CN101508843B - 无卤阻燃增强聚对苯二酰对苯二胺复合材料 - Google Patents

无卤阻燃增强聚对苯二酰对苯二胺复合材料 Download PDF

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CN101508843B
CN101508843B CN2008102415282A CN200810241528A CN101508843B CN 101508843 B CN101508843 B CN 101508843B CN 2008102415282 A CN2008102415282 A CN 2008102415282A CN 200810241528 A CN200810241528 A CN 200810241528A CN 101508843 B CN101508843 B CN 101508843B
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terephthaloyl
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徐东
贺永
杨海灵
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Polymer Science Anhui New Material Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/88—Thermal treatment of the stream of extruded material, e.g. cooling
    • B29C48/918—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling
    • B29C48/9185—Thermal treatment of the stream of extruded material, e.g. cooling characterized by differential heating or cooling in the direction of the stream of the material
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/04—Particle-shaped
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/36—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders
    • B29C48/40—Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die using screws surrounded by a cooperating barrel, e.g. single screw extruders using two or more parallel screws or at least two parallel non-intermeshing screws, e.g. twin screw extruders
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25—Component parts, details or accessories; Auxiliary operations
    • B29C48/92—Measuring, controlling or regulating
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C2948/92—Measuring, controlling or regulating
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C2948/00—Indexing scheme relating to extrusion moulding
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    • B29C2948/92819—Location or phase of control
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00—Indexing scheme relating to extrusion moulding
    • B29C2948/92—Measuring, controlling or regulating
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Abstract

本发明提供了一种无卤阻燃增强高温尼龙聚对苯二酰对苯二胺(PPA)复合材料，其组成按重量配比为(％)：PPA 35～70％；增强剂5～35％；主抗氧剂0.2～0.5％；辅助抗氧剂0.2～0.5％；阻燃剂A 7～10％；阻燃剂B 15～25％；润滑剂0.5～1％。本发明是针对目前全球最热的环保要求而设计的聚对苯二酰对苯二胺新产品，本发明不含卤素，在使用过程中不会因其材料的分解而放出有害气体，对大气和水等无污染，且阻燃性好，电绝缘性能优异，漏电起痕值高，比重低，机械性能优良，可与一般的有卤耐高温阻燃材料相媲美。本发明可广泛应用于家电配件、电子产品配件等。

Description

无卤阻燃增强聚对苯二酰对苯二胺复合材料
技术领域
本发明涉及一种无卤阻燃增强聚对苯二酰对苯二胺复合材料，尤其涉及一种可用于注塑成型各种有环保阻燃要求的以及供出口用的电子电气设备、家电产品、汽车配件的无卤阻燃增强聚对苯二酰对苯二胺复合材料。
背景技术
现有技术中，聚对苯二酰对苯二胺是一种由对苯二酸和对苯二胺缩聚而成的均匀热塑性高分子聚合物，该材料热变形温度高达300℃以上，连续使用温度可达170℃，能满足所需的短期和长期的热性能。它不仅具有高钢性、高强度极佳的尺寸精度及稳定性和低翘曲性良好的耐化学性物性受吸水率影响极小良好的表面质量、易成型的特点，还可以在宽广的温度范围内和高湿度环境中保持其优越的机械特性-强度、硬度、耐疲劳性及抗蠕变性，广泛应用于各种电子电器产品和汽车配件，特别适用于需要过SMT制程的高温连接器元件。由于其优异的性价比，在高温材料市场上是PA46，PA6T，PA9T的优异替代品。目前的阻燃高温尼龙所用的阻燃剂近80％为含卤阻燃剂，由于含溴阻燃剂效率高、用量少，对材料的性能影响小，且价格适中，其效能/价格比非其他阻燃剂所能匹敌，因此我国供出口的电子电气类产品中70％～80％都用此类阻燃剂。但近年来溴系阻燃剂受到二恶英问题的困扰，同时用其(溴一锑系统)阻燃的高分子材料在热裂解及燃烧时会生成大量的烟尘及腐蚀性气体，目前欧盟和日本已相继出台法令禁止使用此类的阻燃剂。欧盟已在2006年7月1日起全面实施ROHS指令，该法令要求投放欧盟的电子电气产品不得含有多溴二苯醚、多溴联苯；日本也出台了相应的标准JISC0950，SONY公司出台的SONY-SS-00259标准对阻燃剂的要求更为严格；在美国，个别州政府立法针对溴系阻燃剂的使用。以上法令和标准严重制约了我国电子电气产品的出口，因此必须大力发展无卤阻燃材料才能适应国际市场的发展趋势，为了提升产品质量，配合国际标准的要求，中国版RoHS的《电子信息产品污染控制管理办法》也从2007年3月1日起正式实施。
发明内容
本发明所要解决的技术问题是提供一种环保、安全、阻燃性好、电绝缘性能优异、机械性能高的无卤阻燃增强聚对苯二酰对苯二胺复合材料。
为实现上述目的，本发明所采用的技术方案为：
一种无卤阻燃增强聚对苯二酰对苯二胺复合材料，其组成按重量配比为(％)：
聚对苯二酰对苯二胺    35～70％；
增强剂                5～35％；
主抗氧剂              0.2～0.5％；
辅助抗氧剂            0.2～0.5％；
阻燃剂A               7～10％；
阻燃剂B      15～25％；
润滑剂       0.5～1％。
所述的增强剂为玻璃纤维，玻璃纤维的加入大大增强了复合材料材料的强度。
所述的主抗氧剂为N，N-双-[3-(3，5-二叔丁基-4-羟基苯基)丙酰基]己二胺。所述的辅助抗氧剂为有机亚磷酸酯，所述有机亚磷酸酯为三(2，4-二叔丁基苯基)亚磷酸酯。抗氧剂的加入可以提高材料在加工过程中的抗热分解的能力，防止材料老化。
所述的阻燃剂A为三聚氰胺磷酸盐，阻燃剂B为次磷酸酯。所述阻燃剂可以和组合物中的其他组分很好的融合，使组合物的阻燃性能达到UL94V-0级，和含卤阻燃产品的阻燃性能相当，且本发明不含卤素，属环保型产品，因此完全可以替代含卤阻燃产品，具有广阔的应用前景。
所述的润滑剂为蒙旦蜡，所述蒙旦蜡为褐煤蜡酸-1-甲基-1，3-丙二基酯与脂肪酸-褐煤蜡钙盐的共混物。所述润滑剂能促进各组分的熔融，有效地改进了所述复合材料熔融体的流动性，减小了加工过程中复合材料溶体与加工机械间的摩擦，同时具有较好的脱模作用，缩短了注塑周期。
一种如上所述无卤阻燃增强聚对苯二酰对苯二胺复合材料制备方法，
a：按重量配比称取上述各原料，混合均匀；
b：将a中混合好的原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度280-320℃，二区温度280-330℃，三区温度280-330℃，四区温度280-330℃，机头275-310℃，停留时间1~2min，压力为12-18MPa。
本发明的有益效果为：本发明所提供的无卤阻燃增强聚对苯二酰对苯二胺复合材料不含卤素，在使用过程中不会因其材料的分解而放出有害气体，对大气和水等无污染，且阻燃性好，电绝缘性能优异，漏电起痕值高，比重低，机械性能优良，可与有卤阻燃材料相媲美，可广泛应用于家电配件、电子产品配件、汽车配件等。
具体实施方式
本发明中提供的一种无卤阻燃增强尼龙复合材料，其包括以下重量份比例的组分：聚对苯二酰对苯二胺35～70％；增强剂5～35％；主抗氧剂0.2～0.5％；辅助抗氧剂0.2～0.5％；阻燃剂A 7～10％；阻燃剂B 15～25％；润滑剂0.5～1％。在本发明中，聚对苯二酰对苯二胺的CAS NO.为97162-59-9，所述增强剂采用玻璃纤维(CAS NO.为65997-17-2)，所述主抗氧剂采用有机亚磷酸酯，具体为三(2，4-二叔丁基苯基)亚磷酸酯(CAS NO.为31570-04-4)，所述辅助抗氧剂为N，N-双-[3-(3，5-二叔丁基-4-羟基苯基)丙酰基]己二胺(CASNO.为23128-74-7)，所述阻燃剂采用三聚氰胺磷酸盐(CAS NO.为218768-84-4)和次膦酸酯(CAS NO.为6303-21-5)，所述润滑剂采用蒙旦腊，具体为褐煤蜡酸-1-甲基-1，3-丙二基酯(CAS NO.73138-44-0)与脂肪酸-褐煤蜡钙盐(CAS NO.为68308-22-5)的共混物。
为便于对本发明进一步理解，现结合具体实施例对本发明进行详细描述。
实施例1：
将聚对苯二酰对苯二胺重量比为39.5％；(以下均为重量比)增强剂35％；主抗氧剂0.3％；辅助抗氧剂0.2％；阻燃剂A 7％；阻燃剂B 17％；润滑剂1％。放入双螺杆挤出机中混合，双螺杆挤出机的螺杆直径为30～90mm，螺杆长度与直径的比例设定为36～40，加工工艺如下：双螺杆挤出机一区温度280℃，二区温度310℃，三区温度320℃，四区温度300℃，机头300℃，停留时间1～2min，压力为12-18MPa。
实施例2：将聚对苯二酰对苯二胺重量比为56.7％；(以下均为重量比)增强剂15％；主抗氧剂0.2％；辅助抗氧剂0.4％；阻燃剂A7％；阻燃剂B 20％；润滑剂0.7％。放入双螺杆挤出机中混合，双螺杆挤出机的螺杆直径为30～90mm，螺杆长度与直径的比例设定为36～40，加工工艺如下：双螺杆挤出机一区温度280℃，二区温度310℃，三区温度320℃，四区温度300℃，机头300℃，停留时间1～2min，压力为12-18MPa。
实施例3：将聚对苯二酰对苯二胺重量比为59.6％；(以下均为重量比)增强剂5％；主抗氧剂0.5％；辅助抗氧剂0.5％；阻燃剂A 9％；阻燃剂B 25％；润滑剂0.4％。放入双螺杆挤出机中混合，双螺杆挤出机的螺杆直径为30～90mm，螺杆长度与直径的比例设定为36～40，加工工艺如下：双螺杆挤出机一区温度280℃，二区温度310℃，三区温度320℃，四区温度300℃，机头300℃，停留时间1～2min，压力为12-18MPa。
实施例4：将聚对苯二酰对苯二胺重量比为68％；(以下均为重量比)增强剂6％；主抗氧剂0.2％；辅助抗氧剂0.3％；阻燃剂A 10％；阻燃剂B 15％；润滑剂0.5％。放入双螺杆挤出机中混合，双螺杆挤出机的螺杆直径为30～90mm，螺杆长度与直径的比例设定为36～40，加工工艺如下：双螺杆挤出机一区温度280℃，二区温度310℃，三区温度320℃，四区温度300℃，机头300℃，停留时间1～2min，压力为12-18MPa。
表1
  原料名称  实施例1(wt％)  实施例2(wt％)  实施例3(wt％)   实施例4(wt％)
  聚对苯二酰对苯二胺   39.5   56.7   59.6   68
  玻璃纤维   35   15   5   6
  辅助抗氧剂   0.2   0.4   0.5   0.3
  主抗氧剂   0.3   0.2   0.5   0.2
  三聚氰胺磷酸盐   7   7   9   10
  次膦酸酯   17   20   25   15
  蒙旦蜡   1   0.7   0.4   0.5
将上述四个实施例制备的无卤阻燃增强聚对苯二酰对苯二胺复合材料样品测试性能，其结果和采用标准如表2所示，与传统的溴-锑阻燃体系测试结果对比可知，本发明复合材料的机械性能接近传统的溴-锑阻燃体系的机械性能，且阻燃效果和含卤体系的阻燃效果相当，耐电弧CTI值高于含卤体系，故本发明产品性能完全达到家电配件、电子产品配件等对塑料材料的性能需求，具有广阔的应用前景。
表2
  测试项目   测试标准   实施例1   实施例2   实施例3   实施例4   溴-锑阻燃体系(35％玻璃纤维)
  密度(g/cm3)   ISO1183   1.50   1.35   1.25   1.24   1.67
  垂直成型收缩率(％)   ISO 294-4   0.4   0.7   1.4   1.3   0.6
  平行成型收缩率(％)   ISO 294-4   0.3   0.5   0.9   0.8   0.3
  拉伸强度(Mpa)   ISO527   170   140   100   96   180
  断裂伸长率(％)   ISO527   2   3   5   5   3
  弯曲强度(Mpa)   ISO178   260   225   150   145   275
  弯曲模量(Mpa)   ISO178   9800   8100   4000   3800   10000
  缺口冲击强度(KJ/m2)   ISO180   14   10   5   4.5   15
  无缺口冲击强度(KJ/m2)   ISO180   60   40   18   16   65
  熔点(℃)   ISO3146-C   305-315   305-315   305-315   305-315   305-315
  热变形温度(66psi)   ISO75-1   295   290   290   290   300
  热变形温度(264psi)   ISO75-2   290   285   280   275   290
  0.8mm阻燃等级   ISO1210/UL94   V-0   V-0   V-0   V0   V-0
  灼热丝(℃)   IEC695-2-1   960   960   960   960   960
  耐电弧CTI(Volt)   UL-746A   600   550   500   500   300
以上对本发明所提供的一种无卤阻燃增强聚对苯二酰对苯二胺复合材料进行了详细介绍，本文中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处，综上所述，本说明书内容不应理解为对本发明的限制。

Claims (4)

1.一种无卤阻燃增强聚对苯二酰对苯二胺复合材料，其特征在于，
其组成按重量配比为(％)：
聚对苯二酰对苯二胺  35～70％；
增强剂              5～35％；
主抗氧剂            0.2～0.5％；
辅助抗氧剂          0.2～0.5％；
阻燃剂A             7～10％；
阻燃剂B             15～25％；
润滑剂              0.5～1％；
其中，所述主抗氧剂为有机亚磷酸酯，所述有机亚磷酸酯为三(2，4-二叔丁基苯基)亚磷酸酯；所述辅助抗氧剂为N，N-双-[3-(3，5-二叔丁基-4-羟基苯基)丙酰基]己二胺；所述阻燃剂A为三聚氰胺磷酸盐，阻燃剂B为次膦酸盐。
2.根据权利要求1所述的无卤阻燃增强聚对苯二酰对苯二胺复合材料，其特征在于：所述的增强剂为玻璃纤维。
3.根据权利要求1所述的无卤阻燃增强聚对苯二酰对苯二胺复合材料，其特征在于：所述的润滑剂为蒙旦蜡，所述蒙旦蜡为褐煤蜡酸-1-甲基-1，3-丙二基酯与脂肪酸-褐煤蜡钙盐的共混物。
4.一种如权利要求1所述无卤阻燃增强聚对苯二酰对苯二胺复合材料制备方法，
a：按重量配比称取上述各原料，混合均匀；
b：将a中混合好的原料投入到双螺杆挤出机的加料斗，经熔融挤出，造粒；加工工艺如下：双螺杆挤出机一区温度280-320℃，二区温度280-330℃，三区温度280-330℃，四区温度280-330℃，机头275-310℃，停留时间1～2min，压力为12-18MPa。
CN2008102415282A 2008-12-23 2008-12-23 无卤阻燃增强聚对苯二酰对苯二胺复合材料 Expired - Fee Related CN101508843B (zh)

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