CN1972993A - 轮胎用橡胶组合物以及使用它的充气轮胎 - Google Patents
轮胎用橡胶组合物以及使用它的充气轮胎 Download PDFInfo
- Publication number
- CN1972993A CN1972993A CNA200580017854XA CN200580017854A CN1972993A CN 1972993 A CN1972993 A CN 1972993A CN A200580017854X A CNA200580017854X A CN A200580017854XA CN 200580017854 A CN200580017854 A CN 200580017854A CN 1972993 A CN1972993 A CN 1972993A
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- Prior art keywords
- acid
- polyethers
- rubber
- tire
- alcohol
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Abstract
一种轮胎用橡胶组合物，其包含100重量份橡胶，1－30重量份具有式(I)的聚醚(E1)和/或其衍生物(E2)以及10－180重量份填料：R1－{(OCH2CH2CH2CH2)m(OA)n－OH}q(I)，其中R1是从具有1－6个羟基的C1－C24化合物中除去至少1个羟基后的残基，A是除1，4－亚丁基以外的C2－C24亚烷基，q是1－6的整数，以及m和n独立地是1－600的整数，其具有优异的加工性、二氧化硅分散性、耐磨损性和潮湿制动性能等。
Description
技术领域
本发明涉及轮胎用橡胶组合物以及使用它的充气轮胎。
背景技术
长久以来已知将填料，如炭黑和二氧化硅用于增强橡胶。当炭黑用于增强橡胶时，可以制成耐磨损性优异的轮胎。与炭黑相比，二氧化硅在高温(60℃左右)下具有较低的tanδ，这是滚动阻力的指数，而在低温(0℃左右)下具有高tanδ，这是潮湿路面上抓地力(grip on wet roads)的指数。因此，例如当用于轮胎胎面胶组合物时，可以制成滚动阻力低而抓地力高的轮胎(例如参见日本未审专利公开(kokai)No.10-273559和日本未审专利公开(kokai)No.6-248116)。
发明内容
然而，难以将大量填料混合至橡胶中，而且混合加工性差，因此存在以下问题：不可能充分保证橡胶组合物的特性，如耐磨损性、低滚动阻力和抓地性能。
因此，本发明的目的在于提供具有改善的加工性、耐磨损性、滚动阻力和抓地力的轮胎用橡胶组合物以及充气轮胎。
根据本发明，提供一种轮胎用橡胶组合物，其包含100重量份橡胶、1-30重量份式(I)的聚醚(E1)和/或其衍生物(E2)以及10-180重量份填料：
R1-{(OCH2CH2CH2CH2)m(OA)n-OH}q (I)
其中R1是从具有1-6个羟基的C1-C24化合物中除去至少1个羟基后的残基，A是除1，4-亚丁基以外的C2-C24亚烷基，q是1-6的整数，m和n独立地是1-600的整数。
根据本发明的轮胎用橡胶组合物和充气轮胎即使在混入大量填料时也具有优异的加工性、耐磨损性、滚动阻力和抓地性能的性能特征。
实施发明的最佳方式
本发明人为达到上述目的而进行了深入研究，从而发现其中混有特定的含聚醚链的化合物的橡胶组合物具有优异的加工性、耐磨损性、滚动阻力和抓地性能，由此完成本发明。
即，本发明提供轮胎用橡胶组合物以及将该橡胶组合物用于胎面的充气轮胎，该组合物包含100重量份橡胶，其中混入1-30重量份式(I)的聚醚(E1)和/或其衍生物(E2)以及10-180重量份填料。注意的是，在式(I)中，R1是从具有1-6(优选1-3)个羟基的C1-C24、优选C1-C20化合物中除去至少1个羟基后的残基，A是除1，4-亚丁基以外的C2-C24、优选C2-C16亚烷基，q是1-6、优选1-3的整数，m和n独立地是1-600的整数，优选地m是3-100的整数，n是5-150的整数。
可用于本发明的轮胎用橡胶组合物中的橡胶可以是任何可交联的橡胶组分。这种可交联的橡胶的例子例如是天然橡胶(NR)、各种丁二烯橡胶(BR)、各种苯乙烯-丁二烯共聚物橡胶(SBR)、聚异戊二烯橡胶(IR)、丁基橡胶(IIR)、卤化丁基橡胶、丙烯腈丁二烯橡胶、氯丁橡胶、乙烯-丙烯共聚物橡胶、乙烯-丙烯-二烯三元共聚物橡胶、苯乙烯-异戊二烯共聚物橡胶、苯乙烯-异戊二烯-丁二烯共聚物橡胶、异戊二烯-丁二烯共聚物橡胶、氯磺化聚乙烯、丙烯酸类橡胶、表氯醇橡胶、聚硫橡胶、硅橡胶、氟橡胶、聚氨酯橡胶等。这些可以单独使用或以其任意的混合物使用。当使用混合物时，混合比例没有特别限制。
本发明中的聚醚(E1)是上述通式(I)所示的化合物。式(I)中的R1是从具有1-6个羟基的C1-C24化合物中除去至少1个羟基、优选除去所有羟基后的残基。可以提及直链或支化或脂环族的1-6元醇的残基、1-6元酚的残基和1-6元芳基脂族醇的残基。为举例说明这些醇类或酚类，可以提及以下的(e1)-(e6)。
(e1)一元醇：
直链或支化的C1-C24脂族饱和一元醇：
甲醇，乙醇，丙醇(如正丙醇、异丙醇)，丁醇，戊醇，己醇，庚醇，辛醇(如正辛醇、2-乙基己基醇)，壬醇，癸醇，十一烷醇，十二烷醇，十三烷醇(如正十三烷醇、异十三烷醇)，十四烷醇，十五烷醇，十七烷醇，十八烷醇，十九烷醇，二十烷醇，二十一烷醇，二十二烷醇，二十三烷醇，二十四烷醇等；
直链或支化的C3-C24脂族不饱和一元醇(顺式-或反式-)：
链烯基醇(如1-、2-和异丙烯醇，丁烯醇，戊烯醇，己烯醇，庚烯醇，壬烯醇，癸烯醇，十一碳烯醇，十二碳烯醇，十三碳烯醇，十四碳烯醇，十五碳烯醇，十六碳烯醇，十七碳烯醇，十八碳烯醇，十九碳烯醇，二十碳烯醇，二十一碳烯醇，二十二碳烯醇，二十三碳烯醇和二十四碳烯醇等)；和炔基醇(戊炔醇等)；
C4-C24脂环族一元醇：
环戊醇、环己醇等；
(e2)二元醇：
C2-C24脂族二元醇：
亚烷基二醇(如乙二醇，丙二醇，1，3-、1，4-和1，2-丁二醇，新戊二醇，1，6-己二醇，1，2-和1，8-辛二醇，异丁二醇，3-甲基-1，5-戊二醇，2，2，4-三甲基-1，3-戊二醇，2，2-二甲基-1，3-丙二醇，2-丁基-2-乙基-1，3-丙二醇，2，5-二甲基己烷-2，5-二醇等)；
C4-C18脂环族二元醇：
亚环烷基二醇(如1，4-环己烷二醇，1，4-环己烷二甲醇等)和氢化双酚(如氢化双酚A，氢化双酚F等)；和
杂环二元醇：
1，4，3，6-双脱水山梨糖醇(sorbitel)等；
(e3)3-6元醇：
C3-C24三元链烷三醇(如甘油，1，2，3-丁三醇，1，2，3-戊三醇，2-甲基-1，2，3-丙三醇，2-甲基-2，3，4-丁三醇，2-乙基-1，2，3-丁三醇，2，3，4-戊三醇，2，3，4-己三醇，4-丙基-3，4，5-庚三醇，2，4-二甲基-2，3，4-戊三醇，五甲基甘油，1，2，4-丁三醇，1，2，4-戊三醇，三羟甲基乙烷，三羟甲基丙烷等)；C5-C24四元至六元链烷多元醇及其分子内或分子间的脱水物(如季戊四醇，二季戊四醇，山梨糖醇，甘露糖醇，1，5-、3，6-和1，4-脱水山梨糖醇，二甘油等)；以及糖类及其衍生物(如蔗糖，葡萄糖，甘露糖，果糖，甲基糖苷等)；
(e4)一元酚：
C6-C24一元酚[如苯酚，烷基酚(如邻-、间-或对甲酚，间-或对二甲酚，2，6-二甲基苯酚，邻-、间-或对乙基苯酚，对正丁基苯酚，对辛基苯酚，对壬基苯酚等)，单硬脂基苯酚，单苄基苯酚等]；
(e5)2-6元酚：
C6-C24的2-6元酚[如单环多元酚{如二元酚(如邻苯二酚，间苯二酚，氢醌等)，单环三元至六元酚(如三羟基苯，四羟基苯，六羟基苯等)}，和双酚(双酚A，双酚F等)]；
(e6)1-6元芳基脂族醇：
C7-C24芳烷基醇(如苄醇，苯乙醇等)；C8-C24经取代的芳烷基醇(如邻-、间-或对-甲基苄醇和对正丁基苯乙醇等)
其中优选(e1)-(e3)，其中更优选C1-C20的物质，特别优选1-3元醇；从与疏水热塑性树脂的良好溶解性的观点，特别优选C3-C18直链或支化的脂族饱和的或不饱和的一元醇。如果少于24个碳原子，则流动性好，因此混合加工性优异。
式(I)中的A是除1，4-亚丁基以外的C2-C24亚烷基。例如，可以提及亚乙基，1，2-和1，3-亚丙基，1，2-和2，3-亚丁基和异亚丁基，亚十一碳烷基等。这些可以是两种或多种的任意混合物。聚合类型可以是无规聚合或嵌段聚合，但是从流动性优异的观点，优选该聚合物具有无规聚合的部分。其中，优选C2-C16亚烷基，更优选亚乙基、1，2-亚丙基和1，2-亚丁基；从可捏合性/加工性的观点特别优选1，2-亚丙基和1，2-亚丁基。
式(I)中的m和n是1-600，优选m是3-100，n是5-150。进而，m与n的优选比例(m/n)是5/95-95/5。
在聚醚(E1)中，-(OCH2CH2CH2CH2)m-与-(OA)n-可以是无规结合或嵌段结合的，但是从低温流动性的观点，优选无规结合部分存在。q优选是1-3，从与疏水性橡胶的良好溶解性的观点，特别优选是1。如果q在6以内，则流动特性优异。
本发明中聚醚(E1)优选具有10以下，更优选1-8，特别优选2-6的HLB。如果在该范围内，增强填料的分散性优异。
本发明中提及的HLB值指的是通过小田(Oda)法基于有机概念图(organic conception diagram)计算出的值。计算方法例如在“Techniqueof Emulsification and Solubilization”(1976，Kogaku Tosho K.K.)中有描述。此外，用于得到HLB的有机值和无机值可以由Organic ConceptionDiagram-Fundamentals and Application，[1984，Sankyo Shuppan K.K.]中所述的无机族表(1974，Fujita等的报道值)得出。
聚醚(E1)具有优选500-30,000、更优选1,000-10,000、特别优选1,500-6,000的重均分子量(Mw)。如果Mw是500以上，增强填料的分散性优异，而如果是30,000以下，则难以增加粘度，而这从处理的观点看是有益的。此处，“Mw”是通过凝胶渗透色谱(GPC)(色谱柱：TSKGelG2000，G3000，G4000HXL，溶剂：四氢呋喃)测定的值。
至于制备聚醚(E1)的方法，可以提及的方法是：在催化剂存在下，优选在30-120℃的温度下，优选在0-0.6MPa的压力下，例如四氢呋喃(以下称作“THF”)和至少一种C2-C24环氧烷(以下称作“AO”)单独地、无规地或作为嵌段加成键接到由R1(OH)q表示的具有1-6个羟基的C1-C24化合物上。需要的话，可以通过除去催化剂得到聚醚。
至于催化剂，可以使用已知的催化剂，但是在AO中，在具有4元环(如氧杂环丁烷)或5元环(如THF)的AO的单独加成反应或与3元环(如环氧乙烷、环氧丙烷等)的共聚加成反应的情况下，以及在具有3元环的AO相互单独加成反应的情况下，优选的催化剂范围不同。
在具有4或5元环的AO的单独加成反应或具有4或5元环的AO与具有3元环的AO之间的共聚加成反应的情况下，作为催化剂，例如可以提及路易斯酸，如BF3、BCl3、AlCl3、FeCl3和SnCl3及其络合物[例如BF3醚络合物、BF3四氢呋喃络合物(BF3-THF)]；质子酸，如H2SO4、HClO4；高氯酸碱金属盐，如KClO4、NaClO4；高氯酸碱土金属盐，如Ca(ClO4)2、Mg(ClO4)2；除了上述以外的高氯酸金属盐，如Al(ClO4)3；等等。其中，优选BF3醚络合物和BF3THF络合物(BF3-THF)。
在具有3元环的AO的加成反应的情况下，作为催化剂，除了上述催化剂以外，可以提及碱性催化剂，例如氢氧化物(如碱金属或碱土金属氢氧化物，如KOH、NaOH、CsOH、Ca(OH)2)；氧化物(如碱金属或碱土金属氧化物，如K2O、CaO、BaO)；碱金属(如Na、K等)及其氢化物(如NaH、KH等)；胺类，如三乙胺、三甲胺等。其中优选KOH、NaOH、CsOH、BF3醚络合物和BF3THF络合物(如BF3·THF)。
作为加成后的AO，列举具有式(I)的那些，其中A是C2-C24亚烷基。例如，可以提及环氧乙烷(以下称作“EO”)、环氧丙烷(以下称作“PO”)、1，2-环氧丁烷、2，3-环氧丁烷、1，1-二甲基环氧丁烷、环氧十一烷等。其中优选EO、PO和1，2-环氧丁烷，特别优选PO和1，2-环氧丁烷。这些可以一起使用。聚合的形式可以是无规的或嵌段的。
THF的加成摩尔数m是3-100，而AO的加成摩尔数n优选是5-150。此外，THF和AO可以无规加成或嵌段加成，但是从低温流动性优异的观点优选无规加成。在THF加成中，更优选至少80重量％是无规加成。
至于本发明中的聚醚衍生物(E2)，可以提及聚醚(E1)的烷基醚产物(E21)或羧酸酯化产物(E22)，聚醚(E1)与多异氰酸酯的反应产物(E23)，或聚醚(E1)与多卤化物的反应产物(E24)。
在聚醚的烷基醚产物(E21)中，优选C1-C8烷基醚产物，例如可以提及具有甲基、乙基、正丙基、正丁基、正己基、正辛基等的醚产物，优选甲基醚产物。
烷基醚产物(E21)可以通过聚醚(E1)与卤代烷基(C1-C8)在碱(例如碱金属的氢氧化物，如KOH、NaOH、CsOH等)的存在下反应而制成。卤代烷基的量基于聚醚(E1)的羟基以当量比优选是卤代烷基/羟基＝1/1-5/1，特别是1.2/1-4/1。此外，碱的添加量相对于聚醚(E1)的羟基以当量比优选是碱/羟基＝1/1-10/1，特别优选1.2/1-5/1。需要的话，反应可以用溶剂如甲苯、苯进行。该醚化反应可以在常压下或在减压下进行。醚化反应的进行状态可以通过反应体系的碱值、粘度、反应体系的数均分子量等判断。
羧酸的酯化产物(E22)是通过聚醚(E1)与选自C2-C22羧酸、羧酸酐、含C1-C4烷基的羧酸烷基酯和C2-C22羧酸酰卤中的至少一种酯化剂(a)之间的反应得到的酯化产物。
至于酯化剂(a)，可以提及以下物质。
(a1)C2-C22脂族一元羧酸：
乙酸，丙酸，硫代丙酸，丁酸，己酸，月桂酸，肉豆蔻酸，棕榈酸，油酸等；
(a2)C2-C22脂族二元羧酸：
草酸，丙二酸，琥珀酸，丙烷二羧酸，硫代二丙酸，四氢化邻苯二甲酸，甲基四氢化邻苯二甲酸酐，六氢化邻苯二甲酸酐，hymic acid(即2-降冰片烯-2，3-二羧酸酐)，四溴邻苯二甲酸，四氯邻苯二甲酸等；
(a3)C3-C22脂族三元至四元或更高级羧酸：
丙烷三羧酸，甲基环己烷三羧酸，环己烯三羧酸，甲基环己烯三羧酸，环己烷四羧酸等；
(a4)芳族一元羧酸：
苯甲酸，苯乙酸，萘羧酸；
(a5)芳族二元羧酸：
邻苯二甲酸，间苯二甲酸，对苯二甲酸，萘二羧酸，亚二甲苯基二羧酸等；
(a6)芳族三元至四元或其它羧酸：
苯三羧酸，苯四羧酸，萘四羧酸等；
(a7)上述(a2)、(a3)、(a5)或(a6)的酸酐
(a8)上述(a1)-(a6)的低级烷基酯
例如，甲酯、乙酯、丙酯、丁酯、C1-C4烷基酯
(a9)上述(a1)-a6)的酰卤(氯，溴等)：
酯化剂(a)可以包含1-3个、优选1个杂原子(硫、磷等)。
酯化剂(a)中，优选(a2)、(a5)和(a7)，更优选草酸(酐)、丙二酸(酐)、琥珀酸(酐)、丙烷二羧酸(酐)、硫代二丙酸、四氢化邻苯二甲酸(酐)、甲基四氢化邻苯二甲酸酐、六氢化邻苯二甲酸(酐)、hymic acid(酐)、降冰片烯二羧酸(酐)、邻苯二甲酸(酐)、间苯二甲酸和对苯二甲酸，特别优选草酸(酐)、丙二酸(酐)、琥珀酸(酐)、丙烷二羧酸(酐)和硫代二丙酸。使用这些物质的聚醚衍生物(E2)具有低粘度，并且容易处理。
聚醚(E1)与酯化剂(a)之间的反应条件可以是一般的酯化反应条件。例如，在单级合成方法的情况下，可以使用酯化催化剂，优选酸催化剂(例如对甲苯磺酸、硫酸等)。合成优选在50-150℃下、更优选70-130℃下进行8-20小时。聚醚(E1)和酯化剂(a)的官能团当量比(E1)/(a)优选是0.5-2.0，更优选0.9-1.5。如果该比例是0.5以上，则未反应的(a)不会大量残留，而且不必冲洗或进行其它处理；如果是2.0以下，则聚醚衍生物(E2)润滑能力优良。此外，需要的话，可以将溶剂，如甲苯、苯用于反应。酯化反应可以在常压、减压或加压下进行，但是优选减压，因为可缩短反应时间。减压的程度在反应的最后阶段中优选是30mmHg以下，特别优选10mmHg以下。酯化反应的进行状态可以通过从反应体系中蒸馏出的水、低级醇的量、反应体系的酸值、粘度、反应体系的数均分子量等判断。
作为可用于聚醚(E1)与多异氰酸酯的反应产物(E23)中的多异氰酸酯(b)，可以使用二至六或更高的多异氰酸酯。可以提及过去用于聚氨酯制备的那些。具体地，可以提及下列(b1)-(b4)。
(b1)芳族多异氰酸酯：
1，3-和/或1，4-苯二异氰酸酯，2，4-和/或2，6-甲苯二异氰酸酯(TDI)，粗制TDI，2，4’-和/或4，4’-二苯基甲烷二异氰酸酯(MDI)，4，4’-联苯二异氰酸酯，3，3，-二甲基-4，4’-联苯二异氰酸酯，3，3’-二甲基-4，4’-二苯基甲烷二异氰酸酯等；
(b2)脂族多异氰酸酯：
亚乙基二异氰酸酯，四亚甲基二异氰酸酯，六亚甲基二异氰酸酯(HDI)，十二亚甲基异氰酸酯，2，2，4-三甲基六亚甲基二异氰酸酯，赖氨酸二异氰酸酯，2，6-二异氰酸酯甲基己酸酯，双(2-异氰酸酯乙基)富马酸酯等；
(b3)脂环族多异氰酸酯：
异佛尔酮二异氰酸酯(IPDI)，二环己基甲烷-4，4’-二异氰酸酯(氢化MDI)，亚环己基二异氰酸酯，甲基亚环己基二异氰酸酯(氢化TDI)等；
(b4)芳族脂族多异氰酸酯：
间-和/或对亚二甲苯基二异氰酸酯(XDI)，α，α，α’，α’-四甲基亚二甲苯基二异氰酸酯(TMXDI)等；
其中，优选芳族多异氰酸酯(b1)和脂族多异氰酸酯(b2)，更优选1，3-和/或1，4-亚苯基二异氰酸酯，2，4-和/或2，6-甲苯二异氰酸酯(TDI)，粗制TDI，2，4’-和/或4，4’-二苯基甲烷二异氰酸酯(MDI)，亚乙基二异氰酸酯，四亚甲基二异氰酸酯和六亚甲基二异氰酸酯(HDI)。
聚醚(E1)与多异氰酸酯(b)之间的反应条件可以是一般的氨酯化(urethanation)反应条件。例如，可以使用氨酯化催化剂，优选过渡金属催化剂(例如二月桂酸二丁基锡等)，优选在50-150℃下、更优选70-130℃下合成8-20小时。聚醚(E1)和多异氰酸酯(b)的官能团当量比(E1)/(b)优选是0.5-2.0，更优选0.9-1.5。如果是0.5-2.0，聚醚衍生物(E2)的润滑性能良好。此外，根据需要，可以将甲苯、二甲苯、二甲基甲酰胺、乙酸丁酯或其它溶剂用于该反应。氨酯化反应可以在任何常压或压力下进行。氨酯化反应的进行状态可以从反应体系的异氰酸酯基团含量、粘度、反应体系的数均分子量等判断。
作为可用于聚醚与多卤化物的反应产物(E24)中的多卤化物(c)，可以提及二至四或更高的C1-C5氯化物或溴化物，特别是(c1)和(c2)。
(c1)C1-C2多卤化物：
二氯甲烷，二氯乙烷，二溴甲烷，二溴乙烷，三氯乙烯等；
(c2)C3或更高级的多卤化物：
1，3-二氯丙烷，1，3-三氯丙烷，1，2-二溴丁烷等。在多卤化物(c)中，优选C1-C2多卤化物(C1)。特别地，使用二氯甲烷或二氯乙烷的聚醚衍生物(E2)的粘度偏低，而且易于处理。
聚醚(E1)与多卤化物(c)的反应在一般的酯化反应条件下进行。例如，碱，优选无机碱(例如氢氧化钠或氢氧化钾)以基于卤素0.9-1.5当量的用量加入，并且体系优选在50-150℃、更优选70-130℃下进行6-24小时。聚醚(E1)和多卤化物(c)的官能团当量比(E1)/(c)优选是0.5-2.0，更优选0.9-1.5。如果是0.5-2.0，聚醚衍生物(E2)的润滑性能优异。此外，需要的话，可以将溶剂，如甲苯、苯用于该反应。酯化反应可以在常压和减压下进行。酯化反应的进行状态可以从反应体系的碱值、粘度、反应体系的数均分子量等判断。
聚醚(E1)和/或聚醚衍生物(E2)相对于100重量份的所述橡胶成分的重量比例是1-30重量份，优选2-15重量份。如果(E1)和/或(E2)的存在量少于1重量份，则橡胶组合物的加工性差，并且无法充分增强，因此例如耐磨损性等劣化。如果多于30重量份，则橡胶组合物的硬度变得太低，而且例如强度降低。
根据本发明的轮胎用橡胶组合物可以使用适用作合成或天然树脂的增强填料的已知填料。作为填料，可以提及金属氧化物、金属氢氧化物、金属碳酸盐、金属磺酸盐、金属硅酸盐、金属氮化物、碳或其它填料。
作为金属氧化物，可以提及例如二氧化硅、硅藻土、氧化铝、氧化锌、氧化钛、氧化钙、氧化镁、氧化铁、氧化锡、氧化锑等。
作为金属氢氧化物，可以提及例如氢氧化钙、氢氧化镁、氢氧化铝、碱式碳酸镁等。
作为金属碳酸盐，可以提及例如碳酸钙、碳酸镁、碳酸锌、碳酸钡、片钠铝石、水滑石等。
作为金属硫酸盐，可以提及例如硫酸钙、硫酸钡、石膏纤维等。
作为金属硅酸盐，可以提及例如硅酸钙、滑石、高岭土、粘土、云母、蒙脱石、膨润土、活化粘土、海泡石、水铝英石、绢云母、玻璃纤维、玻璃珠、二氧化硅基中空小球等。
作为金属氮化物，可以提及例如氮化铝、氮化硼、氮化硅等。
作为碳，可以提及例如炭黑、石墨、碳纤维、中空碳球、木炭粉、富勒烯(fullerrene)等。
作为其它填料，可以提及例如多种其它金属粉末(如金、银、铜、锡等)，钛酸钾，钛酸锆酸铅，硼酸铝，硫化钼，碳化硅，不锈钢纤维，硼酸锌，矿渣纤维，Teflon(注册商标)粉，锯末，纸浆，橡胶粉末，芳族聚酰胺(aramide)纤维，淀粉等。
这些填料可以单独使用或者以两种或更多种组合使用。这些填料中，从增强能力，如耐磨损性的观点优选炭黑和二氧化硅，更优选二氧化硅。
增强填料基于100重量份的橡胶组分的重量比是10-180重量份，优选30-100重量份。如果填料的混合量小于10重量份，无法使橡胶充分增强，因此例如耐磨损性等易于劣化。相反地，如果超过180重量份，硬度变得太高，而加工性易于降低。
填料的形状没有特别限制，但是可以提及纤维状、针状、片状、球状、粒状(即不规则形状，以下相同含义)、tetrapots、中空球状等。此外，需要的话，可以在其表面上用处理剂处理填料。作为表面处理剂，可以使用已知的表面处理剂。例如，可以提及硅烷偶联剂、钛酸酯偶联剂、铝酸酯偶联剂、油或脂肪、聚乙二醇型阴离子表面活性剂、多元醇型阴离子表面活性剂、蜡、脂肪酸、羧酸偶联剂、磷酸偶联剂等。
作为硅烷偶联剂，可以提及例如双(3-三乙氧基甲硅烷基丙基)四硫化物、双(3-三甲氧基甲硅烷基丙基)四硫化物、双(3-甲基二甲氧基甲硅烷基丙基)四硫化物、双(3-三乙氧基甲硅烷基乙基)四硫化物、双(3-三乙氧基甲硅烷基丙基)二硫化物、双(3-三甲氧基甲硅烷基丙基)二硫化物、双(3-三乙氧基甲硅烷基丙基)三硫化物、3-巯基-丙基三甲氧基硅烷、3-巯基丙基三乙氧基硅烷、乙烯基三乙氧基硅烷、乙烯基三甲氧基硅烷、3-氨基丙基三乙氧基硅烷、3-氨基丙基三甲氧基硅烷、3-巯基丙基甲基二甲氧基硅烷、γ-环氧丙氧基-丙基三甲氧基硅烷、γ-环氧丙氧基丙基甲基二乙氧基硅烷、3-三甲氧基甲硅烷基丙基-N，N-二甲基氨甲酰基-四硫化物、3-三甲氧基甲硅烷基丙基-苯并噻唑基四硫化物、3-三甲氧基-甲硅烷基-丙基甲基丙烯酰基单硫化物、γ-氯丙基三甲氧基硅烷、乙烯基三(β-甲氧基乙氧基)硅烷、γ-甲基丙烯酰氧丙基-三甲氧基硅烷和β-(3，4-环氧环己基)乙基三甲氧基硅烷等。这些可以单独使用或多种一起使用。
作为钛酸酯偶联剂，可以提及例如异丙基三异硬脂酰基等。作为铝酸酯偶联剂，可以提及例如乙酰烷氧基铝二异丙氧化物等。
作为油或脂肪，可以提及例如芳香油、石蜡油、椰子油、米糠油、豆油、亚麻籽油、水合蓖麻油、红花油、桐油等。作为聚乙二醇型阴离子表面活性剂，可以提及例如高级醇环氧乙烷加合物、脂肪酸环氧乙烷加合物、高级烷基胺环氧乙烷加合物、聚丙二醇环氧乙烷加合物等。作为多元醇型阴离子表面活性剂，可以提及例如聚环氧乙烷、甘油脂肪酸酯、季戊四醇脂肪酸酯、山梨糖醇或脱水山梨糖醇脂肪酸酯、多元醇烷基醚和链烷醇胺脂族酰胺等。
至于蜡，可以提及例如聚丙烯马来酸酯、聚乙烯马来酸酯等。作为脂肪酸，可以提及例如硬脂酸、油酸、亚油酸(linolic acid，linoleic acid)、桐酸等。
作为羧酸偶联剂，可以提及例如羧化聚丁二烯、羧化聚异戊二烯等。至于磷酸偶联剂，可以提及例如磷酸基偶联剂，如磷酸单辛基酯、磷酸单(2，6-二甲基-7-辛烯基)酯、磷酸单(6-巯基己基)酯、磷酸单(2-甲基丙烯酰氧丙基)酯等。
当使用表面处理剂时，其添加量基于100重量份橡胶优选是1-20重量份，更优选2-10重量份。
在混合添加剂时，作为混合方法，可以使用普通的已知方法。通常，可以采用合适的例如捏合机、密闭式混合机、班伯里密炼机、滚筒等混合块状、球状或粉状的成分，然后压制成形。此外，需要的话，可以以其通常的配合量适当地添加通常用于橡胶工业中的任意配合剂，例如硫化促进剂(如醛-氨-胺类、硫脲类、胍类、噻唑类、亚磺酰胺类、秋兰姆类、二硫代氨基甲酸盐类、xantogen acid盐类、二硫代磷酸盐类等)，硫化剂(硫等)，防焦烧剂(有机酸、N-亚硝基化合物等)，着色剂，UV吸收剂，常用增塑剂(如邻苯二甲酸类、苯偏三酸类、磷酸类、环氧类等)，软化剂，抗氧化剂，有机过氧化物等。
混合时成分的添加顺序没有特别限制。可以将聚醚(E1)和/或其衍生物(E2)与填料混合，然后将其混入橡胶中，或者同时混合聚醚(E1)和/或其衍生物(E2)、填料和橡胶。
至于本发明橡胶组合物的成型方法，可以提及注射成型、压缩成型、压延成型(calendaring)、中空模塑、旋转成型、挤出、吹塑、膜成型(如铸造、拉幅、膨胀等)、硫化压制成型等。基于应用，可以采用任意方法。
实施例
实施例用于进一步解释本发明，但是本发明绝不限于这些实施例。注意的是以下“份”表示“重量份”。
用于实施例中的配合剂如下：
S-SBR：Bayer的溶液聚合SBR VSL5025(油增塑oil extension37.5phr)
BR：Nippon Zeon的BR 1220
填料(炭黑)：Tokai Carbon的N234
填料(二氧化硅)：Rhodia的Z1165MP
硅烷偶联剂：Degussa的双-[3-(三乙氧基甲硅烷基)-丙基]四硫化物(即Si69)
锌白：Seido Chemical(Zinc White No.3)
硬脂酸：NOF Corporation的Beads Stearic Acid
抗氧化剂6C：Flexsys的N-苯基-N’-(1，3-二甲基丁基)-对亚苯基二胺(SANTOFLEX 6PPD)
操作油：Fuji Kosan的Aromatics 3
硫：Hosoi Chemical Industrial的油增塑硫
硫化促进剂CZ：Ouchi Shinko Chemical Industrial制的N-环己基-2-苯并噻唑基亚磺酰胺(Noccelar CZ-G)
硫化促进剂DPG：Ouchi Shinko Chemical Industrial二苯胍(NoccelarD)
聚醚E1：在下列合成例1中合成的1，4-丁二醇的THF 14.3mol/EO20.4mol无规加合物
合成例1
向玻璃高压釜中装入90份1，4-丁二醇(1.0mol)，1032份THF(14.3mol)和12.8份BF3-THF，并在35-50℃下经过10小时由耐压滴液漏斗滴加896份EO(20.4mol)。此后，所得到的混合物在50℃下反应5小时，接着冷却。进而，加入7.4份48％NaOH水溶液，然后在30mmHg以下蒸馏出未反应的物质。此后，使用吸附处理剂(Kyowa Chemical Industry Kyoward600和Kyoward 1000，以下相同)进行处理，然后过滤所得到的混合物，接着在减压下脱水(即130℃，30mmHg以下，1小时，以下相同)以获得2000份1，4-丁二醇的THF 14.3mol/EO 20.4mol无规加成产物(聚醚E1)。
聚醚E2：在下列合成例2中合成的月桂醇的THF 6.5mol/PO 10.0mol无规加成产物
合成例2
向玻璃高压釜中装入186份月桂醇(1.0mol)，468份四氢呋喃(THF)(6.5mol)和7.9份BF3-THF，并且在35-50℃下经过10小时由耐压滴液漏斗滴加580份(10.0mol)PO。此后，所得到的混合物在50℃下反应5小时，接着冷却。进而，加入4.8份48％NaOH水溶液，然后用吸附处理剂进行处理，将所得到的混合物过滤，并在130℃和30mmHg以下的减压真空下脱水，以获得1230份月桂醇的THF 6.5mol/PO 10.0mol无规加成产物(聚醚E2)。
聚醚E3：在下列合成例3中由合成的聚醚E2和琥珀酸得到的酯
合成例3
装入1234份合成例2中得到的聚醚E2(1.0mol)、59份琥珀酸(0.5mol)、4.8份对甲苯磺酸1水合物和3.2份连二磷酸，并在100-120℃下反应(酯化)12小时，同时使氮气通过溶液，并除去反应中生成的水。所得到的混合物用吸附处理剂进行处理，并过滤以除去对甲苯磺酸1水合物和连二磷酸，然后在减压下脱水以获得1100份室温下为液体并且酸值(根据JIS K 1557测定)为3.0的聚醚化合物(聚醚E3)。
聚醚E4：在以下合成例4中合成的月桂醇的EO 19.0mol加合物
合成例4
向玻璃高压釜中装入186份(1.0mol)月桂醇和3.3份KOH。在105℃下经过33小时由耐压滴液漏斗滴加836份EO(19.0mol)。此后，所述成分在130℃下反应10小时，接着冷却。进而，所得到的混合物用吸附处理剂处理，过滤，然后在130℃和30mmHg以下的减压中脱水以获得1000份月桂醇的EO 19.0mol加合物(聚醚E4)。
聚醚E5：Sanyo Chemical Industries聚丙二醇“Newpol PP-2000”
聚醚E6：Sanyo Chemical Industrial聚乙二醇“PEG-4000S”
就物理性能来评价在下列实施例中得到的未硫化的母料、轮胎胎面胶组合物和采用该胎面用组合物形成的尺寸P205/60R15的充气轮胎。
(1)门尼粘度：将未硫化的母料用于在100℃下根据JIS K 6300测定门尼粘度，并评价捏合性/加工性。门尼粘度的值表示为相对于标准例的值100的指数。该值越小，混合/力加工能力越好。
(2)ΔG′：将α-Technology RPA2000用于测量应变剪切应力G’。未硫化橡胶用于在160℃下硫化20分钟，并在0.28％-30.0％的应变下测量G’。差值(G’0.28(MPa)-G’30.0(MPa))表示为指数。该值越小，二氧化硅的分散越好。
(3)潮湿制动性能：各个轮胎在撒有水的沥青路面上以40km/h的初速度行驶，然后将车辆制动。测量此时的制动距离，并相对于标准例的100进行指数化。该值越大，显示的制动性越好。
(4)滚动阻力：测量在80km/h的车辆速度下滚动阻力的值，并相对于标准例的100进行指数化。该值越小，显示的滚动阻力值越低。
(5)耐磨损性：在负荷相当于JATMA(1998年鉴)中规定的最大负荷能力的88％以及气压为200kPa的条件下，各个轮胎在干路面上行驶10000km，然后将各个轮胎的磨损相对于标准例的磨损指数化。该值越大，显示的耐磨损性越好。
标准例，实施例1-3和比较例1-3
将表I中所示各配方中除硫化体系以外的成分在1.8L密闭式混合机中混合3-5分钟。当机中内容物达到165±5℃时，放出混合物。然后通过8-英寸敞开式滚筒将该混合物，即母料，与硫化促进剂和硫混合，以得到橡胶组合物。该组合物用于评价门尼粘度和ΔG′。另一方面，该橡胶组合物用作胎面以通过常规方法制备尺寸P205/60R15轮胎，然后评价其混合/加工性以及物理性能。结果示于表I中。
表I
| 标准例 | 实施例 | 比较例 | |||||
| 1 | 2 | 3 | 1 | 2 | 3 | ||
| 配方(重量份)S-SBRBR炭黑二氧化硅硅烷偶联剂锌白硬脂酸抗氧化剂6C操作油硫硫化促进剂CZ硫化促进剂DPG聚醚E1聚醚E2聚醚E3聚醚E4 | 96.2530.0010705.632.52101.51.71---- | 96.2530.0010705.632.52101.51.715--- | 96.2530.0010705.632.52101.51.71-5-- | 96.2530.0010705.632.52101.51.71--5- | 96.2530.0010705.632.52101.51.71---5 | 96.2530.0010705.632.52101.51.71---- | 96.2530.0010705.632.52101.51.71---- |
| 聚醚E5聚醚E6 | -- | -- | -- | -- | -- | 5- | -5 |
| 橡胶物理性能(指数)门尼粘度ΔG′ | 100100 | 9374 | 9077 | 8875 | 9895 | 9597 | 9396 |
| 轮胎性能(指数)潮湿制动性能滚动阻力耐磨损性 | 100100100 | 10785105 | 10688105 | 10686104 | 1029898 | 1019897 | 10210096 |
工业应用性
本发明的轮胎用橡胶组合物和充气轮胎具有优异的加工性、经济性(即低滚动阻力)和安全性(即高抓地力)，因此可以用于汽车轮胎等。
Claims (6)
1.一种轮胎用橡胶组合物，其包含100重量份橡胶，1-30重量份式(I)的聚醚(E1)和/或其衍生物(E2)以及10-180重量份填料：
R1-{(OCH2CH2CH2CH2)m(OA)n-OH}q (I)
其中R1是从具有1-6个羟基的C1-C24化合物中除去至少1个羟基后的残基，A是除1，4-亚丁基以外的C2-C24亚烷基，q是1-6的整数，m和n独立地是1-600的整数。
2.权利要求1的轮胎用橡胶组合物，其中所述聚醚(E1)是HLB为10或更小以及重均分子量为500-30,000的聚醚。
3.权利要求1或2的轮胎用橡胶组合物，其中所述聚醚衍生物(E2)是所述聚醚(E1)的烷基醚化产物或羧酸酯化产物或者是聚醚(E1)与多异氰酸酯或多卤化物的反应产物。
4.权利要求3中所述的轮胎用橡胶组合物，其中所述酯化产物是由所述聚醚(E1)与选自C2-C22羧酸、C2-C22羧酸酐、具有C1-C4烷基的羧酸烷基酯和C2-C22羧酸酰卤中的至少一种化合物的反应得到的酯化产物。
5.权利要求1-4中任一项的轮胎用橡胶组合物，其中所述填料是炭黑和/或二氧化硅。
6.一种充气轮胎，其使用权利要求1-5中任一项的橡胶组合物作为其胎面。
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| PCT/JP2005/010207 WO2005118705A1 (ja) | 2004-06-01 | 2005-05-27 | タイヤ用ゴム組成物及びそれを用いた空気入りタイヤ |
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| CN107108969B (zh) * | 2014-11-28 | 2019-11-22 | 住友橡胶工业株式会社 | 轮胎用橡胶组合物及充气轮胎 |
| CN107638991A (zh) * | 2017-09-28 | 2018-01-30 | 高祥桐 | 一种用于管道内径焊缝的密封装置 |
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| Publication number | Publication date |
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| US8722781B2 (en) | 2014-05-13 |
| EP1754750A1 (en) | 2007-02-21 |
| EP1754750A4 (en) | 2009-08-26 |
| KR20070052701A (ko) | 2007-05-22 |
| WO2005118705A1 (ja) | 2005-12-15 |
| CN1972993B (zh) | 2011-02-16 |
| US20080097023A1 (en) | 2008-04-24 |
| JP4810798B2 (ja) | 2011-11-09 |
| JP2005343963A (ja) | 2005-12-15 |
| EP1754750B1 (en) | 2011-09-21 |
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