CN1767944B - 具有改进耐候性的热塑性树脂弹性体/橡胶层压材料及使用它的充气轮胎 - Google Patents
具有改进耐候性的热塑性树脂弹性体/橡胶层压材料及使用它的充气轮胎 Download PDFInfo
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- CN1767944B CN1767944B CN2004800091128A CN200480009112A CN1767944B CN 1767944 B CN1767944 B CN 1767944B CN 2004800091128 A CN2004800091128 A CN 2004800091128A CN 200480009112 A CN200480009112 A CN 200480009112A CN 1767944 B CN1767944 B CN 1767944B
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- rubber
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- elastomer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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Abstract
本发明公开了一种具有改进耐候性的热塑性树脂弹性体/橡胶层压制品,该层压制品含有热塑性树脂弹性体组合物和橡胶层。其通过层压两层或更多层包括含有100重量份橡胶和0.1~20重量份抗氧化剂的橡胶层和含有热塑性树脂弹性体组合物的层并进行加热和压制所述堆叠的层而得到。由此所述抗氧化剂从所述橡胶层迁移至含有热塑性树脂弹性体组合物的层。本发明还提供了采用所述层压制品作为内衬层的充气轮胎。
Description
技术领域
本发明涉及一种热塑性树脂弹性体组合物层和橡胶层的层压材料,更具体地,涉及一种具有改进耐候性的热塑性弹性体/橡胶层压材料,该层压材料适用于例如充气轮胎的内衬层,同时还涉及使用该层压材料的充气轮胎。
背景技术
在橡胶层的表面上具有使用热塑性树脂和弹性体的组合物层(即热塑性弹性体组合物层)的热塑性弹性体/橡胶层例如在日本专利No.3217239等中作了描述,并具有例如柔韧性、低温耐久性等特性。然而,在其表面上具有热塑性弹性体/橡胶组合物的弹性体/橡胶层压材料当以暴露于外部的状态使用时会受到UV光、热、氧气和臭氧等的影响,并且所述热塑性树脂弹性体组合物层会老化,由此形成裂纹并出现耐候性方面的其它问题。因此,当预先将抗氧化剂混入该组合物中以改进热塑性树脂弹性体组合物的耐老化性能并同时混合热塑性树脂和弹性体时,抗氧化剂可起到促进剂的作用。特别地,当使用橡胶作为弹性体时,会发生橡胶的过早硫化,因此存在的问题是不能获得具有所需物理性能的组合物。
发明概述
据此,本发明的目的是消除现有技术的上述问题,并提供一种具有改进耐候性的热塑性树脂弹性体/橡胶层压材料。
按照本发明,提供了一种含有橡胶层和热塑性树脂弹性体组合物层的热塑性弹性体/橡胶层压材料,所述橡胶层含有100重量份橡胶和0.1~20重量份预混入其中的抗氧化剂,该层压材料是通过层压至少两层所述橡胶层和热塑性树脂弹性体组合物层、之后通过平压硫化该层压材料而得到的,由此所述抗氧化剂从所述橡胶层迁移至所述热塑性树脂弹性体组合物层以改进耐候性,另外本发明还提供了使用该层压材料作为内衬层的充气轮胎。
按照本发明,当制备热塑性树脂弹性体组合物层和橡胶层的层压材料时,预先将抗氧化剂、优选基于胺的抗氧化剂混入所述橡胶层,在其上层压含有热塑性树脂和弹性体的组合物层,之后通过例如平压硫化该层压材料,由此所述抗氧化剂从所述橡胶层迁移至所述热塑性树脂弹性体组合物层,并因此可改进热塑性树脂弹性体组合物层的耐候性。通过例如平压硫化含有混入其中的抗氧化剂的未硫化橡胶,这样抗氧化剂从橡胶层迁移至热塑性树脂弹性体组合物层,结果得到含有迁移的抗氧化剂的热塑性树脂弹性体组合物和硫化橡胶的层压材料。通过排布该层压材料使得所述热塑性弹性体组合物层接触外部空气,可以明显地抑制由紫外光、热、氧气和臭氧等的影响所导致的层压材料的老化和生成裂纹等问题。
实施发明的最佳方式
按照本发明的层压材料的橡胶层包括任何可用于轮胎的二烯基橡胶,例如天然橡胶(NR)、聚异戊二烯橡胶(IR)、多种苯乙烯-丁二烯共聚物橡胶(SBR)、多种聚丁二烯橡胶(BR)、丙烯腈-丁二烯共聚物橡胶(NBR)、氯丁二烯橡胶(CR)等.这些橡胶可以单独或以其任何混合物的形式使用.此外,还可以少量使用含有非二烯基橡胶的共混物,所述非二烯基橡胶例如为丁基橡胶(IIR)、乙烯-丙烯-二烯三元共聚物橡胶(EPDM)等.
按照本发明的层压材料的热塑性树脂弹性体层包含弹性体共混入其中的
热塑性树脂。作为所述热塑性树脂,可提及基于聚酰胺的树脂(如尼龙6(N6)、尼龙66(N66)、尼龙11(N11)、尼龙12(N12)、尼龙610(N610)、尼龙612(N612)等)、基于聚酯的树脂(如聚对苯二甲酸丁二醇酯(PBT)、聚对苯二甲酸乙二醇酯(PET)、聚间苯二甲酸乙二醇酯(PEI)等)、基于聚腈的树脂(如聚丙烯腈(PAN)、聚甲基丙烯腈等)、基于聚甲基丙烯酸酯的树脂(如聚甲基丙烯酸甲酯(PMMA)、聚甲基丙烯酸乙酯等)、基于聚乙烯基类的树脂(如聚醋酸乙烯酯、聚乙烯醇(PVA)、聚偏氯乙烯(PDVC)、聚氯乙稀(PVC)等)、基于纤维素的树脂(如醋酸纤维素和乙酸丁酸纤维素)、基于氟的树脂(如聚偏氟乙烯(PVDF)、聚氟乙烯(PVF)等)、基于酰亚胺的树脂(如芳族聚酰亚胺(PI))等。
按照本发明,作为与所述热塑性树脂共混的弹性体,例如可提及二烯基橡胶及其氢化物(如NR、IR、SBR、BR、NBR等)、基于烯烃的橡胶(如乙烯丙烯橡胶(EPDM、EPM)、IIR等)、丙烯酸酯橡胶(ACM)、含卤素的橡胶(如Br-IIR、Cl-IIR、异丁烯对甲基苯乙烯共聚物的溴化物(Br-IPMS)等)、硅氧烷橡胶(如甲基乙烯基硅氧烷橡胶、二甲基硅氧烷橡胶等)、含硫橡胶(如聚硫橡胶)、氟橡胶(如基于偏氟乙烯的橡胶、含氟的基于乙烯基醚的橡胶)、热塑性弹性体(如基于苯乙烯的弹性体、基于烯烃的弹性体、基于酯的弹性体、基于聚氨酯的弹性体和基于聚酰胺的弹性体)等。这些可以单独或以其任何两种的混合物形式使用。
当与所述热塑性树脂混合时,上述弹性体组分还可以动态硫化。这里“动态硫化”是指将所述弹性体组分精细分散在所述热塑性树脂中并同时交联和固定所述弹性体组分的方法。在动态硫化的情形中,硫化剂、硫化助剂的类型和硫化条件(温度和时间)等可根据所添加的弹性体组分的组成而适当确定,并且没有特殊的限制。作为硫化剂,可使用常用的橡胶硫化剂(或交联剂)。具体地,作为基于硫的硫化剂,可以使用其量例如约0.5~4phr(基于100重量份的橡胶组分(聚合物)的重量份)的硫磺粉、沉淀硫磺等。
此外,作为基于有机过氧化物的硫化剂,可提及过氧化苯甲酰、叔丁基氢过氧化物、过氧化2,4-二氯苯甲酰等,作为基于硫脲的硫化促进剂,可提及亚乙基硫脲、二乙基硫脲等。
此外,作为硫化助剂,可以一起使用常用的橡胶助剂。例如可使用锌白(约5phr(即基于100重量份弹性体的重量份))、硬脂酸、油酸及其锌盐等(约2~4phr)。所述热塑性弹性体组合物的制备方法包括通过双螺杆挤出机等预先将所述热塑性树脂组分和弹性体组分(对于橡胶而言,是未硫化的)熔融混合和将其分散在所述热塑性树脂中由此形成连续相(或基体相),其中所述弹性体组分作为分散相(或畴)分散。当硫化所述弹性体组分时,也可以在混合的同时加入硫化剂,以使该弹性体组分动态硫化。此外,在混合过程中可加入所述热塑性树脂或弹性体组分用的多种混合试剂(除硫化剂外),但优选地在混合前将其预混合。对用于混合热塑性树脂和弹性体组分的混合机器没有特殊的限制,但可以使用螺杆挤出机、捏和机、Banbury混合机、双螺杆挤出机等。作为熔融混合的条件,温度可以是所述热塑性树脂熔融的任何温度或者更高的温度。此外当混合时,剪切速率优选为1000~7500秒-1.总混合时间为30秒至10分钟.此外当加入硫化剂时,加入后的硫化时间优选为15秒至5分钟.将由上述方法制备的热塑性弹性体组合物通过挤出成型或压延成型制成片状膜.膜的形成方法可以是由热塑性树脂或热塑性弹性体形成膜的常规方法.
如此获得的膜具有的结构使得热塑性树脂(A)基质中分散有作为分散相(或畴)的弹性体组分(B)。通过采用这种具有分散结构的形态,热塑性加工成为可能,且该膜具有足够的柔韧性。此外由于所述树脂层作为连续相的作用,可以赋予足够的刚性。此外,不管弹性体组分的量如何,在成型时可以获得与热塑性树脂相同程度的成型性,因此可以通过常用的树脂成型机器(通过挤出机或压延成型)形成膜。
当共混所述热塑性树脂和弹性体时,对热塑性树脂(A)与弹性体组分(B)的特定比例没有特殊的限制,可以由膜厚、抗空气渗透性和柔韧性的平衡而适当地确定,但是(A)/(B)重量比的优选范围为10/90~90/10,更优选15/85~90/10。
按照本发明,作为预先混入橡胶层一侧的抗氧化剂,优选使用例如基于胺的抗氧化剂,如基于萘胺的抗氧化剂如苯基-2-萘胺、苯基-1-萘胺,基于二苯胺的抗氧化剂如4,4′-α,α-二甲基苄基)二苯胺、对-(对-甲苯磺酰胺)-二苯胺,基于对苯二胺的抗氧化剂如N,N′-二苯基-对-苯二胺、N-异丙基-N′-苯基-对苯二胺,但也可以使用它们的衍生物或混合物。
按照本发明,基于100重量份所述橡胶,混入所述橡胶层中的抗氧化剂的量为0.1~20重量份,优选0.1~10重量份。若混入的量太少,则不能获得所需的耐候性,而若其量太大,则会不希望地出现喷霜。
可以通过过去使用的一般方法制备本发明的热塑性树脂弹性体组合物层和橡胶层的层压材料。例如,可通过涂覆、层压、共挤出等制备。此外,对粘接热塑性树脂弹性体组合物层与橡胶层的方法没有特殊的限制,但是例如可以使用粘合剂、接合剂、直接粘接或任何其它适用的方法。
含有热塑性弹性体树脂组合物的层与基于100重量份的橡胶已预先混入0.1~20重量份抗氧化剂的橡胶层不一定必须直接接触。只要通过加热和压制抗氧化剂可以迁移至热塑性树脂弹性体组合物中,则可以通过夹于所述两层之间的具有其它材料的层而层压所述层。
除了必要的组分外,按照本发明的热塑性树脂弹性体组合物或者橡胶组合物还可以含有任何通常混入热塑性弹性体组合物或橡胶组合物中的添加剂。例如,可以混入炭黑、二氧化硅、或其它填料;硫化或交联剂;硫化或交联促进剂;多种类型的油;抗氧化剂;增塑剂;或其它多种类型的常用于轮胎或其它通用橡胶应用中的添加剂。这些添加剂可以通过常规的方法用于混合和硫化以获得组合物以及用于硫化或交联。这些添加剂的混入量可以是常规的混入量,只要不会损害本发明的目的即可。
实施例
现在通过实施例对本发明作进一步解释,但本发明的范围决不限于这些实施例。
实施例1~11和对比实施例1
片状热塑性树脂弹性体组合物样品的制备
通过Banbury密炼机在初始温度40℃下将0.3重量份ZnO、1.2重量份硬脂酸锌和0.6重量份硬脂酸混合至100重量份的部分溴化的聚异丁烯-对甲基苯乙烯共聚物中(BIMS:Exxpro 89-4)5分钟以制备橡胶母料。因此,通过橡胶造粒机将该橡胶母料造粒。通过双螺杆挤出机在220℃下将50重量份如此获得的橡胶粒料、13重量份尼龙6、66共聚物(Toray AmylanCM6041)和25重量份尼龙11(Atofina Rilsan BMNO)进行动态硫化5分钟,然后造粒。通过T-模具挤出如此获得的粒料,形成0.1mm厚的膜。
橡胶片样品的制备
将表I所示配方中除了硫化促进剂和硫以外的组分通过1升密炼机混合5分钟,当达到165±5℃时出料,得到母料。通过开炼机将硫化促进剂和硫磺混合入母料中,得到片状橡胶组合物。
物理性能的评价方法
用表II所列配方的基于橡胶的接合剂刷涂上述制备的片状热塑性树脂弹性体组合物,干燥,并与上述制备的片状橡胶组合物(即2mm片材)层压,然后在190℃下硫化10分钟。将所得的热塑性树脂弹性体组合物和橡胶的层压材料(即用于胎体用途)进行冲压,得到用于通过JIS No.2哑铃的恒定应变疲劳实验的样品。
之后,通过开放结构碳弧光灯如下述进行样品退化实验。
按照JIS K6266的SA方法所述的程序,对热塑性树脂弹性体组合物和橡胶层压体的层压材料样品进行退化实验。放置样品使得热塑性树脂弹性体组合物一侧面向光源。实验温度为63℃,连续辐照该光,并将水喷洒在实验片的表面上,每102分钟循环18分钟。退化时间为48小时、96小时和168小时。在上述时间取出的样品通过下述的恒定应变疲劳实验评价其耐久性能。结果列于表I。
恒定应变疲劳实验方法
对退化实验后的每一样品进行恒定应变疲劳实验,在20℃下以6.7Hz的循环对样品施加40%重复伸长应变,并评价其耐久性能。当热塑性树脂弹性体的表面裂开时被认为是评价的终点。以1000万次重复疲劳循环终止评价。
表II:基于橡胶的接合剂
材料名称 | 制造商和等级 | 混入量(重量份) |
天然橡胶 | RSS #3 | 80 |
SBR1502 | Nippon Zeon Nipol 1502 | 20 |
FEF炭黑 | Chubu Carbon HTC#100 | 50 |
硬脂酸 | NOF Corp.Beads Stearic Acid NY | 2 |
氧化锌 | Seido Chemical Zinc White #3 | 3 |
硫磺 | Karuizawa Refinery sulfur powder | 3 |
硫化促进剂NS | Ouchi Shinko Chemical IndustrialNoccelar NS-P | 1 |
芳香油 | Showa Shell Oil Desolex #3 | 2 |
六甲氧基甲基化的三聚氰胺 | Mitsui Cytec CYREZ-964RPC | 5 |
间苯二酚-甲醛树脂 | Indspec Chemical Penacolite ResinB-18-S | 10 |
苯酚甲醛树脂 | Hitachi Chemical Hitanol 1502Z | 1 |
甲苯 | 试剂级甲苯 | 1000 |
工业实用性
如上所述,按照本发明,通过层压具有所需物理性能的热塑性树脂和弹性体的组合物以及向其中预混入抗氧化剂的未硫化橡胶组合物,可以使抗氧化剂从临近的橡胶层迁移至热塑性树脂弹性体层,由此改进了耐候性,因此其非常适用作例如充气轮胎的内衬层。
Claims (7)
1.一种含有橡胶层和动态硫化的热塑性树脂弹性体组合物层的热塑性树脂弹性体/橡胶层压材料,所述橡胶层含有100重量份橡胶和2~10重量份预混入其中的抗氧化剂,该层压材料是通过层压所述橡胶层和动态硫化的热塑性树脂弹性体组合物层这至少两层、之后通过加热和压制而得到的,由此所述抗氧化剂从所述橡胶层迁移至所述动态硫化的热塑性树脂弹性体组合物层以改进耐候性,其中所述抗氧化剂选自N-苯基-N’-(1,3-二甲基-丁基)-对-苯二胺和N-苯基-N’-异丙基-对苯二胺,热塑性树脂弹性体组合物包含至少一种选自基于聚酰胺的树脂、基于聚酯的树脂、基于聚腈的树脂,基于聚甲基丙烯酸酯的树脂、聚醋酸乙烯酯、聚乙烯醇、聚偏氯乙烯、聚氯乙烯、基于氟的树脂和基于酰亚胺的树脂的热塑性树脂(A)和至少一种选自二烯基橡胶及其氢化物、丙烯酸酯橡胶、含卤素的橡胶、硅氧烷橡胶、含硫橡胶、氟橡胶和热塑性弹性体的弹性体(B)。
2.权利要求1的层压材料,其中在所述热塑性树脂弹性体组合物中,热塑性树脂(A)和弹性体(B)的重量比(A)/(B)为10/90~90/10。
3.权利要求1或2的层压材料,其中所述热塑性树脂(A)为至少一种基于聚酰胺的树脂。
4.权利要求1的层压材料,其中所述含卤素的橡胶是溴化丁基橡胶和氯化丁基橡胶。
5.权利要求1或2的层压材料,其中形成所述橡胶层的橡胶为至少一种选自以下的橡胶:天然橡胶、苯乙烯-丁二烯共聚物橡胶、聚丁二烯橡胶、氯丁二烯橡胶、丁基橡胶和乙烯-丙烯-二烯三元共聚物橡胶。
6.权利要求1的层压材料,其中所述抗氧化剂为N-苯基-N’-(1,3-二甲基-丁基)-对-苯二胺。
7.一种使用权利要求1~6中任一项的层压材料作为内衬层的充气轮胎。
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