | 单位 | 实施例16 | 实施例17 | 实施例18 | 比较例19 | 比较例20 | 比较例21 | |
阻挡层(1)层配合组成 | 聚酰胺树脂(a)种类聚酰胺树脂配合量 | -体积% | N6-440 | N6-565 | N6-560 | 6T/1265 | N6-470 | N6-365 |
PPS树脂(b)种类PPS树脂配合量 | -体积% | PPS-460 | PPS-535 | PPS-440 | PPS-435 | PPS-330 | PPS-535 | |
有机硅烷化合物 | 重量份 | 0.8 | 0.8 | 0.6 | 0.8 | 0.6 | 0.8 | |
聚酰胺树脂/PPS树脂的熔融粘度比(混炼温度:℃) | 7.0(300) | 9.5(270) | 10.0(300) | 2.4(320) | 1.1(300) | 9.5(270) | ||
(2)层 | 热塑性树脂层(相邻层) | 2-1 | 2-1 | 2-1 | 2-1 | 2-2 | 2-3 | |
(3)层 | 粘合层 | 3-1 | 3-1 | 3-1 | 3-1 | 3-2 | 3-2 | |
阻挡层的相分离结构 | 连续层 | PPS | PPS | PPS | PPS和PA | PA | PPS | |
分散相 | PA | PA | PA | - | PPS带状分散 | PA | ||
气醇阻挡性 | 气醇透过率(g·mm/m2·24h·atm) | 0.37 | 0.37 | 0.30 | 0.32 | 0.41 | 0.29 | |
成型品层间粘合强度(kg/10mm) | 2.0 | 3.7 | 2.6 | 2.5 | 4.0 | 4.5 |
由实施例13~21规定了特定相分离结构的本发明叠层结构体,具有高的气醇阻挡性,层间粘合性优良,实用价值高。另外,同样,把实施例中得到的材料加工成多层吹塑中空成型体也具有良好的特性。
产业上利用的可能性
本发明的热塑性树脂结构体,气体和/或液体阻挡性良好,特别是即使在高湿下,其耐透过性及刚性良好,所以,可推广到各种用途上,例如,适于电气·电子相关仪器、精密机械相关仪器、办公用仪器、汽车·车辆的相关部件、建材、包装材料、家具和日用杂货等。另外,本发明的叠层结构体,即使对气醇等也具有高的阻挡性,而且可用以制成强度、耐久性、成型加工性也优良的塑料容器、管状体,适于制作汽车汽油罐、化学剂液输送及贮存用容器、配管类、食品用、医用包装材料及容器等。
Claims (16)
1.一种热塑性树脂结构体,其特征是,实质上是采用由(a)聚酰胺树脂5~80体积%及(b)聚亚苯基硫醚树脂95~20体积%组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成(b)聚亚苯基硫醚树脂成为基体相(连续相)、(a)聚酰胺树脂成为分散相的相结构。
2.权利要求1中所述的热塑性树脂结构体,其特征是,(a)聚酰胺树脂和(b)聚亚苯基硫醚树脂的混合比率分别为55~80体积%及45~20体积%。
3.权利要求1中所述的热塑性树脂结构体,其特征是,(a)聚酰胺树脂和(b)聚亚苯基硫醚的混合比率分别为60~75体积%及40~25体积%。
4.一种热塑性树脂结构体,其特征是,是采用由(a)聚酰胺树脂15~85体积%及(b)聚亚苯基硫醚85~15体积%组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成由(b)聚亚苯基硫醚树脂构成的相和由(a)聚酰胺树脂构成的相都是实质的连续相的相结构。
5.一种热塑性树脂结构体,其特征是,是采用由(a)聚酰胺树脂55~95体积%及(b)聚亚苯基硫醚树脂45~5体积%组成的树脂组合物构成的,并且,在用电子显微镜观察到的树脂相分离结构中,形成由由(a)聚酰胺树脂构成的连续相和由(b)聚亚苯基硫醚树脂构成的带状分散相构成的相结构。
6.权利要求1~5中任何1项所述的热塑性树脂结构体,其特征是,相对于(a)成分的聚酰胺树脂及(b)成分的聚亚苯基硫醚树脂的合计量100重量份,含有(c)无机填料0.5~200重量份。
7.一种成型品,其特征是,是权利要求1~6中任1项所述的热塑性树脂结构体的成型品,是采用从注射成型、注射压缩成型、压缩成型中选择的至少一种方法成型的。
8.一种化学剂液或气体的输送用或贮存用容器,其特征是,是加工权利要求1~7中任1项所述的热塑性树脂结构体而得到的。
9.一种化学剂液或气体的输送用或贮存用容器的附属部件,其特征是,是加工权利要求1~7中任1项所述的热塑性树脂结构体而得到的。
10.一种叠层结构体,其特征是,权利要求1~6中的任1项所述的热塑性树脂结构体构成阻挡层。
11.根据权利要求10所述的叠层结构体,其特征是,在阻挡层的一面或两面上构成相邻层,构成该相邻层的树脂层是由与构成阻挡层的热塑性树脂结构体不同的热塑性树脂层构成的。
12.根据权利要求11所述的叠层结构体,其特征是,构成相邻层的热塑性树脂是从聚烯烃树脂、热塑性聚酯树脂、聚酰胺树脂、聚碳酸酯树脂、ABS树脂中选择的至少1种树脂。
13.根据权利要求11所述的叠层结构体,其特征是,构成相邻层的热塑性树脂是高密度聚乙烯。
14.根据权利要求11所述的叠层结构体,其特征是,在阻挡层和相邻层之间构成粘合层。
15.根据权利要求10~14中的任1项所述的叠层结构体,其特征是,是采用共挤出成型法成型的。
16.根据权利要求10~15中的任1项所述的叠层结构体,其特征是,使用共挤出成型法成型为多层管或多层吹塑中空成型体。
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EP (1) | EP1262526B1 (zh) |
KR (1) | KR100612754B1 (zh) |
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CN104817831A (zh) * | 2015-05-21 | 2015-08-05 | 国网智能电网研究院 | 一种电气绝缘热塑性树脂组合物及其制备方法 |
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CN101765639B (zh) * | 2008-01-31 | 2012-09-05 | Dic株式会社 | 聚亚芳基硫醚树脂组合物、其制造方法和表面安装用电子部件 |
CN104817831A (zh) * | 2015-05-21 | 2015-08-05 | 国网智能电网研究院 | 一种电气绝缘热塑性树脂组合物及其制备方法 |
CN111755874A (zh) * | 2019-03-28 | 2020-10-09 | 株式会社自动网络技术研究所 | 连接器装置 |
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KR100612754B1 (ko) | 2006-08-18 |
KR20020039369A (ko) | 2002-05-25 |
WO2001027203A1 (fr) | 2001-04-19 |
DE60027927D1 (de) | 2006-06-14 |
CN1211434C (zh) | 2005-07-20 |
DE60027927T2 (de) | 2007-01-04 |
EP1262526A4 (en) | 2003-07-09 |
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