CN106189126B - 一种高热变形温度低成型周期阻燃增强pet材料及制备方法 - Google Patents
一种高热变形温度低成型周期阻燃增强pet材料及制备方法 Download PDFInfo
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Abstract
本发明公开一种高热变形温度低成型周期阻燃增强PET材料，由以下重量份的原材料组成：PET树脂40‑55份；玻璃纤维25‑40份；阻燃剂10‑18份；增韧剂1‑3份；相容剂0.5‑1.5份；成核剂0.5‑0.9份；结晶促进剂0.5‑1.2份；润滑剂0.2‑0.6份；抗氧剂0.2‑0.6份。本发明所使用的原料均来自市售，来源广泛，液晶高分子作为结晶促进剂，添加量少，制备方法简单，可操作性强，易于大规模工业化生产，产品极具性价比；本发明制备的阻燃增强PET材料对注塑成型要求低，无需用油温机，能耗低；同时，注塑成型周期可大大缩短，效率高；本发明阻燃增强PET材料可满足电工电器行业高耐热和阻燃要求。
Description
技术领域
本发明涉及高分子材料领域，具体是一种高热变形温度低成型周期阻燃增强PET材料及制备方法。
背景技术
聚对苯二甲酸乙二醇酯(PET)材料具有很高的介电常数和电绝缘性，且该特性受温度和湿度影响较小，因此PET材料在电工电器领域具有不错的应用前景。
PET材料在电工电器领域使用时，通常需对其进行阻燃增强改性，以满足强度和阻燃性能方面的要求。但是，改性PET在工程塑料改性领域，一直是一个重难点。由于PET为半结晶性聚合物，其结晶速度缓慢，导致其收缩率大，注塑成型周期长，热变形温度不高，无法满足材料设计要求。在实际应用中，还带来了脱模困难、零件脱模后偏软和变形等诸多问题。
改性PET材料结晶慢、成型周期长的主要原因为PET的玻璃化转变温度Tg较高(约78℃)，在注塑成型过程中，热的PET熔体在遇到较冷的模具型腔时，分子运动能力受到大幅抑制，导致结晶无法快速进行。
解决该问题，从注塑工艺来说，需将模温设定在90℃以上，以利于PET结晶，但该方法对设备要求较高，能耗也大；从改性PET配方上来说，需提高PET的成核能力和降低PET的玻璃化转变温度Tg，即对PET进行增塑。常规的成核剂和结晶促进剂(增塑剂)有滑石粉、蒙脱土、稀土、苯甲酸钠等，结晶促进剂有聚乙二醇、褐煤酸、乙烯基离子聚合物等。其中，最有效的为苯甲酸钠和聚乙二醇复配体系，但它们的高效来自于其对PET的分解作用，降低了PET的玻璃化转变温度，在注塑过程中，存在流延明显的问题。
发明内容
本发明的目的在于提供一种高热变形温度低成型周期阻燃增强PET材料及制备方法，利用有机化纳米改性蒙脱土协同热致性液晶高分子作为PET的结晶成核剂，成功地使阻燃增强PET材料的热变形温度达到225℃，同时缩短了成型周期。
本发明的目的可以通过以下技术方案实现：
一种高热变形温度低成型周期阻燃增强PET材料，其特征在于，由以下重量份的原材料组成：
PET树脂 40-55份；
玻璃纤维 25-40份；
阻燃剂 10-18份；
增韧剂 1-3份；
相容剂 0.5-1.5份；
成核剂 0.5-0.9份；
结晶促进剂 0.5-1.2份；
润滑剂 0.2-0.6份；
抗氧剂 0.2-0.6份。
所述PET树脂特性粘度在0.8-0.95dl/g之间。
所述玻璃纤维为直径为7-10um的无碱E级短切玻纤原丝。
所述阻燃剂为锑酸钠与溴系阻燃剂以重量比1:3-5的复配，所述溴系阻燃剂为十溴二苯乙烷、溴化聚苯乙烯或溴化环氧树脂。
所述增韧剂为密度为0.88-0.94g/cm3、在190℃/2.16Kg下熔融指数为5-30g/10min的甲基丙烯酸缩水甘油酯接枝乙烯-辛烯共聚物、乙烯与甲基丙烯酸甲酯或者丙烯酸丁酯共聚物的至少一种。
所述相容剂为苯乙烯-马来酸酐共聚物或苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯共聚物。
所述成核剂为有机纳米改性蒙脱土；所述结晶促进剂为分子量在5000-20000之间的热致性液晶高分子。
所述润滑剂为硬脂酸季戊四醇酯、酸化聚乙烯蜡中的至少一种。
所述抗氧剂为β-(3,5-二叔丁基-4-羟基苯基)丙酸正十八碳醇酯、三[2.4-二叔丁基苯基]亚磷酸酯的至少一种。
本发明还提供一种高热变形温度低成型周期阻燃增强PET材料的制备方法，包括以下步骤：
(1)按配比，将PET树脂、阻燃剂、增韧剂、相容剂、成核剂、结晶促进剂、抗氧剂和润滑剂一起加入高速搅拌机中混合2-5min，得混合物料；
(2)将混合物料经过主喂料斗加入到啮合式平行同向双螺杆挤出机中，并在侧喂料处加入玻璃纤维，经熔融、挤出、切粒得到阻燃增强PET材料；其中，双螺杆挤出机料筒温度230-245℃，螺杆转速为300-400r/min，真空度为-0.04-0.1MPa。
本发明成核剂为纳米层状蒙脱土，它与聚酯材料具有非常好的亲和性，同时它的片层结构非常有利于作为聚酯结晶的晶核模板，纳米蒙脱土的加入，大大降低了PET的结晶过冷度；结晶促进剂为热致性液晶聚合物，它是一种含大量芳环的聚酯，在融融状态下有序排列。其添加到PET材料中作为结晶促进剂，它的自发取向特性有效地对PET分子链进行增塑和润滑，降低了PET材料的玻璃化转变温度，增加了PET材料在低温时的结晶能力，因此降低了成型周期，获得了很高的热变形温度。利用液晶高分子作为PET的结晶促进剂，极大地提高了PET的低温结晶能力。利用本发明方法制备得到的阻燃增强PET材料具有高热变形温度(1.8MPa热变形温度可达到225℃，达到杜邦阻燃增强PET FR530相同水平)、低注塑成型周期的优异特性，在电工电器领域，它将成为断路器、电动工具等零件外壳的理想选材。
本发明的有益效果：
1、本发明所使用的原料均来自市售，来源广泛。液晶高分子作为结晶促进剂，添加量少，制备方法简单，可操作性强，易于大规模工业化生产，产品极具性价比；
2、本发明制备的阻燃增强PET材料对注塑成型要求低，无需用油温机，将模具温度设定在90℃以上，能耗低；同时，注塑成型周期可大大缩短，效率高；
3、本发明制备的阻燃增强PET材料可满足电工电器行业要求高耐热和阻燃要求。
具体实施方式
下面结合具体实施例对本发明作进一步详细描述。
本发明所用原料均可通过购买得到。
按照以下制备方法制备实施例1-3，各组分的配比如表1所示。
(1)按配比，将PET树脂40-55份、阻燃剂10-18份、增韧剂1-3份、相容剂0.5-1.5份、成核剂0.5-0.9份、结晶促进剂0.5-1.2份、抗氧剂0.2-0.6份和润滑剂0.2-0.6份一起加入高速搅拌机中混合2-5min，得混合物料；
(2)将混合物料经过主喂料斗加入到啮合式平行同向双螺杆挤出机中，并在侧喂料处加入25-40份的玻璃纤维，经熔融、挤出、切粒得到阻燃增强PET材料；其中，双螺杆挤出机料筒温度230-245℃，螺杆转速为300-400r/min，真空度为-0.04-0.1MPa。
表1具体实施例中制备原料的组成
将上述实施例1～3制备的阻燃增强PET复合材料的密度、拉伸强度、弯曲模量、悬臂梁缺口冲击强度、热变形温度、阻燃性、成型周期、玻璃化转变温度、体积电阻率等进行检测，其检测标准与性能检测结果如表2所示。
表2复合材料性能
从表2可看出，本发明实施例1-3制备的高热变形温度低成型周期阻燃增强PET复合材料具有较高的机械性能、热变形温度和较低的成型周期，可以满足电工电器行业对材料的性能要求。
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实施案例做出各种修改，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案例，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 (9)
1.一种高热变形温度低成型周期阻燃增强PET材料，其特征在于，由以下重量份的原材料组成：
PET树脂40-55份；
玻璃纤维25-40份；
阻燃剂10-18份；
增韧剂1-3份；
相容剂0.5-1.5份；
成核剂0.5-0.9份；
结晶促进剂0.5-1.2份；
润滑剂0.2-0.6份；
抗氧剂0.2-0.6份；
所述成核剂为有机纳米改性蒙脱土；所述结晶促进剂为分子量在5000-20000之间的热致性液晶高分子。
2.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述PET树脂特性粘度在0.8-0.95dl/g之间。
3.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述玻璃纤维为直径为7-10μm的无碱E级短切玻纤原丝。
4.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述阻燃剂为锑酸钠与溴系阻燃剂以重量比1:3-5的复配，所述溴系阻燃剂为十溴二苯乙烷、溴化聚苯乙烯或溴化环氧树脂。
5.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述增韧剂为密度为0.88-0.94g/cm3、在190℃/2.16Kg下熔融指数为5-30g/10min的甲基丙烯酸缩水甘油酯接枝乙烯-辛烯共聚物、乙烯与甲基丙烯酸甲酯或者丙烯酸丁酯共聚物的至少一种。
6.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述相容剂为苯乙烯-马来酸酐共聚物或苯乙烯-丙烯腈-甲基丙烯酸缩水甘油酯共聚物。
7.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述润滑剂为硬脂酸季戊四醇酯、酸化聚乙烯蜡中的至少一种。
8.根据权利要求1所述的高热变形温度低成型周期阻燃增强PET材料，其特征在于，所述抗氧剂为β-（3,5-二叔丁基-4-羟基苯基）丙酸正十八碳醇酯、三[2.4-二叔丁基苯基]亚磷酸酯的至少一种。
9.一种制备如权利要求1所述的高热变形温度低成型周期阻燃增强PET材料的方法，其特征在于，包括以下步骤：
（1）按配比，将PET树脂、阻燃剂、增韧剂、相容剂、成核剂、结晶促进剂、抗氧剂和润滑剂一起加入高速搅拌机中混合2-5min，得混合物料；
（2）将混合物料经过主喂料斗加入到啮合式平行同向双螺杆挤出机中，并在侧喂料处加入玻璃纤维，经熔融、挤出、切粒得到阻燃增强PET材料；其中，双螺杆挤出机料筒温度230-245℃，螺杆转速为300-400r/min，真空度为-（0.04-0.1）MPa。
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