CN113601808B - 一种纤维增强聚酯复合材料的制备方法 - Google Patents
一种纤维增强聚酯复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种纤维增强聚酯复合材料的制备方法,采用纤维增强聚酯复合材料的加工设备,所述的方法具体为:先将无机纤维和聚酯纤维通过特定装置混合分散,再与润滑剂和抗氧剂等助剂分散混合,最后输送到螺杆挤出机进行挤出成型制备得到纤维增强聚酯复合材料。该方法解决了高纤维增强改性过程中的纤维外露问题,能够实现纤维增强聚酯复合材料中纤维与树脂的充分分散浸润,制备得到综合性能和表面外观质量俱佳的复合材料。同时,本发明还公开了实施该方法的加工设备。
Description
技术领域
本发明涉及复合材料领域,具体涉及一种纤维增强聚酯复合材料的制备方法。
背景技术
聚酯是一种由多元醇和多元酸通过缩聚反应制备得到的高分子材料。一般而言,聚酯主要是指聚对苯二甲酸乙二醇酯(PET)和聚对苯二甲酸丁二酯(PBT)等线性热塑性树脂。其具有熔点高、耐热性能出色、电绝缘性能和尺寸稳定性等特点,被广泛应用于电子电器、汽车和家电等领域。
目前,为了进一步显著提高聚酯材料的强度和耐热性,发挥其高熔点和高结晶性能优势,一般而言通过添加一定含量的无机纤维与其进行螺杆挤出改性手段,即可制备得到高强度、高模量和高耐热性的纤维增强聚酯复合材料。在螺杆挤出改性过程中,树脂通常以粒子或者粉末形式、纤维通常以短切纤维束或连续纤维束形式加入到螺杆挤出机中,通过螺杆的高速剪切混合作用来实现树脂与纤维的相互浸润和粘结。由于物料在螺杆挤出机的停留时间短(通常在1-2min)、纤维束形式(纤维根数在1000根以上)存在的纤维难以均匀分散、纤维和树脂难以形成良好的浸润包覆等原因,纤维增强聚酯复合材料的实际性能远远低于理论值,复合材料的性能提高还存在很大的提升空间。
目前,通常采用对纤维进行表面处理的方法来提高纤维增强聚酯复合材料的综合力学性能。如专利申请201810435929中提到了一种碳纤维增强聚酯复合材料的制备方法。该方法是通过先将碳纤维表面包覆热固性树脂上浆剂,在250-350℃条件下进行热处理后,再进行螺杆挤出制备得到拉伸强度在160-220Mpa,弯曲强度在240-290Mpa的高强度碳纤维增强聚酯复合材料。该专利技术的关键在于通过对碳纤维进行表面化学改性来实现纤维与树脂之间结合力和浸润效果的提高,从而达到提高聚酯复合材料的综合性能的目的。但是该技术并没有从根本上解决纤维束形式的纤维与树脂之间的良好浸润包覆问题。
发明内容
有鉴于此,本发明的目的在于提供一种纤维增强聚酯复合材料的制备方法,将纤维与聚酯树脂充分浸润包覆,该方法能够实现同等密度下更高综合性能的纤维增强聚酯复合材料的制备,同时,本发明还公开了实施该方法的加工设备。
一种纤维增强聚酯复合材料的加工设备,包括依次布置的第一传送带、纤维混合装置、第二传送带和双螺杆挤出机;
所述的第一传送带上方设有用于将无机纤维丝和聚酯纤维丝切割成预设长度的切割机构;
所述的纤维混合装置包括进料牵引带、表面布满倒钩的主动辊 、主动辊 型腔和主动辊 位置调节器;
所述的第二传送带上方设有撒粉装置,所述的撒粉装置包括喂料螺杆和振荡器。
作为优选,所述的第一传送带上方设有用于将无机纤维丝和聚酯纤维丝切割成预设长度的切割机构;所述的切割机构包括相对布置的牵引压辊和切割辊。
作为优选,所述纤维混合装置包括进料牵引带、表面布满倒钩的主动辊 、主动辊型腔和主动辊 位置调节器;所述的主动辊 设置在所述主动辊 型腔内。为了保证无机纤维和聚酯纤维的充分分散混合和分散混合效率,可以通过调节主动辊 位置调节器,调整主动辊 和主动辊 型腔之间的距离来实现分散速率和分散混合效率之间的匹配。
所述撒粉装置是由喂料小螺杆和振荡器组成。物料通过小螺杆的转速实现计量下料,再通过振动器实现均匀的撒粉下料。
所述的纤维增强聚酯复合材料的加工设备还包括:依次设置的冷却装置、切粒机、过滤网和储料罐;所述的冷却装置与所述双螺杆挤出机的挤出口连接。
为实现上述目的,本发明提供如下技术方案:一种纤维增强聚酯复合材料的制备方法,该复合材料按重量百分比(wt%)由以下组分组成:
进一步优选为:
在上述的纤维增强聚酯复合材料中,所述聚酯纤维为聚对苯二甲酸乙二醇酯(PET)纤维或聚对苯二甲酸丁二醇酯(PBT)纤维或聚对苯二甲酸1.3 丙二醇酯(PTT)纤维;所述聚酯纤维的直径为1-10dtex,纤维长度为 10-100mm。
在上述的纤维增强聚酯复合材料中,所述无机纤维为玻璃纤维、碳纤维和玄武岩纤维;所述无机纤维的直径为1-20dtex,纤维长度为10-100mm。
在上述的纤维增强聚酯复合材料中,所述抗氧剂为受阻酚类抗氧剂和亚磷酸酯类抗氧剂的任意组合。
在上述的纤维增强聚酯复合材料中,所述润滑剂为介酸酰胺、油酸酰胺、聚乙烯蜡、季戊四醇硬脂酸酯。
在上述的纤维增强聚酯复合材料的制备方法中,所述的方法包括如下步骤:
步骤1:将无机纤维和聚酯纤维通过切割机构切割成为预设长度的短切无机纤维和短切聚酯纤维,之后通过第一传送带传送进入纤维混合装置混合,得到第一混合物;
步骤2:第一混合物进入到第二传送带,第二传送带上方的撒粉装置将润滑剂和抗氧剂等助剂与第一混合物分散混合得到第二混合物;
步骤3:将第二混合物输送到双螺杆挤出机的加料口,进行挤出成型即可制备得到纤维增强聚酯复合材料。
步骤1中,将一定比例的纤维束状聚酯连续纤维和无机连续纤维先通过切割机将聚酯和无机纤维裁剪成预定长度,再将这两种纤维加入到纤维混合装置中,让两种纤维得到充分蓬松化处理分散,形成纤维混合物。
所述的切割机构的切割条件为:切纱速率为2~8Hz,切纱时间为 0.3~3min;切纱长度为:10~60mm;最优选为,切纱速率为5Hz,切纱时间为1min;切纱长度为:30mm。
所述的纤维混合装置的混合条件为:主动辊 的速率为1000~3000转/min,主动辊与主动辊 型腔的间距为5~30mm,进一步优选为,主动辊 的速率为 1500转/min,主动辊与主动辊 型腔的间距为10mm。
步骤2中,将纤维混合物通过传送带装置,传送带中间上方设置撒粉机,将助剂体系均匀撒在纤维混合物中,形成混合物。所述的撒粉装置的撒粉下料的条件为:控制撒粉下料速度为20~100g/min,振动器频率为2~8Hz,进一步优选为,控制撒粉下料速度为50g/min,振动器频率为5Hz,
步骤3中,所述的双螺杆挤出机的料筒后部(即进料口一端)的温度为 160℃-220℃,料筒中部的温度为220℃-260℃,料筒前部(即出料口一端) 的温度为200℃-240℃,机头温度为250-270℃,螺杆转速为100~300r/min(最优选为150r/min)。
本发明步骤1的目的是使纤维束形式(上千根单纤维)的无机纤维和聚酯纤维能够被充分打散成单根纤维或者多根单纤维分散水平,使无机纤维和聚酯纤维得到充分的分散和混合,实现聚酯纤维和无机纤维在微米尺度上的充分接触和分散。
在上述的纤维增强聚酯复合材料的制备方法中,所述的步骤2的目的是使润滑剂和抗氧剂能够以粉末形式分散在纤维混合物中,实现基本的预分散,有利于后续挤出塑化过程中,实现树脂、纤维与助剂的三相充分分散。
与现有技术相比,本发明具有如下优点:
本发明纤维增强聚酯复合材料的加工设备中,先将无机纤维和聚酯纤维通过特定装置混合分散,再与润滑剂和抗氧剂等助剂分散混合,最后输送到螺杆挤出机进行挤出成型制备得到纤维增强聚酯复合材料,可连续化生产,解决了高纤维增强改性过程中的纤维外露问题,能够实现纤维增强聚酯复合材料中纤维与树脂的充分分散浸润,制备得到综合性能和表面外观质量俱佳的复合材料。
本发明的方法采用无机纤维和聚酯纤维纤维混合预处理工序和助剂撒粉分散工序,能够使无机纤维和聚酯树脂在挤出成型工序前实现微米尺寸上的分散,大大提高了聚酯树脂与无机纤维的接触面积,从而能够有效避免挤出成型过程中由于挤出停留时间短、无机纤维束难以充分打散实现与树脂体系的均匀分散问题,从本质上解决了高纤维填充含量下的纤维与树脂分散问题。从而本发明具有如下优点:
1、复合材料的综合力学性能更高。
2、制品的表面外观质量好,高光泽,无浮纤。
3、螺杆挤出加工条件更加温和可控。
4、可实现更高纤维含量的螺杆挤出加工,对螺杆挤出设备磨损小。
附图说明
图1为本发明的加工设备实施例的结构示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
加工设备实施例
本实施例主要阐述用于实现本发明目的的加工设备,后续实施例再描述具体的复合材料及其制备方法。
本发明的加工设备如下(参阅图1):
如图1所示,一种纤维增强聚酯复合材料的加工设备,包括依次布置的切割装置2、传送带1、纤维混合装置3、传送带4、撒粉装置5和双螺杆挤出机6、冷却装置7、切粒机8、过滤网9、储料罐10;
所述的传送带1上方设有用于将无机纤维丝A和聚酯纤维丝B切割成预设长度的切割机构2;
所述的切割机构2包括相对布置的牵引压辊21和切割辊22;
所述纤维混合装置3主要是由进料牵引带、表面布满倒钩的主动辊 32、主动辊 型腔33和主动辊 位置调节器34组成;为了保证无机纤维和聚酯纤维的充分分散混合和分散混合效率,可以通过调节主动辊 位置调节器34,调整主动辊 32和主动辊 型腔33之间的距离来实现分散速率和分散混合效率之间的匹配。
所述撒粉装置5是由喂料小螺杆51和振荡器52组成。物料通过小螺杆 51的转速实现计量下料,再通过振动器52实现均匀的撒粉下料。
本发明实施例和对比例见下表1:
表1实施例物料配方表(质量百分比)
其中,实施例1-3和对比例2中,聚酯采用PBT连续纤维,纤维直径为 5.5dtex;实施例4-6和对比例1,3中,聚酯采用PET连续纤维,纤维直径为 5.5dtex;对比例4中,聚酯采用仪征化纤的牌号为BG802的PET聚酯切片;碳纤维采用日本东丽化学的T300,玻璃纤维采用重庆巨石的无碱玻璃纤维 EDR14-2000。
如表1所示为实施例1-6和对比例1-3的物料配方表。
实施例1-6的制备方法:
步骤1:将无机纤维和聚酯纤维先切割再混合,得到第一混合物;
步骤1具体包括如下子步骤:
步骤1-1:将一定比例丝状的无机纤维A和丝状的聚酯纤维B经过压辊并通过切割机构2切割成为预设长度的短切无机纤维和短切聚酯纤维;调节切割机构切纱速率为5Hz,切纱时间为1min;切纱长度为:30mm。
步骤1-2:短切碳纤维和短切聚酯纤维通过传送带进入纤维混合装置3,设定主动混合,辊的速率为1500转/min,主动混合辊与型腔间距为10mm;即可制备得到纤维混合物(即第一混合物)。
步骤2:将纤维混合物经传送带4经过撒粉装置5,控制撒粉下料速度为50g/min,振动器频率为5Hz,得到第二混合物。
步骤3:将第二混合物经加料口进入双螺杆挤出机,进行挤出成型,得到纤维增强聚酯复合材料粒子,经注塑制成标准样条进行性能检测。其中,挤出机料筒后部的温度为160℃-220℃,料筒中部的温度为220℃-260℃,料筒前部的温度为200℃-240℃,机头温度为250-270℃,螺杆转速为150r/min。
对比例1-3的制备方法为:
(1)将一定比例丝状的无机纤维和丝状的聚酯纤维经过压辊并通过切割机构切割成为预设长度的短切无机纤维和短切聚酯纤维;调节切割机构切纱速率为5Hz,切纱时间为1min;切纱长度为:30mm;
(2)将步骤(1)得到的混合纤维与抗氧剂和润滑剂经过高速分散机混合,通过双螺杆挤出机熔融挤出,得到纤维增强聚酯复合材料粒子,经注塑制成标准样条进行检测。其中,挤出机料筒后部的温度为160℃-220℃,料筒中部的温度为220℃-260℃,料筒前部的温度为200℃-240℃,机头温度为 250-270℃,螺杆转速为300r/min。
对比例4的制备方法为:
(1)将玻璃纤维、PET切片和助剂加入到高速混合机中充分混合均匀;
(2)将步骤(1)得到的均混物通过双螺杆挤出机熔融挤出,经牵引、冷却、切粒、干燥,得到纤维增强聚酯复合材料粒子,经注塑制成标准样条进行检测。其中,挤出机料筒后部的温度为200℃-220℃,料筒中部的温度为240℃-265℃,料筒前部的温度为230℃-240℃,机头温度为260℃,螺杆转速为300r/min。
测试项目和测试方法及结果见下表2:
表2
其中,表面外观的测试是通过观察100mm*2mm圆盘外观的光泽性和是否有浮纤来评判。其评价标准具体为:1:最差(大量浮纤,表面粗糙);2:较差(有浮纤,表面粗糙);3:一般(少量浮纤);4:较好(无浮纤);5:最好(无浮纤,表面光泽)。
从实施例1-6和对比例1-4的数据可知,与常规依靠螺杆挤出来实现无机纤维与树脂纤维共混分散(对比例1-3)、无机纤维与树脂切片共混分散的技术(对比例4)相比,采用本发明的工艺路线(含纤维混合装置)制备得到的玻璃纤维增强和碳纤维聚酯复合材料(实施例1-6)在纤维填充量和密度同等的前提下,拉伸强度、弯曲强度和模量提升了25%以上,缺口冲击强度也有30%左右的提高,同时表面质量也有了显著的提升,采用本发明技术的50%和60%纤维增强聚酯复合材料的表面质量可以达到无浮纤的效果,解决高纤维增强复合材料过程中纤维易析出的技术难题。
从上述实施例和对比例中可以得出结论:本发明的方法采用无机纤维和聚酯纤维纤维混合预处理工序,使无机纤维和聚酯树脂在挤出成型工序前实现微米尺寸上的分散,从本质上解决了高纤维填充含量下的纤维与树脂分散问题,通过试验证实,该方法制备得到的纤维增强复合材料综合力学性能更好,不存在表面纤维析出等问题。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。
Claims (3)
1.一种纤维增强聚酯复合材料的制备方法,其特征在于,采用纤维增强聚酯复合材料的加工设备,包括依次布置的第一传送带、纤维混合装置、第二传送带和双螺杆挤出机以及依次设置的冷却装置、切粒机、过滤网和储料罐,所述的冷却装置与所述双螺杆挤出机的挤出口连接;
所述的第一传送带上方设有用于将无机纤维丝和聚酯纤维丝切割成预设长度的切割机构,所述的切割机构包括相对布置的牵引压辊和切割辊;
所述的纤维混合装置包括表面布满倒钩的主动辊、主动辊型腔和主动辊位置调节器,所述的主动辊设置在所述主动辊型腔内;
所述的第二传送带上方设有撒粉装置,所述的撒粉装置包括喂料螺杆和振荡器;所述的纤维增强聚酯复合材料采用以下重量百分比原料:
聚酯纤维: 38.5-94.4%;
无机纤维: 5-60%;
抗氧剂: 0.2-2%;
润滑剂: 0.2-3%;
所述的聚酯纤维为聚对苯二甲酸乙二醇酯纤维或聚对苯二甲酸丁二醇酯纤维或聚对苯二甲酸1,3丙二醇酯纤维;
所述的无机纤维为玻璃纤维、碳纤维、玄武岩纤维中的至少一种;
该方法包括以下步骤:
步骤一:将无机纤维和聚酯纤维通过切割机构切割成为预设长度的短切无机纤维和短切聚酯纤维,之后通过第一传送带传送进入纤维混合装置混合,得到第一混合物;
所述的切割机构的切割条件为:切纱速率为2~8Hz,切纱时间为0.3~3min;切纱长度为:10~60mm;
所述的纤维混合装置的混合条件为:主动辊的速率为1000~3000转/min,主动辊与主动辊型腔的间距为5~30mm;
步骤二:第一混合物进入到第二传送带,第二传送带上方的撒粉装置将润滑剂和抗氧剂与第一混合物分散混合得到第二混合物;
步骤三:将第二混合物输送到双螺杆挤出机的加料口,进行挤出成型即可制备得到纤维增强聚酯复合材料。
2.根据权利要求1所述的纤维增强聚酯复合材料的制备方法,其特征在于,步骤二中,所述的撒粉装置的撒粉下料的条件为:控制撒粉下料速度为20~100g/min,振动器频率为2~8Hz。
3.根据权利要求1所述的纤维增强聚酯复合材料的制备方法,其特征在于,步骤三中,所述的双螺杆挤出机的料筒后部的温度为160℃-220℃,料筒中部的温度为220℃-260℃,料筒前部的温度为200℃-240℃,机头温度为250-270℃,螺杆转速为100~300r/min。
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CN102161817A (zh) * | 2011-05-17 | 2011-08-24 | 深圳市科聚新材料有限公司 | 一种碳纤维增强聚酯复合材料及其制备方法 |
CN103467757A (zh) * | 2013-09-30 | 2013-12-25 | 金发科技股份有限公司 | 一种纤维增强热塑性复合材料及其制备方法 |
CN105802146A (zh) * | 2016-04-07 | 2016-07-27 | 苏州市鼎立包装有限公司 | 聚酯纤维柔性打包带及其制备方法 |
CN107083581A (zh) * | 2017-05-16 | 2017-08-22 | 江苏田园新材料股份有限公司 | 一种车用pbt复合材料及其制备方法 |
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