CN112812414B - 一种氟硅聚合物加工助剂母粒及其制备方法 - Google Patents
一种氟硅聚合物加工助剂母粒及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种氟硅聚合物加工助剂母料,以质量百分比计,包括以下组分:聚合物树脂40%‑60%、硅橡胶20%‑40%、抗氧剂0.2%‑2%、含氟聚合物5%‑25%、引发剂0.01%‑0.1%。本发明还公开了该氟硅聚合物加工助剂母粒的制备方法。与现有技术相比,本发明的氟硅聚合物加工助剂母料具有起效快、耐黄变性能好,在聚烯烃产品的加工时能有效改善制品外观、性能等优点。
Description
技术领域
本发明涉及高分子材料技术领域,具体涉及一种氟硅聚合物加工助剂母粒及其制备方法。
背景技术
在聚烯烃的挤出加工过程中,不论是有缺陷的外观还是频繁的停机清除模头结焦都是让人难以接受的,而含氟聚合物加工助剂PPA可以解决这些问题,但含氟聚合物加工助剂PPA要起到上述效果需在挤出机内部的腔体、模头表面与聚合物熔体间形成一层稳定的润滑层。而对于普通的含氟聚合物加工助剂PPA而言,这一稳定的润滑层形成至少需要1小时左右的时间,这段时间一般也被称之为起效时间,在这一稳定的润滑层形成前所生产的制品品质都会有瑕疵。同时,现有的普通含氟聚合物加工助剂PPA基本是通过聚乙二醇和含氟弹性体复配的方式得到,低分子量的聚乙二醇耐热性差,容易氧化分解,在长时间挤出加工过程中,模头处容易有结焦现象。
因此,如何找到一种新的加工助剂来解决目前含氟聚合物加工助剂PPA起效时间长、耐黄变性差、力学性能不佳的问题成为制得高性能塑料制品的关键。
发明内容
本发明所要解决的技术问题之一是:针对现有技术存在的不足,提供一种氟硅聚合物加工助剂母粒,将含氟聚合物与橡胶进行接枝反应对聚合物树脂基体进行协同改性,采用的含氟聚合物不仅具有柔顺的大分子链,优越加工性能,制得的母粒耐黄变性能好,起效快,力学性能好。
本发明所要解决的技术问题之二是,提供一种氟硅聚合物加工助剂母粒的制备方法,在加工前首先对含氟聚合物在一定温度下进行预处理,将含氟聚合物中的水分、低分子量组分挥发,有效改善了母粒的耐黄变性能,且该方法操作简单,对设备要求低。
为解决上述第一个技术问题,本发明采用的技术方案是:
一种氟硅聚合物加工助剂母粒,以质量百分比计,包括以下组分:
聚合物树脂40%-60%,
硅橡胶20%-40%,
抗氧剂0.2%-2%,
含氟聚合物5%-25%,
引发剂0.01%-0.1%。
作为上述技术方案的优选,所述聚合物树脂为EVA、LLDPE、LDPE、HDPE、ULDPE、XHDPE、XLLDPE、PP中的一种。
作为上述技术方案的优选,所述聚合物树脂的熔融指数为(1-10)g/10min。
作为上述技术方案的优选,所述抗氧剂为抗氧剂1010、抗氧剂1076、抗氧剂215、抗氧剂168、抗氧剂300、抗氧剂626、抗氧剂1098、抗氧剂3114中的一种或几种混合。
作为上述技术方案的优选,所述含氟聚合物是己内酯、含氟弹性体及界面分散剂的共聚物;所述共聚物是己内酯、含氟弹性体和界面分散剂的质量比为6:3:1的共聚物。
作为上述技术方案的优选,所述含氟聚合物是己内酯、含氟弹性体及界面分散剂的共聚物;所述界面分散剂为滑石粉、硅藻土、碳酸钙、二氧化硅中的一种或多种混合。
作为上述技术方案的优选,所述含氟弹性体是偏二氟乙烯与六氟丙烯的共聚物、偏二氟乙烯、六氟丙烯与四氟乙烯的三元共聚物、四氟乙烯、偏二氟乙烯与丙烯的三元共聚物中的一种或多种混合。
作为上述技术方案的优选,所述含氟聚合物的分子量1000-100000。
作为上述技术方案的优选,所述硅橡胶为二甲基硅橡胶、甲基乙烯基硅橡胶、甲基苯基乙烯基硅橡胶,所述硅橡胶的分子量为200000-2000000。
作为上述技术方案的优选,所述引发剂为过氧化二异丙苯.
为解决上述第二个技术问题,本发明采用的技术方案如下:
一种氟硅聚合物加工助剂母粒的制备方法,包括以下步骤:
(1)按质量百分比称取聚合物树脂、硅橡胶、抗氧剂、含氟聚合物和引发剂,并将含氟聚合物在烘箱中预处理30min-60min;
(2)将聚合物树脂、硅橡胶、含氟聚合物、抗氧剂在高速搅拌机或密炼机中混合1-10min,然后加入引发剂后再混合5-10min,制得混合物料;
(3)将步骤(2)制得的混合物料置于双螺杆挤出机中熔融挤出造粒,制得氟硅聚合物用加工助剂母粒。
作为上述技术方案的优选,所述双螺杆挤出机的长径比为40:1-52:1;所述挤出造粒时的条件为:各段温度如下:加料段40-60℃,输送段120-170℃,熔融段170-200℃,机头170-200℃,整个挤出过程的停留时间为1-3min,模头压力为4-14MPa,挤出机末端抽真空排气,排气真空度为-0.08MPa至-0.1MPa。
由于采用了上述技术方案,本发明的有益效果是:
本发明通过引发剂过氧化二异丙苯,将含氟聚合物、硅橡胶在双螺杆挤出机中进行反应接枝,形成氟硅大分子链。在聚烯烃的挤出加工过程中借助氟硅大分子链的柔顺性,能快速的形成连续的润滑涂层,很好的解决挤出过程中起效时间慢的问题。
与现有的含氟聚合物加工助剂相比,本发明制得的氟硅聚合物加工助剂有优越的耐黄变性能。本发明将含氟聚合物在烘箱中进行预处理,水份、低分子等组分挥发,使得加工助剂母料的耐黄变性能比现有含氟聚合物加工助剂有明显的提升。
具体实施方式
下面结合实施例进一步阐述本发明。应理解,这些实施例仅用于说明本发明而不用于限制本发明的范围。
实施例1
(1)按质量称取抗氧剂1010 1kg,抗氧剂168 1kg,甲基乙烯基硅橡胶23kg,LLDPE(熔指1g/10min,190℃)60kg,含氟聚合物15kg,过氧化二异丙苯0.01kg,将含氟聚合物在烘箱中150℃下预处理30min;
(2)将上述称取的LLDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂168依次放入高速搅拌机中搅拌3min,搅拌速率50rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌8min,得到混合物料;
(4)选用长径比为40:1的双螺杆挤出机,向上述双螺杆挤出机中加入步骤(3)制得的混合物料,并设置加料段温度60℃,输送段温度150℃,熔融段温度185℃,机头温度185℃,螺杆转速265rpm,模头压力为10MPa,挤出机末端抽真空,真空度为-0.08MPa;
(5)上述准备工作完毕,挤出造粒,制得母粒-1。
实施例2
(1)按质量称取抗氧剂1010 0.5kg,抗氧剂168 1.5kg,甲基乙烯基硅橡胶38kg,LLDPE(熔指1g/10min,190℃)40kg,含氟聚合物20kg,过氧化二异丙苯0.01kg,将含氟聚合物在烘箱中160℃下预处理60min;
(2)将上述称取的LLDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂168依次放入高速搅拌机中搅拌4min,搅拌速率50rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌10min后得到混合物料;
(4)选用长径比为52:1的双螺杆挤出机,并将上述制得的混合物料加入到双螺杆挤出机中,设置加料段温度55℃,输送段温度145℃,熔融段温度180℃,机头温度180℃,螺杆转速300rpm,模头压力为10MPa,挤出机末端抽真空,真空度为-0.1MPa;
(5)上述准备工作完毕,挤出造粒,制得母粒-2。
实施例3
(1)按质量称取抗氧剂1076 0.5kg,抗氧剂168 0.5kg,抗氧剂3114 0.5kg,甲基乙烯基硅橡胶36kg,LLDPE(熔指5g/10min,190℃)47.5kg,含氟聚合物15kg,过氧化二异丙苯0.01kg,将含氟聚合物在烘箱中165℃下预处理40min;
(2)将上述称取的LLDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1076、抗氧剂168、抗氧剂3114依次放入密炼机中60℃下密炼4min,密炼机速率50rpm;
(3)开启密炼机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为50:1的双螺杆挤出机,将上述制得的混合物料加入到双螺杆挤出机中,设置加料段温度50℃,输送段温度145℃,熔融段温度185℃,机头温度185℃,螺杆转速250rpm,模头压力为8MPa,挤出机末端抽真空,真空度为-0.08MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-3。
实施例4
(1)按质量称取抗氧剂1076 0.5kg,抗氧剂168 1.0kg,甲基乙烯基硅橡胶38kg,LDPE(熔指1g/10min,190℃)40kg,含氟聚合物20.5kg,过氧化二异丙苯0.01kg,将含氟聚合物在烘箱中155℃下预处理30min;
(2)将上述称取的LDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1076、抗氧剂168依次放入密炼机中60℃密炼5min,密炼机速率50rpm;
(3)开启密炼机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,将上述制得的混合物料加入到双螺杆挤出机中,设置加料段温度50℃,输送段温度145℃,熔融段温度190℃,机头温度190℃,螺杆转速250rpm,模头压力为8MPa,挤出机末端抽真空,真空度为-0.1MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-4。
实施例5
(1)按质量称取抗氧剂1076 1.0kg,抗氧剂618 0.5kg,抗氧剂1098 0.5kg,甲基乙烯基硅橡胶25kg,LDPE(熔指3g/10min,190℃)48kg,含氟聚合物25kg,过氧化二异丙苯0.02kg,将含氟聚合物在烘箱中155℃下预处理45min;
(2)将上述称取的LDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1076、抗氧剂618、抗氧剂1098依次放入密炼机中55℃密炼7min,密炼机速率50rpm;
(3)开启密炼机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,将上述制得的混合物料加入到双螺杆挤出机中,设置加料段温度55℃输送段温度155℃,熔融段温度200℃,机头温度200℃,螺杆转速300rpm,模头压力为8MPa,挤出机末端抽真空,真空度为-0.1MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-5。
实施例6
(1)按质量称取抗氧剂215 0.5kg,抗氧剂168 0.5kg,抗氧剂1098 0.5kg,甲基乙烯基硅橡胶23.5kg,LLDPE(熔指8g/10min,190℃)55kg,含氟聚合物20kg,过氧化二异丙苯0.02kg,将含氟聚合物在烘箱中155℃下预处理45min;
(2)将上述称取的LLDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂3114、抗氧剂168、抗氧剂1098依次放入高速搅拌机中搅拌4min,搅拌速率40rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,加入上述制得的混合物料,设置加料段温度55℃,输送段温度145℃,熔融段温度190℃,机头温度200℃,螺杆转速200rpm,模头压力为12MPa,挤出机末端抽真空,真空度为-0.1MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-6。
实施例7
(1)按质量称取抗氧剂1010 0.5kg,抗氧剂618 0.5kg,抗氧剂3114 0.5kg,甲基乙烯基硅橡胶27.5kg,LLDPE(熔指10g/10min,190℃)56kg,含氟聚合物15kg,过氧化二异丙苯0.05kg,并将含氟聚合物在烘箱中160℃下预处理50min;
(2)将上述称取的LLDPE、甲基乙烯基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂618、抗氧剂3114依次放入高速搅拌机中搅拌4min,搅拌速率40rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,加入上述制得的混合物料,设置加料段温度50℃,输送段温度155℃,熔融段温度200℃,机头温度200℃,螺杆转速300rpm,模头压力为14MPa,挤出机末端抽真空,真空度为-0.09MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-7。
实施例8
(1)按质量称取抗氧剂1076 1.0kg,抗氧剂168 0.5kg,二甲基硅橡胶30kg,PP(熔指10g/10min,190℃)48.5kg,含氟聚合物20kg,过氧化二异丙苯0.05kg,将含氟聚合物在烘箱中160℃下预处理50min,;
(2)将上述称取的PP、二甲基硅橡胶、含氟聚合物、抗氧剂1076、抗氧剂168依次放入高速搅拌机中搅拌4min,搅拌速率40rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,加入上述制得的混合物料,设置加料段温度60℃,输送段温度160℃,熔融段温度190℃,机头温度190℃,螺杆转速350rpm,模头压力为6MPa,挤出机末端抽真空,真空度为-0.09MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-8。
实施例9
(1)按质量称取抗氧剂1010 0.5kg,抗氧剂168 0.5kg,二甲基硅橡胶30kg,XHDPE44kg、含氟聚合物25kg,过氧化二异丙苯0.05kg,将含氟聚合物在烘箱中155℃下预处理45min;
(2)将上述称取的XHDPE、二甲基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂168依次放入高速搅拌机中搅拌4min,搅拌速率40rpm;
(3)开启高速搅拌机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,加入上述制得的混合物料,设置加料段温度60℃,输送段温度160℃,熔融段温度190℃,机头温度190℃,螺杆转速350rpm,模头压力为8MPa,挤出机末端抽真空,真空度为-0.09MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-9。
实施例10
(1)按质量称取抗氧剂1010 1.0kg,抗氧剂168 0.5kg,甲基苯基乙烯基硅橡胶28.5kg,XHDPE 60kg、含氟聚合物10kg,过氧化二异丙苯0.08kg,将含氟聚合物在烘箱中155℃下预处理45min;
(2)将上述称取的XHDPE、甲基苯基乙烯基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂168依次放入密炼机中55℃密炼7min,密炼机速率40rpm;
(3)开启密炼机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,并加入上述制得的混合物料,设置加料段温度60℃,输送段温度160℃,熔融段温度190℃,机头温度190℃,螺杆转速350rpm,模头压力为10MPa,挤出机末端抽真空,真空度为-0.09MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-10。
实施例11
(1)按质量称取抗氧剂1010 1.0kg,抗氧剂168 0.5kg,甲基苯基乙烯基硅橡胶35.5kg,EVA 58kg,含氟聚合物5kg,过氧化二异丙苯0.1kg,将含氟聚合物在烘箱中155℃下预处理65min;
(2)将上述称取的EVA、甲基苯基乙烯基硅橡胶、含氟聚合物、抗氧剂1010、抗氧剂168依次放入密炼机中55℃密炼10min,密炼机速率40rpm;
(3)开启密炼机密封盖,加入过氧化二异丙苯,继续搅拌5min后得到混合物料;
(4)选用长径比为42:1的双螺杆挤出机,并加入上述制得的混合物料,设置加料段温度60℃,输送段温度160℃,熔融段温度190℃,机头温度190℃,螺杆转速350rpm,模头压力为6MPa,挤出机末端抽真空,真空度为-0.1MPa;
(5)上述准备工作完毕,挤出造粒,得到母粒-11。
应用实施例:
将上述实施例1-实施例11制得的母料应用在聚乙烯薄膜体系中,配方如表1所示,采用的聚乙烯LLDPE 1001AV(美国埃克森美孚化工提供)。
表1
将上述聚乙烯、母粒、抗氧剂168在高速搅拌机中混合5分钟,高速搅拌机的搅拌转速为400转/分;将混合好的物料通过长径比为28:1的FBSI-25/28吹膜机进行吹膜,工艺参数为:一区160℃、二区175℃、三区195℃、四区-六区195℃、过渡体区195℃、模头温度195℃,吹膜数据如表2所示;薄膜的性能如表3所示。其中,母料粒径按GB/T 27596-2011标准进行检验;耐黄变温度按HG/T 3689-2014标准进行检验;拉伸强度按ASTM D-638标准进行检验;透光率和雾度按GB/T 2410-2008标准进行检验;透射率按HG/T 5077-2016标准进行检验;光泽度按ASTM D2457进行检验;起效时间是指开机后至螺杆机的主机电流呈现稳定值的时间,开机后越短的时间内达到稳定电流值,说明起效时间短、起效快。
表2
从表2测试结果可以看出,用本发明所制备的氟硅聚合物加工助剂母料在聚乙烯体系进行吹膜试验时,与空白样相比较,各个实验组在添加母粒后,起效时间、熔体压力、主机电流均呈现明显下降趋势,模头结焦情况有所改善。分析其原因,主要在于:氟硅聚合物加工助剂母料借助氟硅分子链的柔顺性和优异的改善加工特性,在腔体、模口处快速的形成连续的润滑涂层,很好的解决熔体压力高、主机电流大、模头结焦、黑点等问题。氟硅聚合物加工助剂母料在聚合物加工树脂中能够形成连续、均匀的低表面能聚合物“涂层”结构,可以使被加工的聚合物畅通地滑过界面,明显降低加工时的剪切应力,从而对树脂加工性能、产品质量、能源消耗、生产效率、机械磨损都有不同程度的改善。与现有技术相比,本发明的氟硅聚合物加工助剂母料具有起效时间快、耐黄变温度性能优异、添加量少等特点。
表3
从表3可以看到,本发明所制备的氟硅聚合物加工助剂母料添加到聚乙烯体系中,与空白样相比较,各个实验组在添加母粒后,拉伸强度有明显的提升。在雾度方面,采用本发明母粒的实验组低于空白样,而体系的透光率、透射率及光泽度方面均有明显的上升,其中透光率提2%以上,光泽度提升40%左右。分析其原因主要在于:本发明制得的氟硅聚合物加工助剂母料借助氟硅分子链的柔顺性和易于析出流平成膜的特性,提高农膜表面光泽度、透光率、透射率,提高产品拉伸强度,稳定产品质量。
此外,应理解上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。
Claims (8)
2.根据权利要求1所述的一种氟硅聚合物加工助剂母粒,其特征在于:所述聚合物树脂的熔融指数为(1-10)g/10min。
3.根据权利要求1所述的一种氟硅聚合物加工助剂母粒,其特征在于:所述抗氧剂为抗氧剂1010、抗氧剂1076、抗氧剂215、抗氧剂168、抗氧剂300、抗氧剂626、抗氧剂1098、抗氧剂3114中的一种或几种混合。
4.根据权利要求1所述的一种氟硅聚合物加工助剂母粒,其特征在于:所述含氟聚合物的分子量1000-100000。
5.根据权利要求1所述的一种氟硅聚合物加工助剂母粒,其特征在于:所述硅橡胶的分子量为200000-2000000。
6.根据权利要求1所述的一种氟硅聚合物加工助剂母粒,其特征在于:所述引发剂为过氧化二异丙苯。
7.根据权利要求1至6任一所述的一种氟硅聚合物加工助剂母粒的制备方法,其特征在于,包括以下步骤:
(1)按质量百分比称取聚合物树脂、硅橡胶、抗氧剂、含氟聚合物和引发剂,并将含氟聚合物在烘箱中预处理30min-60min;
(2)将聚合物树脂、硅橡胶、含氟聚合物、抗氧剂在高速搅拌机或密炼机中混合1-10min,然后加入引发剂后再混合5-10min,制得混合物料;
(3)将步骤(2)制得的混合物料置于双螺杆挤出机中熔融挤出造粒,制得氟硅聚合物用加工助剂母粒。
8.根据权利要求7所述的一种氟硅聚合物加工助剂母粒的制备方法,其特征在于:所述双螺杆挤出机的长径比为40:1-52:1;所述挤出造粒时的条件为:各段温度如下:加料段40-60℃,输送段120-170℃,熔融段170-200℃,机头170-200℃,整个挤出过程的停留时间为1-3min,模头压力为4-14MPa,挤出机末端抽真空排气,排气真空度为-0.08MPa至-0.1MPa。
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