CN102702715A - 一种高流动性玻纤增强无卤阻燃pc树脂及其制备方法 - Google Patents

一种高流动性玻纤增强无卤阻燃pc树脂及其制备方法 Download PDF

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CN102702715A
CN102702715A CN2012102211559A CN201210221155A CN102702715A CN 102702715 A CN102702715 A CN 102702715A CN 2012102211559 A CN2012102211559 A CN 2012102211559A CN 201210221155 A CN201210221155 A CN 201210221155A CN 102702715 A CN102702715 A CN 102702715A
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flame retardant
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刘福军
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DONGGUAN SONG SHEN PLASTICS TECHNOLOGY Co Ltd
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Abstract

本发明涉及PC树脂改性技术领域，特别是涉及一种高流动性玻纤增强无卤阻燃PC树脂及其制备方法，该种高流动性玻纤增强无卤阻燃PC树脂，它由以下重量百分比的原料组成：PC树脂30-70%、玻璃纤维10-35%、AS树脂5-30%、阻燃剂8-15%、增韧剂5-10%、抗氧剂0.2-1.5%，以上原料经共混挤出造粒制得，本发明制得的种高流动性玻纤增强无卤阻燃PC在满足材料UL94V0阻燃的基础上，耐热性、加工流动性、抗冲击性能优异；本发明的制备方法工艺简单、成本低。

Description

一种高流动性玻纤增强无卤阻燃PC树脂及其制备方法
技术领域
本发明涉及PC树脂改性技术领域，特别是涉及一种高流动性玻纤增强无卤阻燃PC树脂及其制备方法。
背景技术
聚碳酸酯PC具有冲击强度高，透明，无毒，介电性能优良抗蠕变性和尺寸稳定性等优点，在电气，汽车工业，医疗器械，建筑和照明用具等领域已广泛应用。虽然聚碳酸酯PC的阻燃等级为UL94-V-2。但是仍可燃烧，且燃烧时有热熔体滴下，容易引起附近材料着火，难以满足阻燃防火要求。因此，在实际应用中要对PC进行阻燃处理。
如专利号为ZL200810038154.4的中国发明公开了一种低发烟量无卤阻燃PC/ABS合金及其制备方法，按重量百分比称取聚碳酸酯(PC)40-75%，丙烯晴-丁二烯-苯乙烯共聚物(ABS)10-40%，复合阻燃剂10-15%，复合降烟剂0.2-2%，相容剂2-16%，低发烟促进剂1-6%，稳定剂0.1-0.5%，润滑剂0.1-0.6%，以上专利和其它现有技术要使PC树脂达到V0级别阻燃，都添加了很大量的阻燃剂和其它助剂，导致改性PC树脂的耐热性急剧下降，加工流动性较差。
发明内容
本发明的目的在于针对现有技术的不足，提供了一种高流动性玻纤增强无卤阻燃PC树脂及其制备方法，该种高流动性玻纤增强无卤阻燃PC树脂耐热性好、加工流动性强，该种高流动性玻纤增强无卤阻燃PC树脂的制备方法工艺简单、成本低。
本发明的目的是这样实现的：一种高流动性玻纤增强无卤阻燃PC树脂，它由以下重量百分比的原料组成：
PC树脂              30-70%
玻璃纤维             10-35%
AS树脂              5-30%
阻燃剂               8-15%
增韧剂              5-10%
抗氧剂              0.2-1.5%。
优选的，它由以下重量百分比的原料组成：
PC树脂              30-64%
玻璃纤维             15-35%
AS树脂              5-30%
阻燃剂               10-15%
增韧剂               5-10%
抗氧剂              1-1.5%。
更为优选的，它由以下重量百分比的原料组成：
PC树脂              45%
玻璃纤维             15%
AS树脂              19%
阻燃剂               15%
增韧剂               5%
抗氧剂              1%。
其中，所述ＰＣ树脂为一种通用型号芳香族聚碳酸酯，密度为1.１-1.6g/cm3。
其中，所述玻璃纤维的直径为10μm-13μm。
其中，所述AS树脂中苯乙烯含量为30%-50%。
其中，所述阻燃剂为双酚A双（磷酸二苯酯）（BDP）。
其中，所述增韧剂为甲基丙烯酸甲酯、丁二烯、及苯乙烯的三元共聚物（MBS）。
其中，所述抗氧剂为四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯，三［2.4-二叔丁基苯基］亚磷酸酯，2-叔丁基-6-(3-叔丁基-5-甲基-2-羟苯基)-4-甲基苯基丙烯酸酯中的一种或任意几种。
本发明通过调节玻璃纤维的含量来有效改善材料的耐热性能，通过调节AS树脂的含量来有效改善材料的加工流动性。
上述高流动性玻纤增强无卤阻燃PC树脂的制备方法，它包括以下制备步骤：
步骤A、将PC 树脂和AS树脂在80℃烘烤1小时，备用;
步骤B、将烘烤后的PC树脂、将烘烤后的AS树脂、阻燃剂、增韧剂、抗氧剂按比例加入高速混合机中高速共混5-10min，得到共混物；
步骤C、将玻璃纤维和步骤B得到的共混物经双螺杆挤出机挤出造粒；
步骤D、将步骤C得到的粒子在100℃ 烘烤1-2小时，即得成品。
其中，所述步骤C双螺杆挤出机的具体工艺参数为：一区温度 210-200℃，二区温度210-200℃，三区温度210-200℃，四区温度210-200℃，五区温度210-200℃，六区温度 190-200℃，七区温度190-200℃，八区温度190-200℃，九区温度190-200℃，模头温度190-195℃ ，停留时间2-3min，压力12-18MPa，螺杆转速 280-350R/min。
本发明的有益效果为：本发明制备的高流动性玻纤增强无卤阻燃PC树脂，在满足材料UL94 V0阻燃的基础上，耐热性、加工流动性、抗冲击性能优异；本发明的制备方法工艺简单、成本低。
具体实施方式
下面通过实施例对本发明作进一步说明，但本发明的实施范围并不限于此。
实施例1。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将30㎏烘烤后的PC树脂、将30㎏烘烤后的AS树脂、15㎏BDP、5㎏MBS、0.2㎏四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯加入高速混合机中高速共混10min，得到共混物，再将19.8㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤2小时，即得成品。双螺杆挤出机的具体工艺参数为：一区温度 210℃，二区温度200℃，三区温度205℃，四区温度210℃，五区温度200℃，六区温度 195℃，七区温度200℃，八区温度190℃，九区温度200℃，模头温度195℃ ，停留时间2min，压力12MPa，螺杆转速 280R/min。
实施例2。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将70㎏烘烤后的PC树脂、将5㎏烘烤后的AS树脂、8.5㎏BDP、5㎏MBS、0.5㎏四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯、0.5㎏三［2.4-二叔丁基苯基］亚磷酸酯、0.5㎏2-叔丁基-6-(3-叔丁基-5-甲基-2-羟苯基)-4-甲基苯基丙烯酸酯加入高速混合机中高速共混8min，得到共混物，再将10㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤1小时，即得成品。双螺杆挤出机的具体工艺参数为：一区温度200℃，二区温度210℃，三区温度200℃，四区温度210℃，五区温度200℃，六区温度 190℃，七区温度200℃，八区温度190℃，九区温度200℃，模头温度195℃ ，停留时间3min，压力18MPa，螺杆转速350R/min。
实施例3。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将50㎏烘烤后的PC树脂、将20㎏烘烤后的AS树脂、10㎏BDP、5.8㎏MBS、0.2㎏三［2.4-二叔丁基苯基］亚磷酸酯加入高速混合机中高速共混8min，得到共混物，再将14㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤2小时，即得成品。双螺杆挤出机的具体工艺参数为：一区温度 205℃，二区温度200℃，三区温度205℃，四区温度210℃，五区温度205℃，六区温度 195℃，七区温度200℃，八区温度195℃，九区温度195℃，模头温度190℃ ，停留时间2min，压力15MPa，螺杆转速 320R/min。
实施例4。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将45㎏烘烤后的PC树脂、将19㎏烘烤后的AS树脂、15㎏BDP、5㎏MBS、1㎏2-叔丁基-6-(3-叔丁基-5-甲基-2-羟苯基)-4-甲基苯基丙烯酸酯加入高速混合机中高速共混8min，得到共混物，再将15㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤2小时，即得成品。双螺杆挤出机的具体工艺参数为：一区温度 210℃，二区温度200℃，三区温度210℃，四区温度208℃，五区温度210℃，六区温度 198℃，七区温度195℃，八区温度200℃，九区温度190℃，模头温度193℃ ，停留时间3min，压力18MPa，螺杆转速 330R/min。
实施例5。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将40㎏烘烤后的PC树脂、将10㎏烘烤后的AS树脂、10㎏BDP、10㎏MBS、0.5㎏四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯、0.5㎏三［2.4-二叔丁基苯基］亚磷酸酯加入高速混合机中高速共混10min，得到共混物，再将29㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤1小时，即得成品。双螺杆挤出机的具体工艺参数为：：一区温度 205℃，二区温度200℃，三区温度205℃，四区温度210℃，五区温度205℃，六区温度 195℃，七区温度200℃，八区温度195℃，九区温度195℃，模头温度190℃ ，停留时间2min，压力15MPa，螺杆转速 320R/min。
实施例6。
将PC 树脂和AS树脂在80℃烘烤1小时，然后将40㎏烘烤后的PC树脂、将15㎏烘烤后的AS树脂、13.5㎏BDP、5㎏MBS、1㎏四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯、0.5㎏2-叔丁基-6-(3-叔丁基-5-甲基-2-羟苯基)-4-甲基苯基丙烯酸酯加入高速混合机中高速共混5min，得到共混物，再将25㎏玻璃纤维和上述共混物经双螺杆挤出机挤出造粒，得到的粒子在100℃ 烘烤2小时，即得成品。双螺杆挤出机的具体工艺参数为：一区温度200℃，二区温度210℃，三区温度200℃，四区温度210℃，五区温度200℃，六区温度 190℃，七区温度200℃，八区温度190℃，九区温度200℃，模头温度195℃ ，停留时间3min，压力17MPa，螺杆转速340R/min。
说明：实施例1-6所用的ＰＣ树脂为一种通用型号芳香族聚碳酸酯，密度为1.1-1.6g/cm3；玻璃纤维的直径为10μm-13μm；AS树脂中苯乙烯含量为30%-50%；阻燃剂为双酚A双（磷酸二苯酯）（BDP）；增韧剂为甲基丙烯酸甲酯、丁二烯、及苯乙烯的三元共聚物（MBS）。
本发明产品的性能评价方式及实行标准：
按照上述方法完成造粒的粒子放入80℃的鼓风烘箱中干燥1-2小时，然后再将干燥好的粒子在注射成型机上进行注射成型制样。
拉伸性能测试按ISO-527-2进行，试样尺寸150*10*4mm ，拉伸速度为50mm/min；弯曲强度按ISO 178进行，试样尺寸80*10*4mm ，弯曲速度为2mm/min，跨距为64mm；
简支梁冲击强度按ISO 179进行，试样尺寸80*6*4mm，缺口深度为试样厚度的三分之一；
热变形温度按ISO 75进行，试样尺寸120*10*3mm，载荷为1.8MPa； 
熔融指数按照ISO1133，试样为粒子状，加工流动性通过熔融指数进行评价。
实施例1-6产品性能参数见表1。
                                                
Figure 365093DEST_PATH_IMAGE001
。
通过表1可以看出本发明制备的高流动性玻纤增强无卤阻燃PC树脂耐热性、加工流动性、抗冲击性能优异。
最后应当说明的是，以上实施例仅用以说明本发明的技术方案，而非对本发明保护范围的限制，尽管参照较佳实施例对本发明作了详细地说明，本领域的普通技术人员应当理解，可以对本发明的技术方案进行修改或者等同替换，而不脱离本发明技术方案的实质和范围。

Claims (10)

1.一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于: 它由以下重量百分比的原料组成：
PC树脂              30-70%
玻璃纤维             10-35%
AS树脂              5-30%
阻燃剂               8-15%
增韧剂              5-10%
抗氧剂              0.2-1.5%。
2.根据权利要求1所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：它由以下重量百分比的原料组成：
PC树脂              30-64%
玻璃纤维             15-35%
AS树脂              5-30%
阻燃剂               10-15%
增韧剂               5-10%
抗氧剂              1-1.5%。
3.根据权利要求2所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：它由以下重量百分比的原料组成：
PC树脂              45%
玻璃纤维             15%
AS树脂              19%
阻燃剂               15%
增韧剂               5%
抗氧剂              1%。
4.根据权利要求1-3任一项所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：所述玻璃纤维的直径为10μm-13μm。
5.根据权利要求1-3任一项所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：所述AS树脂中苯乙烯含量为30%-50%。
6.根据权利要求1-3任一项所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：所述阻燃剂为双酚A双（磷酸二苯酯）。
7.根据权利要求1-3任一项所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：所述增韧剂为甲基丙烯酸甲酯、丁二烯及苯乙烯的三元共聚物。
8.根据权利要求1-3任一项所述的一种高流动性玻纤增强无卤阻燃PC树脂，其特征在于：所述抗氧剂为四[β-（3，5-二叔丁基-4-羟基苯基）丙酸]季戊四醇酯，三［2.4-二叔丁基苯基］亚磷酸酯，2-叔丁基-6-(3-叔丁基-5-甲基-2-羟苯基)-4-甲基苯基丙烯酸酯中的一种或任意几种。
9.权利要求1-8任一项所述的高流动性玻纤增强无卤阻燃PC树脂的制备方法，其特征在于：它包括以下制备步骤：
步骤A、将PC 树脂和AS树脂在80℃烘烤1小时，备用；
步骤B、将烘烤后的PC树脂、将烘烤后的AS树脂、阻燃剂、增韧剂、抗氧剂按比例加入高速混合机中高速共混5-10min，得到共混物；
步骤C、将玻璃纤维和步骤B得到的共混物经双螺杆挤出机挤出造粒；
步骤D、将步骤C得到的粒子在100℃ 烘烤1-2小时，即得成品。
10.根据权利要求9所述的一种高流动性玻纤增强无卤阻燃PC的制备方法，其特征在于：所述步骤C双螺杆挤出机的具体工艺参数为：一区温度 210-200℃，二区温度210-200℃，三区温度210-200℃，四区温度210-200℃，五区温度210-200℃，六区温度 190-200℃，七区温度190-200℃，八区温度190-200℃，九区温度190-200℃，模头温度190-195℃ ，停留时间2-3min，压力12-18MPa，螺杆转速 280-350R/min。
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