CN101506431B - 织物涂覆用硅橡胶组合物及涂覆硅橡胶的织物 - Google Patents
织物涂覆用硅橡胶组合物及涂覆硅橡胶的织物 Download PDFInfo
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- CN101506431B CN101506431B CN2007800303252A CN200780030325A CN101506431B CN 101506431 B CN101506431 B CN 101506431B CN 2007800303252 A CN2007800303252 A CN 2007800303252A CN 200780030325 A CN200780030325 A CN 200780030325A CN 101506431 B CN101506431 B CN 101506431B
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B60—VEHICLES IN GENERAL
- B60R—VEHICLES, VEHICLE FITTINGS, OR VEHICLE PARTS, NOT OTHERWISE PROVIDED FOR
- B60R21/00—Arrangements or fittings on vehicles for protecting or preventing injuries to occupants or pedestrians in case of accidents or other traffic risks
- B60R21/02—Occupant safety arrangements or fittings, e.g. crash pads
- B60R21/16—Inflatable occupant restraints or confinements designed to inflate upon impact or impending impact, e.g. air bags
-
- C—CHEMISTRY; METALLURGY
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Abstract
织物涂覆用硅橡胶组合物,其特征在于,该硅橡胶组合物是无溶剂的氢化硅烷化反应固化性组合物,其具有在100~500Pa·s范围内的25℃下的粘度,并且含有烷氧基硅烷和锆螯合物,但不含有有机钛化合物,该烷氧基硅烷含有甲基丙烯酰基或丙烯酰基。和用织物涂覆用硅橡胶组合物涂覆的织物。
Description
技术领域
本发明涉及适合涂覆织物的硅橡胶组合物、用该组合物涂覆的织物和涂覆织物的制造方法。更具体地说,本发明涉及适合形成涂覆层的硅橡胶组合物,其牢固地粘附于难以粘附的织物例如中空织造织物的表面并且涂覆后即使将该涂覆织物长时间暴露于高温和高湿度后也能够维持该涂覆层与该织物的牢固粘附。本发明还涉及上述织物的制造方法并且涉及由其制造的涂覆织物。
背景技术
将用硅橡胶涂覆织物用硅橡胶组合物用于制造例如车辆安全气囊。但是,将常规的这种类型的硅橡胶组合物施涂到难以粘附的材料例如中空织造织物上时,它们不提供涂覆层与织物的足够的粘合强度并且在长时间使用和存储后容易从织物基材剥离。
此外,使用常规的用硅橡胶涂覆的织物遇到问题。更具体地说,将该产品长时间暴露于高温和高湿度后,涂覆层与织物的粘合强度与制造后即刻的粘合强度相比变低。另一方面,在车辆安全气囊的情况下,要求即使在折叠状态下长期存储后该安全气囊也应可靠地膨胀并且保持其保存加压气体的功能。
日本未审专利申请公开(以下称为“公开”)2006-2093公开了含有热塑性树脂颗粒的固化性有机聚硅氧烷组合物,该热塑性树脂颗粒包括特定的有机金属化合物。
公开H08-209068公开了氢化硅烷化固化性涂覆组合物,其含有:含有环氧基的烷氧基硅烷、有机钛化合物、金属螯合物和作为粘合促进剂的用硅烷醇基封端的烯基官能聚有机硅氧烷。
公开H09-87585公开了用于涂覆织物的氢化硅烷化固化性液体硅橡胶组合物,其包括有机聚硅氧烷树脂、含有环氧基的有机硅化合物和有机钛化合物。
公开2002-88307公开了用于涂覆纤维基材的涂覆组合物,其包括烷氧基硅烷、水和金属络合物。
公开2005-82669公开了用于安全气囊的硅橡胶组合物,其可用加成反应或者用有机过氧化物固化并且包括在一个分子中含有脲基的有机硅化合物或者用有机硅化合物改性的异氰脲酸酯和后者的水解缩合产物。
但是,当将上述复合物用于在难以粘附的材料例如中空织造织物上形成涂覆层时,它们不提供涂覆层与织物的足够的粘合,并且将该涂覆织物在高温和高湿度的条件下保存时它们的粘合性能降低。
发明内容
本发明目的在于解决现有技术的问题,并且本发明的目的是提供硅橡胶组合物,其能够在难以粘附的织物例如中空织造织物的表面上形成涂覆层,该涂覆层牢固地粘附于织物,并且其适合用于制造具有即使在高温和高湿度的条件下将该涂覆织物保持长时间后也能保持与该织物的牢固粘合的涂覆层的涂覆织物。另一目的是提供用上述硅橡胶组合物涂覆的织物。
本发明的上述目的通过以下实现:
织物涂覆用硅橡胶组合物,其特征在于,该硅橡胶组合物是无溶剂的氢化硅烷化反应固化性组合物,其具有在100~500Pa·s范围内的25℃下的粘度,并且含有烷氧基硅烷和锆螯合物,但不含有有机钛化合物,该烷氧基硅烷含有甲基丙烯酰基或丙烯酰基;或者上述织物涂覆用硅橡胶组合物还包括含有环氧基的烷氧基硅烷。
根据项[1]的织物涂覆用硅橡胶组合物,其包括以下组分:
100质量份的含有烯基的有机聚硅氧烷(A),其在一分子中含有至少两个烯基并且具有在100~1,000,000mPa·s范围内的25℃下的粘度;
有机氢化聚硅氧烷(B)(其以这样的量使用,即组分(B)的键接硅的氢原子与组分(A)的烯基的摩尔比在(0.7∶1.0)~(5.0∶1.0)的范围内);
氢化硅烷化催化剂(C)(以足以固化该组合物的量使用);
0.1~50质量份的增强二氧化硅细粉末(D);
0.1~2质量份的烷氧基硅烷(E),其含有甲基丙烯酰基或丙烯酰基;和
0.01~0.5质量份的锆螯合物(F)。
根据项[2]的织物涂覆用硅橡胶组合物,其还包括含有环氧基的烷氧基硅烷(相对于100质量份组分(A),其量为0.1~2质量份)。
用根据项[1]、[2]或[3]的织物涂覆用硅橡胶组合物涂覆的织物。
根据项[4]的织物,其中该织物具有中空织造结构。
根据项[4]或[5]的织物,其用作安全气囊材料。
制造涂覆织物的方法,其包括如下步骤:将根据项[1]、[2]或[3]的织物涂覆用硅橡胶组合物施涂到织物上,然后通过固化上述组合物而在该织物上形成硅橡胶涂覆层。
根据项[7]的制造涂覆织物的方法,其中该织物具有中空织造结构。
本发明的硅橡胶组合物在难以粘附的织物例如中空织造织物上形成与该织物牢固粘附的涂覆层。即使将该涂覆织物长时间暴露于高温和高湿度的条件后该涂覆层也能保持与该织物的牢固粘合。本发明的涂覆织物的特征在于,提供与织物牢固粘附并且即使将该涂覆织物长时间暴露于高温和高湿度的条件后也能保持该牢固粘合的涂覆层。本发明的用于制造涂覆织物的方法的特征在于,制造工艺的高效率。
具体实施方式
本发明的硅橡胶组合物含有烷氧基硅烷和锆螯合物,但不含有有机钛化合物,该烷氧基硅烷含有甲基丙烯酰基或丙烯酰基。此外,该组合物是可通过氢化硅烷化反应固化的无溶剂型组合物,并且具有在100~500Pa·s范围内的25℃下的粘度。
含有甲基丙烯酰基或丙烯酰基的烷氧基硅烷是该组合物的不可缺少的组分,其赋予该组合物与难以粘附的织物例如中空织造织物牢固粘合性。含有甲基丙烯酰基或丙烯酰基的烷氧基硅烷可以是本领域中公知的物质。该化合物的具体实例如下:甲基丙烯酰氧基甲基-三甲氧基硅烷、3-甲基丙烯酰氧基丙基-三甲氧基硅烷、3-甲基丙烯酰氧基丙基-甲基二甲氧基硅烷、3-甲基丙烯酰氧基丙基-二甲基甲氧基硅烷、3-甲基丙烯酰氧基丙基-三乙氧基硅烷、3-甲基丙烯酰氧基丙基-甲基二乙氧基硅烷、3-甲基丙烯酰氧基异丁基-三甲氧基硅烷、或类似的甲基丙烯酰氧基取代的烷氧基硅烷;3-丙烯酰氧基丙基-三甲氧基硅烷、3-丙烯酰氧基丙基-甲基二甲氧基硅烷、3-丙烯酰氧基丙基-二甲基甲氧基硅烷、3-丙烯酰氧基丙基-三乙氧基硅烷、或类似的含有丙烯酰氧基取代的烷基的烷氧基硅烷。
锆螯合物是赋予该组合物与难以粘附的织物例如中空织造织物更好粘合并且使该组合物即使在该织物长期暴露于高温和高湿度的条件后也保持该性能的组分,该织物通过用上述组合物的涂覆层涂覆并固化而形成。该锆螯合物组成在本领域是公知的并且可以由下述的具体实例表示:四乙酰丙酮锆(IV)、六氟乙酰丙酮锆(IV)、三氟乙酰丙酮锆(IV)、四(乙基三氟乙酰丙酮)锆、四(2,2,6,6-四甲基-庚二酮合)锆、二丁氧基双(乙基丙酮)锆(IV)、二异丙氧基双(2,2,6,6-四甲基-庚二酮合)锆、或类似的具有用作配体的β-二酮(包括其烷基取代和氟取代的形式)的锆络合物。其中,最优选的化合物是锆的乙酰丙酮合物(包括烷基取代和氟取代的形式)络合物。
此外,优选进一步将该组合物与含有环氧基的烷氧基硅烷结合。与上述含甲基丙烯酰基或丙烯酰基的烷氧基硅烷和锆螯合物结合,该含环氧基的烷氧基硅烷也有助于改善与难以粘附的织物例如中空织造织物的粘合。上述含环氧基的烷氧基硅烷在本领域是已知的并且可以由以下具体化合物表示:3-环氧丙氧基丙基三甲氧基硅烷、3-环氧丙氧基丙基三乙氧基硅烷、3-环氧丙氧基丙基甲基二甲氧基硅烷、4-环氧丙氧基丁基三甲氧基硅烷、5,6-环氧己基三乙氧基硅烷、2-(3,4-环氧环己基)乙基三甲氧基硅烷、或2-(3,4-环氧环己基)乙基三乙氧基硅烷。
本发明的组合物的特征还在于不含钛有机化合物。如果将该组合物中配合有机钛化合物,这会削弱该组合物与中空织造织物的粘合并且如果将用该组合物的固化层涂覆的织物长时间暴露于高温和湿度的条件下会使该性能恶化。
有机钛化合物的实例如下:钛酸四异丙酯、钛酸四丁酯、钛酸四辛酯、或类似的有机钛酸酯;醋酸钛或类似的有机钛酸盐;二异丙氧基双(乙酰丙酮)钛、二异丙氧基双(乙酰乙酸酯)钛、或类似的钛螯合物。
本发明的组合物具有在100~500Pa·s范围内的25℃下的粘度并且包括不需要用于粘度调节的溶剂的可氢化硅烷化反应固化的无溶剂液体硅橡胶组合物。该组合物的优点在于对于将其施涂到织物的表面上中的处理极其方便,改进生产率,并且阻止在涂覆层中形成缺陷。
以下是本发明的组合物的优选实施方案的具体说明。
含烯基的有机聚硅氧烷(A)是本发明的组合物的主要组分之一。该组分在一分子中含有至少两个烯基。优选组分(A)具有线型分子结构。但是,在不与本发明的目的矛盾的范围内,组分(A)可以具有部分支化的分子结构,或者可以包含具有环状、支化、网状或树枝状分子结构的含烯基的有机聚硅氧烷的混合物。对于组分(A)在25℃下的粘度并无特别限制,但可以建议该组分具有100~1,000,000mPa·s的粘度,优选具有300~100,000mPa·s的粘度。从降低粘度和改进物理性能的观点出发,建议组分(A)中烯基的含量在0.02~1.9质量%的范围内。
该烯基可以由乙烯基、烯丙基、丁烯基、戊烯基、己烯基和庚烯基表示,其中优选乙烯基。另外,组分(A)中含有的烯基以外的键接硅的有机基团可以例示甲基、乙基、丙基、丁基、戊基、己基或者类似的烷基;苯基、甲苯基、二甲苯基或类似的芳基;或3-氯丙基、3,3,3-三氟丙基或类似的卤代基团。最优选甲基和苯基。另外,组分(A)的分子末端上可以含有少量的羟基、甲氧基、乙氧基或者类似的烷氧基。
组分(A)的具体实例如下:分子两端用二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷;分子两端用二甲基乙烯基甲硅烷氧基封端的甲基乙烯基硅氧烷和二甲基硅氧烷的共聚物;分子两端用三甲基甲硅烷氧基封端的甲基乙烯基硅氧烷和二甲基硅氧烷的共聚物;部分或全部的甲基用乙基、丙基或类似的烷基;苯基、甲苯基或类似的芳基;3,3,3-三氟丙基或类似的卤化烷基替代的上述的有机聚硅氧烷;或两种或更多种上述化合物的混合物。从容易获得降低的粘度和改进的物理性能的观点出发,最优选分子两端用二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷。
组分(B)是一分子中含有平均2个键接硅的氢原子的有机氢化聚硅氧烷形式的固化剂。当在下述组分(C)的存在下使用该组分时,其与组分(A)反应并且将该组合物交联。对于组分(B)的分子结构无特别限制,其可以具有线型、支化、环状或三维网状分子结构。对于组分(A)在25℃下的粘度并无特别限制,但可以建议该组分具有1~100,000mPa·s的粘度。组分(B)中使用的键接硅的有机基团可以例示甲基、乙基、丙基、丁基、戊基、己基或类似的烷基;苯基、甲苯基、二甲苯基或类似的芳基;3-氯丙基、3,3,3-三氟丙基或类似的卤代烷基,其中优选甲基和苯基。
建议组分(B)的使用量使组分(B)的键接硅的氢原子的摩尔数与组分(A)的烯基的摩尔数的比在(0.7∶1.0)~(5.0∶1.0)的范围内,优选在(0.9∶1.0)~(2.5∶1.0)的范围内,并且最优选在(0.9∶1.0)~(2.0∶1.0)的范围内。如果组分(B)的含量低于建议的下限,这可能不提供该组合物的充分固化程度或该组合物的涂覆层与织物的充分的粘合强度。另一方面,如果组分(B)的用量超过建议的上限,这可能降低涂覆产物的固化后的物理性能,例如伸长率。
组分(B)可以例示下列化合物:分子两端用三甲基甲硅烷氧基封端的甲基氢化聚硅氧烷;分子两端用三甲基甲硅烷氧基封端的甲基氢化硅氧烷和二甲基硅氧烷的共聚物;分子两端用二甲基氢化甲硅烷氧基封端的二甲基硅氧烷;分子两端用二甲基氢化甲硅烷氧基封端的甲基氢化硅氧烷和二甲基硅氧烷的共聚物;分子两端用二甲基苯基甲硅烷氧基封端的甲基氢化硅氧烷和甲基苯基硅氧烷的共聚物;环状甲基氢化聚硅氧烷;由(CH3)2HSiO1/2硅氧烷单元和SiO4/2单元组成的共聚物;由(CH3)2HSiO1/2硅氧烷单元、(CH3)3SiO1/2硅氧烷单元和SiO4/2单元组成的共聚物;其中部分或全部甲基替代为乙基、丙基或类似的烷基;苯基、甲苯基或类似的芳基;3,3,3-三氟丙基或类似的卤代烷基的上述有机聚硅氧烷;或两种或更多种的上述有机聚硅氧烷的混合物。
氢化硅烷化催化剂(C)用于加速组分(A)的烯基和组分(B)的键接硅的氢原子之间的氢化硅烷化反应。优选的组分(C)为其催化作用高效并且相对容易得到的铂系催化剂。该催化剂可以例示以下物质:细粉末状铂;氯铂酸或氯铂酸的醇溶液;氯铂酸的烯烃络合物;氯铂酸和烯基硅氧烷的络合物;铂-二酮络合物;二氧化硅、氧化铝、碳或类似载体上的金属铂;或含有铂化合物的热塑性树脂粉末。这些以外的属于铂族系的催化剂可以例示铑、钌、铱或钯化合物。例如,这些催化剂可以由下式表示:RhCl(PPh3)3、RhCl(CO)(PPh3)2、Ru3(CO)12、IrCl(CO)(PPh3)2和Pd(PPh3)4(其中,Ph表示苯基)。
相对于组分(A)的106质量份,通常应以金属铂为0.1~500质量份、优选1~50质量份的量添加组分(C)。如果组分(C)的添加量低于建议的下限,反应不会充分进行,另一方面,如果添加量超过建议的上限,这在经济上不合理。
增强细二氧化硅粉末(D)是用于提高通过固化上述加成固化性液体硅橡胶组合物而得到的成型硅橡胶产品的机械强度而添加的组分。该组分可以例示干法二氧化硅、沉淀二氧化硅或例如用有机硅化合物对其表面进行了疏水处理的上述二氧化硅。建议该增强细二氧化硅粉末的比表面积等于或超过50m2/g。相对于100质量份的组分(A),可以将增强细二氧化硅粉末以0.1~50质量份、优选5~40质量份的量加入组合物中。
含有甲基丙烯酰基或丙烯酰基的烷氧基硅烷(E)是赋予组合物与难以粘附的材料例如中空织造织物的改进的粘合的组分。这些含有甲基丙烯酰基或丙烯酰基的烷氧基硅烷可以例示前面已提及的相同的化合物。相对于组分(A)的100质量份,建议以0.1~2质量份、优选0.5~2质量份的量将组分(E)添加到组合物中。如果组分(E)以小于建议的下限的量添加,与难以粘附的材料的粘合的改进可能不充分,另一方面,如果添加的量超过建议的上限,这可能改变涂覆层的颜色。
锆螯合物(F)是赋予组合物与难以粘附的材料例如中空织造织物更好的粘合性的组分。此外,该组分使将施涂到织物上的组合物固化后形成的涂覆层即使长时间暴露于高温和高湿度的条件后也保持与织物的牢固粘合。该锆螯合物可以由与以上给出的相同的实例表示。相对于组分(A)的100质量份,建议以0.01~0.5质量份、优选0.05~0.5质量份的量添加组分(F)。如果组分(F)以小于建议的下限的量使用,这可能不提供固化的组合物与难以粘附的材料例如中空织造织物足够牢固的粘合,或者可能不会使将施涂到织物上的组合物固化后形成的涂覆层在长时间暴露于高温和高湿度的条件后保持与织物的牢固粘合。另一方面,如果组分(F)的含量超过建议的上限,这可能使该组合物的固化产物的物理性能降低,或者可能使将施涂到织物上的组合物固化后得到的硅橡胶层的颜色改变。
如果将上述组分(E)和(F)进一步与含有环氧基的烷氧基硅烷(G)结合,能够进一步改进该组合物与难以粘附的材料例如中空织造织物的粘附。适合的含有环氧基的烷氧基硅烷(G)可以例示与前面提及的相同的化合物。相对于组分(A)的100质量份,可以以0.1~2质量份、优选0.5~2质量份的量添加该组分。
为了提高储存稳定性或工业可处理性,该组合物可以含有例如3,5-二甲基-1-己炔-3-醇、3,5-二甲基-1-辛炔-3-醇、2-苯基-3-丁炔-2-醇或类似的炔类化合物;3-甲基-3-戊烯-1-炔、3,5-二甲基-3-己烯-1-炔或类似的烯炔化合物;苯并三唑或类似的三唑化合物;膦、硫醇、肼或类似的固化抑制剂。对于这些化合物能够使用的量没有特别限制,但通常相对于100质量份的组分(A),它们应当加入0.001~5质量份的量。最优选地,相对于组分(A)的100质量份,该固化抑制剂应当以0.01~10质量份的量加入。
为了改进固化产物的物理性能,该组合物可以进一步与以下物质结合:1,3,5,7-四甲基-1,3,5,7-四乙烯基环四硅氧烷、1,3,5,7-四甲基-1,3,5,7-四己烯基环四硅氧烷、分子两端用二甲基羟基甲硅烷氧基封端的甲基乙烯基硅氧烷、分子两端用二甲基羟基甲硅烷氧基封端的二甲基硅氧烷和甲基乙烯基硅氧烷的共聚物、分子两端用三甲基甲硅烷氧基封端的甲基乙烯基硅氧烷低聚物、或一分子中以等于或大于5质量%的量含有乙烯基的类似的有机聚硅氧烷化合物。相对于组分(A)的100质量份,这些有机聚硅氧烷可以以0.1~1质量份的量添加。尽管对上述有机聚硅氧烷的粘度无特别限制,但建议具有0.5~50mPa·s范围内的粘度。
在不与本发明的目的矛盾的范围内,该组合物可以进一步与以下物质结合:由(CH3)2ViSiO1/2硅氧烷单元和SiO4/2硅氧烷单元(其中Vi表示乙烯基)组成的有机聚硅氧烷,由(CH3)3SiO1/2硅氧烷单元、(CH3)2ViSiO1/2单元和SiO4/2硅氧烷单元(其中Vi表示乙烯基)组成的有机聚硅氧烷,或硅橡胶组合物中的其他常规添加剂例如石英粉末、硅藻土、碳酸钙、碳酸镁或类似的增重填料;氧化铈、氢氧化铈、氧化铁或类似的耐热添加剂;氧化铁红、氧化钛、炭黑或类似的颜料;阻燃剂;和不具有烯基且不具有软化点的有机聚硅氧烷树脂。
对于适于制备本发明的硅橡胶组合物的方法没有特别限定,并且该组合物可以通过将组分(A)~(E)混合而制备,如需要,可与其它任意组分混合。但是,可首先通过加热和混合组分(A)的一部分与组分(D)来制备二氧化硅母料,然后在该母料中加入组分(A)的其余部分和组分(B)、(C)和(E)。如果该组合物含有任意组分,可在二氧化硅母料的制备过程中将它们与其它组分混合,如果加热和混合这些任意组分改变它们的性能,优选地,可以将它们与组分(A)的其余部分和组分(B)、(C)和(E)一起与二氧化硅母料结合。另外,在制备该二氧化硅母料时,可以加入上述的有机硅化合物,并且可以对组分(D)进行原位表面处理。该组合物可以通过使用双辊塑炼机、捏合混合机、罗斯(Ross)混合机、或者任何其他常规的捏合或混合设备来制备。
为了得到更好的存储稳定性,本发明的硅橡胶组合物可以包括双份液体硅橡胶组合物,其由含有组分(A)、(C)和(D)且不含组分(B)的组合物(I)和由组分(A)、(B)和(D)组成且不含组分(C)的组合物(II)组成。组分(E)可以与组合物(I)混合或者与组合物(II)混合。
本发明的涂覆织物是涂覆有本发明的组合物的织物。该织物可以包括尼龙6、尼龙66、尼龙46或者类似的聚酰胺纤维织物;聚对苯二甲酸乙二醇酯、聚对苯二甲酸丁二醇酯或类似的聚酯纤维织物;聚丙烯腈纤维织物、芳族聚酰胺纤维织物、聚醚-酰亚胺纤维织物、聚砜类纤维织物、碳纤维织物、人造丝纤维织物、聚乙烯纤维织物、或由上述纤维制成的无纺布。在上述织物中,从低成本和强度的观点出发,最优选聚酰胺纤维织物或聚酯纤维织物。
尽管对于织物结构不作特别限定,但为了得到更好的生产率和需要的厚度,通常应为平织物。由于本发明的组合物适合形成具有与难以粘附的材料牢固的粘合的涂覆层,因此建议将该组合物用于施涂在中空织造织物上,该中空织造织物具有在其织物结构中织出的袋状体。应注意决定与中空织造织物的难粘合性的因素之一是该中空织造织物的复杂质地。因此,有必要检查在实施涂覆前对该织物仔细洗涤并完全干燥。
将本发明的硅橡胶组合物施涂到织物上的方法可包括喷涂、凹版辊涂布、棒涂、刮刀涂布、patting、丝网印刷、浸涂或任何其它常规的工艺。该组合物的涂覆量可以在25~150g/m2的范围内。施涂到织物上的组合物的固化可在150~200℃的温度下进行,并且在该温度下的固化时间大约为1~2分钟。
通常,本发明组合物的织物涂覆层包括单层。但如果需要,在织物上可形成任意层数。设置这样的附加层以用于改进触感,提高材料的耐磨性能,或提高涂覆产品的强度。附加涂覆层可以例示塑料膜、织物、无纺布、或者由其它弹性涂覆材料形成的层。
实施例
参照实施例进一步说明本发明,其中所有份数均为质量份并且所有粘度均在25℃下测定。实施例中,Me代表甲基并且Vi代表乙烯基。
[硅橡胶的物理性能的测定方法]
通过在150℃下、20MPa的压力下对硅橡胶组合物进行加压固化5min,制备2mm厚的固化硅橡胶试样。硅橡胶的硬度根据JIS K6253使用A型硬度计测定。拉伸强度和伸长率根据JIS K6251测定。另外,100%伸长率时产生的应力根据JIS K6251测定作为100%模量。
[粘合耐久性的测定方法]
将具有中空织造结构、经线密度46根/英寸和纬线密度46根/英寸的尼龙66织物片涂覆50μm厚的硅橡胶组合物层,并且通过将涂覆有该组合物的织物在170℃下的加热炉中保持2分钟从而形成硅橡胶涂覆织物。根据JIS K6404-6利用Scott揉性测试机在1kgf负荷下使得到的硅橡胶涂覆织物经受1000次载荷循环,然后观察硅橡胶涂覆层的表面上的状况。将不含有任何变化的表面评定为等级5,将含有轻微条状痕迹的表面评定为等级4,将具有轻微和部分硅橡胶涂覆层剥离的织物评定为等级3,将具有明显的硅橡胶涂覆层的部分剥离的织物评定为等级2,将在织物整个表面具有显著的硅橡胶涂覆层剥离的织物被评定为等级1。对采用与上述同样的方法制造但却在温度80℃且Rh湿度95%的条件下将该织物保持10天后的硅橡胶涂覆织物,通过利用Scott测试机进行相同的粘合耐久性测试并使用与上述那些同样的评价标准。
[涂覆织物的颜色变化]
目视观察在织物的表面上由本发明的组合物形成的涂覆层中是否出现黄褐色。如果没有观察到该变色则涂覆织物合格,如果观察到该变色则不合格。
[制造例1]
将Ross混合机填充以下组分:100份的分子两端用二甲基乙烯基甲硅烷氧基封端且粘度为40,000mPa·s的二甲基聚硅氧烷;40份的BET比表面积为225m2/g的气相法二氧化硅;7份的六甲基二硅氮烷;2份的水;和0.2份的分子两端用二甲基羟基甲硅烷氧基封端且粘度为20mPa·s的二甲基硅氧烷和甲基乙烯基硅氧烷的共聚物(10.9质量%的乙烯基含量)。将这些组分在室温下混合均匀后,对得到的混合物在200℃下在减压下加热处理2小时,由此制备可流动的二氧化硅母料1。
以下给出在随后的比较例和实施例中用作组合物组分的材料的名称和量。
(1)二氧化硅母料
制造例1中制备的二氧化硅母料。该母料含有下述的组分:71份的成分(a-1)、0.1份的乙烯基硅氧烷低聚物和29份的组分(D),组分(D)为气相法二氧化硅,相对于100份的二氧化硅母料。
(2)组分(A)
(a-1):粘度为40,000mPa·s且分子两端用二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷;乙烯基的含量大约为0.09质量%。
(a-2):粘度为2,000mPa·s且分子两端用二甲基乙烯基甲硅烷氧基封端的二甲基聚硅氧烷;乙烯基的含量大约为0.2 3质量%。
(a-3):粘度为350mPa·s且分子两端用二甲基乙烯基甲硅烷氧基封端的甲基乙烯基硅氧烷和二甲基硅氧烷的共聚物;乙烯基的含量大约为1.17质量%。
(3)组分(B)
(b-1):运动粘度为5.5mm2/s且分子两端用三甲基甲硅烷氧基封端的甲基氢化硅氧烷和二甲基硅氧烷的共聚物;键接硅的氢原子的含量大约为0.73质量%。
(b-2):运动粘度为9.5mm2/s且分子两端用二甲基氢化甲硅烷氧基封端的二甲基聚硅氧烷;键接硅的氢原子的含量大约为0.16质量%。
(4)组分(C)
铂系催化剂:铂的1,3-二乙烯基四甲基二硅氧烷的络合物的1,3-二乙烯基四甲基二硅氧烷溶液;金属铂的含量大约为4000ppm。
(5)粘合促进剂
通过按表1中给出的比例将各种组分均匀混合来制备粘合促进剂AD-1至AD-10。以下给出表1中所示的适当组分的名称和量。
组分(E)
E:3-甲基丙烯酰氧基丙基三甲氧基硅烷
组分(F)
f-1:四乙酰丙酮锆(商品名:Orgatix ZC-150;由Matsumoto SeiyakuKogyo Co.,Ltd.提供)
f-2:四(乙基三氟乙酰乙酸)锆
组分(G)3-环氧丙氧丙基三甲氧基硅烷
其他有机金属化合物
m-1:醋酸锆(商品名:Orgatix B-115;由Matsumoto Seiyaku KogyoCo.,Ltd.提供)
m-2:铝络合物(商品名:Orgatix AL135;由Matsumoto Seiyaku KogyoCo.,Ltd.提供)
m-3:乳酸钛(商品名:Orgatix TC-310;由Matsumoto Seiyaku KogyoCo.,Ltd.提供)
m-4:钛酸四异丙酯(商品名:Orgatix TA-10;由Matsumoto SeiyakuKogyo Co.,Ltd.提供)
(6)添加剂
固化抑制剂:3,5-二甲基-1-辛炔-3-醇
有机硅树脂:由下式(Me3SiO1/2)n(Me2ViSiO1/2)m(SiO4/2)r表示的有机聚硅氧烷;数均分子量=4300;乙烯基的大致含量=1.9质量%;(n+m)/r=0.71
环状硅氧烷低聚物:环状甲基乙烯基聚硅氧烷;粘度=3.5mPa·s;乙烯基的大致含量=30.7质量%
乙烯基硅氧烷低聚物:粘度为20mPa·s且分子两端用二甲基羟基甲硅烷氧基封端的甲基乙烯基硅氧烷和二甲基硅氧烷的共聚物;乙烯基的含量=约10.9质量%
[实施例1~5]
硅橡胶组合物通过以表2中所示的量均匀混合各种组分而制备。将得到的硅橡胶组合物的物理性能、它们的粘合强度、用硅橡胶涂覆的中空织造织物的粘合耐久性的测定结果示于表2中。
[比较例1]
以与实施例1中同样的方式制备硅橡胶组合物,不同之处在于将实施例1中使用的1.2份的粘合赋予剂AD-1替换为1.7份的AD-8。
[实施例6和7、比较例2~7]
以与实施例1中同样的方式制备硅橡胶组合物,不同之处在于将以1.2份的量使用的粘合促进剂AD-1替换为以表3中所示的量使用的AD-2~AD-10。采用上述方法对用各种硅橡胶组合物涂覆的中空织造织物的粘合耐久性进行测定。将结果示于表3中。
[表1]
AD-1 | AD-2 | AD-3 | AD-4 | AD-5 | AD-6 | AD-7 | AD-8 | AD-9 | AD-10 | |
E(份) | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | 0.6 | |
G(份) | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | |
f-1(份) | 0.1 | 0.7 | 0.1 | 0.1 | ||||||
f-2(份) | 0.1 | |||||||||
m-1(份) | 0.1 | |||||||||
m-2(份) | 0.1 | |||||||||
m-3(份) | 0.1 | |||||||||
m-4(份) | 0.1 |
[表2]
实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 比较例1 | |
二氧化硅母料 | 48 | 61.5 | 52.5 | 65 | 60 | 48 |
A-1 a-1(份)a-2(份)a-3(份) | 48 | 35 | 43.78 | 25 | 48 | 48 |
B b-1(份)b-2(份)b-3(份) | 21 | 1.5 | 0.231.10.18 | 1.91.9 | 2.1 | 2.1 |
C铂类催化剂(份) | 0.3 | 0.2 | 0.2 | 0.2 | 0.3 | 0.3 |
粘结促进剂 AD-1(份)AD-8(份) | 1.2 | 1.2 | 0.65 | 1.2 | 1.2 | 1.8 |
固化抑制剂 (份)有机硅树脂 (份)环状硅氧烷低聚物(份)乙烯基硅氧烷低聚物(份) | 0.040.20.3 | 0.040.20.15 | 10.050.1 | 0.040.20.15 | 0.048.50.15 | 0.040.20.3 |
粘度 Pa·s硬度密度 g/cm3拉伸强度 MPa | 85261.056 | 120291.0910 | 88181.065 | 120271.110 | 125261.18 | 170271.056 |
相对伸长率 % | 830 | 940 | 1100 | 1000 | 650 | 680 |
粘合耐久性初始 | 5 | 5 | 5 | 5 | 5 | 5 |
暴露于热和湿度后 | 5 | 5 | 5 | 5 | 5 | 5 |
涂覆层的颜色变化 | 合格 | 合格 | 合格 | 合格 | 合格 | 不合格 |
[表3]
实施例6 | 实施例7 | 比较例2 | 比较例3 | 比较例4 | 比较例5 | 比较例6 | 比较例7 | |
粘合促进剂 | ||||||||
AD-2(份) | 1.2 | |||||||
AD-3(份) | 1.2 | |||||||
AD-4(份) | 1.2 | |||||||
AD-5(份) | 1.2 | |||||||
AD-6(份) | 1.2 | |||||||
AD-7(份) | 1.1 | |||||||
AD-9(份) | 0.7 | |||||||
AD-10(份) | 0.6 | |||||||
粘合耐久性 | ||||||||
初始 | 5 | 5 | 3 | 3 | 1 | 1 | 3 | 1 |
暴露于热和湿度后 | 3 | 5 | 1 | 2 | 1 | 1 | 1 | 1 |
实施例1~6与比较例4和5的比较表明,含有含甲基丙烯酰氧基的烷氧基硅烷(E)、锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与含有含甲基丙烯酰氧基的烷氧基硅烷(E)和含环氧基的烷氧基硅烷(G)并且含有有机钛化合物而不是锆螯合物(F)的织物涂覆用硅橡胶组合物相比,在其粘合耐久性方面具有优势,粘合耐久性在初始阶段和暴露于热和湿度后均保持优异。
实施例1~6与比较例6的比较表明,含有含甲基丙烯酰氧基的烷氧基硅烷(E)、锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与含有含甲基丙烯酰氧基的烷氧基硅烷(E)和含环氧基的烷氧基硅烷(G)并且不含锆螯合物(F)的织物涂覆用硅橡胶组合物相比,在其粘合耐久性方面具有优势,粘合耐久性在初始阶段和暴露于热和湿度后均保持优异。
实施例1~6与比较例2的比较表明,含有含甲基丙烯酰氧基的烷氧基硅烷(E)、锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与含有含甲基丙烯酰氧基的烷氧基硅烷(E)和含环氧基的烷氧基硅烷(G)并且含有有机锆化合物而不是锆螯合物(F)的织物涂覆用硅橡胶组合物相比,在其粘合耐久性方面具有优势,粘合耐久性在初始阶段和暴露于热和湿度后均保持优异。
实施例1~6与比较例3的比较表明,含有含甲基丙烯酰氧基的烷氧基硅烷(E)、锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与含有含甲基丙烯酰氧基的烷氧基硅烷(E)和含环氧基的烷氧基硅烷(G)并且含有铝螯合物而不是锆螯合物(F)的织物涂覆用硅橡胶组合物相比,在其粘合耐久性方面具有优势,粘合耐久性在初始阶段和暴露于热和湿度后均保持优异。
实施例1与比较例1的比较表明,含有适当量的锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与含有过剩量的锆螯合物的织物涂覆用硅橡胶组合物相比,在组合物的固化产物的物理性能和外观上具有优势,原因是涂覆层不易变色。
实施例1与比较例7的比较表明,含有含甲基丙烯酰氧基的烷氧基硅烷(E)、锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物与不含有含甲基丙烯酰氧基的烷氧基硅烷(E)并且含有锆螯合物(F)和含环氧基的烷氧基硅烷(G)的织物涂覆用硅橡胶组合物相比,在其粘合耐久性方面具有优势,粘合耐久性在初始阶段和暴露于热和湿度后均保持优异。
工业应用性
本发明的硅橡胶组合物由于其使织物在较长时间内保持预定的压力而适用作织物涂覆用组合物。因此,该组合物可用于涂覆应用在车辆侧帘安全气囊、飞机紧急出口座席、充气救生艇及类似物的结构中的织物。本发明的涂覆织物可应用在车辆侧帘安全气囊、飞机紧急出口座席、充气救生艇等的结构中。
Claims (7)
1.织物涂覆用硅橡胶组合物,该硅橡胶组合物是无溶剂的氢化硅烷化反应固化性组合物,其具有在100~500Pa·s范围内的25℃下的粘度,其包括以下组分,但不含有有机钛化合物:
100质量份的含有烯基的有机聚硅氧烷(A),其在一分子中含有至少两个烯基并且具有在100~1,000,000mPa·s范围内的25℃下的粘度;
有机氢化聚硅氧烷(B),其以这样的量使用,即组分(B)的键接硅的氢原子与组分(A)的烯基的摩尔比在(0.7∶1.0)~(5.0∶1.0)的范围内;
氢化硅烷化催化剂(C),以足以固化该组合物的量使用;
0.1~50质量份的增强二氧化硅细粉末(D);
0.1~2质量份的烷氧基硅烷(E),其含有甲基丙烯酰基或丙烯酰基;和
0.01~0.5质量份的锆螯合物(F)。
2.根据权利要求1所述的织物涂覆用硅橡胶组合物,其还包括含有环氧基的烷氧基硅烷,相对于100质量份组分(A),其量为0.1~2质量份。
3.用根据权利要求1~2任一项所述的织物涂覆用硅橡胶组合物涂覆的织物。
4.根据权利要求3所述的织物,其中该织物具有中空织造结构。
5.根据权利要求3或4所述的织物,其用作安全气囊材料。
6.制造涂覆织物的方法,其包括如下步骤:将根据权利要求1~2任一项所述的织物涂覆用硅橡胶组合物施涂到织物上,然后通过固化上述组合物而在该织物上形成硅橡胶涂覆层。
7.根据权利要求6所述的制造涂覆织物的方法,其中该织物具有中空织造结构。
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EP2053161A1 (en) | 2009-04-29 |
PT2053161E (pt) | 2012-07-20 |
TW200833789A (en) | 2008-08-16 |
KR101439112B1 (ko) | 2014-09-12 |
ES2388081T3 (es) | 2012-10-08 |
KR20090045338A (ko) | 2009-05-07 |
EP2053161A4 (en) | 2011-04-13 |
EP2053161B1 (en) | 2012-05-16 |
US20100190396A1 (en) | 2010-07-29 |
JP5372510B2 (ja) | 2013-12-18 |
JPWO2008020635A1 (ja) | 2010-01-07 |
WO2008020635A1 (fr) | 2008-02-21 |
PL2053161T3 (pl) | 2012-10-31 |
CN101506431A (zh) | 2009-08-12 |
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