CN111363317A - 车灯反射镜用高耐热高光泽pbt复合材料及其制备方法 - Google Patents
车灯反射镜用高耐热高光泽pbt复合材料及其制备方法 Download PDFInfo
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- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 24
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- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical class O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 18
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Abstract
本发明公开一种车灯反射镜用高耐热高光泽PBT复合材料及其制备方法,PBT复合材料包含以下重量百分比的组份:57.2‑88.9wt%的PBT、5‑20wt%的PET、5‑20wt%的硅酸钙、0‑10wt%的偶合剂改质滑石粉、0.1‑0.3wt%的抗氧化剂,0.5‑1.5wt%的流动助剂以及0.5‑1.0wt%的成核剂;其制备方法是将各原料成分加入到押出机后进行熔融塑化,通过押出机模头挤出后水冷拉条造粒,得到具有出色的耐热性和良好的表面光泽性的PBT复合材料,适用于制作具备高耐热高光泽的车灯反射镜。
Description
技术领域
本发明涉及一种高耐热高光泽PBT复合材料,特别是一种适用于制作具备高耐热高光泽的车灯反射镜的PBT复合材料。
背景技术
汽车的车灯由灯座、灯泡、反射镜、装饰圈和配光镜组成。而且,车灯分照明灯(大灯、雾灯及倒车灯)和信号灯(转弯信号灯、警示灯及尾灯)。不同车灯需要具备的耐热程度不同,故对于材料的选择要求也不同。其中,为满足大灯与雾灯为点灯功率最高的需求,这两个车灯的材料应具有较高的耐热性,而车灯的反射镜为车灯内受热温度最高的塑料部件,则必须兼具良好的耐热性与表面光泽性。
制造车灯的材料,为避免车灯因频繁使用导致短时间温度超过120度,致使灯体变形,影响车灯的安全使用,现有技术采用以PC、PC/ABS材料为主制造车灯。但是,近年随着不同车型的车灯温度的升高,制造车灯的传统材料,已汰换为价格昂贵的耐热的PPS、PEI等树脂,而汽车制造业却基于降低成本的考虑,又逐渐发展采用PBT复合材料取代PPS、PEI树脂制作新型的汽车车灯。
发明内容
有鉴于此,本发明的主要目的在于提供一种PBT复合材料,适用于制作具备高耐热高光泽的车灯反射镜,基于材料的总重量,PBT复合材料包含以下成份且各成分的总和为100wt%:
1. 57.2-88.9wt%的PBT;
2. 5-20wt%的PET;
3. 5-20wt%的硅酸钙;
4. 0-10wt%的偶合剂改质滑石粉;
5. 0.1-0.3wt%的抗氧化剂;
6. 0.5-1.5wt%的流动助剂;及
7. 0.5-1.0wt%的成核剂。
本发明的PBT复合材料,保持了PBT良好的加工性、耐低温性、耐候性、耐化学品性,且改善了PET的结晶性和成型加工性,尤其是兼具有出色的耐热性和良好的表面光泽性。
本发明的另一主要目的在于提供一种高耐热高光泽的PBT复合材料的制备方法,包括以下步骤:
步骤一、按上述所述的重量百分比称取各个组分;
步骤二、将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌10-20分钟,放入押出机主进料斗中;
步骤三、将硅酸钙和滑石粉按比例混合后,放入混料机中搅拌5-10分钟,放入押出机侧进料斗中;
步骤四、经双螺杆押出机熔融挤出,造粒,制得PBT复合材料;押出机的螺杆长度(L)及螺杆直径(D)的L/D的比值介于30-52;双螺杆押出机的加热条件,设定五个温度加热区:第一区温度为210-230℃,第二区温度为230-250℃,第三区温度为230-265℃,第四区温度为230-260℃,第五区温度为230-265℃,螺杆转速200-350rpm。
本发明的PBT复合材料具有下列的有益功效:
1.具有出色的耐热性和良好的表面光泽性;
2.在真空镀铝时无需喷涂底漆,可直接进行金属蒸镀处理,进一步降低了加工成本。
3.在流动性方面进行了改进,可以制造出更薄的反射镜,带来更短的加工周期时间。
为使能更进一步了解本发明的特征及技术内容,请参阅以下有关本发明的详细说明。
具体实施方式
为了使本发明的技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
本发明的PBT复合材料,适用于制作具备高耐热高光泽的车灯反射镜,基于材料的总重量,PBT复合材料包含以下成份且各成分的总和为100wt%:
1. 57.2-88.9wt%的PBT;
2. 5-20wt%的PET;
3. 5-20wt%的硅酸钙;
4. 0-10wt%的偶合剂改质滑石粉;
5. 0.1-0.3wt%的抗氧化剂;
6. 0.5-1.5wt%的流动助剂;及
7. 0.5-1.0wt%的成核剂。
其中,所述PBT的功能是作为主料,在机械强度及流动性起主导主用。所述PET的功能是作为辅助底料,在材料耐热性上有辅助效果。无机填料为硅酸钙与偶合剂处理的滑石粉,其功能是增加材料的机械性能、提升材料的耐热、抗翘曲能力及提升材料表面的光泽度。抗氧化剂的功能是减少材料在加工过程中的氧化。流动助剂的功能是减少料与料之间的摩擦,并提升产品表面光泽性。成核剂的功能是完善和提升PET的结晶效果和结晶速度,提升材料的耐热性能。
在下述各个具体实施例中,PBT优选的相对密度为1.30-1.35g/cm3,熔点为220-230℃,特性黏度(IV)为0.85-1.2dL/g。来源可购自商业上的中国台湾长春或日本三菱公司的市售商品。
PET优选的相对密度为1.35-1.40g/cm3,熔点为250-260℃,其特性黏度(IV)为0.65-0.85dL/g。来源可购自商业上的中国台湾南亚或力丽公司的市售商品。
无机填料优选为硅酸钙与偶合剂处理的滑石粉按1:0.25至1:1.5的含量比例混合。硅酸钙优选平均粒径3-8μm,滑石粉优选平均粒径1-4μm。
所述偶合剂处理的滑石粉是取98.5wt%的滑石粉和1.5wt%的硅烷偶合剂或钛酸酯偶合剂,经过10-60分钟的高速搅拌而制成。
抗氧化剂选自四(3,5-二叔丁基-4-羟基)苯丙酸季戊四醇酯、三(2,4-二叔丁基)亚磷酸苯酯及3-(3,5-二叔丁基-4-羟基苯基)丙酸正十八烷醇酯中的一种或者几种混合而成。(市售型号1010、BASF 168、BASF 1076等)。
流动助剂选自二甲基硅氧烷与聚酯共聚物或邻苯二甲酸系聚酯中的一种(市售型号TEGOMER H-Si 6441P、DIC A55等)。
成核剂选自由长链线型饱和羧酸钠盐、长链线型饱和羧酸钙盐和芳香族羧酸金属钠盐或镁盐中的一种以上。
实施例1
本实施例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 89wt%、PET 5wt%、硅酸钙5wt%、抗氧化剂0.3wt%、流动助剂0.5wt%及成核剂0.2wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌10分钟,放入押出机主进料斗中。硅酸钙放入押出机侧进料斗中,再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为210℃,第二区温度为240℃,第三区温度为250℃,第四区温度为250℃,第五区温度为255℃,螺杆转速200rpm。
实施例2
本实施例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 78.8wt%、PET 10wt%、硅酸钙10wt%、抗氧化剂0.3wt%、流动助剂0.5wt%及成核剂0.4wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌12分钟,放入押出机主进料斗中。硅酸钙放入押出机侧进料斗中,再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为220℃,第二区温度为245℃,第三区温度为250℃,第四区温度为255℃,第五区温度为260℃,螺杆转速为250rpm。
实施例3
本实施例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 63.1wt%、PET 15wt%、硅酸钙20wt%、抗氧化剂0.3wt%、流动助剂1wt%及成核剂0.6wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌15分钟,放入押出机主进料斗中。硅酸钙放入押出机侧进料斗中,再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为230℃,第二区温度为250℃,第三区温度为255℃,第四区温度为255℃,第五区温度为260℃,螺杆转速为300rpm。
实施例4
本实施例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 62.9wt%、PET 15wt%、硅酸钙10wt%、偶合剂改质的滑石粉10wt%、抗氧化剂0.3wt%、流动助剂1wt%及成核剂0.8wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌12分钟,放入押出机主进料斗中。将硅酸钙和滑石粉按比例混合后,放入混料机中搅拌8分钟,放入押出机侧进料斗中。再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为230℃,第二区温度为250℃,第三区温度为245℃,第四区温度为245℃,第五区温度为260℃,螺杆转速为350rpm。
实施例5
本实施例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 57.2wt%、PET 20wt%、硅酸钙15wt%、偶合剂改质的滑石粉5wt%、抗氧化剂0.3wt%、流动助剂1.5wt%及成核剂1.0wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌12分钟,放入押出机主进料斗中。将硅酸钙和滑石粉按比例混合后,放入混料机中搅拌5分钟,放入押出机侧进料斗中。再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为230℃,第二区温度为250℃,第三区温度为245℃,第四区温度为250℃,第五区温度为260℃,螺杆转速为350rpm。
比较例1
本比较例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 58.1wt%、PET 15wt%、PC 5wt%、硅酸钙20wt%、抗氧化剂0.3wt%、流动助剂1wt%及成核剂0.6wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、PC、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌15分钟,放入押出机主进料斗中。硅酸钙放入押出机侧进料斗中,再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为230℃,第二区温度为255℃,第三区温度为260℃,第四区温度为260℃,第五区温度为265℃,螺杆转速为300rpm。
比较例2
本比较例的车灯反射镜用高耐热高光泽PBT复合材料,由下述重量份数的原料制成:
PBT 63.7wt%、PET 15wt%、硅酸钙10wt%、玻璃纤维10wt%、抗氧化剂0.3wt%、流动助剂1.0wt%及成核剂0.8wt%。
其制备方法如下:
按重量份数称取上述原料,将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌12分钟,放入押出机主进料斗中。将硅酸钙和玻璃纤维按比例混合后,放入混料机中搅拌5分钟,放入押出机侧进料斗中。再经过双螺杆押出机挤出,造粒。其中押出机的双螺杆分成五个区段温度:第一区温度为230℃,第二区温度为250℃,第三区温度为245℃,第四区温度为245℃,第五区温度为260℃,螺杆转速为350rpm。
性能测试及评价:
将上述实施例1-5及比较例1-2制备的粒子物料在鼓风干燥箱中110-120℃干燥4小时,然后再将干燥好的粒子材料在射出机上进行射出成型制样,射出成型模温控制在80-100℃。测试所处的室温环境为23℃,根据下述方法进行物性评估:
1.拉伸强度:
按ASTM D638标准进行检验。试样尺寸(mm):(165±2)×(19±0.2)×(3.2±0.2),拉伸速度为50mm/min。
2.弯曲强度和弯曲模数:
按ASTM D790标准进行检验。试样类型试样尺寸(mm):(127±2)×(12.7±0.2)×(3.2±0.2),弯曲速度为13mm/min。
3.缺口冲击强度:
按ASTM D256标准进行检验。试样尺寸(mm):(63.5±2)×(12.7±0.2)×(3.2±0.2);缺口角度45±1°,半径0.25±0.12mm,缺口深度10.16±0.05mm。
4.热变形温度:
按ASTM D648标准进行检验。试样尺寸(mm):(127±2)×(12.7±0.2)×(3.2±0.2);升温速率为120℃/hr,压力为1.82MPa(4.6kg/cm2),设定形变量为0.254mm。
5.光泽度测试:
按ASTM D2457,测试选用60°角,试样尺寸为100×100×2mm。
下表1列出了本发明的PBT复合材料的多个实施例与比较例。通过对实施例1-5及比较例1-2所制备的复合材料,进行成型,对比分析:
1.比较例1与实施例3相比,比较例1的PBT复合材料导入PC材料表面光泽性提升,但热变形温度却下降过多,不适合用于制作具备高耐热高光泽的车灯反射镜,;
2.比较例2与实施例1-5相比,比较例2的PBT复合材料导入玻璃纤维,PC材料表面的表面光泽度远优于比较例2的成型制件;
3.通过对以上分析,本发明所制备的复合材料,以特定的量掺合偶合剂处理的滑石粉与硅酸钙有效提升热性质(实施例4的热变形温度达186℃),导入流动助剂有效提升表面光泽性(实施例5的光泽度达99.2%),以特定的量掺合PBT树脂与PET树脂,车灯反射镜的机械性能、耐热性及表面光泽性可获得改善。
表1实施例1-5及比较例1-2的原料的重量组成及材料性能测试数据
以上所公开的内容仅为本发明的优选可行实施例,并非因此局限本发明的权利要求书的保护范围,所以凡是运用本发明说明书内容所做的等效技术变化,均包含于本发明的权利要求书的保护范围内。
Claims (9)
1.一种车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,基于PBT复合材料的总重量,所述车灯反射镜用高耐热高光泽PBT复合材料包含以下成份:
1)57.2-88.9wt%的PBT;
2)5-20wt%的PET;
3)5-20wt%的硅酸钙;
4)0-10wt%的偶合剂改质滑石粉;
5)0.1-0.3wt%的抗氧化剂;
6)0.5-1.5wt%的流动助剂;及
7)0.5-1.0wt%的成核剂。
2.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述PBT的相对密度为1.30-1.35g/cm3,熔点为220-230℃,其特性黏度(IV)为0.85-1.2dL/g。
3.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述PET的相对密度为1.35-1.40g/cm3,熔点为250-260℃,其特性黏度(IV)为0.65-0.85dL/g。
4.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述硅酸钙与所述偶合剂改质滑石粉按1:0.25至1:1.5的含量比例混合;所述硅酸钙的平均粒径为3-8μm,所述偶合剂改质滑石粉的平均粒径为1-4μm。
5.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述偶合剂改质滑石粉是取98.5wt%的滑石粉和1.5wt%的硅烷偶合剂或钛酸酯偶合剂,经过10-60分钟的高速搅拌而制成。
6.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述抗氧化剂选自四(3,5-二叔丁基-4-羟基)苯丙酸季戊四醇酯、三(2,4-二叔丁基)亚磷酸苯酯及3-(3,5-二叔丁基-4-羟基苯基)丙酸正十八烷醇酯中的一种以上。
7.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述流动助剂选自二甲基硅氧烷与聚酯共聚物及邻苯二甲酸系聚酯中的一种以上。
8.根据权利要求1所述的车灯反射镜用高耐热高光泽PBT复合材料,其特征在于,所述成核剂选自长链线型饱和羧酸钠盐、长链线型饱和羧酸钙盐和芳香族羧酸金属钠盐或镁盐中的一种以上。
9.一种根据权利要求1至8中任一项所述的车灯反射镜用高耐热高光泽PBT复合材料的制备方法,其特征在于,所述制备方法包括以下步骤:
步骤一、称取PBT、PET、抗氧化剂、流动助剂及成核剂各个组分的重量百分比;
步骤二、将PBT、PET、抗氧化剂、流动助剂及成核剂按比例混合后,放入高速混料机中搅拌10-20分钟,放入押出机主进料斗中;
步骤三、将硅酸钙和偶合剂改质滑石粉按比例混合后,放入混料机中搅拌5-10分钟,放入押出机侧进料斗中;
步骤四、经双螺杆押出机熔融挤出,造粒,制得PBT复合材料;双螺杆押出机的加热条件,设定五个温度加热区:第一区温度为210-230℃,第二区温度为230-250℃,第三区温度为230-265℃,第四区温度为230-260℃,第五区温度为230-265℃,螺杆转速200-350rpm。
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WO2002092688A1 (fr) * | 2001-04-26 | 2002-11-21 | Mitsubishi Rayon Co., Ltd. | Composition de resine de polyester thermoplastique et reflecteurs de lumiere fabriques a partir de cette composition |
CN101724229A (zh) * | 2008-10-16 | 2010-06-09 | 上海红京印实业有限公司 | 一种车灯用极高耐热聚酯合金及其制备方法 |
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