CN114729245A - 用于轮胎帘子线的粘合剂组合物、轮胎帘子线和轮胎 - Google Patents
用于轮胎帘子线的粘合剂组合物、轮胎帘子线和轮胎 Download PDFInfo
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- CN114729245A CN114729245A CN202180006471.1A CN202180006471A CN114729245A CN 114729245 A CN114729245 A CN 114729245A CN 202180006471 A CN202180006471 A CN 202180006471A CN 114729245 A CN114729245 A CN 114729245A
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Abstract
本发明涉及一种用于轮胎帘子线的粘合剂组合物、轮胎帘子线和轮胎,所述粘合剂组合物包含环氧化合物、胶乳、重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂、胺化合物和水,所述轮胎帘子线包括由上述粘合剂组合物形成的粘合层,所述轮胎包括上述轮胎帘子线。
Description
技术领域
本发明涉及一种用于轮胎帘子线的粘合剂组合物、轮胎帘子线和轮胎。
背景技术
为了增强橡胶结构的强度,使用纤维增强材料。例如,在橡胶轮胎中,聚酯纤维、聚酰胺纤维、芳族聚酰胺纤维或聚乙烯醇纤维等可以用作增强材料。并且,在一些情况下,根据纤维,纤维与橡胶之间的粘合性不好,因此,将粘合剂涂布在纤维的表面上以增补纤维与橡胶之间的粘合性。例如,为了改善用于轮胎帘子线的聚酯纤维(原帘子线)与轮胎橡胶之间的粘合强度,将粘合剂涂布在聚酯纤维上。
一般而言,在用于上述目的的粘合剂中,包括含有间苯二酚-甲醛或由其衍生的成分的橡胶(或胶乳)。然而,包含已知为致癌物的间苯二酚(一种酚)和甲醛的RF已知对人体有害。而且,对于包含RF的粘合剂废液,通常要求特定的后续管理和后续处理成本。
同时,作为在纤维增强材料上涂布上述粘合剂组合物的方法,可以考虑浸渍或喷涂。在这个准备过程中,构成粘合剂组合物的各个组分应在该组合物中包含的溶剂中均匀地混合和分散。并且,即使在浸渍或喷涂其中各个组分均匀混合并分散的组合物后,该组合物也应当以适当的量均匀地涂覆在纤维增强材料的表面上。如果组合物的组分没有充分混合或者组合物的流动性由于过度使用溶剂而过度增加,则粘合强度不能得到确保。
发明内容
技术问题
本发明的一个目的是提供一种环境友好的用于轮胎帘子线的粘合剂组合物,该粘合剂组合物能够显著提高轮胎橡胶和轮胎帘子线之间的粘合强度和耐热粘合强度。
本发明的另一目的是提供一种轮胎帘子线,其对轮胎橡胶具有高粘合强度和耐热粘合性,因此,能够改善轮胎的耐久性。
本发明的还一目的是提供一种包括上述轮胎帘子线的轮胎。
技术方案
于此本发明提供一种用于轮胎帘子线的粘合剂组合物,包含:环氧化合物;胶乳;重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂;胺化合物;和水。
于此本发明还提供一种轮胎帘子线,包括:纤维基底;和在所述纤维基底上形成的粘合层,且该粘合层由上述用于轮胎帘子线的粘合剂组合物形成。
于此本发明还提供一种轮胎帘子线,包括:纤维基底;和在所述纤维基底上形成的粘合层,且该粘合层包含环氧化合物、胶乳、重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂和胺化合物。
于此本发明还提供一种包括上述轮胎帘子线的轮胎。
下文,将详细地说明根据本发明特定实施方案的用于轮胎帘子线的粘合剂组合物、轮胎帘子线和轮胎。
如于此所使用的,重均分子量是指由GPC方法测量的聚苯乙烯换算的重均分子量。在测量由GPC测量的聚苯乙烯换算的重均分子量的过程中,可以使用公知的分析设备、检测器(如折射率检测器)和分析柱子,并且可以应用通常应用的温度条件、溶剂和流速。
作为测量条件的具体实例,用于分析的0.05%-LiCl/DMF溶液通过称量2.12g无水氯化锂(LiCl)、放入1l的容量瓶中并溶解在N,N-二甲基甲酰胺(DMF)中而制得。将0.0250g(25mg)的诸如聚氨酯树脂的聚合物样品加入小瓶中,将10ml的0.05%-LiCl/DMF加入并溶解。然后,使用孔径为0.45μm的注射器过滤器过滤该溶液,并将100μl溶液引入GPC中,作为GPC的流动相,使用LiCl/DMF并以1.0mL/min的流速引入;作为柱子,1个Agilent PLgel5μmGuard(7.5x 50mm)和2个Agilent PLgel 5μm Mixed D(7.5x 300mm)串联连接;作为检测器,使用Agilent 1260Infinity II***,RI检测器;测量温度为40℃。
对于标准物质,将0.0050g(5mg)的聚苯乙烯加入小瓶中,将5ml的0.05%-LiCl/DMF加入并溶解,并通过上述方法进行测量。通过PS 842000、193000、65000、16200和4000绘制校准曲线。
根据本发明的一个实施方案,提供一种用于轮胎帘子线的粘合剂组合物,包含:环氧化合物;胶乳;重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂;胺化合物;和水。
本发明人通过实验证实,应用于轮胎帘子线的粘合剂组合物即使包含常见的聚氨酯树脂,也不能充分确保粘合强度,而在使用具有预定重均分子量的脂环族聚氨酯树脂的情况下,粘合强度和耐热粘合强度能够得到显著改善,特别是,可以表现出与轮胎橡胶的高粘合强度和耐热粘合性,因此,能够改善轮胎的耐久性,从而完成本发明。
更具体地,由于用于轮胎帘子线的粘合剂组合物中包含的脂环族聚氨酯树脂的重均分子量(Mw)为250,000至350,000,所以用于轮胎帘子线的粘合剂组合物在室温下可以具有与胶乳相似的粘度,即使在高温下也不发生水解,并且该组合物具有高粘合性且在搅拌过程中稳定。
具体地,聚氨酯的重均分子量(Mw)的下限可以是,例如255,000以上、260,000以上、265,000以上、270,000以上、275,000以上、280,000以上、285,000以上、290,000以上、295,000以上、300,000以上或者305,000以上。并且,聚氨酯的重均分子量(Mw)的上限可以是,例如345,000以下、340,000以下、335,000以下、330,000以下、325,000以下、320,000以下、315,000以下、310,000以下、305,000以下或者300,000以下。
如果脂环族聚氨酯树脂的重均分子量(Mw)低,则用于轮胎帘子线的粘合剂组合物的粘度可能会相对低,因此,可能不能表现出充分的粘合性能,并且可能不能确保与轮胎橡胶的高粘合强度和耐热粘合性。
如果脂环族聚氨酯树脂的重均分子量(Mw)高,则用于轮胎帘子线的粘合剂组合物的粘度可能会显著增加,因此,其它组分可能会不均匀混合,因此,可能会难以确保均匀的粘合强度。并且,如果脂环族聚氨酯树脂的重均分子量(Mw)高,则脂环族聚氨酯树脂本身可能会预先反应或者与其它组分反应以形成凝胶,因此,可能会干扰均匀粘合剂溶液的制备,并且可能会产生产品的外观缺陷。
同时,所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂保护或捕获下面描述的胺化合物,因此使得由粘合剂组合物形成的粘合层(或涂层)的能够稳定固化。并且,由于聚氨酯具有优异的与橡胶或胶乳组分的亲和力,其有助于粘合剂组合物与包括橡胶的被粘物的稳定粘合,因此确保了优异的与被粘物的粘合强度(特别是,耐热粘合强度)。此外,在使用水分散的聚氨酯的情况下,还可以确保聚氨酯的耐磨性和弹性。
所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂包含脂环结构,因此,不仅可以提高用于轮胎帘子线的粘合剂组合物和由其制备的轮胎帘子线的机械强度和尺寸稳定性,而且可以提高耐热性和疲劳性能。
相反,在用于轮胎帘子线的粘合剂组合物包含在分子中含有芳基的芳族聚氨酯树脂的情况下,使用其制备的轮胎帘子线的拉伸强度或耐疲劳性可能会劣化,或者用于轮胎帘子线的粘合剂组合物的均匀性或均质性可能会劣化,因此,粘合强度可能会劣化。
所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂可以包含多异氰酸酯与多元醇之间的反应产物,该多异氰酸酯包含一个或更多个碳数为4至30的脂环基,更具体地,其可以包含二异氰酸酯与多元醇之间的反应产物,该二异氰酸酯包含一个或更多个碳数为4至30的脂环基并且包含总碳数为4至40的中心基团。
脂环族二异氰酸酯可以是4,4’-二环己基甲烷二异氰酸酯(H12MDI)、异佛尔酮二异氰酸酯(IPDI)、1,4-亚环己基二异氰酸酯或其混合物。
作为多元醇的实例,可以提及聚酯多元醇、聚醚多元醇和聚碳酸酯多元醇等。
所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂可以还包含:醇类物质,例如乙二醇(EG)、1,4-丁二醇(BD)、1,6-己二醇(HD)和三羟甲基丙烷(TMP)等;和增链剂,例如乙二胺(EDA)和二乙醇胺等。
同时,所述脂环族聚氨酯树脂可以是分散在水(H2O)中的聚氨酯。对在水分散的聚氨酯中包含的水的含量不特别限定。例如,在水分散的聚氨酯中水的含量可以为40wt%至80wt%,其它含量可以由聚氨酯占据。根据情况,少量的已知添加剂可以以约10wt%以下、约5wt%以下或约1wt%以下的含量包含在水分散的聚氨酯中。
更具体地,所述脂环族聚氨酯树脂可以是由脂环族聚氨酯离聚物形成的水分散的脂环族聚氨酯树脂。
所述由脂环族聚氨酯离聚物形成的水分散的脂环族聚氨酯树脂可以如下制备:由如4,4’-二环己基甲烷二异氰酸酯(H12MDI)等的脂环族多异氰酸酯、1,6-己二醇(HD)和二羟甲基丁酸(DMBA)等制备聚酯聚氨酯(PU),并用三乙胺(TEA)中和,然后将其分散在水中并在水中用乙二胺(EDA)进行链增长。
更具体地,所述脂环族聚氨酯树脂可以包含1mol%至20mol%的来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分。
在所述脂环族聚氨酯树脂中,来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分连接脂环族聚氨酯树脂表面上的离子官能团,从而提高了在水中分散过程中整个分子的稳定程度,从而用于轮胎帘子线的粘合剂组合物可以在高温下具有粘合强度和柔韧性。
如果在脂环族聚氨酯树脂中来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分的含量太小,则脂环族聚氨酯树脂的聚合度可能会降低,或者可能不能充分确保分子量。
如果在脂环族聚氨酯树脂中来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分的含量太大,则用于轮胎帘子线的粘合剂组合物的粘度可能会增大,或者在组合物中可能会形成淤泥(sludge)。
同时,所述用于轮胎帘子线的粘合剂组合物可以包含0.5wt%至10wt%的重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂。
如果与环氧化合物相比,所述用于轮胎帘子线的粘合剂组合物包含低含量的脂环族聚氨酯树脂,则粘合性能和疲劳性能可能会劣化,并且粘合性能可能会显著劣化。如果与环氧化合物相比,用于轮胎帘子线的粘合剂组合物包含过量含量的脂环族聚氨酯树脂,则用于轮胎帘子线的粘合剂组合物的浓度可能会显著增加,因此,在施用粘合剂组合物的过程中可能会产生淤泥或可能会产生凝胶,并且可能会产生产品的外观缺陷。
同时,所述用于轮胎帘子线的粘合剂组合物可以满足在室温下使用乌氏粘度计测量的粘度在2.50至2.85的范围内。
“室温”是温度没有特别升高或降低的状态,例如,它可以是指在15℃至30℃范围内的温度。具体地,在上述温度范围内,室温可以是17℃以上、19℃以上、21℃以上或23℃以上且29℃以下或27℃以下的温度。
并且,在整个说明书中,除非特别定义,否则进行数值性质的评价的温度可以是室温。
具体地,所述粘合剂组合物的粘度的下限可以是,例如2.51以上、2.52以上、2.53以上、2.54以上、2.55以上、2.56以上、2.57以上、2.58以上、2.59以上、2.60以上、2.61以上、2.62以上、2.63以上、2.64以上、2.65以上、2.66以上、2.67以上、2.68以上、2.69以上或者2.70以上。
并且,所述粘合剂组合物的粘度的上限可以是,例如2.84以下、2.83以下、2.82以下、2.81以下、2.80以下、2.79以下、2.78以下、2.77以下、2.76以下、2.75以下、2.74以下、2.73以下、2.72以下或者2.71以下。
在所述用于轮胎帘子线的粘合剂组合物满足上述粘度范围的情况下,如下面试验所示,可以确保最佳的吸附率(pick up rate),可以改善加工性和生产率,并且可以提供优异的粘合强度。
特别地,已证实,考虑到火灾的风险、对人体的危害和组合物的其它组分的分散性等,使用水(H2O)代替有机溶剂作为粘合剂组合物或组合物中包含的各成分的分散介质时,粘合剂组合物的粘度可能会降低,并且可能不能确保充分的粘合强度。
所述环氧化合物起到固化剂的作用,因此当热处理粘合剂时形成三维网状结构,并赋予由粘合剂组合物形成的涂层粘合强度和层稳定性。
假设满足上面说明的总组合物的粘度范围,则对粘合剂组合物中包含的环氧化合物的种类不特别限制。例如,可以使用缩水甘油醚类化合物,如二甘醇-二缩水甘油醚、聚乙二醇-二缩水甘油醚、聚丙二醇-二缩水甘油醚、新戊二醇-二缩水甘油醚、1,6-己二醇-二缩水甘油醚、甘油-聚缩水甘油醚、三羟甲基丙烷-聚缩水甘油醚、聚甘油-聚缩水甘油醚、季戊四醇-聚缩水甘油醚、二甘油-聚缩水甘油醚和山梨醇-聚缩水甘油醚等;线性酚醛型环氧树脂,如苯酚线性酚醛型环氧树脂或甲酚线性酚醛型环氧树脂等;以及双酚型环氧树脂,如双酚A型环氧树脂或双酚F型环氧树脂等。
并且,假设满足上面说明的总组合物的粘度范围,则可以使用已知的或市售的环氧化合物。例如,作为环氧化合物,可以使用来自Nagase的EX614B、来自Kolon的KETL6000、来自Ipox Chemicals的CL16或来自Raschig的GE500等。
上面建议的市售的山梨醇聚缩水甘油醚的环氧当量(g/EQ)可以为120~300g/eq,并且如果山梨醇聚缩水甘油醚的当量小于120,则环氧树脂的聚合单元可能会较小,因此可能会难以在异氰酸酯之间形成网络结构。并且,如果山梨醇聚缩水甘油醚的当量大于300,则每单位分子的环氧量可能会相对不足,因此,粘合强度可能会劣化。
所述用于轮胎帘子线的粘合剂组合物可以包含0.1wt%至10wt%的环氧化合物。
在所述用于轮胎帘子线的粘合剂组合物中包含的胶乳是考虑到组合物的用途而使用的组分。
具体地,所述粘合剂组合物可以用于如橡胶复合物、橡胶结构或橡胶增强材料的被粘物成分,并且在使用胶乳的情况下,其可以有利于确保与被粘物的亲合性、相容性或粘合强度。根据情况,粘合剂组合物中包含的胶乳组分可以与被粘物的橡胶组分相同。
根据一个实例,所述胶乳可以不包含间苯二酚-甲醛或由其衍生的组分。即,所述粘合剂组合物可以是无RF的组合物。因此,与使用RF胶乳的现有技术相比,可以提供对人体无害的环境友好的粘合剂组合物。并且,使用这种粘合剂组合物具有降低后续管理和后续处理成本的优点。
对可以用于所述粘合剂组合物中的胶乳的种类不特别限制,只要其不包含间苯二酚-甲醛或由其衍生的组分并且满足上述说明的总组合物的粘度即可。
根据一个实例,作为所述胶乳,可以使用天然橡胶胶乳、乙烯基-吡啶-苯乙烯-丁二烯共聚物胶乳(VP胶乳)、苯乙烯-丁二烯类共聚物胶乳、丙烯酸酯类共聚物胶乳、丁基橡胶胶乳、氯丁橡胶胶乳或它们的改性胶乳。对于改性胶乳,对改性胶乳的方法或者胶乳的具体种类不限制。例如,可以使用通过用羧酸等改性乙烯基-吡啶-苯乙烯-丁二烯类共聚物而得到的改性胶乳。
也可以使用市售的胶乳,只要可以满足下面描述的总组合物的粘度即可。例如,作为VP胶乳,可以使用商业产品如来自Denaka的LM-60、来自APCOTEX的VP-150、来自NipponA&L的VB-1099或者来自Closlen的5218或0653等。
根据一个实例,包含一种或多种上述胶乳的胶乳组分可以用于粘合剂组合物中。
根据一个实例,所述用于轮胎帘子线的粘合剂组合物可以包含1.0wt%至30wt%的胶乳。在满足上述范围的情况下,其可以有利于确保与含橡胶的被粘物(所述粘合剂组合物用于该含橡胶的被粘物)的亲合性、相容性或粘合强度。
根据一个实例,胶乳在溶解于溶剂(水或有机溶剂)中时,可以与组合物的其它组分混合。
在所述用于轮胎帘子线的粘合剂组合物中包含的胺化合物起到固化剂的作用。由于胺化合物引起的固化或促进固化,可以形成稳定的涂层。
在所述用于轮胎帘子线的粘合剂组合物中,考虑到取决于使用重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂和溶剂(水)而导致的粘度下降,可以使用一种或更多种胺化合物。具体地,所述粘合剂组合物可以包含至少具有链结构的胺化合物。
根据一个实例,具有链结构的胺化合物可以是一种来自乙二胺和硬脂酸的反应的化合物。于此,胺化合物的碳数可以是8至20(产品名称:来自Lonza的AcrawaxTM C分散液)。所述胺化合物可以以固态或液态存在,并且在其以固体存在的情况下,可以使用用于将其分散成液体的溶剂。
此外,不特别限制胺化合物的种类,并且根据本发明的一个实例,可以用作固化剂的胺化合物可用作所述胺化合物,而不受限制。作为所述胺化合物,例如,可以使用脂环族胺、脂族胺和芳族胺中的至少一种。
更具体地,根据本发明的一个实例,来自DAEJUNG的哌嗪、来自Kukdo Chemical的G640和来自Huntsman Corporation的HK511等可以用作所述胺化合物。
考虑到用于轮胎帘子线的粘合剂组合物的固化促进作用,具有链结构的胺化合物与脂环族胺化合物的重量比可以为1:1至3:1或7:1。
所述用于轮胎帘子线的粘合剂组合物可以包含0.1wt%至10wt%的胺化合物。
所述用于轮胎帘子线的粘合剂组合物可以包含水(H2O)。
具体地,考虑到对人体的危害和火灾的风险,所述用于轮胎帘子线的粘合剂组合物使用水作为溶剂,而不是有机溶剂(如甲苯或乙醇)。即,所述用于轮胎帘子线的粘合剂组合物可以是水基组合物(water-based composition)或水性组合物。
根据一个实例,在粘合剂组合物中用作溶剂的水可以是软化水。
根据一个实例,基于测量了粘度的组合物的总重量,水的含量可以是50wt%以上,或者65wt%以上。具体地,水的含量的下限可以是,例如70wt%以上、75wt%以上或者80wt%以上。并且,水的含量的上限可以是,例如95wt%以下、85wt%以下或者75wt%以下。在满足上述范围的情况下,构成该组合物的每个组分可以充分分散在溶剂中。
根据一个实例,在总组合物中水的含量可以是指作为溶剂混合的水的含量。
根据一个实例,在总组合物中水的含量可以不仅包括作为溶剂混合的水的含量,而且还可以包括在其它组分中混合的水的含量,例如用于分散重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂的水。
同时,所述用于轮胎帘子线的粘合剂组合物还可以包含一种或更多种选自异氰酸酯类化合物、氮丙啶类化合物和金属螯合化合物的交联剂。
不特别限制用于赋予粘合强度和内聚强度的交联剂的种类,可以使用例如异氰酸酯类化合物、氮丙啶类化合物、环氧类化合物和金属螯合化合物等的常见化合物。
所述用于轮胎帘子线的粘合剂组合物可以包含1wt%至20wt%含量的交联剂。
当热处理粘合剂时,交联剂形成三维网状结构,从而向由粘合剂组合物形成的涂层赋予粘合强度和层稳定性。
对异氰酸酯的种类不特别限制,但是可以考虑如上所述的总组合物的粘度范围来选择异氰酸酯的种类。例如,作为所述异氰酸酯,可以使用包含脂环基的化合物,即脂环族异氰酸酯。与非芳族多异氰酸酯相比,芳族多异氰酸酯可以确保高反应速率,因此,其可以有利于提高水性组合物的低粘度。
根据一个实例,在异氰酸酯化合物中包含的芳基可以是苯基,作为包含这种芳基的异氰酸酯,例如,可以使用亚甲基二苯基多异氰酸酯或多亚甲基多苯基多异氰酸酯(polymethylene polyphenyl polyisocyanate)等。
根据一个实例,所述异氰酸酯化合物可以是封端异氰酸酯。封端异氰酸酯化合物可以通过向多异氰酸酯化合物中加入已知封端剂的反应来制备。作为这样的封端剂,可以使用如下化合物:例如,酚,如苯酚、苯硫酚、氯苯酚、甲酚、间苯二酚、对仲丁基苯酚、对叔丁基苯酚、对仲戊基苯酚、对辛基苯酚、对壬基苯酚;仲醇或叔醇,如异丙醇和叔丁醇等;芳族仲胺,如二苯基胺和二甲基苯胺等;邻苯二甲酰亚胺;内酰胺,如δ-戊内酰胺等;己内酰胺,如ε-己内酰胺;活性亚甲基化合物,如丙二酸二烷基酯、乙酰丙酮和乙酰乙酸烷基酯等;肟,如丙酮肟、甲基乙基酮肟和环己酮肟等;碱性氮化合物,如3-羟基吡啶,和酸性亚硫酸钠等。
更具体地,市售的水分散的封端异氰酸酯产品,例如来自EMS的IL-6、来自MEISEIChemical的DM-6500等可以用作异氰酸酯。
并且,假设满足上述总组合物的粘度范围,则可以使用已知的或者市售的异氰酸酯化合物。例如,可以使用市售的水分散的封端异氰酸酯产品,例如来自EMS的IL-6或来自MEISEI Chemical的DM-6500等。
同时,根据本发明的另一个实施方案,提供一种轮胎帘子线,包括:纤维基底;和在所述纤维基底上形成的粘合层,且该粘合层由根据一个实施方案的粘合剂组合物形成。
对于根据上述实施方案的用于轮胎帘子线的粘合剂组合物的详细说明,应用上述的说明。
所述用于轮胎帘子线的粘合剂组合物不包含间苯二酚-甲醛或其衍生的组分,因此是环境友好的,并且它可以显著地提高轮胎橡胶和轮胎帘子线之间的粘合强度或耐热粘合强度,因此它对轮胎橡胶具有高粘合强度或耐热粘合强度,并且可以提高轮胎的耐久性。并且,根据本公开,提供一种包括上述轮胎帘子线的轮胎。
虽然不限制轮胎帘子线的具体用途,但是由于包括粘合层,所以可以实现更高的与混合帘子线的粘合性,并且它可以适用于需要更高的耐热性粘合性的大型轮胎。
根据本发明的又一个实施方案,提供一种轮胎帘子线,包括:纤维基底;和在所述纤维基底上形成的粘合层,且该粘合层包含环氧化合物、胶乳、重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂和胺化合物。
所述用于轮胎帘子线的粘合剂组合物不包含间苯二酚-甲醛或其衍生的组分,因此是环境友好的,并且它可以显著地提高轮胎橡胶和轮胎帘子线之间的粘合强度或耐热粘合强度,因此它对轮胎橡胶具有高粘合强度或耐热粘合强度,并且可以提高轮胎的耐久性。并且,根据本公开,提供了一种包括上述轮胎帘子线的轮胎。
所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂可以包含多异氰酸酯与多元醇之间的反应产物,该多异氰酸酯包含一个或更多个碳数为4至30的脂环基。
所述脂环族聚氨酯树脂可以包含1mol%至20mol%的来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分。
所述纤维基底可以是包括聚酯纤维的原帘子线(raw cord)。
虽然不限制轮胎帘子线的具体用途,但是由于包括粘合层,所以可以实现更高的与混合帘子线的粘合性,并且它可以适用于需要更高的耐热性粘合性的大型轮胎。
同时,根据本发明的又一个实施方案,提供一种包括上述轮胎帘子线的轮胎。
充气轮胎可以包括:胎面部;一对胎肩部,分别围绕胎面部延伸至两侧;一对胎侧部,延伸至各自胎肩部;一对胎圈部,分别延伸至各自胎侧部;胎体层,形成在胎面部、胎肩部、胎侧部和胎圈部的内部;帘子线,位于胎体层的内部;带束部,位于胎面部的内表面与胎体层之间;和内衬,粘合至胎体层的内侧。
有益效果
根据本公开内容,可以提供一种环境友好的用于轮胎帘子线的粘合剂组合物,该粘合剂组合物可以显著地提高轮胎橡胶和轮胎帘子线之间的粘合强度和耐热粘合强度;可以提供一种轮胎帘子线,该轮胎帘子线与轮胎橡胶具有高的粘合强度和耐热粘合强度,因此,能够改善轮胎的耐久性;以及可以提供一种包括上述轮胎帘子线的轮胎。
附图说明
图1是示出试验例1中使用的乌氏粘度计的示意图。
具体实施方式
在下面的实施例中将更详细地说明本发明。然而,提供这些实施例仅用于举例说明本发明,本发明的范围不局限于此。
[实施例和比较例:用于轮胎帘子线的粘合剂组合物和轮胎帘子线的制备]
实施例1
(1)水分散的聚氨酯树脂的合成
以下面表1中所示的摩尔比,引入聚酯多元醇(重均分子量:2000)、二醇(1,6-己二醇)和二羟甲基丁酸(DMBA),并在75±5℃和大气压下混合4小时。
而后,以下面表1中所示的摩尔比,将4,4’-二环己基甲烷二异氰酸酯(H12MDI)加入到混合物中,反应2小时以制备脂环族聚氨酯预聚物。
将上述制备的预聚物的反应温度降至60℃,并将中和剂(三乙醇胺,TEA)引入到溶剂(丙酮)中以分散。于此,使用搅拌器来分散,且搅拌器的RPM保持在1000至1500。分散完成之后,对预聚物减压以除去丙酮。
向中和的预聚物中引入蒸馏水,使得固含量变为60%。而后,加入增链剂(乙二胺,EDA)以制备水分散的脂环族聚氨酯(重均分子量:308,000g/mol)。
(2)用于轮胎帘子线的粘合剂组合物的制备
各组分以如下面表4中所示的含量比例(wt%)混合,并在约20℃的温度搅拌24小时,以制备各实施例和比较例的组合物。
(3)轮胎帘子线的制备
使用聚酯纱线制备2股捻数为360TPM的初捻纱111、112(Z方向),然后,将2股初捻纱111、112以360TPM的捻数一起进行二次加捻,制得合股纱线(1650dtex/2股)。这样制备的合股纱线用作原帘子线110。
将由聚酯构成的原帘子线110浸渍在第一涂布溶液中,然后分别在150℃的干燥温度和240℃的固化温度下处理1分钟以形成第一涂层211,从而向原帘子线110提供反应活性基团。
然后,为了向其上形成有第一涂层211的原帘子线110提供粘合剂组合物,将其上形成有第一涂层211的原帘子线110浸渍在第二涂布溶液中,然后干燥并固化。于此,通过分别在150℃的干燥温度和235℃的固化温度下处理1分钟来进行干燥和固化。第一涂布溶液浸渍工序和第二涂布溶液浸渍工序连续进行,其中张力为0.5g/d。从而,轮胎帘子线201以浸渍帘子线的形式制得。
实施例2至10
(1)水分散的聚氨酯树脂的合成
除了如下面表1或表2中所示改变所使用的组分的摩尔比之外,通过与实施例1相同的方法制备水分散的脂环族聚氨酯。
(2)用于轮胎帘子线的粘合剂组合物的制备
各组分以如下面表4或表5中所示的含量比例(wt%)混合,并在约20℃的温度搅拌24小时,以制备各组合物。
(3)轮胎帘子线的制备
除了改变用于轮胎帘子线的粘合剂组合物之外,通过与实施例1相同的方法制备轮胎帘子线。
比较例1至5
(1)水分散的聚氨酯树脂的合成
除了如下面表3中所示改变所使用的组分的摩尔比之外,通过与实施例1相同的方法制备水分散的脂环族聚氨酯。
于此,比较例1至4中分别使用的水分散的脂环族聚氨酯树脂的重均分子量如表3中所示,并且在比较例5中,使用亚甲基二苯基二异氰酸酯(MDI)芳族二异氰酸酯代替4,4’-二环己基甲烷二异氰酸酯。
(2)用于轮胎帘子线的粘合剂组合物的制备
各组分以如下面表6中所示的含量比例(wt%)混合,并在约20℃的温度搅拌24小时,以制备各组合物。
(3)轮胎帘子线的制备
除了改变用于轮胎帘子线的粘合剂组合物之外,通过与实施例1相同的方法制备轮胎帘子线。
[表1]
(单位:摩尔比) | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
(A)聚酯多元醇 | 1 | 0.5 | 2 | 1 | 1 |
(B)二元醇 | 0.2 | 0.2 | 0.2 | 1 | 2 |
(C)DMBA | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
(D)H<sub>12</sub>MDI | 2 | 2 | 2 | 2 | 2 |
(E)EDA | 1 | 1 | 1 | 1 | 1 |
(F)TEA | 7 | 7 | 7 | 7 | 7 |
Mw(g/mol) | 308,000 | 286,000 | 346,000 | 316,000 | 322,000 |
[表2]
(单位:摩尔比) | 实施例6 | 实施例7 | 实施例8 | 实施例9 | 实施例10 |
(A)聚酯多元醇 | 1 | 1 | 1 | 1 | 1 |
(B)二元醇 | 6 | 8 | 0.2 | 0.2 | 0.2 |
(C)DMBA | 0.8 | 0.8 | 3 | 0.8 | 0.8 |
(D)H<sub>12</sub>MDI | 2 | 2 | 2 | 2 | 2 |
(E)EDA | 1 | 1 | 1 | 4 | 1 |
(F)TEA | 7 | 7 | 7 | 7 | 5 |
Mw(g/mol) | 337000 | 342000 | 299000 | 319000 | 299000 |
[表3]
(单位:摩尔比) | 比较例1 | 比较例2 | 比较例3 | 比较例4 | 比较例5 |
(A)聚酯多元醇 | 0.1 | 2.5 | 1 | 1 | 1 |
(B)二元醇 | 0.2 | 0.2 | 0 | 12 | 0.2 |
(C)DMBA | 0.8 | 0.8 | 0.8 | 0.8 | 0.8 |
(D)H<sub>12</sub>MDI | 2 | 2 | 2 | 2 | - |
(D)MDI | - | - | - | - | 2 |
(E)EDA | 1 | 1 | 1 | 1 | 1 |
(F)TEA | 7 | 7 | 7 | 7 | 7 |
Mw(g/mol) | 231000 | 364000 | 217000 | 379000 | 315000 |
[表4]
(单位:wt%) | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 |
(A)胶乳 | 14.7 | 14.7 | 14.7 | 14.7 | 14.7 |
(B)水分散的聚氨酯 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
(C)胺化合物 | 1.8 | 1.8 | 1.8 | 1.8 | 1.8 |
(D)增链剂 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
(E)环氧化合物 | 1.7 | 1.7 | 1.7 | 1.7 | 1.7 |
(F)异氰酸酯 | 3.4 | 3.4 | 3.4 | 3.4 | 3.4 |
(G)溶剂 | 76.5 | 76.5 | 76.5 | 76.5 | 76.5 |
TSC | 23.5 | 23.5 | 23.5 | 23.5 | 23.5 |
[表5]
(单位:wt%) | 实施例6 | 实施例7 | 实施例8 | 实施例9 | 实施例10 |
(A)胶乳 | 14.7 | 14.7 | 14.7 | 14.7 | 14.7 |
(B)水分散的聚氨酯 | 1.5 | 1.5 | 1.5 | 1.5 | 1.5 |
(C)胺化合物 | 1.8 | 1.8 | 1.8 | 1.8 | 1.8 |
(D)增链剂 | 0.4 | 0.4 | 0.4 | 0.4 | 0.4 |
(E)环氧化合物 | 1.7 | 1.7 | 1.7 | 1.7 | 1.7 |
(F)异氰酸酯 | 3.4 | 3.4 | 3.4 | 3.4 | 3.4 |
(G)溶剂 | 76.5 | 76.5 | 76.5 | 76.5 | 76.5 |
TSC | 23.5 | 23.5 | 23.5 | 23.5 | 23.5 |
[表6]
<表4至表6的说明>
(A)胶乳:来自Closlen的VP胶乳0653
(C)胺化合物:来自Lonza的AcrawaxTM C分散液(D)增链剂:哌嗪
(E)环氧化合物:来自NAGASE的EX614B(山梨醇聚缩水甘油醚,环氧含量:167g/eq,粘度(mPa·s):21,200)
(F)异氰酸酯:来自EMS的IL-6
(G)溶剂:软化水
TSC:总固含量
[试验例]
试验例1:实施例和比较例的组合物的粘度的测量
使用乌氏粘度计在室温(约25℃)测量上述制备的实施例和比较例的每个组合物的粘度。
将组合物放置于恒温水槽(约25℃)中30分钟,然后使用乌氏粘度计测量。具体地,通过以下过程,将一定量的软化水加入乌氏粘度计中并测量软化水的粘度性质,并通过相同的方法测量组合物的粘度性质,然后基于已经测量的软化水的粘度性质计算出相对粘度。
粘度的具体测量方法如下,测量结果示于表7中。
(1)将样品(组合物或软化水)引入乌氏粘度计的A管中。
(2)在将恒温水槽设定在25℃后,将其固定,使C部分浸入水槽中,并放置30分钟。
(3)使用移液管吸注器将样品定位到C部分的中间。
(4)样品向下流动,测量从当样品液面通过B的上刻度线直到样品液面通过B的下刻度线的时间。
(5)将测量到的时间应用于相对粘度计算公式,以计算出相对粘度。
<相对粘度计算公式>:
T1/T0
T1:从当组合物通过B的上刻度线直到组合物通过B的下刻度线的时间T0:从当软化水通过B的上刻度线直到软化水通过B的下刻度线的时间试验例2:粘合强度的评价
对于在实施例和比较例中制备的每个轮胎帘子线,为了评价每单位面积的粘合强度,根据ASTM D4393测量轮胎帘子线的粘合剥离强度。具体地,将厚度为0.6mm的橡胶片、帘子线层和厚度为0.6mm的橡胶片顺序层叠以制备试样,然后,将其在170℃在60kg/cm2的压力下硫化15分钟以制备试样。
然后,将硫化后的试样切割以制备宽度为1英寸的试样。对于所制备的试样,使用万能试验机(Instron)在25℃、125mm/min的速度下测试剥离强度,从而测量轮胎帘子线的粘合强度。于此,将剥离过程中产生的负荷的平均值评定为粘合强度。进行粘合强度的评价,并汇总于下面表7中。
试验例3:耐热疲劳性的评价
对于在实施例和比较例中制备的每个轮胎帘子线,测量实施例和比较例的每个组合物的耐疲劳性。
具体地,将厚度为0.6mm的橡胶片、帘子线层、厚度为0.6mm的橡胶片、帘子线层和厚度为0.6mm的橡胶片顺序层叠以制备试样,然后,将其在170℃在60kg/cm2的压力下硫化15分钟以制备试样。然后,将硫化后的试样切割以制备宽度为1英寸的试样。所制备的试样的疲劳性可以通过对于轮胎帘子线垫试样的未挠曲部分和挠曲部分,橡胶化合物与轮胎帘子线的粘合强度以及对界面的观察来评价。
在疲劳试验机中,附着宽度为1英寸的试样,然后在100℃下预热30分钟。然后,建立在180rpm和60kg的负载下100,000次循环的试验机条件,并且使用1英寸挠曲辊(FlexingRoller)。在疲劳评价结束后,将试样从试验机中取出并在室温下放置12小时,然后使用万能试验机(Instron)在25℃、125mm/min下进行剥离强度测试。
根据下面式1测定耐热疲劳性,其结果示于下面表7中。
[式1]
疲劳性(%)=(对于挠曲部分的粘合强度的测量结果)*100/(对于未挠曲部分的粘合强度的测量结果)
[表7]
粘度(RV) | 粘合强度(%) | 耐热疲劳性(%) | |
实施例1 | 2.71 | 100 | 100 |
实施例2 | 2.64 | 97 | 100 |
实施例3 | 2.82 | 97 | 98 |
实施例4 | 2.73 | 100 | 99 |
实施例5 | 2.76 | 100 | 95 |
实施例6 | 2.79 | 100 | 95 |
实施例7 | 2.81 | 100 | 99 |
实施例8 | 2.74 | 100 | 100 |
实施例9 | 2.54 | 100 | 97 |
实施例10 | 2.60 | 99 | 98 |
比较例1 | 2.41 | 75 | 72 |
比较例2 | 2.88 | 75 | 79 |
比较例3 | 2.44 | 72 | 81 |
比较例4 | 2.89 | 76 | 80 |
比较例5 | 2.92 | 77 | 79 |
如表7中所示,证实了:实施例的用于轮胎帘子线的粘合剂组合物具有2.50至2.85范围内的粘度,并且当施用时,可以提高轮胎帘子线对胎体层的粘合强度,并确保优异的耐热粘合强度和耐热疲劳性。
相反,证实了:当应用比较例的用于轮胎帘子线的粘合剂组合物时,不能确保轮胎帘子线对胎体层的充分的粘合强度,并且耐热粘合强度和耐热疲劳性相对低。
Claims (16)
1.一种用于轮胎帘子线的粘合剂组合物,包含:环氧化合物;胶乳;重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂;胺化合物;和水。
2.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂包含多异氰酸酯与多元醇之间的反应产物,该多异氰酸酯包含一个或更多个碳数为4至30的脂环基。
3.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述脂环族聚氨酯树脂是由脂环族聚氨酯离聚物形成的水分散的脂环族聚氨酯树脂。
4.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述脂环族聚氨酯树脂包含1mol%至20mol%的来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分。
5.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,在室温下使用乌氏粘度计测量的粘度在2.50至2.85的范围内。
6.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述粘合剂组合物包含0.5wt%至10wt%的重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂。
7.根据权利要求6所述的用于轮胎帘子线的粘合剂组合物,其中,所述粘合剂组合物包含:
0.1wt%至10wt%的环氧化合物;
1wt%至30wt%的胶乳;
0.5wt%至10wt%的重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂;
0.1wt%至10wt%的胺化合物;和
50wt%至95wt%的水。
8.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述胺化合物包括具有链结构的胺化合物。
9.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述用于轮胎帘子线的粘合剂组合物还包含一种或更多种选自异氰酸酯类化合物、氮丙啶类化合物和金属螯合化合物的交联剂。
10.根据权利要求1所述的用于轮胎帘子线的粘合剂组合物,其中,所述用于轮胎帘子线的粘合剂组合物包含50wt%以上的水。
11.一种轮胎帘子线,包括:
纤维基底;和
在所述纤维基底上形成的粘合层,且该粘合层由权利要求1所述的粘合剂组合物形成。
12.一种轮胎帘子线,包括:
纤维基底;和
在所述纤维基底上形成的粘合层,且该粘合层包含环氧化合物、胶乳、重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂和胺化合物。
13.根据权利要求12所述的轮胎帘子线,其中,所述重均分子量(Mw)为250,000至350,000的脂环族聚氨酯树脂包含多异氰酸酯与多元醇之间的反应产物,该多异氰酸酯包含一个或更多个碳数为4至30的脂环基。
14.根据权利要求12所述的轮胎帘子线,其中,所述脂环族聚氨酯树脂包含1mol%至20mol%的来自一个或更多个选自二羟甲基丁酸和二羟甲基丙酸的化合物的部分。
15.根据权利要求12所述的轮胎帘子线,其中,所述纤维基底是包括聚酯纤维的原帘子线。
16.一种轮胎,包括权利要求12所述的轮胎帘子线。
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