CN117946576A - 双组份聚氨酯树脂及其制备方法和应用 - Google Patents
双组份聚氨酯树脂及其制备方法和应用 Download PDFInfo
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- CN117946576A CN117946576A CN202311338954.9A CN202311338954A CN117946576A CN 117946576 A CN117946576 A CN 117946576A CN 202311338954 A CN202311338954 A CN 202311338954A CN 117946576 A CN117946576 A CN 117946576A
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Abstract
双组份聚氨酯树脂及其制备方法和应用涉及材料领域。双组份聚氨酯树脂,包括以下重量份的原料:异氰酸酯、聚合物多元醇、扩链剂、内脱模剂、抗静电剂、催化剂、消泡剂、除水剂。聚氨酯拉挤复合材料的制备方法,将待复合的增强材料浸入双组份聚氨酯树脂中以进行浸润得到复合初料,之后将复合初料以1~5cm/s的速度通过具有三段温区的模具以进行固化,三段温区依次为温度为100℃的预热区、温度为140℃凝胶区、温度为150℃固化区,复合初料从预热区进入,经过凝胶区后从固化区输出得到聚氨酯拉挤复合材料。本发明的聚氨酯拉挤复合材料降低了电阻率,使得静电喷涂成为可能。
Description
技术领域
本发明涉及材料领域,尤其涉及是树脂。
背景技术
静电喷涂是利用高压静电电场使带负电的涂料微粒沿着电场相反的方向定向运动,将涂料微粒吸附在工件表面的一种喷涂方法。它可以显著减少飞散在空气中的漆雾,节省涂料,并且降低对环境的污染,改善喷漆工人的劳动条件,消除职业病,而且可以使喷涂工艺机械化、连续化,减少废品率,获得优异的涂膜性能,大大提高生产效率,改善劳动条件,从而获得可观的社会经济效益。此外,由于静电喷涂可以方便的涂覆于锐边或者隐藏的面上,降低了漏涂的概率,提高了型材的整体耐久性。
传统的拉挤复合材料基体树脂一般为不饱和聚酯、环氧树脂和乙烯基树脂等。体积电阻率普遍大于1012欧姆.米,接近绝缘材料,非常不导电,难以采用静电喷涂工艺。
发明内容
本发明的目的在于提供一种双组份聚氨酯树脂,系生产聚氨酯拉挤复合材料的原料之一;
本发明的目的还在于提供双组份聚氨酯树脂的制备方法,用于制备双组份聚氨酯树脂;
本发明的目的还在于提供一种聚氨酯拉挤复合材料,该材料允许静电喷涂;
本发明的目的还在于提供聚氨酯拉挤复合材料的制备方法,用于制备聚氨酯拉挤复合材料;
本发明所解决的技术问题可以采用以下技术方案来实现:
双组份聚氨酯树脂,其特征在于,包括以下重量份的原料:
优选,所述内脱模剂和所述抗静电剂为二合一,为内脱模抗静电二合一添加剂;所述内脱模抗静电二合一添加剂是脂肪酸酯、可再生植物脂肪酸的乙氧基化烷基胺衍生、基于聚乙二醇脂肪酸酯的混合物、脂肪酸酰胺或高单甘油单硬脂酸酯。
为了进一步改进加工性和最终复合材料的相应性能,双组份聚氨酯树脂的原料还可以包括阻燃剂、分散剂、无机填料、抗紫外线剂、抗水解助剂。
双组份聚氨酯树脂的制备方法,其特征在于,包括如下步骤:步骤1、按照权利要求1-7中任意一项所述的双组份聚氨酯树脂的原料的重量份称取各原料,备用;步骤2、将聚合物多元醇、扩链剂混合后在110~120℃条件下进行真空脱水1.5~5小时进行真空脱水,冷却后加入内脱模剂、抗静电剂、催化剂、消泡剂、除水剂,以120~400r/min的速率进行搅拌30~400分钟至各组分混合均匀得到B料,采用静态混合器将作为A料的异氰酸酯与B料混合均匀,得到双组份聚氨酯树脂。
聚氨酯拉挤复合材料,其特征在于,由双组份聚氨酯树脂和增强材料共混拉挤制备而成。
聚氨酯拉挤复合材料的制备方法,其特征在于,将待复合的增强材料浸入双组份聚氨酯树脂中以进行浸润得到复合初料,浸润时间为0.5~3分钟,之后将复合初料以1~5cm/s的速度通过具有三段温区的模具以进行固化,所述三段温区依次为温度为100℃的预热区、温度为140℃凝胶区、温度为150℃固化区,复合初料从预热区进入,经过凝胶区后从固化区输出得到聚氨酯拉挤复合材料。
有益效果:
1.传统的聚氨酯树脂以及相应拉挤复合材料接近绝缘体。本发明的双组份聚氨酯树脂及其复合材料大幅降低了电阻率,使得静电喷涂成为可能,更经济,更高效率,全自动化涂装成为可能,相较于传统的离线手动或半自动喷涂工艺,合格率更高,耐久性更好。
2.本发明同现有技术相比使用了抗静电剂能或者具有抗静电功能的内脱模剂,使得拉挤制备的型材具有抗静电功能,同时低电阻方便后续的有机涂层采用静电喷涂,适合水性涂料,溶剂型涂料和粉末涂料。
3.本发明聚氨酯拉挤复合材料具有机械性能高,耐腐蚀、耐老化、生产效率高、无苯乙烯挥发等诸多优点。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面进一步阐述本发明。
关于双组份聚氨酯树脂
双组份聚氨酯树脂,包括以下重量份的原料:
其中,所述异氰酸酯为MDI-50、MDI-100、液化MDI、改性MDI、PAPI中的至少一种。其中,优选其NCO含量为28-32%、平均官能度为2-3%,另外,改性MDI优选采用氨酯改性MDI和/或碳化二亚胺改性MDI,MDI型异氰酸酯中NCO基团含量高,反应活性高,可与多元醇快速聚合,尤其适合快速拉挤工艺。
所述聚合物多元醇为聚醚多元醇和/或聚酯多元醇。其中,聚醚多元醇的起始剂优选采用为乙二醇、丙二醇、丙三醇、三羟基丙烷、季戊四醇、木糖醇、山梨醇、蔗糖中的至少一种。聚醚多元醇的分子量优选为20~4500;聚酯多元醇优选采用常规聚酯多元醇、聚己内酯多元醇和聚碳酸酯二醇中的至少一种,优选聚酯多元醇的分子量为500-2000。
所述扩链剂为乙二醇、1,4丁二醇、1,6己二醇、一缩二乙二醇、HQEE-L、MOCA、DMTDA、DETDA中的至少一种。选用小分子醇作为扩链剂,可以提高聚氨酯拉挤复合材料制品的强度和硬度。
所述内脱模剂包括有机氟化物类(如聚四氟乙烯,PTFE、FEP、PFA),硅氧烷类化合物、硅油和硅树脂,蜡(油)脱模剂,界面活化剂体系,硬脂酸锌、硬脂酸铵和石蜡磷酸酯、卵磷酸、硬脂酸盐类、三乙醇胺油,伯胺、仲胺和有机磷酸酯与酯肪酸的共聚体的混合物等。所述抗静电剂为内掺型抗静电剂,主要为表面活性剂型,包括阳离子型(季铵盐),阴离子型(磷酸盐、磺酸盐),非离子型(脂肪酸多元醇酯,据氧化乙烯加成物),两性型(甜菜碱类,内铵盐,丙氨酸盐)以及高分子型(聚丙烯酸衍生物,包括聚环氧乙烷、聚醚酯酰胺、含季铵盐的(甲基)丙烯酸酯共聚物和含亲水基的有机硅等)。优选,所述内脱模剂为含有磷酸酯、卵磷酸、硬脂酸盐类、三乙醇胺油,有机脂肪酸和胺类的混合溶液,可保证拉挤线速度达到最快,同时可提高增强材料的浸润性,降低复合材料与模具表面的磨损。内脱模剂是将其直接加入到树脂中,在一定加工温度条件下,从树脂基体渗出扩散到固化制品表面,在模具和制品之间形成一层隔离膜,起到脱模作用。
所述催化剂为叔胺催化剂和/或有机金属化合物催化剂,如二月桂酸二丁基锡、二甲基锡、二丁基锡、辛酸亚锡、单丁基氧化锡、二巯基乙酸二丁基锡、巯基乙酸异辛酯丁基锡、巯基乙酸异辛酯二丁基锡、巯基丙酸二丁基锡中的一种或几种。优选,叔胺催化剂可以是包括三亚乙基二胺,双(二甲氨基乙基)醚、环己基甲基叔胺中的至少一种,有机金属化合物催化剂优选有机重金属催化剂,可以是有机锡催化剂、有机锌催化剂、有机铋催化剂、铋-锌复配催化剂中的至少一种,催化剂在常温下对聚氨酯树脂反应几乎不起催化作用,但在100℃时可以加快聚氨酯树脂的反应速度,这样可以保证常温下采用聚氨酯树脂制备聚氨酯拉挤复合材料时拥有较长的适用期,高温时具有较快的固化成型速度。
所述消泡剂为有机硅消泡剂、聚合物消泡剂、有机氟消泡剂中的至少一种。其中,有机硅和聚合物消泡剂,可以使体系内的小气泡迅速聚集形成大气泡,在浮力作用下快速上升到表面,然后破裂。同时,有机硅、聚合物消泡剂还具有防止制品表面缺陷的功能。
所述除水剂为分子筛干燥剂、噁唑烷除水剂、碳化二亚胺除水剂中的至少一种。其中,碳化二亚胺类除水剂优选聚碳化二亚胺、N,N`-二环己基碳化二亚胺、1,3-二环己基碳化二亚胺中的至少一种。
所述抗静电剂,它通过离子化基团或极性基团的离子传导或吸湿作用,构成泄漏电荷通道,达到抗静电的目的,一是在塑料表面形成导电层,从而降低其表面电阻率,使已经产生的静电荷迅速泄漏;二是赋予塑料表面具有一定的润滑性,降低摩擦系数.从而抑制和减少静电荷的产生。所述的抗静电剂包括,阳离子型(季铵盐),阴离子型(磷酸盐、磺酸盐),非离子型(脂肪酸多元醇酯,据氧化乙烯加成物),两性型(甜菜碱类,内铵盐,丙氨酸盐)以及高分子型(聚丙烯酸衍生物,包括聚环氧乙烷、聚醚酯酰胺、含季铵盐的(甲基)丙烯酸酯共聚物和含亲水基的有机硅等),表面活性剂型抗静电剂加入,也提高了后续保护涂层的润湿和流平性。
可以,内脱模剂和静电剂二合一,为内脱模抗静电二合一添加剂。内脱模抗静电二合一添加剂可以是脂肪酸酯,可再生植物脂肪酸的乙氧基化烷基胺衍生,基于聚乙二醇脂肪酸酯的混合物,脂肪酸酰胺,阴离子(烷烃磺酸钠)和非离子化合物(乙氧基化烷基胺)的混合物,高单甘油单硬脂酸酯等。这类添加剂用作润滑剂、防粘连剂、滑爽剂和抗静电剂。对加工产生积极影响。它具有低挥发性和高相容性。赋予最终产品改进的流变特性、优化的机械输出和改进的表面光洁度。它将可能导致火灾或爆炸的放电风险降至最低。它可以减少影响复合材料产品性能和外观的灰尘积聚。改善运输、包装和储存过程中的操作。改善表面光洁度。防止由分离过程引起的表面缺陷。还通过减少摩擦和允许更有效的加工来改进注塑成型工艺。有助于最大限度地缩短周期时间并允许连续生产。
为了进一步改进加工性和最终复合材料的相应性能,还可加入阻燃剂。以提高材料的阻燃性。所述阻燃剂选自间苯二酚双膦酸脂、三(3-羟丙基)氧化膦、磷酸三乙酯、磷酸三丁酯、磷酸三异辛酯、磷酸铵、多聚磷酸盐、三聚氰胺、三聚氰胺盐、十溴二苯乙烷、溴代三甲基苯基氧化茚、五溴氯环己烷、1,2-双(四溴邻苯二甲酰亚胺)乙烷、四氯邻苯二甲酸酐、氟硅酸盐中的至少一种。进一步优选地,所述阻燃剂为磷酸三丁酯和氟硅酸盐的组合,质量比优选为(2-5):1。所述阻燃剂的添加量为5-20%。
为了进一步改进加工性和最终复合材料的相应性能,还可加入分散剂。所述分散剂为聚丙烯酰胺、羧甲基纤维素、聚乙烯蜡、聚丙烯-高分子二氧化硅共聚蜡中的任意一种。
为了进一步改进加工性和最终复合材料的相应性能,还可加入无机填料。所述无机填料选自包括但不限于滑石粉、高岭土、硅酸盐、长石、云母、硅灰石、碳酸钙、硫酸钡、氧化硅、氧化钛、氢氧化铝、氮化硼、氮化铝、玻璃微珠中的至少一种。优选,所述无机填料为碳酸钙和氢氧化铝的组合。其中,碳酸钙可以降低配方成本,氢氧化铝可以提高阻燃性。无机填料的添加量为5-35%。
为了进一步改进加工性和最终复合材料的相应性能,还可加入抗紫外线剂。所述抗紫外线剂为酯类、酮类、三嗪类、胺类中的一种或几种。抗紫外线剂抗紫外线助剂是通过吸收或反射紫外线的能量来保护塑料表面的材料。一般来说,它能够将紫外线分解为无害的热能,从而消除它对产品的危害。另外,抗紫外线助剂还可以在材料表面形成一层保护膜,起到遮挡和反射紫外线的作用。抗紫外线剂的在0.5-1.0%
为了进一步改进加工性和最终复合材料的相应性能,还可加入抗水解助剂等。抗水解助剂优选为双(2,6-二异丙基苯)碳二亚胺,其原理是与水解产物羧酸或水反应,阻止自催化水解的降解发生,提高聚合物的使用寿命,特别是高温潮湿及酸碱环境等苛刻条件下抗水解或耐水解稳定性能的提升,添加量为0.7-1.5%。
关于双组份聚氨酯树脂的制备方法
双组份聚氨酯树脂的制备方法,包括如下步骤:步骤1、按照所述重量份称取各原料,备用;步骤2、将聚合物多元醇、扩链剂混合后在110~120℃条件下进行真空脱水1.5~5小时进行真空脱水,冷却后加入内脱模剂、抗静电剂(或者,脱模抗静电二合一添加剂)、催化剂、消泡剂、除水剂,有其他添加剂的,在该处一并添加进来。以120~400r/min的速率进行搅拌30~400分钟至各组分混合均匀得到B料,采用静态混合器将作为A料的异氰酸酯与B料混合均匀,得到双组份聚氨酯树脂。
关于聚氨酯拉挤复合材料的制备方法
聚氨酯拉挤复合材料由双组份聚氨酯树脂和增强材料共混拉挤制备而成。具体制备方法如下:将待复合的增强材料浸入双组份聚氨酯树脂中以进行浸润得到复合初料,浸润时间为0.5~3分钟,之后将复合初料以1~5cm/s的速度通过具有三段温区的模具以进行固化,所述三段温区依次为温度为100℃的预热区、温度为140℃凝胶区、温度为150℃固化区,复合初料从预热区进入,经过凝胶区后从固化区输出得到聚氨酯拉挤复合材料。
复合初料进入模具预热区后,双组份聚氨酯树脂的温度逐渐升高,粘度逐渐下降,使增强材料进一步浸润在双组份聚氨酯树脂中,通过凝胶区时,双组份聚氨酯树脂受热发生交联反应,逐渐变硬,开始具有一定的强度,进入固化区后继续固化,并保证出模时达到一定的固化度。
待复合的增强材料为玻璃纤维、碳纤维、聚酯纤维、芳纶纤维、天然纤维、芳香族聚酰胺纤维、尼龙纤维、玄武岩纤维、硼纤维、碳化硅纤维、石棉纤维、晶须、硬质颗粒、金属纤维、高强高模聚乙烯纤维或其组合。优选,待复合的增强材料为玻璃纤维、碳纤维或芳纶纤维。
增强材料浸入双组份聚氨酯树脂前可以经预浸液改性,所述预浸液由硅烷偶联剂、具有至少一个c4-c18链且至少带一个极性基团的咪唑啉铵盐、溶剂组成。经过改性后的纤维提高了分散性和其与树脂的结合力,使复合材料的弹性模量被显著增强。
聚氨酯拉挤复合材料中增强材料的含量为80%以上。
性能测试:
双组份聚氨酯树脂的原料含量和重量份,如下表:
聚氨酯拉挤复合材料的原料以及制备出的聚氨酯拉挤复合材料的体积电阻率,如下表:
从上表中可以看出:
1.实施例1、实施例2、实施例3在均采用双组份聚氨酯树脂1的情况下,混合金属纤维后的体积电阻率小于碳纤维,小于玻璃纤维,故优选增强纤维为金属纤维。
2.实施例1、实施例4、实施例5、实施例6、实施例7在增强纤维形同的情况下,所采用的树脂不同,说明优选双组份聚氨酯树脂1下的原料组分。
本发明的聚氨酯拉挤复合材料可以通过静电喷涂的涂料涂覆。其中,适合的涂料包括各类可采用静电喷涂工艺的涂料(包括底漆和面漆),如溶剂型,无溶剂性,高固含的单组份,双组分或者多组分液体涂料以及低温粉末涂料等。当为水性涂料时,静电喷涂的涂料包括单组份水性聚氨酯涂料,双组分羟基丙烯酸-聚氨酯涂料、双组分氟碳涂料、水性氟烯烃-乙烯基醚涂料、聚偏氟乙烯涂料、水性单或双组分环氧涂料。当为溶剂型或高固含或无溶剂型涂料时,静电喷涂的涂料包括双组分羟基丙烯酸-聚氨酯涂料、双组分氟碳涂料、氟烯烃-乙烯基醚涂料、聚偏氟乙烯涂料、单或双组分环氧涂料。当为粉末涂料时,静电喷涂的涂料包括热塑性(如聚乙烯、聚丙烯、聚酯、聚氯乙烯、氯化聚醚、聚酰胺系、纤维素系、聚酯系,氟树脂粉末等。)和热固性两大类(如环氧树脂系、环氧-聚酯系、聚酯系、聚氨酯系、丙烯酸树脂系等)。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (10)
1.双组份聚氨酯树脂,其特征在于,包括以下重量份的原料:
2.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,所述内脱模剂和所述抗静电剂为二合一,为内脱模抗静电二合一添加剂;
所述内脱模抗静电二合一添加剂是脂肪酸酯、可再生植物脂肪酸的乙氧基化烷基胺衍生、基于聚乙二醇脂肪酸酯的混合物、脂肪酸酰胺或高单甘油单硬脂酸酯。
3.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,还包括阻燃剂。
4.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,还包括分散剂。
5.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,还包括无机填料。
6.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,还包括抗紫外线剂。
7.根据权利要求1所述的双组份聚氨酯树脂,其特征在于,还包括抗水解助剂。
8.双组份聚氨酯树脂的制备方法,其特征在于,包括如下步骤:
步骤1、按照权利要求1-7中任意一项所述的双组份聚氨酯树脂的原料的重量份称取各原料,备用;
步骤2、将聚合物多元醇、扩链剂混合后在110~120℃条件下进行真空脱水1.5~5小时进行真空脱水,冷却后加入内脱模剂、抗静电剂、催化剂、消泡剂、除水剂,以120~400r/min的速率进行搅拌30~400分钟至各组分混合均匀得到B料,采用静态混合器将作为A料的异氰酸酯与B料混合均匀,得到双组份聚氨酯树脂。
9.聚氨酯拉挤复合材料,其特征在于,由双组份聚氨酯树脂和增强材料共混拉挤制备而成。
10.聚氨酯拉挤复合材料的制备方法,其特征在于,将待复合的增强材料浸入双组份聚氨酯树脂中以进行浸润得到复合初料,浸润时间为0.5~3分钟,之后将复合初料以1~5cm/s的速度通过具有三段温区的模具以进行固化,所述三段温区依次为温度为100℃的预热区、温度为140℃凝胶区、温度为150℃固化区,复合初料从预热区进入,经过凝胶区后从固化区输出得到聚氨酯拉挤复合材料。
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