CN103772919A - 一种无卤阻燃玻纤增强pet组合物及其制备方法 - Google Patents

一种无卤阻燃玻纤增强pet组合物及其制备方法 Download PDF

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CN103772919A
CN103772919A CN201210393487.5A CN201210393487A CN103772919A CN 103772919 A CN103772919 A CN 103772919A CN 201210393487 A CN201210393487 A CN 201210393487A CN 103772919 A CN103772919 A CN 103772919A
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polyethylene terephthalate
glass fiber
fiber reinforced
halogen
nucleator
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邓悦欢
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Hefei Genius New Materials Co Ltd
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Abstract

本发明属于工程塑料领域，涉及一种玻纤增强PET组合物及其制备方法。该组合物由包括以下重量份的组分制成：聚对苯二甲酸乙二醇酯100份，无卤阻燃剂5-25份，玻璃纤维20-100份，成核剂1-5份，抗氧剂0.1-0.5份，润滑改性剂1-3份，偶联剂0.1-0.2份。本发明可以使聚对苯二甲酸乙二醇酯在机械性能下降很小的幅度的情况下获得了很好的阻燃性能，并且本发明具有配方简单，工艺简便易行，加工成型性能好，制品易脱模，表观好的特点。

Description

一种无卤阻燃玻纤增强PET组合物及其制备方法
技术领域
本发明属于工程塑料领域，涉及一种玻纤增强PET组合物及其制备方法。
背景技术
聚对苯二甲酸乙二醇酯(PET)是一种性能非常优异的材料，由于其具有很好的力学性能，良好的着色性，耐化学腐蚀性等，因而广泛地应用于建筑行业、汽车行业、电气行业。但是由于PET是一种能够燃烧高分子材料，极限氧指数在21-23，在分类上属于易燃或可燃高分子材料，并且在燃烧时容易产生滴落，造成火势蔓延的严重后果，因此严重地限制了PET在各个行业内的应用。
长期以来，市场上大部分的阻燃PET工程塑料使用的是有卤的阻燃剂，主要是溴系的阻燃剂，包括十溴二苯醚、八溴二苯醚、四溴双酚A等，这些阻燃剂具有阻燃效果好、添加量少、对树脂基体机械性能影响小的优点，因而使用非常广泛。然而，有卤阻燃剂在燃烧时会受热分解出大量对人体有害卤化氢气体，极易对人体造成二次伤害，鉴于有卤阻燃剂的毒性和环保原因，欧盟2003年颁布了WEEE和RoHS两个指令，对有卤阻燃剂的使用作出了严格的限制。因此，开发无卤阻燃PET不仅有着巨大的经济价值，更是与时俱进，实现可持续发展的必然要求。
发明内容
本发明的一个目的是提供了一种无卤阻燃改性的PET组合物及其制备方法，该方法对PET进行无卤阻燃改性，可以制得玻纤增强无卤阻燃PET工程塑料。
为实现上述目的，本发明采用以下技术方案：
一种玻纤增强PET组合物，由包括以下重量份的组分制成：
聚对苯二甲酸乙二醇酯(PET)  100份，
无卤阻燃剂                 5-25份，
玻璃纤维                   20-100份，
成核剂                     1-5份，
抗氧剂                     0.1-0.5份
润滑改性剂                 1-3份，
偶联剂                     0.1-0.2份。
所述的聚对苯二甲酸乙二醇酯(PET)为特性粘数0.65-0.82dl/g；该粘度范围具有结晶速率快，加工性能好的特点，使用该粘度范围PET可使本发明的组合物具有优良的机械性能和加工成型性能。
所述的无卤阻燃剂选自苯代三聚氰胺（BG）、含磷热致性液晶高分子（TLCP）或六（4-硝基苯氧基）环三聚磷腈（HNCP）中的一种或一种以上。
所述的玻璃纤维为经过表面处理的连续玻璃纤维，优选巨石集团产988连续玻璃纤维、988A连续玻璃纤维或990连续玻璃纤维三种牌号的连续玻璃纤维。
所述的成核剂为surlyn树脂成核剂、纳米凹凸棒有机无机复配成核体系或表面有机化处理的无定形粉末和接枝的小分子聚合物复配的有机体系。
所述的成核剂优选为杜邦产牌号8920的surlyn树脂。
所述的纳米凹凸棒有机无机复配成核体系优选江苏玖川纳米科技有限公司产牌号MT502A成核剂；所述的表面有机化处理的无定形粉末和接枝的小分子聚合物复配的有机体系优选市售牌号ADD301的PET专用成核剂。
所述的抗氧剂为烷基多酚类抗氧剂，优选由四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯（抗氧剂1010）和三［2.4-二叔丁基苯基］亚磷酸酯（抗氧剂168）以重量比1:1复配而成的复配抗氧剂。
所述的润滑改性剂为硅酮粉，优选余姚凯姆立华塑胶科技有限公司售SK20R硅酮粉。
所述的偶联剂为硅烷偶联剂、钛酸酯类偶联剂，优选γ-氨丙基三乙氧基硅烷（硅烷偶联剂KH550）。
一种上述玻纤增强PET组合物的制备方法，包括以下步骤：
（1）原料混合
将聚对苯二甲酸乙二醇酯(PET)、无卤阻燃剂置于80-120℃烘箱中烘干后，按上述配比称取以下重量份的各组分原料，聚酯PET100份，无卤阻燃剂5-25份，玻璃纤维20-100份，成核剂1-5份，抗氧剂0.1-0.5份，润滑改性剂1-3份，偶联剂0.1-0.2份；将聚酯PET、无卤阻燃剂与成核剂、抗氧剂、润滑改性剂、偶联剂加入到高混机中，在常温下连续高速搅拌5分钟左右，混合均匀；
（2）挤出造粒
将步骤（1）中得到的原料混合物加入到双螺杆挤出机的料斗中，同时在双螺杆挤出机的玻纤加入口卷入连续玻纤，熔融挤出造粒；得到本发明的无卤阻燃PET组合物。
所述的步骤（2）中挤出工艺如下所示：从喂料口到机头共十段挤出温度分别为190~230℃、250~260℃、250~260℃、245~255℃、245~255℃、240~250℃、240~250℃、250~260℃、250~260℃、255~265℃，机头温度为260~270℃；螺杆转速为250~300r/min。
本发明具有以下有益效果：
本发明可以使聚对苯二甲酸乙二醇酯(PET)在机械性能下降很小的幅度的情况下获得了
很好的阻燃性能，并且本发明具有配方简单，工艺简便易行，加工成型性能好，制品易脱模，表观好的特点。
具体实施方式
以下结合具体实施例来说明本发明所涉及的方法和工艺，下列实施例仅用于说明本发明的操作过程及配方，并不限定本发明的保护范围。
实施例1-9中的聚对苯二甲酸乙二醇酯(PET)为仪征石化产牌号为SB500的PET树脂，特性粘数0.65dl/g；抗氧剂为抗氧1010和抗氧168以重量比1:1复配而成的复配抗氧剂；所述的玻璃纤维为巨石集团生产的玻纤，包括牌号为988；成核剂为杜邦产牌号8920的surlyn树脂；硅酮粉为余姚凯姆立华塑胶科技有限公司售SK20R硅酮粉。
实施例1-9
（1）将聚对苯二甲酸乙二醇酯(PET)、无卤阻燃剂置于80-120℃烘箱中烘干后，将聚酯PET、无卤阻燃剂、成核剂、抗氧剂、润滑改性剂、偶联剂按配方计量后，加入到高混机中，在常温下连续高速搅拌5分钟，得到混合均匀的原料混合物，其中以聚酯PET100重量份计，无卤阻燃剂5-25重量份，玻纤20-100重量份，成核剂1-5重量份，抗氧剂0.1-0.5重量份，润滑改性剂1-3重量份，偶联剂0.1-0.2份；实施例1-9的具体配方参数见表1；
（2）然后将步骤（1）中得到的原料混合物加入到双螺杆挤出机的料斗中，同时在玻纤加入口加入连续玻纤，按照上述挤出工艺挤出造粒。得到本发明的无卤阻燃PET组合物。
其中，步骤（2）中挤出机为南京瑞亚弗斯特高聚物设备有限公司产型号TSE-35A的同向双螺杆挤出机，该挤出机螺杆公称螺杆35mm，长径比44，转速60-600r/min。
步骤（3）所述注塑机为震德塑料机械厂有限公司制造型号CJ80M2V塑料注射成型机，注塑工艺为一段温度245~250℃，射胶速度50~99%，压力99~88%、二段温度250~255℃，射胶速度45~88%，压力88~77%、三段温度245~250℃、射胶速度40~77%，压力77~66%，保压一段时间6~8S，压力40~50%，保压二段时间4~6S，压力50~60%；冷却时间6~8S，模具温度90~120℃。
将步骤（2）中得到粒料在80-120℃的烘箱内烘6-10小时，然后注塑成ASTM标准样条。进行力学性能与燃烧性能测试。测试标准及性能数据见表2。
对比例1-3
将聚对苯二甲酸乙二醇酯(PET)、成核剂、抗氧剂、润滑改性剂、偶联剂按配方计量后，加入到高混机中，在常温下连续高速搅拌5分钟左右，得到混合均匀的原料混合物，其中以聚酯PET100重量份计，玻纤20-100重量份，成核剂1-5重量份，抗氧剂0.1-0.5重量份，润滑改性剂1-3重量份，偶联剂0.1-0.2份。然后将原料混合物加入到双螺杆挤出机的料斗中，同时在玻纤加入口加入连续玻纤，按照上述挤出工艺挤出造粒。对比例1-3的具体配方参数见表1。
将上述粒料在80-120℃的烘箱内烘6-10小时，然后按照上述注塑工艺注塑标准样条，进行力学性能与燃烧性能测试，测试标准及性能数据见表2。
表1
Figure BDA00002264811200041
表2
拉伸强度/Mpa 弯曲强度/Mpa 阻燃级别
测试标准 ASTM ASTM UL-94
实施例1 94.4 112.6 3.2mm V-2
实施例2 95.7 118.6 3.2mmV1
实施例3 108.8 155.9 3.2mm V-0
实施例4 125.2 189.4 3.2mmV1
实施例5 153.9 227.5 3.2mm V-0
实施例6 120 183.1 3.2mm V-0
实施例7 96.3 117.2 3.2mmV1
实施例8 105.9 158.7 3.2mm V-0
实施例9 118.6 179.6 3.2mm V-0
对比例1 99.1 122.9 Not rated
对比例2 114.5 160.3 Not rated
对比例3 137.2 201.6 Not rated
结合表1和表2可以看出，添加了无卤阻燃剂的实施例在机械性能下降很小的幅度的情况下获得了很好的阻燃性能。
上述的对实施例的描述是为便于该技术领域的普通技术人员能理解和应用本发明。熟悉本领域技术的人员显然可以容易地对这些实施例做出各种修改，并把在此说明的一般原理应用到其他实施例中而不必经过创造性的劳动。因此，本发明不限于这里的实施例，本领域技术人员根据本发明的揭示，不脱离本发明范畴所做出的改进和修改都应该在本发明的保护范围之内。

Claims (10)

1.一种玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：由包括以下重量份的组分制成：
聚对苯二甲酸乙二醇酯  100份，
无卤阻燃剂            5-25份，
玻璃纤维              20-100份，
成核剂                1-5份，
抗氧剂                0.1-0.5份
润滑改性剂            1-3份，
偶联剂                0.1-0.2份。
2.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的聚对苯二甲酸乙二醇酯为特性粘数0.65-0.82dl/g。
3.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的无卤阻燃剂选自苯代三聚氰胺、含磷热致性液晶高分子或六（4-硝基苯氧基）环三聚磷腈中的一种或一种以上。
4.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的玻璃纤维为经过表面处理的连续玻璃纤维，优选988连续玻璃纤维、988A连续玻璃纤维或990连续玻璃纤维。
5.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的成核剂为surlyn树脂成核剂、纳米凹凸棒有机无机复配成核体系或表面有机化处理的无定形粉末和接枝的小分子聚合物复配的有机体系。
6.根据权利要求5所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的成核剂为杜邦产牌号8920的surlyn树脂；
或所述的纳米凹凸棒有机无机复配成核体系优选MT502A成核剂；
或所述的表面有机化处理的无定形粉末和接枝的小分子聚合物复配的有机体系优选ADD301的PET专用成核剂。
7.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的抗氧剂为烷基多酚类抗氧剂，优选由四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯和三［2.4-二叔丁基苯基］亚磷酸酯以重量比1:1复配而成的复配抗氧剂。
8.根据权利要求1所述的玻纤增强聚对苯二甲酸乙二醇酯组合物，其特征在于：所述的润滑改性剂为硅酮粉；
或所述的偶联剂为硅烷偶联剂、钛酸酯类偶联剂，优选硅烷偶联剂γ-氨丙基三乙氧基硅烷。
9.一种上述权利要求1-8中任一所述的玻纤增强聚对苯二甲酸乙二醇酯组合物的制备方法，其特征在于：包括以下步骤：
（1）原料混合
将聚对苯二甲酸乙二醇酯(PET)、无卤阻燃剂置于80-120℃烘箱中烘干后，按上述配比称取以下重量份的各组分原料，聚酯PET100份，无卤阻燃剂5-25份，玻璃纤维20-100份，成核剂1-5份，抗氧剂0.1-0.5份，润滑改性剂1-3份，偶联剂0.1-0.2份；将聚对苯二甲酸乙二醇酯、无卤阻燃剂与成核剂、抗氧剂、润滑改性剂、偶联剂加入到高混机中，在常温下连续高速搅拌5分钟左右，混合均匀；
（2）挤出造粒
将步骤（1）中得到的原料混合物加入到双螺杆挤出机的料斗中，同时在双螺杆挤出机的玻纤加入口卷入连续玻纤，熔融挤出造粒；得到本发明的玻纤增强聚对苯二甲酸乙二醇酯组合物。
10.根据权利要求9所述的制备方法，其特征在于：所述的步骤（2）中挤出工艺如下所示：从喂料口到机头共十段挤出温度分别为190~230℃、250~260℃、250~260℃、245~255℃、245~255℃、240~250℃、240~250℃、250~260℃、250~260℃、255~265℃，机头温度为260~270℃；螺杆转速为250~300r/min。
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