CN102020833A - 高成型速率、高流动的增强阻燃聚酯及其生产方法 - Google Patents
高成型速率、高流动的增强阻燃聚酯及其生产方法 Download PDFInfo
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Abstract
本发明公开了一种高成型速率、高流动的增强阻燃聚酯及其生产方法,由包括半结晶性热塑性聚酯、主阻燃剂、阻燃协效剂、增韧剂、低粘环状聚酯、抗氧剂、成核剂、润滑剂、填充改性剂、其它助剂制成。本发明高成型速率高流动的增强阻燃聚酯具有快速的成型周期、高流动性、脱模效力高、节能、机械性能好等优点。
Description
技术领域
本发明涉及一种阻燃聚酯及其生产方法。
背景技术
热塑性增强阻燃聚酯PBT聚对苯二甲酸丁二酯)因其良好的电绝缘性能被广泛用于电子、电器行业。随着制造水平的提高,电子、电器产品的小型化,搭载在上面的电子元器件产品也面临着小型化、轻量化和薄壁化的趋势,工程塑料PBT做为零部件的外壳使用时要求也越来越小和薄,比如说在制作继电器外壳与电容器外壳时,要求注塑周期短,注塑速度快,注塑能力强,一模可出几十甚至上百个小型、薄壁制件,通常的阻燃聚酯材料不具备如此高的流动性和快速的脱模能力。
发明内容
本发明的目的在于提供一种适合快速注塑成型及薄壁化的具有高成型速率、高流动的增强阻燃聚酯及其生产方法。
本发明的技术解决方案是:
一种高成型速率、高流动的增强阻燃聚酯,其特征是:以重量份数计,由包括下列重量份的组分制成:
半结晶性热塑性聚酯 100份
主阻燃剂 10-40份
阻燃协效剂 3-20份
增韧剂 0-30份
低粘环状聚酯 0.1-30份
抗氧剂 0.1-5.0份
成核剂 0.1-2.0份
润滑剂 0.2-8.0份
填充改性剂 0-160份
其它助剂 0-10.0份。
所述的半结晶性热塑性聚酯是聚对苯二甲酸丁二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸-1,4-环己烷二甲酯中的一种;
所述主阻燃剂为溴化环氧、十溴二苯乙烷、溴化聚碳、溴化聚苯、聚溴化苯乙烯、三-(三溴苯氧基)-三嗪、聚溴化五溴苄基酯、磷(膦)氮系阻燃剂中的一种或几种;
所述的阻燃协效剂为三氧化二锑、锑酸钠、五氧化二锑中的一种或几种;
所述的增韧剂为橡胶类弹性体、核-壳类冲击改性剂、二元或三元烯烃类共聚物、烯烃类接枝改性共聚物中的一种或几种;
所述的低粘环状聚酯为对苯二甲酸环丁二醇酯树脂;
所述的抗氧剂包括主抗氧剂和辅助抗氧剂,主抗氧剂为酚类抗氧剂,辅助类抗氧剂为亚磷酸酯类抗氧剂;
所述的成核剂为有机和无机成核剂的混和物(如德国公司的Clariant公司生产的P250);
所述的润滑剂为季戊四醇硬脂酸酯、超高分子量的固态硅氧烷产品、氧化聚乙烯蜡、德国COGNIS公司LOXIOL EP861中的一种或几种;
所述的填充改性剂为玻璃纤维、玻璃微珠、玻璃矿物纤维、碳纤维、云母、高岭土、碳酸钙、硫酸钙、硫酸钡、滑石粉、硅酸钙、晶须中的一种或多种;
所述的其它助剂为抗滴落剂聚四氟乙烯(即4F)、色母粒中的一种或几种。
磷(膦)氮系阻燃剂是MPP、MC、EXOLIT OP 1240、RDP;橡胶类弹性体为EPDM、POE;核-壳类冲击改性剂为MBS、SBS。
一种高成型速率、高流动的增强阻燃聚酯,由包括下列重量份的组分制成:
半结晶性热塑性聚酯 100份
主阻燃剂 14-30份
阻燃协效剂 4-15份
增韧剂 2-20份
低粘环状聚酯 0.1-14份
抗氧剂 0.1-1.5份
成核剂 0.5-1.4份
润滑剂 0.5-3.0份
玻璃纤维 0-80份
其它助剂 0-5.0份;
所述的半结晶性聚酯是聚对苯二甲酸丁二醇酯,密度为1.31-1.35g/cm3,粘度为0.7-1.2d1/g,熔融温度220-230℃;
所述的主阻燃剂为溴化环氧、聚溴化五溴苄基酯(如死海溴公司的FR1025)中的一种或二种;
所述的阻燃协效剂为三氧化二锑;
所述的增韧剂为核壳类抗冲改性剂;
所述的抗氧剂为主抗氧剂1010或抗氧剂168;
所述的玻璃纤维直径为5-20微米,是经过复合偶联剂处理的玻纤。
所述核壳类抗冲改性剂为美国罗姆哈斯公司生产的MBS或二元烯烃类共聚物(如法国阿科码公司35BA40)。
所述的半结晶性聚酯聚对苯二甲酸丁二醇酯,其粘度为0.75-0.85dl/g。
一种高成型速率、高流动的增强阻燃聚酯的生产方法,其特征是:将半结晶性聚酯、主阻燃剂、阻燃协效剂、增韧剂、抗氧剂、成核剂、润滑剂、低粘环状聚酯和其它助剂按重量组分配比,在高速混和机中混和均匀以后,送入双螺杆挤出机中的主喂料中,填充改性剂随后在侧向喂料中加入,经挤出、冷却、切粒、干燥、包装而制成。
双螺杆挤出机螺杆的长径比为25-50∶1,螺杆设定温度为180-240℃,螺杆转速设定为200-600转/分。
本发明高成型速率高流动的增强阻燃聚酯具有如下几个优点
1、快速的成型周期。为了提高PBT产品的结晶度,加快成型速度,缩短成型周期,本发明中添加了兼具有机和无机成核能力的成熟产品,如德国公司的Clariant公司生产的P250,可使成型周期由15S缩短为13S,在相同时间内可多生产15%以上的产品。
2、高流动性。本发明中的聚酯材料具有非常好的流动性,可完成薄壁制件的注塑,充模充分,厚度可达0.3mm以下。主要是以对苯二甲酸环丁二醇酯树脂(CBT树脂)为主,辅代以低粘度的PBT树脂和具有内外润滑功能的润滑剂(如LOXIOL EP861)来实现的。
CBT树脂在常温下为固态,190℃时它就会变得象水一样的液体(相同条件下,其粘度仅为PBT的万分之二),这将非常有利于快速和极佳地润湿填料/纤维增强材料,并可在很低的压力下成型。极少的添加量就可大幅提高树脂的流动性,而几乎不影响力学性能,同时还可降低共混能耗和提高产能。
3、脱模效力高。本发明由于成核剂的引入与内、外润滑剂的配合,赋予了材料非常优良的脱模效果,提高了成型速率。
4、节能。由于CBT树脂和润滑剂以及低粘度PBT树脂的三重作用,使得注塑可在较低的温度和压力下进行,节约了能源。
5、机械性能好。尤其是代表韧性的冲击强度,正常情况下,流动性好的材料则韧性偏低,韧性好的材料则流动性偏差,但本发明实现了韧性和流动性的高度统一。
下面结合实施例对本发明作进一步说明。
具体实施方式
将半结晶性聚酯、主阻燃剂、阻燃协效剂、增韧剂、抗氧剂、成核剂、润滑剂、低粘环状聚酯和其它助剂按重量组分配比,在高速混和机中混和均匀以后,送入双螺杆挤出机中的主喂料中,填充改性剂随后在侧向喂料中加入,经挤出、冷却、切粒、干燥、包装而制成高成型速率、高流动的增强阻燃聚酯。
双螺杆挤出机螺杆的长径比为25-50∶1,螺杆设定温度为180-240℃,螺杆转速设定为200-600转/分。
具体实施例1-7及比较例的各组分用量见表(表中用量为重量份)。
上述各实施例制得产品测试性能如下表所示:
各比较例得到的产品测试性能如下表所示:
上述实施例的用量和组分可以变化,如:
以重量份数计,由包括下列重量份的组分制成:
半结晶性热塑性聚酯 100份
主阻燃剂 10-40份(例10、25、40)
阻燃协效剂 3-20份(例3、15、20)
增韧剂 0-30份(例1、15、30)
低粘环状聚酯 0.1-30份(例1、15、30)
抗氧剂 0.1-5.0份(例1、3、5)
成核剂 0.1-2.0份(例0.2、1、2)
润滑剂 0.2-8.0份(例0.5、5、8)
填充改性剂 0-160份(例1、80、150)
其它助剂 0-10.0份(例1、5、10)。
所述的半结晶性热塑性聚酯是聚对苯二甲酸丁二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸-1,4-环己烷二甲酯中的一种;
所述主阻燃剂为溴化环氧、十溴二苯乙烷、溴化聚碳、溴化聚苯、聚溴化苯乙烯、三-(三溴苯氧基)-三嗪、聚溴化五溴苄基酯、磷(膦)氮系阻燃剂中的一种或几种;
所述的阻燃协效剂为三氧化二锑、锑酸钠、五氧化二锑中的一种或几种;
所述的增韧剂为橡胶类弹性体、核-壳类冲击改性剂、二元或三元烯烃类共聚物、烯烃类接枝改性共聚物中的一种或几种;
所述的低粘环状聚酯为对苯二甲酸环丁二醇酯树脂;
所述的抗氧剂包括主抗氧剂和辅助抗氧剂,主抗氧剂为酚类抗氧剂,辅助类抗氧剂为亚磷酸酯类抗氧剂;
所述的成核剂为有机和无机成核剂的混和物(如德国公司的Clariant公司生产的P250);
所述的润滑剂为季戊四醇硬脂酸酯、超高分子量的固态硅氧烷产品、氧化聚乙烯蜡、德国COGNIS公司LOXIOL EP861中的一种或几种;
所述的填充改性剂为玻璃纤维、玻璃微珠、玻璃矿物纤维、碳纤维、云母、高岭土、碳酸钙、硫酸钙、硫酸钡、滑石粉、硅酸钙、晶须中的一种或多种;
所述的其它助剂为抗滴落剂聚四氟乙烯(即4F)、色母粒中的一种或几种。
磷(膦)氮系阻燃剂是MPP、MC、EXOLIT OP 1240、RDP;橡胶类弹性体为EPDM、POE;核-壳类冲击改性剂为MBS、SBS。
Claims (8)
1.一种高成型速率、高流动的增强阻燃聚酯,其特征是:以重量份数计,由包括下列重量份的组分制成:
半结晶性热塑性聚酯 100份
主阻燃剂 10-40份
阻燃协效剂 3-20份
增韧剂 0-30份
低粘环状聚酯 0.1-30份
抗氧剂 0.1-5.0份
成核剂 0.1-2.0份
润滑剂 0.2-8.0份
填充改性剂 0-160份
其它助剂 0-10.0份。
2.根据权利要求1所述的高成型速率、高流动的增强阻燃聚酯,其特征是:所述的半结晶性热塑性聚酯是聚对苯二甲酸丁二醇酯、聚对苯二甲酸丙二醇酯、聚对苯二甲酸乙二醇酯、聚对苯二甲酸-1,4-环已烷二甲酯中的一种;
所述主阻燃剂为溴化环氧、十溴二苯乙烷、溴化聚碳、溴化聚苯、聚溴化苯乙烯、三-(三溴苯氧基)-三嗪、聚溴化五溴苄基酯、磷(膦)氮系阻燃剂中的一种或几种;
所述的阻燃协效剂为三氧化二锑、锑酸钠、五氧化二锑中的一种或几种;
所述的增韧剂为橡胶类弹性体、核-壳类冲击改性剂、二元或三元烯烃类共聚物、烯烃类接枝改性共聚物中的一种或几种;
所述的低粘环状聚酯为对苯二甲酸环丁二醇酯树脂;
所述的抗氧剂包括主抗氧剂和辅助抗氧剂,主抗氧剂为酚类抗氧剂,辅助类抗氧剂为亚磷酸酯类抗氧剂;
所述的成核剂为有机和无机成核剂的混和物;
所述的润滑剂为季戊四醇硬脂酸酯、超高分子量的固态硅氧烷产品、氧化聚乙烯蜡、德国COGNIS公司LOXIOL EP861中的一种或几种;
所述的填充改性剂为玻璃纤维、玻璃微珠、玻璃矿物纤维、碳纤维、云母、高岭土、碳酸钙、硫酸钙、硫酸钡、滑石粉、硅酸钙、晶须中的一种或多种;
所述的其它助剂为抗滴落剂聚四氟乙烯、色母粒中的一种或几种。
3.根据权利要求2所述的高成型速率、高流动的增强阻燃聚酯,其特征是:磷(膦)氮系阻燃剂是MPP、MC、EXOLIT OP 1240、RDP;橡胶类弹性体为EPDM、POE;核-壳类冲击改性剂为MBS、SBS。
4.根据权利要求1所述的高成型速率、高流动的增强阻燃聚酯,其特征是:由包括下列重量份的组分制成:
半结晶性热塑性聚酯 100份
主阻燃剂 14-30份
阻燃协效剂 4-15份
增韧剂 2-20份
低粘环状聚酯 0.1-14份
抗氧剂 0.1-1.5份
成核剂 0.5- 1.4份
润滑剂 0.5-3.0份
玻璃纤维 0-80份
其它助剂 0-5.0份;
所述的半结晶性聚酯是聚对苯二甲酸丁二醇酯,密度为1.31-1.35g/cm3,粘度为0.7-1.2dl/g,熔融温度220-230℃;
所述的主阻燃剂为溴化环氧、聚溴化五溴苄基酯中的一种或二种;
所述的阻燃协效剂为三氧化二锑;
所述的增韧剂为核壳类抗冲改性剂;
所述的抗氧剂为主抗氧剂1010或抗氧剂168;
所述的玻璃纤维直径为5-20微米,是经过复合偶联剂处理的玻纤。
5.根据权利要求4所述的高成型速率、高流动的增强阻燃聚酯,其特征是:所述核壳类抗冲改性剂为美国罗姆哈斯公司生产的MBS或二元烯烃类共聚物。
6.根据权利要求4或5所述的高成型速率、高流动的增强阻燃聚酯,其特征是:所述的半结晶性聚酯聚对苯二甲酸丁二醇酯,其粘度为0.75-0.85dl/g。
7.一种权利要求1所述的高成型速率、高流动的增强阻燃聚酯的生产方法,其特征是:将半结晶性聚酯、主阻燃剂、阻燃协效剂、增韧剂、抗氧剂、成核剂、润滑剂、低粘环状聚酯和其它助剂按重量组分配比,在高速混和机中混和均匀以后,送入双螺杆挤出机中的主喂料中,填充改性剂随后在侧向喂料中加入,经挤出、冷却、切粒、干燥、包装而制成。
8.根据权利要求7所述的高成型速率、高流动的增强阻燃聚酯的生产方法,其特征是:双螺杆挤出机螺杆的长径比为25-50:1,螺杆设定温度为180-240℃,螺杆转速设定为200-600转/分。
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