CN102634194A - 一种阻燃的无机纤维填充的聚酰胺材料的制备方法 - Google Patents

一种阻燃的无机纤维填充的聚酰胺材料的制备方法 Download PDF

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CN102634194A
CN102634194A CN2012101282947A CN201210128294A CN102634194A CN 102634194 A CN102634194 A CN 102634194A CN 2012101282947 A CN2012101282947 A CN 2012101282947A CN 201210128294 A CN201210128294 A CN 201210128294A CN 102634194 A CN102634194 A CN 102634194A
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polyamide material
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叶法冬
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CHANGSHU CITY FADONG PLASTIC INDUSTRY Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03Extrusion 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
    • B29C48/04Particle-shaped
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/36Means for plasticising or homogenising the moulding material or forcing it through the nozzle or die
    • B29C48/395Means 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
    • B29C48/40Means 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/78Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling
    • B29C48/875Thermal treatment of the extrusion moulding material or of preformed parts or layers, e.g. by heating or cooling for achieving a non-uniform temperature distribution, e.g. using barrels having both cooling and heating zones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/25Component parts, details or accessories; Auxiliary operations
    • B29C48/92Measuring, controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92504Controlled parameter
    • B29C2948/92704Temperature
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B29WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29CSHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C2948/00Indexing scheme relating to extrusion moulding
    • B29C2948/92Measuring, controlling or regulating
    • B29C2948/92819Location or phase of control
    • B29C2948/92857Extrusion unit
    • B29C2948/92876Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895Barrel or housing

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  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

一种阻燃的无机纤维填充的聚酰胺材料的制备方法,属于高分子材料制备技术领域。包括以下步骤:按重量份数称取聚已内酰胺树脂 120-125 份、尼龙 66 树脂 50-56 份、偶联剂 1.2-1.8 份、云母 40-52 份和阻燃剂 30-41 份,并且投入高速混合机中混合,而后投入按重量份数称取的抗氧剂 1.0-2.0 份和玻璃纤维 65-76 份,并且继续混合,得到造粒料;将得到的造粒料投入双螺杆挤出机中熔融挤出,并且控制双螺杆挤出机的挤出温度,得到阻燃的无机纤维填充的聚酰胺材料。优点:拉伸强度大于 120MPa ,弯曲强度大于 230MPa, 悬臂梁缺口冲击强度大于 26kj/m 2 , 熔融指数大于 23g/10min ,阻燃性达到 UL-94-V-0 3mm )等级。

Description

一种阻燃的无机纤维填充的聚酰胺材料的制备方法
技术领域
本发明属于高分子材料制备技术领域,具体涉及一种阻燃的无机纤维填充的聚酰胺材料的制备方法。
背景技术
由二元酸与二元胺合成的分子链中含有酰胺键的材料具有优异的性能,广泛用于各行各业中。这类材料具有很好的耐候性,耐温性,但是缺乏对抑制燃烧的特性,并且燃烧产生一些难闻的气味,因此有必要通过合理的原料选择和制备工艺加以改进,对此本申请人作了有益的尝试,下面将要介绍的技术方案便是在这种背景下产生的。
发明内容
本发明的任务在于提供一种阻燃的无机纤维填充的聚酰胺材料的制备方法,该方法工艺步骤十分简便并且能使获得的聚酰胺材料具有优异的机械强度和阻燃性。
本发明的任务是这样来完成的,一种阻燃的无机纤维填充的聚酰胺材料的制备方法,包括以下步骤:
A)制备造粒料,按重量份数称取聚己内酰胺树脂120-125份、尼龙66树脂50-56份、偶联剂1.2-1.8份、云母40-52份和阻燃剂30-41份,并且投入高速混合机中混合,而后投入按重量份数称取的抗氧剂1.0-2.0份和玻璃纤维65-76份,并且继续混合,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,并且控制双螺杆挤出机的挤出温度,得到阻燃的无机纤维填充的聚酰胺材料。
在本发明的一个具体的实施例中,所述的聚己内酰胺树脂树脂是指熔点在220℃的尼龙6树脂。
在本发明的另一个具体的实施例中,所述的尼龙66树脂是指熔点在210℃的树脂。
在本发明的又一个具体的实施例中,所述的偶联剂是指异丙基三乙氧基硅烷。
在本发明的再一个具体的实施例中,所述的云母是指白云母。
在本发明的还有一个具体的实施例中,所述的阻燃剂是指八溴二苯醚。
在本发明的更而一个具体的实施例中,所述的抗氧剂是指双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯。
在本发明的进而一个具体的实施例中,所述的玻璃纤维是指长度为3mm的无碱短切玻璃纤维。
在本发明的又更而一个具体的实施例中,所述的混合的时间为10-13min;所述的继续混合的时间为7-10min。
在本发明的又进而一个具体的实施例中,所述的控制双螺杆挤出机的挤出温度是将温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃。
本发明的制备方法工艺步骤十分简练,得到的阻燃的无机纤维填充的聚酰胺材料具有如下优异的技术指标:拉伸强度大于120MPa,弯曲强度大于230MPa,悬臂梁缺口冲击强度大于26kj/m2,熔融指数大于23g/10min,阻燃性达到UL-94-V-0(3mm)等级。
具体实施方式
实施例1:
A)制备造粒料,按重量份数称取聚己内酰胺树脂树脂即熔点在220℃的尼龙6树脂120.2份、尼龙66树脂(熔点在210℃)50.1份、偶联剂即异丙基三乙氧基硅烷1.2份、云母即白云母40.1份和阻燃剂即八溴二苯醚30.3份,并且投入高速混合机中混合10min,而后投入按重量份数称取的抗氧剂即双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯1.0份和长度为3mm的无碱短切玻璃纤维65.4份,并且继续混合7min,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,双螺杆挤出机的挤出温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃,得到阻燃的无机纤维填充的聚酰胺材料。
实施例2:
A)制备造粒料,按重量份数称取聚己内酰胺树脂树脂即熔点在220℃的尼龙6树脂122.6份、尼龙66树脂(熔点在210℃)51.4份、偶联剂即异丙基三乙氧基硅烷1.5份、云母即白云母45.8份和阻燃剂即八溴二苯醚34.5份,并且投入高速混合机中混合13min,而后投入按重量份数称取的抗氧剂即双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯1.3份和长度为3mm的无碱短切玻璃纤维68.9份,并且继续混合10min,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,双螺杆挤出机的挤出温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃,得到阻燃的无机纤维填充的聚酰胺材料。
实施例3:
A)制备造粒料,按重量份数称取聚己内酰胺树脂树脂即熔点在220℃的尼龙6树脂123.8份、尼龙66树脂(熔点在210℃)53.8份、偶联剂即异丙基三乙氧基硅烷1.6份、云母即白云母48.9份和阻燃剂即八溴二苯醚38.7份,并且投入高速混合机中混合11min,而后投入按重量份数称取的抗氧剂即双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯1.7份和长度为3mm的无碱短切玻璃纤维72.5份,并且继续混合8min,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,双螺杆挤出机的挤出温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃,得到阻燃的无机纤维填充的聚酰胺材料。
实施例4:
A)制备造粒料,按重量份数称取聚己内酰胺树脂树脂即熔点在220℃的尼龙6树脂125.4份、尼龙66树脂(熔点在210℃)55.8份、偶联剂即异丙基三乙氧基硅烷1.8份、云母即白云母51.6份和阻燃剂即八溴二苯醚40.7份,并且投入高速混合机中混合12min,而后投入按重量份数称取的抗氧剂即双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯2.0份和长度为3mm的无碱短切玻璃纤维76份,并且继续混合9min,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,双螺杆挤出机的挤出温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃,得到阻燃的无机纤维填充的聚酰胺材料。
由上述实施例1至4得到的阻燃的无机纤维填充的聚酰胺材料具有下表所示的技术效果。
  测试项目   实施例1   实施例2   实施例3   实施例4
  拉伸强度MPa   120   122   125   127
  弯曲强度MPa   230   234   236   237
  悬臂梁缺口冲击强度kj/m2   26.0   26.3   26.5   26.7
  熔融指数g/10min   23   23.4   23.6   23.9
  阻燃性(UL-94-V-0-3mm)   V-0   V-0   V-0   V-0

Claims (10)

1.一种阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于包括以下步骤:
A)制备造粒料,按重量份数称取聚已内酰胺树脂120-125份、尼龙66树脂50-56份、偶联剂1.2-1.8份、云母40-52份和阻燃剂30-41份,并且投入高速混合机中混合,而后投入按重量份数称取的抗氧剂1.0-2.0份和玻璃纤维65-76份,并且继续混合,得到造粒料;
B)造粒,将由步骤A)得到的造粒料投入双螺杆挤出机中熔融挤出,并且控制双螺杆挤出机的挤出温度,得到阻燃的无机纤维填充的聚酰胺材料。
2.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的聚已内酰胺树脂树脂是指熔点在220℃的尼龙6树脂。
3.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的尼龙66树脂是指熔点在210℃的树脂。
4.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的偶联剂是指异丙基三乙氧基硅烷。
5.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的云母是指白云母。
6.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的阻燃剂是指八溴二苯醚。
7.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的抗氧剂是指双(2,4二叔丁基苯基)季戊四醇二亚磷酸酯。
8.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的玻璃纤维是指长度为3㎜的无碱短切玻璃纤维。
9.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的混合的时间为10-13min;所述的继续混合的时间为7-10min。
10.根据权利要求1所述的阻燃的无机纤维填充的聚酰胺材料的制备方法,其特征在于所述的控制双螺杆挤出机的挤出温度是将温度控制为:一区235℃、二区245℃、三区245℃、四区250℃、五区250℃和六区245℃
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