CN105764999A - 经处理的填料、包含该填料的组合物和由该填料制备的制品 - Google Patents
经处理的填料、包含该填料的组合物和由该填料制备的制品 Download PDFInfo
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- CN105764999A CN105764999A CN201480064858.2A CN201480064858A CN105764999A CN 105764999 A CN105764999 A CN 105764999A CN 201480064858 A CN201480064858 A CN 201480064858A CN 105764999 A CN105764999 A CN 105764999A
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- treated
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- agent
- precipitated silica
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Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/28—Compounds of silicon
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Abstract
本发明包括一种用于生产经处理的填料的方法,其包括(a)用包括处理剂的处理组合物处理包括未经处理的填料(其中该未经处理的填料未被事先干燥)的浆料,从而形成经处理的填料浆料;和(b)使该经处理的填料浆料干燥以生产经处理的填料。处理剂可包括氨基酸或多肽中的至少一种。本发明还涉及通过该方法制备的经处理的填料,以及包括该经处理的填料的橡胶配混组合物和轮胎。
Description
相关申请的交叉参考
本申请要求2013年10月7日提交的美国临时申请号61/887,713的权益,其在此以其全文通过引用并入本文。
关于联邦政府资助的研究和发展的陈述
本发明是基于美国能源部授予的第DE-EE0005359号合约受政府支持作出的。政府在本发明中具有某些权利。
发明领域
本发明涉及一种用于制备经处理的填料的方法,通过该方法生产的经处理的填料,和包含这类经处理的填料的组合物和制品。
发明背景
使用二氧化硅/硅烷填料系统降低滚动阻力和改良客车和卡车轮胎抗湿滑性是本领域已知的。降低滚动阻力造成较少的燃料消耗。
滚动阻力、磨耗和牵引力的同时改良,称为扩大“魔术三角”,需要新的方法开发橡胶复合物。沉淀二氧化硅在生胎(greentire)的出现中扮演重要角色,其与过去的技术相比具有在滚动阻力方面的大的改良。二氧化硅(经由偶联)直接交联成经高度交联的聚合物基质,同时使二氧化硅颗粒间的相互作用最小化,据信对于用于生产客车和卡车轮胎的橡胶的所需动力机械性质极其重要。已注意到在天然橡胶(典型地用于生产卡车轮胎)中,自天然橡胶生物合成而存在的蛋白质优先吸附至二氧化硅表面,干扰原位的偶联反应。可能改良偶联效率的增加的排胶温度(dumptemperature),也已被表明会使天然橡胶降解。因此,在橡胶产业中持续需要经改良的二氧化硅-橡胶偶联材料。
此外,已发现使高表面积填料材料并入橡胶组合物内会造成粘度不令人期望的增加,因此,由于加工问题,限制可被包括在橡胶组合物内的高表面积材料的量。因此,存在用材料处理这类高表面材料(例如,沉淀二氧化硅)的需求,该材料可作为使高表面材料与将其并入于内的聚合物基质更相容,改良加工粘度,和避免高表面材料与聚合物基质相分离。
发明概述
根据本发明,提供了一种用于生产经处理的填料的方法,其包括:(a)用包括处理剂的处理组合物处理包括未经处理的填料(其中该未经处理的填料未被事先干燥)的浆料,由此形成经处理的填料浆料;和(b)使该经处理的填料浆料干燥以生产经处理的填料。处理剂可包括氨基酸和/或多肽中的至少一种。
根据本发明,进一步提供了一种用于生产经处理的沉淀二氧化硅的方法,其包括:(a)使碱金属硅酸盐与酸合并以形成包括未经处理的二氧化硅的浆料,其中,未经处理的二氧化硅未被事先干燥;(b)用包括处理剂的处理组合物处理所述浆料,由此形成经处理的浆料;和(c)使所述经处理的浆料干燥以生产经处理的沉淀二氧化硅。处理剂可包括氨基酸和/或多肽中的至少一种。
根据本发明,进一步提供了一种用于生产经处理的沉淀二氧化硅的方法,其包括:(a)使碱金属硅酸盐与酸合并以形成包括未经处理的二氧化硅的未经处理的浆料,其中未经处理的二氧化硅未被事先干燥;(b)使未经处理的浆料干燥以生产经干燥的沉淀二氧化硅;(c)用包括处理剂和任选的偶联剂和/或任选的非偶联剂的处理组合物形成经干燥的沉淀二氧化硅的水性浆料,以形成经处理的沉淀二氧化硅浆料;和(d)使经处理的沉淀二氧化硅浆料干燥以生产经干燥的经处理的沉淀二氧化硅。处理剂可包括氨基酸和/或多肽中的至少一种。
根据本发明,还提供了通过此处所述方法制备的经处理的填料,以及包括该经处理的填料的橡胶组合物,诸如,橡胶配混组合物,和包括本发明的经处理的填料的橡胶制品。
具体实施方式
如先前所提及,本发明提供了一种用于生产经处理的填料的方法。该方法可包括:(a)用包含处理剂的处理组合物处理可包括未经处理的填料(其中该未经处理的填料未被事先干燥)的浆料,由此形成经处理的填料浆料;和(b)使该经处理的填料浆料干燥以生产经处理的填料。
如此处所使用的,关于填料(诸如,经处理和/或未经处理的填料),术语“未被事先干燥”意指在处理方法前填料未被干燥至小于20重量%的水分含量。出于本发明的目的,未经处理的填料不包括被事先干燥至小于20重量%的水分且然后再次水合的填料。
如此处所使用的,术语“填料”意指可用于聚合物组合物中以改良该聚合物至少一种性质的无机材料,诸如,无机氧化物。如此处所使用的,术语“浆料”意指包括至少填料和水的混合物。
如此处所使用的,除非以其它方式明确和不含糊地限于一个指示物,冠词“一个”、“一”和“该”包括多个指示物。
除非另有指示,此处公开的所有范围或比率应理解为涵盖其中包含的任何和所有子范围或子比率。例如,“1至10”的陈述范围或比率应被认为包括最小值1与最大值10间(且包括端值)的任何和所有子范围,即,以最小值1或更大开始且以最大值10或更小结束的所有子范围或子比率,诸如但不限于1至6.1,3.5至7.8,和5.5至10。
除了在操作实施例中或其中另有指示外,说明书和权利要求书中使用的表示成分、反应条件等的量的所有数值应理解为在所有情况下以术语“约”修饰。
如此处所使用的,聚合物的分子量值,诸如,重均分子量(Mw)和数均分子量(Mn),是通过凝胶渗透色谱法使用合适的标准物,诸如聚苯乙烯标准物测定。
如此处所使用的,多分散性指数(PDI)值表示该聚合物的重均分子量(Mw)与数均分子量(Mn)的比率(即,Mw/Mn)。
如此处所使用的,术语“聚合物”意指均聚物(例如,由单种单体物质制备)、共聚物(例如,由至少二种单体物质制备),和接枝聚合物。
如此处所使用的,术语“(甲基)丙烯酸酯”和相似术语,诸如,“(甲基)丙烯酸酯”,意指甲基丙烯酸酯和/或丙烯酸酯。如此处所使用的,术语“(甲基)丙烯酸”意指甲基丙烯酸和/或丙烯酸。
除非另有指示,此处提及的诸如但不限于授权专利和专利申请的所有文件被认为是以它们的全文“通过引用并入”。
如此处所使用的,“线性或支化”基团的描述,诸如,线性或支化的烷基,在此应理解为包括:亚甲基基团或甲基基团;线性的基团,诸如,线性C2-C36烷基基团;和适当支化的基团,诸如,支化的C3-C36烷基基团。
如此处所使用的,“任选地经取代”的基团的描述意指其中其至少一个氢已任选地被不同于氢的基团替代或取代的基团,该基团包括但不限于烷基基团、环烷基基团、杂环烷基基团、芳基基团,和/或杂芳基基团,该不同于氢的基团是诸如但不限于卤基团(例如,F、Cl、I,和Br)、羟基基团、醚基团、硫醇基团、硫醚基团、羧酸基团、羧酸酯基团、磷酸基团、磷酸酯基团、磺酸基团、磺酸酯基团、硝基基团、氰基基团、烃基基团(包括但不限于:烷基;烯基;炔基;环烷基,包括多稠合环的环烷基和多环烷基;杂环烷基;芳基,包括经羟基取代的芳基,诸如,酚,且包括多稠合环的芳基;杂芳基,包括多稠合环的杂芳基;和芳烷基基团),和胺基团,诸如,N(R11′)(R12′),其中,在一些实施方式中,R11′和R12′各自独立地选自氢、线性或支化的C1-C20烷基、C3-C12环烷基、C3-C12杂环烷基、芳基,和杂芳基。
可用于本发明方法的一些化合物包括在每一情况下可独立地选自烃基和/或经取代的烃基和/或官能烃基(或具有一个或多个官能团的烃基基团)的组和子组。如此处所使用的,且根据一些实施方式,术语“烃基”和相似术语,诸如,“烃基取代基”,意指:线性或支化的C1-C36烷基(例如,线性或支化的C1-C10烷基);线性或支化的C2-C36烯基(例如,线性或支化C2-C10烯基);线性或支化的C2-C36炔基(例如,线性或支化C2-C10炔基);C3-C12环烷基(例如,C3-C10环烷基);C5-C18芳基(包括多环状芳基基团)(例如,C5-C10芳基);和C6-C24芳烷基(例如,C6-C10芳烷基)。
代表性的烷基基团包括但不限于甲基、乙基、丙基、异丙基、丁基、异丁基、仲丁基、叔丁基、戊基、新戊基、己基、庚基、辛基、壬基,和癸基。代表性的烯基基团包括但不限于乙烯基、烯丙基,和丙烯基。代表性的炔基基团包括但不限于乙炔基、1-丙炔基、2-丙炔基、1-丁炔基,和2-丁炔基。代表性的环烷基基团包括但不限于环丙基、环丁基、环戊基、环己基,和环辛基取代基。代表性的芳烷基基团包括但不限于苯甲基和苯乙基。
如此处所使用的术语“经取代的烃基”和相似术语,诸如,“官能烃基”(或具有至少一个官能团的烃基)意指其中其至少一个氢已被不同于氢的基团取代的烃基基团,该不同于氢的基团是诸如但不限于卤基团、羟基基团、醚基团、硫醇基团、硫醚基团、羧酸基团、羧酸酯基团、磷酸基团、磷酸酯基团、磺酸基团、磺酸酯基团、硝基基团、氰基基团、烃基基团(例如,烷基、烯基、炔基、环烷基、芳基,和芳烷基基团)、杂环烷基基团、杂芳基基团,和胺基团,诸如,-N(R11′)(R12′),其中,R11′和R12′各自独立地选自氢、烃基,和经取代的烃基。
根据一些实施方式,如此处所使用的术语“烷基”意指线性或支化的烷基,诸如但不限于线性或支化的C1-C25烷基,或线性或支化的C1-C10烷基,或线性或支化的C2-C10烷基。可选作本发明的各种烷基基团的烷基基团的例子包括但不限于本文先前描述的那些。在一些实施方式中,本发明的各种化合物的烃基(alkyl)基团可包括一个或多个选自-CH=CH-基团和/或一个或多个-C≡C-基团的不饱和连接基,条件是烃基基团不含两个或更多个共轭不饱和连接基。在一些实施方式中,烃基基团不含诸如CH=CH基团和-C≡C-基团的不饱和连接基。
根据一些实施方式,如此处所使用的术语“环烷基”意指是适当的环状的基团,诸如但不限于C3-C12环烷基(包括但不限于环状C5-C7烷基)基团。环烷基基团的例子包括但不限于本文先前描述的那些。根据一些实施方式,如此处所使用的术语“环烷基”还包括:桥接环多环烷基基团(或桥接环多环状烷基基团),诸如但不限于双环[2.2.1]庚基(或降冰片基(norbornyl))和双环[2.2.2]辛基;和稠合环多环烷基基团(或稠合环多环状烷基基团),诸如但不限于八氢-1H-茚基,和十氢萘基。
根据一些实施方式,如此处所使用的术语“杂环烷基”意指为适当环状的基团(在环状环中具有至少一个杂原子),诸如但不限于C3-C12杂环烷基基团或C5-C7杂环烷基基团,且其在环状环中具有至少一个杂原子,诸如但不限于O、S、N、P,和它们的组合。杂环烷基基团的例子包括但不限于咪唑基、四氢呋喃基、四氢吡喃基,和哌啶基。根据一些实施方式,如此处所使用的术语“杂环烷基”还包括:桥接环多环状杂环烷基基团,诸如但不限于7-氧杂双环[2.2.1]庚基;和稠合环多环状杂环烷基基团,诸如但不限于八氢环戊并[b]吡喃基,和八氢1H异色烯基。
如此处所使用的且根据一些实施方式,术语“芳基”包括C5-C18芳基,诸如,C5-C10芳基(且包括多环状芳基基团,包括多环状稠合环芳基基团)。代表性的芳基基团包括但不限于苯基、萘基、蒽基,和三蝶烯基(triptycenyl)。
根据一些实施方式,如此处所使用的术语“杂芳基”意指在环中具有至少一个杂原子的芳基基团,且包括但不限于C5-C18杂芳基,诸如但不限于C5-C10杂芳基(包括稠合环多环状杂芳基基团),且意指在芳香族环中或在稠合环多环状杂芳基基团的情况中的至少一个芳香族环中具有至少一个杂原子的芳基基团。杂芳基基团的例子包括但不限于呋喃基、吡喃基、吡啶基、异喹啉,和嘧啶基。
如此处所使用的,术语“稠合环多环状芳基烷基基团”和相似术语,诸如,稠合环多环状烷基芳基基团、稠合环多环芳基烷基基团,和稠合环多环烷基芳基基团意指包括稠合在一起以形成稠合环结构的至少一个芳基环和至少一个环烷基环的稠合环多环状基团。出于非限制性说明的目的,稠合环多环芳基烷基基团的例子包括但不限于茚基、9H-芴基、环五萘基,和二环戊二烯并苯基(indacenyl)。
如此处所使用的且根据一些实施方式,术语“芳烷基”包括但不限于C6-C24芳烷基,诸如但不限于C6-C10芳烷基,且意指被烷基基团取代的芳基基团。芳烷基基团的例子包括但不限于本文先前描述的那些。
用于本发明方法的适合的未经处理的填料可包括本领域技术人员所知的广泛的各种材料。非限制性的例子可包括在露出表面拥有氧(化学吸附或共价键合)或羟基(结合或游离)的诸如无机颗粒和非晶固体材料的无机氧化物,诸如但不限于F.AlbertCotton等人的AdvancedInorganicChemistry:AComprehensiveText,第四版,JohnWileyandSons,1980的元素周期表的第Ib、IIb、IIIa、IIIb、IVa、IVb(除了碳)、Va、VIa、VIIa和VIII族的第2、3、4、5和6周期的金属的氧化物。适合的无机氧化物的非限制性例子可包括但不限于硅酸铝、二氧化硅,诸如,二氧化硅凝胶、胶体二氧化硅、沉淀二氧化硅,和它们的混合物。
在一些实施方式中,无机氧化物可为二氧化硅。例如,在某些实施方式中,无机氧化物可包括沉淀二氧化硅、胶体二氧化硅,和它们的混合物。如电子显微镜所测量的,二氧化硅可具有少于0.1微米,或大于0.001微米,或从0.01至0.05微米,或从0.015至0.02微米的平均最终颗粒尺寸(ultimateparticlesize)。此外,如通过Brunauer,Emmett,andTeller(BET)方法根据ASTMD1993-91测定的,二氧化硅可具有从25至1000平方米/克,诸如,从75至250平方米/克,或从100至200平方米/克的表面积。在一些实施方式中,填料是沉淀二氧化硅。
如先前提及,未经处理的填料浆料是用包括处理剂的处理组合物处理的。在某些实施方式中,处理剂可充当偶联剂。如此处所使用的术语“偶联剂”意指与(i)存在于填料颗粒表面上(诸如,在二氧化硅表面上)的基团,以及与(ii)存在于聚合物基质(填料并入其中)的组分上的官能团(离子地或共价地)结合的材料。因此,填料颗粒可与聚合物基质内的组分“偶联”。
备选地,在一些实施方式中,处理剂可充当非偶联剂。如此处所使用的术语“非偶联剂”意指用以使经处理的填料与其中最终使用该经处理的填料的聚合物组合物相容的材料。即,非偶联剂可影响经处理的填料颗粒的自由表面能,使经处理的填料颗粒具有与聚合物组合物相似的表面能。这促进经处理的填料并入聚合物组合物内,且可用以改良(诸如,减少)组合物的混合粘度。应注意非偶联剂不被预期超过(beyond)范德华相互作用而与橡胶基质偶联。如此处所使用的,术语“非偶联剂”可与“增容剂”互换地使用。
应注意许多处理剂可同时起到偶联剂以及非偶联剂/增容剂的作用。
用于本发明方法的处理剂包括(i)氨基酸和(ii)多肽,和它们的衍生物中的至少一种。如此处所用的术语“氨基酸”意指具有伯胺(-NH2)和羧酸(-COOH)基团两者的有机化合物。在一些实施方式中,处理剂的氨基酸可以下式(A)表示:
关于式(A),和在一些实施方式中,R选自经取代和未经取代的烃基基团。在一些实施方式中,可选作式(A)的R的经取代的烃基基团的取代基包括但不限于此处所述的那些取代基。
在本发明若干实施方式中使用的氨基酸可选自手性分子(其中其至少一个碳是非对称碳),和/或非手性分子。非手性氨基酸的非限制性例子是甘氨酸。虽然大部分的氨基酸是l-氨基酸(包括蛋白(proteinogenic)氨基酸),如此处所用的术语氨基酸包括氨基酸的1-和d-镜像异构体。
可用于本发明各种实施方式的氨基酸包括蛋白和/或非蛋白的氨基酸。蛋白氨基酸是在转译期间并入蛋白质的氨基酸。蛋白氨基酸包括二十种传统氨基酸(丙氨酸、精氨酸、天冬酰胺、天冬氨酸、半胱氨酸(和它们的氧化产物,包括例如但不限于胱氨酸)、谷氨酸、谷氨酰胺、甘氨酸、组氨酸、异亮氨酸、亮氨酸、赖氨酸、甲硫氨酸、苯丙氨酸、脯氨酸、丝氨酸、苏氨酸、色氨酸、酪氨酸,和缬氨酸)与甲酰基甲硫氨酸、硒代半胱氨酸,和吡咯赖氨酸。
非蛋白氨基酸在转译期间未被并入蛋白质中,虽然其可在转译后并入。非蛋白氨基酸包括天然氨基酸(即,由活生物体制造的那些)和非天然氨基酸(即,合成氨基酸)。如此处所用的,术语“合成氨基酸”意指由于人类干预而设计或产生且在不存在人类干预的情况下无法通过活生物体天然产生的那些氨基酸。非蛋白氨基酸包括但不限于β-氨基酸(例如且不受限地诸如,β-丙氨酸)、d-氨基酸、高氨基酸、丙酮酸衍生物、3-取代的丙氨酸衍生物、甘氨酸衍生物、经环取代的苯丙氨酸和酪氨酸衍生物、二氨基酸,和N-甲基氨基酸。蛋白和非蛋白的氨基酸两者可用于本发明的各种实施方式。
除氨基酸外或作为其替代,可用于本发明方法的处理剂可包括多肽。如此处所用的,术语“多肽”意指其中每对氨基酸残基通过二价肽(-C(=O)NH-)基团结合的一连串两个或更多个氨基酸残基。如此处所用的,术语“氨基酸残基”意指氨基酸单体,或单一氨基酸,它们是多肽的一部分。如此处所用的,术语二价肽基团包括顺式和反式的异构体。包括固体相合成和溶液相合成的多肽合成方法是本领域技术人员熟知的,且描述于,例如,JohnMcMurry的OrganicChemistry(第4版),Brooks/ColePublishingCo.(1996),第27章和L.G.WadeJr.的OrganicChemistry(第5版),PearsonEducaton,Inc.(2003),第24章。
在一些实施方式中,无论是蛋白或非蛋白的,氨基酸包括任选地包括一个或多个取代基(或官能团)(诸如,如上式(A)的R)的侧链。可被包括在氨基酸侧链上的非排他性的一列取代基包括一般类别的烷基、烯基、炔基、苯基、苯甲基、卤基(包括氟、氯、溴,和碘基团)、羟基、羰基、醛、卤甲酰基、碳酸酯、羧酸酯、羧基、酯、甲氧基、氢过氧基、过氧基、醚、半缩醛、半缩酮、缩醛、缩酮、原酸酯、亚甲基二氧基、原碳酸酯、甲酰胺、伯胺、仲胺、叔胺、季铵、亚胺(伯酮亚胺、仲酮亚胺、伯醛亚胺、仲醛亚胺)、酰亚胺、叠氮化物、偶氮、氰酸酯、异氰酸酯、硝酸盐、腈、异腈、亚硝基氧基(nitrosooxy)、硝基、亚硝基、吡啶基、巯基(硫醇)、硫化物、二硫化物、亚磺酰基、磺酰基亚磺基、磺基、硫氰酸酯、异硫氰酸酯、硫羰基(carbonothioyl)、膦基、膦酰基、磷酸酯(盐),和它们的衍生物。如此处所用的,“衍生物”意指盐、开环产物,和经取代的产物。本领域技术人员会领会所有氨基酸按照定义包括至少两个官能团,伯胺和伯羧基基团,并因此侧链无需包括官能团。
在一些实施方式中,处理剂包括具有极性侧链的氨基酸。可在氨基酸的极性侧链上或限定该极性侧链的极性基团的例子包括但不限于羟基、硫醇、羧基、酚、胺、甲酰胺、咪唑,和吲哚基团。具有极性侧链的氨基酸的例子包括但不限于精氨酸、天冬酰胺、天冬氨酸、半胱氨酸、谷氨酸、谷氨酰胺、组氨酸、赖氨酸、丝氨酸、苏氨酸、色氨酸,和酪氨酸。本领域技术人员会了解侧链无需为了呈极性而带电荷,且足够的是侧链被水吸引/对水具吸引性。
在一些实施方式中,可用于本发明的氨基酸的极性侧链是具有例如但不限于羟基、酚、硫醇、咪唑、胍盐、胺,和铵基团的可离子化或经离子化的侧链。具有可离子化或经离子化的侧链的氨基酸的例子包括但不限于半胱氨酸、酪氨酸、天冬氨酸、谷氨酸、赖氨酸、精氨酸,和组氨酸。然而,本领域技术人员会领会前述仅是例示性的,且具有用于与存在于填料颗粒和/或聚合物基质的表面上的基团结合、反应,或相互作用的官能侧链(例如但不限于,极性和/或可离子化/经离子化的侧链)的蛋白或非蛋白的氨基酸可用于本发明的工艺和方法。可用于本发明的氨基酸可如本领域已知的那样来合成(例如,JohnMcMurry的OrganicChemistry(第4版),Brooks/ColePublishingCo.(1996),第27章),或可从任何适合的商业来源获得,例如,从Sigma-AldrichCorp.(St.Louis,MO,USA)和ThermoFisherScientific,Inc.(Waltham,MA,USA)获得。
在一些实施方式中,本发明的处理剂的氨基酸是游离半胱氨酸、胱氨酸、精氨酸、组氨酸、酪氨酸、甲硫氨酸和脯氨酸中的至少一种,且多肽包括半胱氨酸、胱氨酸、精氨酸、组氨酸、酪氨酸、甲硫氨酸,和脯氨酸的残基。在一些另外实施方式中,氨基酸是游离氨基酸,且是半胱氨酸和/或l-精氨酸中的至少一种,且多肽包括半胱氨酸和/或l-精氨酸的残基。
在一些实施方式中,除如上列示的处理剂外,处理组合物可另外包括与该处理剂不同的第一或另外的偶联剂。在某些实施方式中,偶联剂可包括任何的多种有机硅烷。可用于本发明一些实施方式的适合的有机硅烷的例子包括由式(I)表示的那些:
(R1)a(R2)bSiX4-a-b(I)。
关于式(I),R1对于每个“a”独立地是具有1至36个碳原子和官能团的烃基基团。烃基基团的官能团是乙烯基、烯丙基、己烯基、环氧基(环氧乙烷)、缩水甘油氧基、(甲基)丙烯酰氧基、硫化物、异氰酸基(-NCO)、多硫化物、巯基,或卤素。关于式(I),R2对于每个“b”独立地是具有从1至36个碳原子的烃基基团或氢。式(I)的X独立地是卤素或具有1至36个碳原子的烷氧基;下标“a”是0、1、2,或3;下标“b”是0、1,或2;(a+b)是1、2,或3。在一些实施方式中,条件是当b是1时,(a+b)是2或3。在本发明的一些另外的实施方式中,处理组合物进一步包括由式(I)表示的偶联剂,其中,X是烷氧基;a是1;b是0;且R1的烃基的官能团是卤素。
卤基官能有机硅烷(诸如由式(I)表示的那些)的例子包括但不限于(4-氯甲基-苯基)三甲氧基硅烷、(4-氯甲基-苯基)三乙氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三甲氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三乙氧基硅烷、(3-氯-丙烯基)-三甲氧基硅烷、(3-氯-丙烯基)-三乙氧基硅烷、(3-氯-丙基)-三乙氧基硅烷、(3-氯-丙基)-三甲氧基硅烷、三甲氧基-(2-对甲苯基-乙基)硅烷,和/或三乙氧基-(2-对甲苯基-乙基)硅烷。
在某些实施方式中,基于已沉淀的SiO2的总质量计,另外的偶联剂可以范围从0.25至30.0重量%,诸如,1至15重量%,或5至10重量%的量存在于浆料中。
在某些实施方式中,可用于本发明方法的处理组合物还可进一步包括与诸如由式(I)表示的前述任选的有机硅烷偶联剂不同的含硫有机硅烷。此类材料的非限制性例子可包括但不限于由下式(II)表示的有机硅烷:
(R3)c(R4)dSiY4-c-d(II)。
关于式(II),R3对于每个“c”独立地可为具有1至12个碳原子和官能团的烃基基团。官能团可为硫化物、多硫化物,或巯基。关于式(II),R4对于每个“d”独立地可为具有从1至18个碳原子的烃基基团或氢。每个Y可独立地是卤素或具有1至12个碳原子的烷氧基基团。下标“c”可为0、1、2,或3;下标“b”可为0、1,或2;且c+d可为1、2,或3。在一些实施方式中,条件是当b是1时,a+b是2或3。式(II)的R3和R4基团可被选择,使得它们可与其中并入有经处理的填料的聚合物组合物反应。
另外,含硫的有机硅烷可包括下式(III)表示的双(烷氧基甲硅烷基烷基)多硫化物:
Z′-alk-Sn′-alk-Z′(III)。
关于式(III),“alk”表示具有从1至18个碳原子的二价烃基团;n'是从2至12的整数;且Z′是:
其中,R5独立地是具有从1至4个碳原子的烷基基团或苯基,且每个R6独立地是具有从1至8个碳原子的烷氧基基团,具有从5至8个碳原子的环烷氧基基团,或具有从1至8个碳原子的直链或支链烷基巯基基团。R5和R6基团可以相同或不同。此外,二价alk基团可为直链或支链、饱和或不饱和的脂族烃基团,或环状烃基团。双(烷氧基甲硅烷基烷基)-多硫化物的非限制性例子可包括双(2-三烷氧基甲硅烷基乙基)-多硫化物,其中三烷氧基基团可为三甲氧基、三乙氧基、三(甲基乙氧基)、三丙氧基、三丁氧基等,直到三辛氧基,且多硫化物可为二、三、四、五,或六硫化物,或它们的混合物。另外的非限制性例子可包括相对应的双(3-三烷氧基甲硅烷基丙基)-、双(3-三烷氧基甲硅烷基异丁基)、-双(4-三烷氧基甲硅烷基丁基)-等,直到双(6-三烷氧基甲硅烷基-己基)-多硫化物。双(烷氧基甲硅烷基烷基)-多硫化物的另外非限制性例子描述于美国专利号3,873,489,第6栏,第5-55行,和美国专利号5,580,919,第11栏,第11-41行。这类化合物的另外非限制性例子可包括:3,3'双(三甲氧基甲硅烷基丙基)二硫化物、3,3'-双(三乙氧基甲硅烷基丙基)四硫化物、3,3'-双(三甲氧基甲硅烷基丙基)四硫化物、2,2'-双(三乙氧基甲硅烷基乙基)四硫化物、3,3'-双(三甲氧基甲硅烷基丙基)三硫化物、3,3'-双(三乙氧基甲硅烷基丙基)三硫化物、3,3'-双(三丁氧基甲硅烷基丙基)二硫化物、3,3'-双(三甲氧基甲硅烷基丙基)六硫化物,和3,3'-双(三辛氧基甲硅烷基丙基)四硫化物,和它们的混合物。
含硫有机硅烷也可为下式(IV)表示的巯基有机金属化合物:
关于式(IV),M′是硅,L是卤素或-OR8,Q是氢、C1-C12烷基或经卤基取代的C1-C12烷基,R7是C1-C12亚烷基,R8是C1-C12烷基或含有从2至12个碳原子的烷氧基烷基,卤素或(卤)基团是氯、溴、碘,或氟,且n是1、2或3。在非限制性实施方式中,可以使用具有两个巯基基团的巯基有机金属反应物。
有用的巯基有机金属化合物的非限制性例子包括但不限于巯基甲基三甲氧基硅烷、巯基乙基三甲氧基硅烷、巯基丙基三甲氧基硅烷、巯基甲基三乙氧基硅烷、巯基乙基三丙氧基硅烷、巯基丙基三乙氧基硅烷、(巯基甲基)二甲基乙氧基硅烷、(巯基甲基)甲基二乙氧基硅烷、3-巯基丙基-甲基二甲氧基硅烷,和它们的混合物。
在本发明的一些实施方式中,含硫有机硅烷可为巯基有机金属化合物,诸如,不同于用于步骤(a)的处理组合物中的有机硅烷的巯基硅烷,例如,巯基丙基三甲氧基硅烷和/或巯基甲基三乙氧基硅烷。
此外,预期可用于本发明方法的步骤(a)中的不同于由式(I)表示的前述有机硅烷偶联剂的由式(IV)表示的含硫有机硅烷可为其中巯基基团被封端(即,巯基的氢原子被另外的基团替代)的巯基有机金属化合物。经封端的巯基有机金属化合物可具有经由单键与硫直接键合的不饱和杂原子或碳。具体的封端基团的非限制性例子可包括硫代羧酸酯、二硫代氨基甲酸酯、硫代磺酸酯、硫代硫酸酯、硫代磷酸酯、硫代膦酸酯,和硫代亚膦酸酯。
在其中经封端的巯基有机金属化合物作为任选的偶联材料的一些非限制性实施方式中,可将解封端剂(deblockingagent)添加至聚合物化合物混合物以使经封端的巯基有机金属化合物解封端。在其中水和/或醇存在于混合物中的一些非限制性实施方式中,诸如叔胺、路易斯酸或硫醇的催化剂可被用以通过水解或醇解引起和促进封端基团丧失,以释放(liberate)相对应的巯基有机金属化合物。经封端的巯基硅烷的非限制性例子可包括但不限于2-三乙氧基甲硅烷基-1-乙基硫代乙酸酯、3-三甲氧基-甲硅烷基-1-丙基硫代辛酸酯、双-(3-三乙氧基甲硅烷基-1-丙基)-甲基二硫代膦酸酯、3-三乙氧基甲硅烷基-1-丙基二甲基硫代亚膦酸酯、3-三乙氧基甲硅烷基-1-丙基甲基硫代硫酸酯、3-三乙氧基甲硅烷基-1-丙基甲苯硫代磺酸酯,和它们的混合物。
这些任选的含硫有机硅烷的量可广泛改变,且可取决于所选择的特定材料。例如,基于未经处理的填料的重量计,这些任选的含硫有机硅烷的量可为大于0.1%,诸如,基于未经处理的填料的重量计,是从0.5%至25%,或从1%至20%,或从2%至15%。
在某些实施方式中,处理组合物可进一步包括卤基官能有机硅烷,其包括得自以下的拥有卤素官能度和烷二氧基甲硅烷基官能度的单体、二聚、低聚和/或聚合型化合物:(i)含多羟基的化合物,其中,烷二氧基团是经由Si-O键与单一Si原子共价键合以形成环;和/或(ii)烷二氧基团是经由Si-O键与至少两个Si原子共价键合,以形成二聚物、低聚物,或聚合物,其中,相邻的甲硅烷基单元经由桥接烷烷氧基结构彼此键合。这类卤基官能有机硅烷详细描述于2011年1月6日公开的美国公开专利申请号2011/0003922A1,第[0020]至[0057]段,其引述部分在此通过引用并入。
任何前述偶联剂的混合物可用于本发明的方法。
在一些实施方式中,除此处先前所述的处理剂外,处理组合物可任选地进一步包括不同于该处理剂的第一或另外的非偶联剂/增容剂。该另外的非偶联剂/增容剂可选自饱和生物聚合物、饱和脂肪酸、饱和有机酸、饱和聚合物乳液、饱和聚合物涂料组合物,和它们的混合物。该另外的非偶联剂/增容剂可备选地或进一步包括表面活性剂,其选自阴离子型、非离子型,和两性的表面活性剂,和它们的混合物。如此处所用的,术语表面活性剂排除氨基酸表面活性剂。
在一些实施方式中,基于未经处理的填料的总重量(诸如,已被沉淀的SiO2的总质量)计,该另外的非偶联剂//增容剂可以大于1重量%至25重量%的量存在。例如,该另外的非偶联剂/增容剂可选自脂肪酸盐、烷基肌氨酸酯、烷基肌氨酸盐,和它们的混合物。这类物质的具体的非限制性例子可于U.S.7,569,107,第5栏第9行至第7栏第21行发现,其引述部分在此通过引用并入。在本发明的一些实施方式中,该另外的非偶联剂/增容剂可包括选自硬脂酸钠、硬脂酸铵、椰油酸铵、月桂酸钠、椰油酰基肌氨酸钠(sodiumcocylsarcosinate)、月桂酰基肌氨酸钠、牛脂的钠皂、椰子油的钠皂、肉豆蔻酰基肌氨酸钠,和/或硬脂酰基肌氨酸的一种或多种阴离子型表面活性剂。
在一些实施方式中,基于未经处理的填料总重量(诸如,已被沉淀的SiO2总质量)计,该另外的非偶联剂/增容剂是以大于1重量%至最高且包括25重量%的量存在,例如,2.0重量%至20.0重量%,或4重量%至15重量%,或5重量%至12重量%。
在一些实施方式中,该另外的非偶联剂/增容剂可为非偶联有机硅烷。在一些实施方式中,可选作该另外的非偶联剂/增容剂的非偶联硅烷的非限制性例子包括十八烷基三乙氧基硅烷、十八烷基三氯硅烷、十八烷基三甲氧基硅烷、丙基三乙氧基硅烷、丙基三甲氧基硅烷、丙基三氯硅烷、正辛基三甲氧基硅烷、正辛基三乙氧基硅烷、正辛基三氯硅烷、正己基三甲氧基硅烷、正己基三乙氧基硅烷,和/或正己基三氯硅烷。
应理解出于本发明的目的,在一些实施方式中,任何包括如上所述的具有结构(I)的有机硅烷的前述有机硅烷可包括其部分水解物。
用于本发明各种不同实施方式的未经处理的填料可使用任何本领域认可的方法制备。例如,在其中未经处理的填料是未经处理的二氧化硅的情况下,未经处理的填料可通过使可溶性金属硅酸盐的水溶液与酸溶液合并以形成二氧化硅浆料;二氧化硅浆料任选地可被老化;酸或碱可添加至任选地经老化的二氧化硅浆料以调整浆料的pH;二氧化硅浆料可被过滤,任选地清洗,并然后使用本领域认可的技术干燥。根据本发明的各种实施方式,在干燥前,处理组合物(诸如任何上述的那些)可在上述方法的任何步骤添加。
在一些备选的实施方式中,本发明涉及一种用于生产经处理的沉淀二氧化硅的方法,其包括:
(a)使碱金属硅酸盐与酸合并以形成未经处理的浆料;
(b)任选地用包括该处理剂的该处理组合物处理未经处理的浆料,以形成经处理的浆料;
(c)使步骤(a)的未经处理的浆料干燥,或使(b)的经处理的浆料干燥,以在每一情况下产生经干燥的沉淀二氧化硅;
(d)用包括该处理剂的处理组合物形成步骤(c)的经干燥的沉淀二氧化硅的水性浆料,以形成经处理的二氧化硅浆料;和
(e)使经处理的二氧化硅浆料干燥以产生经干燥的经处理的沉淀二氧化硅。
在一些实施方式中且参考如上概述的方法,无论处理组合物是否在干燥前被包括在未经处理的浆料中,可制备经干燥的沉淀二氧化硅(经处理或未经处理)的水性浆料,和然后可添加处理组合物以形成沉淀二氧化硅的经处理的浆料,其随后再次干燥以产生经处理的沉淀二氧化硅。
此外,任何先前实施方式的沉淀二氧化硅可被包括在聚合物共混物中且与此处先前所述的处理组合物配混。
用于形成经处理的二氧化硅的方法的更详细说明可在此处如下的实施例中发现。
可用于本发明的一些实施方式中的适合的金属硅酸盐可包括本领域已知的广泛多种材料。非限制性的例子可包括但不限于硅酸铝(aluminasilicate)、硅酸锂、硅酸钠、硅酸钾,和它们的混合物。金属硅酸盐可以下列结构式表示:M2O(SiO2)x,其中M可为铝(alumina)、锂、钠,或钾,且x范围可为从0.1至4。
可用于本发明的一些实施方式中的适合的酸可选自本领域已知的广泛多种酸。非限制性的例子可包括但不限于矿物酸、有机酸、二氧化碳、硫酸,和它们的混合物。
通过本发明方法制备的经处理的填料适于包括在有机聚合物组合物中。在一些实施方式中,通过本发明方法制备的经处理的填料材料可用于橡胶配混组合物中,诸如,用于制造轮胎和轮胎组件(诸如,轮胎面)的橡胶组合物。
根据本发明方法制备的经处理的填料可包含于其内的聚合物组合物包括但不限于在KirkOthmerEncyclopediaofChemicalTechnology,第四版,1996,第19卷,881-904页中所述的那些,其描述内容在此通过引用并入。根据本发明各种实施方式制备的经处理的填料可与聚合物或其可聚合组分在该聚合物或可聚合组分的物理形式是呈任何液体或可配混形式(诸如,溶液、悬浮液、胶乳、分散体等)时混合。含有本发明的经处理的填料的聚合物组合物可通过本领域已知的任何方式研磨、混合、模制,和任选地固化,以形成聚合物制品。聚合物的种类可包括但不限于热塑性和热固性树脂、橡胶配混物,和具有弹性体性质的其它聚合物。
前述聚合物可包括,例如,醇酸树脂、经油改性的醇酸树脂、不饱和聚酯、天然油(例如,亚麻籽油、桐油、大豆油)、环氧化物、尼龙、热塑性聚酯(例如,聚对苯二甲酸乙二酯、聚对苯二甲酸丁二酯)、聚碳酸酯,即,热塑性和热固性,聚乙烯、聚丁烯、聚苯乙烯、聚丙烯、乙烯丙烯共聚物和三元共聚物、丙烯酸类物质(丙烯酸、丙烯酸酯、甲基丙烯酸酯、丙烯酰胺、它们的盐、氢卤化物等的均聚物和共聚物)、酚醛树脂、聚甲醛(均聚物和共聚物)、聚氨酯、聚砜、多硫化物橡胶、硝基纤维素、丁酸乙烯酯、乙烯基类物质(含有氯乙烯和/或乙酸乙烯酯的聚合物)、乙基纤维素、纤维素乙酸酯和丁酸酯、粘胶人造丝、虫胶、蜡、乙烯共聚物(例如,乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯丙烯酸酯共聚物)、有机橡胶(合成和天然橡胶两者)等。
可用于聚合物组合物中的经处理的填料的量可取决于聚合物组合物和待由该聚合物组合物形成的制品的所需性质广泛变化。例如,基于聚合物组合物总重量计,存在于聚合物组合物中的经处理的填料的量范围可为从5至高达70重量%。
在一些非限制性实施方式中,聚合物组合物可包括有机橡胶。此类橡胶的非限制性例子可包括但不限于天然橡胶;由丁二烯及其同系物和衍生物均聚形成的那些,诸如:顺式-1,4-聚异戊二烯;3,4-聚异戊二烯;顺式-1,4-聚丁二烯;反式-1,4-聚丁二烯;1,2-聚丁二烯;和由丁二烯及其同系物和衍生物与一种或多种含有烯属不饱和度的可共聚合单体(诸如,苯乙烯及其衍生物、乙烯基-吡啶及其衍生物、丙烯腈、异丁烯,和经烷基取代的丙烯酸酯,诸如,甲基丙烯酸甲酯)共聚形成的那些。进一步非限制性例子可包括由各种百分比的苯乙烯和丁二烯组成且使用各种丁二烯异构体(根据需要)的苯乙烯-丁二烯共聚物橡胶(其后称为“SBR”);苯乙烯、异戊二烯和丁二烯聚合物的三元共聚物,和它们的各种异构体;基于丙烯腈的共聚物和三元共聚物橡胶组合物;和基于异丁烯的橡胶组合物;和它们的混合物,例如,在美国专利号4,530,959;4,616,065;4,748,199;4,866,131;4,894,420;4,925,894;5,082,901;和5,162,409中所述。
适合的有机聚合物的非限制性例子可包括乙烯与其它高(high)α烯烃(诸如,丙烯、丁烯-1,和戊烯-1)和二烯单体的共聚物。有机聚合物可为嵌段、无规,或序列,且可通过本领域所知的方法制备,诸如但不限于,乳化(例如,e-SBR)或溶液聚合方法(例如,s-SBR)。用于本发明的聚合物的进一步非限制性例子可包括经部分或完全官能化的那些,包括经偶联或星形支化的聚合物。经官能化的有机橡胶的另外非限制性例子可包括聚氯丁二烯、氯丁基和溴丁基橡胶,以及溴化异丁烯-共聚-对甲基苯乙烯橡胶。在非限制性实施方式中,有机橡胶可为聚丁二烯、s-SBR,和它们的混合物。
聚合物组合物可为可固化橡胶。术语“可固化橡胶”旨在包括天然橡胶及其各种原始和再生形式以及各种合成橡胶。在替换的非限制性实施方式中,可固化橡胶可包括SBR与丁二烯橡胶(BR)的组合、SBR、BR与天然橡胶的组合,和任何先前公开作为有机橡胶的材料的其它组合。在本发明的说明中,除非另有指示,术语“橡胶”、“弹性体”和“橡胶弹性体”可互换使用。术语“橡胶组合物”、“经配混的橡胶”和“橡胶配混物”可互换使用以指代与各种成分和材料共混或混合的橡胶,且这类术语是具有橡胶混合或橡胶配混领域的技术的那些技术人员所熟知的。
包括通过本发明方法生产的经处理的填料且可用于制造无数种橡胶制品的橡胶组合物,该制品诸如,轮胎(其至少一个组件(例如,胎面)包含该经固化的橡胶组合物),以及其它橡胶制品,诸如,鞋底、软管、密封垫、线缆套管、垫片、皮带等。包含通过本发明方法生产的经处理的填料的橡胶组合物特别有利地用于制造轮胎胎面,展现出低滚动阻力和高抗磨性,包括当轮胎胎面基于天然橡胶时。此外,在一些实施方式中,对于含有通过本发明方法生产的经处理的填料的这类天然橡胶组合物可实现较低的固化温度。
本发明的经处理的填料(呈粉末、颗粒、丸粒(pellet)、浆料、水性悬浮液,或溶剂悬浮液)可与基础材料(即,用于待制造的产物中的材料)合并以形成称为母炼胶的混合物。在该母炼胶中,经处理的填料可以比在最终产物中更高的浓度存在。此混合物的等分物(aliquot)典型地在混合操作期间添加至生产尺寸量,以有助于使非常小量的这类添加剂均匀分散至聚合物组合物,例如,塑料、橡胶,和涂料组合物中。
经处理的填料可与乳液和/或溶液聚合物(例如,包含溶液苯乙烯/丁二烯(SBR)的有机橡胶、聚丁二烯橡胶,或它们的混合物)合并以形成母炼胶。一个预期的实施方式是包含有机橡胶、水不可混溶的溶剂、经处理的填料,和任选的加工油的组合的母炼胶。该产物可由橡胶生产商供应至轮胎制造商。轮胎制造商使用母炼胶的益处是经处理的填料均匀分散于橡胶中,这导致生产经配混的橡胶的混合时间最小化。母炼胶可含有每100份橡胶为10至150份(phr)的经处理的二氧化硅,优选从20至130phr,更优选从30至100phr,和最优选从50至80phr。
在下列实施例中更具体地描述本发明,该实施例旨在仅仅是示例性的,因为其中的许多修改和变化对本领域技术人员是明显的。除非另有说明,所有份数和所有百分比是以重量计。
实施例
第1部分-分析测试
本申请的实施例中报导的二氧化硅CTAB表面积值是使用CTAB溶液及其后描述的方法测定。分析是使用装配有Metrohm可互换“Snap-In”50毫升滴定管的Metrohm751Titrino自动滴定器,和装配有550nm过滤器的Brinkmann探针比色计PC910型进行。此外,将MettlerToledoHB43或等价物用于测定二氧化硅的105℃水分损失,和将FisherScientificCentrificTM离心机225型用以分离二氧化硅和残余CTAB溶液。过量的CTAB是通过用OT(磺基琥珀酸二辛基钠,可得自CytecIndustries,Inc.)的溶液自动滴定直到获得最大浊度(其是用探针比色计检测)为止而测定。最大浊度点被取作为相对应于150的毫伏读数。获知给定重量的二氧化硅吸收的CTAB量和CTAB分子占据的空间,二氧化硅的外比表面积被计算,且以干燥重量为基准,以平方米/克报导。
测试和制备所需的溶液包括pH为9.6的缓冲液、鲸蜡基[十六烷基]三甲基溴化铵(CTAB,也称为十六烷基三甲基溴化铵,工业级)、OT,和1N氢氧化钠。pH为9.6的缓冲溶液是通过使3.101克的原硼酸(99%;工业级,结晶)溶于含有500毫升去离子水和3.708克的氯化钾固体(FisherScientific,Inc.,工业级,结晶)的1升容量瓶而制备。使用滴定管,添加36.85毫升的1N氢氧化钠溶液。将该溶液混合且稀释至相应体积(volume)。
CTAB溶液是将11.0克+/-0.005克的粉末状的CTAB用于称皿上而制备。将CTAB粉末转移至2升烧杯,且用去离子水冲洗称皿。将约700毫升的pH为9.6的缓冲溶液和1000毫升的蒸馏水或去离子水添加至2升烧杯,且用磁力搅拌棒搅拌。将大的表面皿置于烧杯上,且在室温搅拌烧杯直到CTAB粉末完全溶解为止。将溶液转移至2升容量瓶,用去离子水冲洗烧杯和搅拌棒。使气泡消散,且用去离子水将溶液稀释至相应体积。添加大的搅拌棒,且将溶液在磁力搅拌器上混合约10小时。CTAB溶液可在24小时后使用,且仅持续15天。使用3.46克+/-0.005克制备OT溶液(将其置于称皿上)。将在称皿上的OT冲洗至含有约1500毫升去离子水和大搅拌棒的2升烧杯内。将OT溶液溶解和冲洗至2升容量瓶内。将溶液稀释至容量瓶的2升体积标记处。在使用前使OT溶液老化最少12天。OT溶液的保存期为从制备日起2个月。
在表面积样品制备前,CTAB溶液的pH经验证并使用1N氢氧化钠溶液调整至9.6+/-0.1的pH。对于测试计算,制备并分析空白样品。用移液管移取5毫升CTAB溶液并将55毫升去离子水添加至150毫升烧杯,且在Metrohm751Titrino自动滴定器上分析。自动滴定器经程序化,用下列参数测定空白组和样品:测量点密度=2,信号漂移=20,平衡时间=20秒,起始体积=0毫升,停止体积=35毫升,且固定端点=150mV。将滴定管尖端和比色计探针刚好置于溶液表面下,如此放置以使得尖端和光探针路径长度完全浸入。尖端和光探针两者均离烧杯底部基本上等距离,且彼此不接触。在最小搅拌(在Metrohm728搅拌器上设定为1)下,在每一空白组和样品测定前,将比色计设定为100%T,且滴定是用OT溶液起始。端点是以150mV时的滴定剂体积(毫升)记录。
为了测试样品的制备,将约0.30克的粉末状二氧化硅称重至含有搅拌棒的50毫升容器内。将颗粒状二氧化硅样品(在研磨和称重前)翻动(riffle)以获得代表性子样品。将咖啡研磨式研磨机用于研磨颗粒状材料。然后,将30毫升的经pH调整的CTAB溶液以移液管移取至含有该0.30克的粉末状二氧化硅的样品容器内。然后,将二氧化硅和CTAB溶液在搅拌器上混合35分钟。当混合完成时,将二氧化硅和CTAB溶液离心处理20分钟,以将二氧化硅与过量的CTAB溶液分离。当离心处理完成时,将CTAB溶液以移液管移取至干净容器内(无分离固体(称为“离心物”))。为了样品分析,将50毫升的去离子水置于含有搅拌棒的150毫升烧杯内。然后,将10毫升的样品离心物以移液管移取至相同烧杯内以供分析。样品是使用与用于空白组溶液相同的技术和程序化程序分析。
在本申请的实施例中报导的BET表面积值是根据Brunauer-Emmet-Teller(BET)方法根据ASTMD1993-03测定。BET表面积是通过使来自MicromeriticsTriStar3000TM仪器进行的氮吸附等温线测量的五个相对压力点拟合而测定。流动Prep-060TM站提供热和连续气流,以制备供分析的样品。在氮吸附前,二氧化硅样品通过在流动氮气(P5等级)内加热至160℃的温度至少一(1)小时而干燥。
在本申请的实施例中报导的碳(C)和硫(S)重量百分比值是使用Flash2000元素分析器测定。安装该系统以监测碳和硫。典型的参数包括:燃烧炉设为950℃,GC炉温度设为65℃,载体氦气流速设为140毫升/分钟,参考氦气流速设为100毫升/分钟,氧流速设为250毫升/分钟,且氧注射时间为5秒。对于给定的操作(run),典型地操作校准标准物、样品,和对照组。向每个中添加8-10毫克的五氧化二钒(V2O5)。样品尺寸在2-4毫克之间,且它们在分析前密封于锡胶囊(tincapsule)中。若对照标准物没有在已知接受值相对±10%内或一式两份的样品操作未相配(相对±5%),则再次分析整个样品操作。
本申请的实施例中报导的硫醇(SH)重量百分比值是使用返滴定法测定。将样品分散于75毫升的2-丙醇中,接着添加过量的0.1N碘溶液。然后,用氮气吹扫测试溶液,封闭,并使其搅拌15分钟。未反应的碘随后用标准化的0.05N硫代硫酸钠返滴定至无色端点。
第2部分-配混物测试程序和设备
实施例A
将水(74.9升)添加至150升反应槽并经由间接蒸气盘管加热加热至87℃。以560毫升/分钟的速率添加硅酸钠(3.0升)以获得2.6g/升的Na2O浓度和7.8的酸值。使用如上所述的Na2O滴定方法和酸值滴定方法通过滴定硅酸钠/水混合物来确定Na2O浓度和酸值。温度在必要时经由间接蒸气盘管加热调整至87℃,并起始沉淀步骤。经由主要槽搅拌器搅拌150升的反应器。主要搅拌器保持开着,并开始同时添加沉淀步骤。在90分钟期间同时添加硅酸钠(50.4升)和3.2升的硫酸。硅酸钠经由接近槽底部的开放管以560毫升/分钟的速率添加,且硫酸在次要高速混合器刀片上直接添加。酸添加速率在90分钟同时添加步骤期间平均为36.0毫升/分钟。
在同时添加步骤结束时,起始100分钟老化步骤。使用硫酸将溶液的pH调整至8.5。关掉次要高速搅拌器。在15-20分钟期间将硬脂酸钠,1244克缓慢喷洒至反应器内。反应混合物在搅拌下完成老化持续100分钟的剩余部分。将温度维持在87℃。老化步骤完全后,添加硫酸以达到4.8的最终批料(batch)pH。
将混合物泵取至压滤机内,并且清洗直到测得的冲洗水导电率小于1000微西门子为止。将预期的起始二氧化硅质量的约75%回收并转移回到150升反应器内。添加约20升的在环境温度的自来水,并使用主要搅拌器再次液化滤饼。在此时,将710克的L-半胱氨酸盐酸盐单水合物以每一百份二氧化硅为~7.0份(PHS)的处理比率添加。用50%NaOH将pH升至4.0,且静置48小时,其后经由压滤机送回直到冲洗水达到1000微西门子的导电率为止。
用水将所得的滤饼再次浆化以形成可泵取的浆料,且使用Niro喷雾干燥器(UtilityModel5,具有FU-1型的旋转雾化器,购自Niro,Inc.)喷雾干燥。使用AlexanderwerkWP120X40碾压机以下列条件粒化经喷雾干燥的粉末;螺杆转速=55rpm,碾压机速度4.5rpm,压碎机速度=55rpm,液压=25巴,和筛网尺寸~7筛目。合成二氧化硅的物理性质概述于表1中,证实了氨基酸半胱氨酸在二氧化硅表面上放置了可测得的硫含量。
表1-物理和化学性质
示范的(model)客车胎面配方I
用于比较实施例A本发明和比较的二氧化硅的示范的客车胎面配方显示于表2中。将装备有4个翼转子(wingrotor)的1.89升(L)KobelcoStewartBollingInc.混合器(“00”型)和Farrel12英寸双辊橡胶混炼机用于根据ASTMD3182-89混合该成分。
使用非生产道(non-productivepass)混合配方,使配混物冷却,接着在双辊混炼机上精混炼(millfinish)。对于第一道(firstpass),将混合器速度调整至85rpm,且起始温度为150°F。将商购自LANXESS的溶液SBR,VSL5228-2(乙烯基含量:52%;苯乙烯含量:28%;经处理的馏出物芳香族萃取物(TDAE)油含量:每百份橡胶是37.5份(phr);门尼粘度(ML(1+4)100℃):50),和商购自TheGoodyearTire&RubberCompany的丁二烯橡胶(BR),BUDENETM1207(顺式1,4含量98%;门尼粘度(ML(l+4)100℃):55),聚合物添加至混合器。进入混合周期内30秒后,将一半的测试二氧化硅与所有的硅烷(若指示)添加至混合器。进入混合周期内另外30秒后,将另一半的测试二氧化硅以及商购自H&RGroupInc.的500TDAE加工油添加至混合器。进入混合周期内另外30秒后,升高柱塞(ram)并清扫斜槽,即,升高入口斜槽上的覆盖物,并将在斜槽中发现的任何材料扫回混合器内,并降低柱塞。进入混合周期内另外30秒后,将商购自ZincCorporationofAmerica的经表面处理的氧化锌、商购自R.E.Carroll的橡胶等级硬脂酸、商购自HarwickStandard的描述为N-(1,3-二甲基丁基)-N'-苯基-对苯二胺的Stangard13抗臭氧剂,和商购自ADDIVANTTMUSA,LLC的Improved的抗臭氧剂烃蜡的组合添加至混合器。在另外30秒后,升高柱塞并清扫斜槽。从向前进入混合周期内150秒,将混合器速度调整达到和/或维持在338°F+/-5°F的温度持续390秒时间范围(timeframe)。在总混合时间约540秒后,在338°F+/-5°F的温度使第一道下降。
将商购自Taber,Inc.的RubberMakers硫(“RM硫”),100%活性,商购自HarwickStandard的CBS,正环己基-2-苯并噻唑次磺酰胺,和商购自HarwickStandardInc.的二苯基胍共混至在双辊橡胶混炼机上的冷却第一道母炼胶内。混炼进行约5分钟,实施5次侧向切割(sidecut)和5次最终道(endpass)。
表2:示范的客车胎面配方I
应力/应变测试样本在150℃固化30”,而所有其它测试样本在150℃固化40”。使用(如上)第2部分所示的程序和设备进行样本制备和测试。化合物性能性质显示于表3中。
表3:示范的客车胎面配方的结果
无偶联剂Si-69的半胱氨酸材料生产了具有比比较对照组更低的门尼粘度ML(1+4)、改良的韧度、相似的滚动阻力和降低的填料-填料相互作用的配混物。当Si-69与半胱氨酸组合使用时,观察到滚动阻力的下降(以在60℃的Tanδ指示),且看到较低的伸长率,这指示强化是通过半胱氨酸提供的。
实施例B
经由硅酸钠的硫酸中和而生产沉淀二氧化硅浆料。过滤和清洗该浆料以产生滤饼。用Cowles刀片混合该滤饼以形成在液体悬浮液中的固体。该液化浆料的固体百分率被确定并用于根据方程式1确定应用于各个实施例的处理量。添加L-精氨酸(98.5%+;SigmaAldrich),且用Cowles刀片混合最少10分钟。然后,在Niro喷雾干燥器(入口温度约400℃.;出口温度约105℃)中干燥该经处理的浆料。经喷雾干燥的粉未的水分含量为4-7重量%。使用AlexanderwerkWP120x40碾压机使用54.5rpm的供料螺杆转速,4.6rpm的碾压机速度,55.0rpm的压碎机速度,1.5mm的筛网间隙,26.2巴的真空压力,和20巴的粒化压力粒化经喷雾干燥的粉未。物理和化学性质显示于表4中。
方程式1:处理(克)=浆料重量(克)*固体(重量%/100)*1.00%
表4-经处理的二氧化硅的物理性质
将二氧化硅混入实施例A指示的橡胶配混物中。橡胶配混物的性质显示于表5中。
表5:示范的客车胎面配方的结果
应注意相对于比较例CE-B.1A,L-精氨酸的存在降低了固化时间(Tc90)。此外,当与Si-69硅烷结合使用时,滚动阻力(在60℃的tanδ)、门尼粘度(ML(1+4))和填料-填料相互作用(以低应变G’指示)降低。
虽然本发明已参考其某些实施方式的具体细节进行了描述,但不旨在这类细节应被视为对本发明范围的限制,除了它们包括在权利要求书中之外。
Claims (30)
1.一种用于生产经处理的填料的方法,包括:
(a)用包含处理剂的处理组合物处理包含未经处理的填料的浆料,从而形成经处理的填料浆料,其中所述未经处理的填料未被事先干燥;和
(b)使所述经处理的填料浆料干燥以生产经处理的填料,其中所述处理剂包含以下的至少一种:
(i)氨基酸;和/或
(ii)多肽。
2.如权利要求1的方法,其中所述未经处理的填料选自硅酸铝、二氧化硅凝胶、胶体二氧化硅、沉淀二氧化硅和它们的混合物。
3.如权利要求1的方法,其中所述填料包括沉淀二氧化硅。
4.如权利要求1的方法,其中所述处理剂包括所述多肽。
5.如权利要求1的方法,其中所述氨基酸是半胱氨酸、胱氨酸、精氨酸、组氨酸、酪氨酸、甲硫氨酸和脯氨酸中的至少一种。
6.如权利要求1的方法,其中所述处理组合物进一步包含有机硅烷偶联剂,其由下式(I)表示:
(R1)a(R2)bSiX4-a-b(I),
其中每个R1独立地是包含1至36个碳原子和官能团的烃基基团,其中所述烃基基团的所述官能团是乙烯基、烯丙基、己烯基、环氧基、缩水甘油氧基、(甲基)丙烯酰氧基、硫化物、异氰酸基、多硫化物、巯基,或卤素;每个R2独立地是具有1至36个碳原子的烃基基团或氢,X独立地是卤素或具有1至36个碳原子的烷氧基;a是0、1、2或3;b是0、1或2;(a+b)是1、2或3;条件是当b是1时,(a+b)是2或3。
7.如权利要求6的方法,其中所述处理组合物进一步包含不同于由式(I)表示的有机硅烷的有机硅烷。
8.如权利要求1的方法,其中所述处理组合物进一步包含偶联剂,所述偶联剂包括选自以下的有机硅烷:(4-氯甲基-苯基)三甲氧基硅烷、(4-氯甲基-苯基)三乙氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三甲氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三乙氧基硅烷、(3-氯-丙烯基)-三甲氧基硅烷、(3-氯-丙烯基)-三乙氧基硅烷、(3-氯-丙基)-三乙氧基硅烷、(3-氯-丙基)-三甲氧基硅烷、三甲氧基-(2-对甲苯基-乙基)硅烷和三乙氧基-(2-对甲苯基-乙基)硅烷和它们的组合。
9.如权利要求1的方法,其中所述处理组合物进一步包含非偶联剂,且其中所述非偶联剂是生物聚合物、脂肪酸、有机酸、聚合物乳液、聚合物涂料组合物和它们的组合中的一种或多种,且其中所述非偶联剂不同于所述处理剂。
10.如权利要求1的方法,其中所述处理组合物进一步包含非偶联剂,所述非偶联剂选自阴离子型表面活性剂、非离子型表面活性剂、两性表面活性剂和它们的组合,且基于未经处理的填料的重量计,所述非偶联剂以大于1重量%至25重量%的量存在。
11.如权利要求1的方法,其中
所述经处理的填料包含经处理的沉淀二氧化硅;和
所述处理组合物进一步包含:
(i)至少一种偶联剂,和
(ii)非偶联剂,其选自阴离子型、非离子性和/或两性表面活性剂,且基于未经处理的填料的重量计,所述非偶联剂以大于1重量%至25重量%的量存在。
12.一种经处理的填料,其通过权利要求1的方法生产。
13.一种橡胶组合物,包含通过权利要求1的方法生产的经处理的填料。
14.如权利要求13的橡胶组合物,其中所述橡胶组合物包含天然橡胶。
15.如权利要求13的橡胶组合物,其中所述橡胶组合物是橡胶配混母炼胶。
16.一种用于生产经处理的沉淀二氧化硅的方法,包括:
(a)使碱金属硅酸盐与酸合并以形成包含未经处理的二氧化硅的浆料,其中所述未经处理的二氧化硅未被事先干燥;
(b)用包含处理剂的处理组合物处理所述浆料,从而形成经处理的浆料;和
(c)使所述经处理的浆料干燥以生产经处理的沉淀二氧化硅,
其中所述处理剂包含以下的至少一种:
(i)氨基酸;和/或
(ii)多肽。
17.如权利要求16的方法,其中所述碱金属硅酸盐包括硅酸铝、硅酸锂、硅酸钠和/或硅酸钾。
18.如权利要求16的方法,其中所述处理剂包含所述多肽。
19.如权利要求16的方法,其中所述氨基酸是半胱氨酸、胱氨酸、精氨酸、组氨酸、酪氨酸、甲硫氨酸和脯氨酸中的至少一种。
20.如权利要求16的方法,其中所述处理组合物进一步包含偶联剂,所述偶联剂包括选自以下的有机硅烷:(4-氯甲基-苯基)三甲氧基硅烷、(4-氯甲基-苯基)三乙氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三甲氧基硅烷、[2-(4-氯甲基-苯基)-乙基]三乙氧基硅烷、(3-氯-丙烯基)-三甲氧基硅烷、(3-氯-丙烯基)-三乙氧基硅烷、(3-氯-丙基)-三乙氧基硅烷、(3-氯-丙基)-三甲氧基硅烷、三甲氧基-(2-对甲苯基-乙基)硅烷和三乙氧基-(2-对甲苯基-乙基)硅烷和它们的组合。
21.如权利要求16的方法,其中所述处理组合物进一步包含非偶联剂,所述非偶联剂选自阴离子型表面活性剂、非离子型表面活性剂、两性表面活性剂和它们的组合,且基于未经处理的填料的重量计,所述非偶联剂是以大于1重量%至25重量%的量存在。
22.一种经处理的沉淀二氧化硅,其是通过权利要求16的方法制备的。
23.一种橡胶组合物,包含通过权利要求16的方法生产的经处理的沉淀二氧化硅。
24.如权利要求23的橡胶组合物,其中所述橡胶组合物是橡胶配混母炼胶。
25.一种用于生产经处理的沉淀二氧化硅的方法,包括:
(a)使碱金属硅酸盐与酸合并以形成包含未经处理的二氧化硅的未经处理的浆料,其中所述未经处理的二氧化硅未被事先干燥;
(b)使所述未经处理的浆料干燥以生产经干燥的沉淀二氧化硅;
(c)用包含处理剂和任选的偶联剂和/或任选的非偶联剂的处理组合物形成所述经干燥的沉淀二氧化硅的水性浆料,以形成经处理的沉淀二氧化硅浆料;和
(d)使所述经处理的沉淀二氧化硅浆料干燥以生产经干燥的经处理的沉淀二氧化硅,
其中所述处理剂包含以下的至少一种:
(i)氨基酸;和/或
(ii)多肽。
26.如权利要求25的方法,其中所述处理剂包含所述多肽。
27.如权利要求25的方法,其中所述氨基酸是半胱氨酸、胱氨酸、精氨酸、组氨酸、酪氨酸、甲硫氨酸和脯氨酸中的至少一种。
28.一种经处理的沉淀二氧化硅,其通过权利要求25的方法制备。
29.一种橡胶组合物,包含通过权利要求25的方法生产的经处理的沉淀二氧化硅。
30.如权利要求29的橡胶组合物,其中所述橡胶组合物是橡胶配混母炼胶。
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