CN101591470B - 一种填充增韧pa66复合材料及其制备方法 - Google Patents

一种填充增韧pa66复合材料及其制备方法 Download PDF

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CN101591470B
CN101591470B CN200810038317A CN200810038317A CN101591470B CN 101591470 B CN101591470 B CN 101591470B CN 200810038317 A CN200810038317 A CN 200810038317A CN 200810038317 A CN200810038317 A CN 200810038317A CN 101591470 B CN101591470 B CN 101591470B
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CN101591470A (zh
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刘正军
张祥福
周文
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Shanghai Pret Composites Co Ltd
Zhejiang Pret New Materials Co Ltd
Chongqing Pret New Materials Co Ltd
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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
    • 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
    • B29C48/88—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
    • B29C48/25—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
    • 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
    • B29C2948/92504—Controlled parameter
    • B29C2948/9258—Velocity
    • B29C2948/9259—Angular velocity
    • 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
    • B29C2948/92504—Controlled parameter
    • B29C2948/92704—Temperature
    • 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
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92885—Screw or gear
    • 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
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92876—Feeding, melting, plasticising or pumping zones, e.g. the melt itself
    • B29C2948/92895—Barrel or housing
    • 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
    • B29C2948/92819—Location or phase of control
    • B29C2948/92857—Extrusion unit
    • B29C2948/92904—Die; Nozzle zone

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  • Mechanical Engineering (AREA)
  • Physics & Mathematics (AREA)
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Abstract

本发明公开了一种填充增韧PA66复合材料及其制备方法，按重量比包括以下组分：PA66树脂50～94.8％，无机填料5～45％，填料处理剂0.01-1％，其他助剂0.1～10％。该方法具体步骤如下：称取这些材料，在高速混料机混合3-5分钟，将混匀的物料加入双螺杆挤出机，自喂料口至挤出模头温度分别是220～240℃，230～250℃，230～250℃，220～250℃，240～270℃，主机转速是40～50赫兹，然后用塑料注塑机制样。该复合材料耐冲击，易加工，平整度好。

Description

一种填充增韧PA66复合材料及其制备方法
技术领域
本发明涉及一种尼龙66复合材料，具体为一种填充增韧PA66复合材料及其制备方法，属于高分子复合材料领域。
背景技术
PA66是很重要的工程塑料，被应用在汽车、电子、建筑等方面。但纯的PA66树脂容易吸水，强度下降很多，限制了它的应用范围。为了克服PA66的这些缺点，一般通用的方法是用无机填料填充PA66，提高复合材料的强度和耐热，降低材料的吸水率，延长材料的使用时间。
由于无机填料与有机的PA66不能完全相容，导致复合材料的冲击性能变差，尤其是材料的无缺口冲击性能。为了提高材料的耐冲性能，国外的研究人员作了一些相关的研究，主要有：Payne等在USP.5013786介绍了用乙烯丙烯酸丁酯作相容剂和增韧剂，30％硅灰石填充PA6缺口冲击为86J/m，弯曲强度为4500MPa；Freeman等在USP.5571851中用氨基硅烷偶联剂处理，40％煅烧石灰填充PA66的缺口冲击为27～52J/m，弯曲模量为5790～5980MPa。
从上述的这些专利可以看出，用增韧剂能提高冲击性能，但强度下降得比较多；而单纯用硅烷偶联剂的话，冲击性能与纯的PA66相类似，不能提高耐冲击性能。
发明内容
本发明所要解决的技术问题在于克服现有技术中存在的上述不足，提供一种填充增韧PA66复合材料及其制备方法。
其发明目的可以通过以下技术方案得以实现。
一种填充增韧PA66复合材料，包括以下组分(重量百分比)：
PA66树脂    50～94.8％
无机填料    5～45％
填料处理剂  0.01～1％
其他助剂    0.1～10％
本发明所述的填充增韧PA66复合材料中PA66树脂是中粘尼龙66，其特征粘数为2.6～2.8。
本发明所述的填充增韧PA66复合材料中无机填料是硅灰石，其长径比为5～40。
本发明所述的填充增韧PA66复合材料中填料处理剂是钛酸酯偶联剂。
本发明所述的填充增韧PA66复合材料中其他助剂是阻燃剂、润滑剂、抗氧剂或颜色助剂。
制备填充增韧PA66复合材料的具体步骤如下：按上述组份配比称取材料，在高速混料机混合3-5分钟，然后将混合均匀的物料加入双螺杆挤出机，自喂料口至挤出模头温度分别是220～240℃，230～250℃，230～250℃，220～250℃，240～270℃，主机转速是40～50赫兹，然后用塑料注塑机制得各种所需产品。
本发明所述的填充增韧PA66复合材料，机械强度高，耐冲击性能好，易加上。
具体实施方式
下面通过实施例和对比例进一步说明本发明，在不违反本发明的宗旨下，本发明应不限于以下实验例具体明示的内容。
实施例和对比例所用原材料如下：
PA66树脂，FYR-27D，中国神马公司；
硅灰石，NYGLOS 10012，美国NYCO公司；
玻璃微珠，050-20-215，法国SOVITEC公司
核壳聚合物MBS，E-920，北京普利宏斌化工材料公司
钛酸酯偶联剂，NDZ-201，浙江杭州沸点公司
硅烷偶联剂，KH-550，南京曙光化工有限公司；
抗氧剂，168和1010，瑞士汽巴精化公司。
按重量百分比称起各种原材料，在高速混合器中干混3～5分钟之后；将混合好的原料置于双螺杆机中(玻璃纤维在排气口加入)，经熔融挤出，造粒。将得到的切片粒子在80℃的鼓风烘箱中干燥8小时后，用宁波海天HT1150B注射成型机制样。
材料的力学性能测试按照ISO标准测试：测试拉伸强度的样条是170*10*4mm，按ISO 527进行，速度为50mm/min；测试弯曲模量的样条是80*10*4mm，按ISO 178进行，速度为2mm/min；测试冲击强度的样条是80*10*4mm，按ISO 179进行，摆锤为4J；测试缺口冲击强度的样条是80*10*4mm，按ISO 179进行，V型缺口，摆锤为4J；测试热变形温度的样条是120*10*4mm，按ISO 75进行，负荷为1.8MPa，升温速度为120℃/h。
实施例1～4
复合材料中各种原材料的重量百分比如表1所示，双螺杆挤出机的温度分别是(自喂料口至挤出模头)：230℃，240℃，245℃，240℃，255℃。主机转速是45赫兹。
表1实施例1-4配方及材料性能表
  1   2   3   4
  PA66(％)   94.5   84.3   69   53.7
  NYGLOS(％)   5   15   30   45
  NDZ-201(％)   0.1   0.3   0.6   0.9
  168(％)   0.2   0.2   0.2   0.2
  1010(％)   0.2   0.2   0.2   0.2
  拉伸强度(MPa)   77   86   96   93
  弯曲模量(MPa)   3010   3640   5760   6270
  冲击强度(kJ/m^2)   不断   不断   不断   不断
  缺口冲击强度(kJ/m^2)   5.3   8.7   8.5   8.3
  热变形温度(℃)   72   82   101.3   107
实施例5～7
复合材料中各种原材料的重量百分比如表2所示，双螺杆挤出机的温度分别是(自喂料口至挤出模头)：230℃，240℃，245℃，240℃，255℃。主机转速是45赫兹。
表2实施例5-7配方及材料性能表
  5   6   7
  PA66(％)   84.5   84.2   84
  NYGLOS(％)   15   15   15
  NDZ-201(％)   0.1   0.4   0.6
  168(％)   0.2   0.2   0.2
  1010(％)   0.2   0.2   0.2
  拉伸强度(MPa)   83.6   86.8   85.9
  弯曲模量(MPa)   3570   3690   3590
  冲击强度(kJ/m^2)   不断   不断   不断
  缺口冲击强度(kJ/m^2)   8.9   8.8   8.4
热变形温度(℃) 81 82.3 82.2
对比例1～5
复合材料中各种原材料的重量百分比如表3所示，双螺杆挤出机的温度分别是(自喂料口至挤出模头)：230℃，240℃，245℃，240℃，255℃。主机转速是45赫兹。
表3  对比例1-4配方及材料性能表
  1   2   3   4   5
  PA66(％)   84.6   81.6   84.3   84.6   84.3
  NYGLOS(％)   15   15   15
  玻璃微珠(％)   15   15
  E-920(％)   3
  KH550(％)   0.3
  NDZ-201   0.3
  168(％)   0.2   0.2   0.2   0.2   0.2
1010(％) 0.2 0.2 0.2 0.2 0.2
  拉伸强度(MPa)   81   73   81   72   74
  弯曲模量(MPa)   3340   3010   3220   2960   3060
  冲击强度(kJ/m^2)   全断   5断1   5断3   5断2   5断1
  缺口冲击强度(kJ/m^2) 3.6 7.9 6.5 6.6 4.5
热变形温度(℃) 77 75 73 67 71
从以上表中的数据可以看出：用钛酸酯偶联剂作为硅灰石和PA66的相容剂，在相对低的挤出温度下，提高主机的转速，达到同步提高无机填料填充PA66复合材料力学性能和冲击性能的目的。

Claims (4)

1.一种填充增韧PA66复合材料，其组成和配比为：
上述组份为重量百分比；其中，所述的无机填料是硅灰石，其长径比为5～40；所述的填料处理剂是钛酸酯偶联剂。
2.根据权利要求1所述的一种填充增韧PA66复合材料，其特征在于：所述的PA66树脂是中粘尼龙66，其特征粘数为2.6～2.8。
3.根据权利要求1所述的一种填充增韧PA66复合材料，其特征在于：所述的其他助剂是阻燃剂、润滑剂、抗氧剂或颜色助剂。
4.一种制备权利要求1所述填充增韧PA66复合材料的方法，具体步骤如下：
按权利要求1所述组份配比称取材料，在高速混料机混合3-5分钟，将混匀的物料加入双螺杆挤出机，自喂料口至挤出模头温度分别是220～240℃，230～250℃，230～250℃，220～250℃，240～270℃，主机转速是40～50赫兹。
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