CN103374197A - 一种高强度碳纤维增强聚醚醚酮复合材料及其制备方法 - Google Patents

一种高强度碳纤维增强聚醚醚酮复合材料及其制备方法 Download PDF

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CN103374197A
CN103374197A CN2012101149315A CN201210114931A CN103374197A CN 103374197 A CN103374197 A CN 103374197A CN 2012101149315 A CN2012101149315 A CN 2012101149315A CN 201210114931 A CN201210114931 A CN 201210114931A CN 103374197 A CN103374197 A CN 103374197A
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马刚
张宇
李婷婷
童艳玲
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Heilongjiang Xinda Enterprise Group Co Ltd
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Abstract

本发明属于特种工程塑料领域，具体涉及一种高强度碳纤增强聚醚醚酮复合材料及其制备方法。复合材料含65-90wt％的聚醚醚酮树脂，0-5wt％的耐高温润滑剂，10-30wt％的高强碳纤维。聚醚醚酮树脂的熔融指数为12-80g/10min，耐高温润滑剂为高分子量聚硅氧烷和科莱恩公司的蒙旦蜡。所使用的碳纤为德国西格里的高强短切碳纤，表面经包覆改性。制得的聚醚醚酮复合材料具有高强度、高模量和高耐热的特点，可广泛应用于航空航天、武器装备以及高端民用领域，例如耐高温接插件等。

Description

一种高强度碳纤维增强聚醚醚酮复合材料及其制备方法
技术领域
本发明属于高性能聚合物领域，具体涉及一种高强度碳纤增强聚醚醚酮复合材料及其制备方法。
背景技术
PEEK是一种典型的热塑性高性能聚合物，具有耐高温、耐溶剂、耐老化、耐水解以及极高的比强度、比模量等性能，特别是在高温高湿的恶劣环境中仍然能保持良好的综合性能，因此，在对材料性能要求越来越高的今天，PEEK及其复合材料的重要性日益凸显。但是如今科技飞速发展，对材料的性能要求也在不断提高，尤其航空航天领域，要求重量轻的同时，还要求极高的强度和模量，很多领域要求非常高的热变形温度，而这些都是纯PEEK树脂无法达到的，所以必须对其进行增强处理。
碳纤是传统的增强填料，对提高强度和耐热性有显著的作用，但是普通碳纤无法满足高端市场对材料的要求，为此本发明选用德国西格里的高强碳纤。碳纤的表面为亲水性，和树脂基的相容性不好，传统的硅烷偶联剂等虽然可以明显改性碳纤和树脂的相容性，但是其耐热等级低，结构上和PEEK相差较大，无法起到增容作用，因此我们选用和PEEK相容性非常好的PES，PEI等树脂溶液来包覆碳纤，可以起到明显的界面增强作用。碳纤在树脂基体中的分散和长径比是其增强效果的关键，通常采用连续碳纤从第一排气口导入的方法引入碳纤，碳纤受到强烈的剪切作用，破损较大，本发明采用短切碳纤，从接近机头口模的第二侧喂料口加入碳纤，碳纤受到的剪切作用较小，可以保持完整，从而具有更高的长径比，更好的增强效果。
PEEK熔体黏度较大，加入碳纤后加工性变差，为此本发明加入了耐高温润滑剂，可以有效的降低熔体黏度，提高碳纤的分散性，并减少碳纤外露的情况，是产品性能更好，外观更美观。
发明内容
本发明的目的是通过失重秤和侧喂料技术加入短切纤维来制备一种具有高强度的聚醚醚酮复合材料。
本发明制备的复合材料具有良好的力学性能、耐热性以及相对较低的成本。
本发明的高强度高耐热聚醚醚酮复合材料，其特征在于：各组分和按100wt％计算，含65-90wt％熔融指数为12-80g/10min的聚醚醚酮树脂，0-5wt％的耐高温偶联剂，10-30wt％的碳纤维。
聚醚醚酮(PEEK)的对数比浓粘度为0.76-0.80，熔融指数为12g/10min、21g/10min和80g/10min其结构式如(I)所示，n为≥1的整数，表示聚合度。
Figure BSA00000703421100021
耐高温润滑剂为高分子量聚硅氧烷和蒙旦蜡。偶联剂可以在增强材料与树脂基体之间形成一个界面层，有效的传递应力，从而提高复合材料的性能。而常用的市售偶联剂难以承受聚醚醚酮高达360℃的加工温度，并且结构也与聚醚醚酮差异较大，因此难以应用在聚醚醚酮行业。为此，我们选用了和PEEK相容性好的几种耐高温树脂包覆改性短切碳纤；
本发明所述的聚醚醚酮复合材料制备步骤为：
(1)将短切碳纤加入反应釜中，加入不同种类的耐高温树脂溶液一种或几种，在100℃条件下搅拌一小时，抽滤，100℃烘干。
(2)将PEEK，耐高温润滑剂和短切碳纤分别加入第一、第二、第三失重秤，从主喂料口加入PEEK和耐高温润滑剂，从第二侧喂料口加入碳纤，通过失重秤精确调节配方中各组分含量，加工温度从320℃～380℃。
(3)将挤出的料条经传送带传输、空气冷切、切粒即得到本发明所述的高强度碳纤增强聚醚醚酮复合材料。
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说明，但本发明并不局限于以下实施例。
实施例1：
设定双螺杆挤出机各工艺段温度为320℃、340℃、355℃、355℃、355℃、355℃、355℃、355℃、350℃、340℃，温度达到设定值后，首先开启第一失重秤，以20Kg/h的喂料速度从主喂料口加入PEEK粉料，其中PEEK熔指为21g/10min，待口模挤出PEEK后，开启第二失重秤，以0.45Kg/h的速度加入耐高温润滑剂，待挤出机运行平稳后，开启侧喂料和第三失重秤，以2.27Kg/h的速度加入短切碳纤，控制双螺杆转速为300～500Rad/min，扭矩不超过80％，机头熔体温度不超过400℃，得到PEEK含量88％，耐高温润滑剂含量2％，碳纤含量10％的复合材料。调整喂料参数，得到不同的配方，配方见表1，各配方性能见表2.
表1不同配方各组分含量
Figure BSA00000703421100031
表2不同配方性能比较
Figure BSA00000703421100032
由表中可以看出，高强碳纤的加入可以显著提高PEEK的强度和耐热性，并且随着碳纤含量的增加，材料的强度和耐热性都在提高，润滑剂含量的增加，可以改善材料的加工性能，提高碳纤的分散性，从而使材料性能有所提高。

Claims (5)

1.一种高强度碳纤维增强聚醚醚酮复合材料，其特征在于：各组分和按100wt％计算，含65-90wt％熔融指数为12-80g/10min的聚醚醚酮树脂，0-5wt％的耐高温润滑剂，10-30wt％的高强短切碳纤维。
2.如权利要求1所述的高强度聚醚醚酮复合材料，其特征在于：各组分和按100wt％计算，含65-90wt％的聚醚醚酮树脂，10-30wt％的高强短切碳纤维，0-5wt％的耐高温润滑剂，耐高温润滑剂为高分子量聚硅氧烷和科莱恩公司的蒙旦蜡中的一种或者两种。
3.如权力要求1中所述的碳纤为德国西格里公司生产的高强度短切碳纤，长度为6mm，表面经耐高温树脂溶液包覆处理。
4.如权力要求3中所述的耐高温树脂溶液具体包括聚醚砜(PES)溶液、聚醚酰亚胺(PEI)、可溶性聚芳醚酮中的一种或几种。
5.如权利要求1所述的高强度聚醚醚酮复合材料的制备方法为：
1)首先将短切碳纤放入反应釜中，加入一种或几种耐高温树脂溶液，其中所含树脂和短切碳纤的质量比为：1∶100～5∶100，在100℃条件下搅拌一小时，抽滤后100℃烘干。
2)将聚醚醚酮树脂、耐高温润滑剂和改性处理后的高强短切碳纤分别放入第一、第二、第三失重秤，通过失重式喂料精确控制配方比例和混合效果；
3)首先开启第一失重秤，在主喂料口加入聚醚醚酮，挤出纯聚醚醚酮树脂，各个工艺段温度分别为320℃、340℃、355℃、355℃、355℃、355℃、355℃、355℃、350℃、340℃；
4)挤出平稳后，开启第二失重秤，在主喂料口加入耐高温润滑剂，加工温度不变。
5)挤出平稳后，开启侧喂料螺杆和第三失重秤，将短切碳纤从第二侧喂料口，即靠近机头口模的位置加入。
6)调整失重秤参数，控制不同碳纤含量配方的挤出，并根据碳纤含量调整挤出温度参数，碳纤含量越高，加工段温度越高，口模温度越低：
7)挤出的料条经传送带传输、空气冷切、切粒机切粒，得到圆柱状颗粒，即为高强度碳纤增强聚醚醚酮复合材料。 
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CN104629254A (zh) * 2015-02-12 2015-05-20 华中科技大学 一种连续纤维增强聚醚醚酮复合材料预浸带的制造方法及设备
CN104927298A (zh) * 2015-06-30 2015-09-23 吉林大学 一种聚醚醚酮基耐磨复合材料、制备方法及其在减摩耐磨方面的应用
CN105199313A (zh) * 2014-06-13 2015-12-30 黑龙江鑫达企业集团有限公司 一种高尺寸稳定性、耐磨性优异的peek阀片复合材料
CN105315474A (zh) * 2014-06-13 2016-02-10 黑龙江鑫达企业集团有限公司 一种利用特制偶联剂处理碳纤维增强peek的制备方法
CN105641752A (zh) * 2016-01-22 2016-06-08 上海雪枫精密机械有限公司 工程塑料及制备方法和在制备外科手术器械中的应用
CN106633627A (zh) * 2017-01-05 2017-05-10 吉林大学 聚醚醚酮/纳米氧化锌/碳纤维耐磨复合材料、制备方法及在机械抛光保持环方面的应用
CN106751443A (zh) * 2016-11-23 2017-05-31 大连路阳科技开发有限公司 金属衬塑耐腐蚀耐摩擦复合材料及制备方法和应用
CN107629401A (zh) * 2017-09-22 2018-01-26 南京肯特复合材料股份有限公司 耐高温防自转十字滑环及其制备方法
CN108125713A (zh) * 2017-12-28 2018-06-08 武汉康斯泰德科技有限公司 长链碳纤维peek外包裹热成型骨固定板及成型方法
CN111732815A (zh) * 2020-07-13 2020-10-02 扬州市维纳复合材料科技有限公司 功能聚醚醚酮碳纤复合材料的制备方法
CN113248863A (zh) * 2021-04-02 2021-08-13 南京聚隆科技股份有限公司 一种可激光焊接的碳纤维改性peek材料及其制备方法
CN113908633A (zh) * 2021-10-25 2022-01-11 安徽欣创节能环保科技股份有限公司 基于高强度滤袋的低阻高效袋式除尘器

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CN105199313A (zh) * 2014-06-13 2015-12-30 黑龙江鑫达企业集团有限公司 一种高尺寸稳定性、耐磨性优异的peek阀片复合材料
CN105315474A (zh) * 2014-06-13 2016-02-10 黑龙江鑫达企业集团有限公司 一种利用特制偶联剂处理碳纤维增强peek的制备方法
CN104629254A (zh) * 2015-02-12 2015-05-20 华中科技大学 一种连续纤维增强聚醚醚酮复合材料预浸带的制造方法及设备
CN104927298A (zh) * 2015-06-30 2015-09-23 吉林大学 一种聚醚醚酮基耐磨复合材料、制备方法及其在减摩耐磨方面的应用
CN105641752A (zh) * 2016-01-22 2016-06-08 上海雪枫精密机械有限公司 工程塑料及制备方法和在制备外科手术器械中的应用
CN106751443A (zh) * 2016-11-23 2017-05-31 大连路阳科技开发有限公司 金属衬塑耐腐蚀耐摩擦复合材料及制备方法和应用
CN106751443B (zh) * 2016-11-23 2019-02-22 大连路阳科技开发有限公司 金属衬塑耐腐蚀耐摩擦复合材料及制备方法和应用
CN106633627A (zh) * 2017-01-05 2017-05-10 吉林大学 聚醚醚酮/纳米氧化锌/碳纤维耐磨复合材料、制备方法及在机械抛光保持环方面的应用
CN107629401A (zh) * 2017-09-22 2018-01-26 南京肯特复合材料股份有限公司 耐高温防自转十字滑环及其制备方法
CN108125713A (zh) * 2017-12-28 2018-06-08 武汉康斯泰德科技有限公司 长链碳纤维peek外包裹热成型骨固定板及成型方法
CN108125713B (zh) * 2017-12-28 2024-02-23 武汉康斯泰德科技有限公司 长链碳纤维peek外包裹热成型骨固定板及成型方法
CN111732815A (zh) * 2020-07-13 2020-10-02 扬州市维纳复合材料科技有限公司 功能聚醚醚酮碳纤复合材料的制备方法
CN113248863A (zh) * 2021-04-02 2021-08-13 南京聚隆科技股份有限公司 一种可激光焊接的碳纤维改性peek材料及其制备方法
CN113248863B (zh) * 2021-04-02 2024-02-27 南京聚隆科技股份有限公司 一种可激光焊接的碳纤维改性peek材料及其制备方法
CN113908633A (zh) * 2021-10-25 2022-01-11 安徽欣创节能环保科技股份有限公司 基于高强度滤袋的低阻高效袋式除尘器

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