CN106977787A - 添加炭化ff 的hdpe/ff 复合材料及其制备方法 - Google Patents
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Abstract
本发明涉及一种添加炭化FF的HDPE/FF复合材料及其制备方法,具体涉及将再生天然纤维进行表面处理,此外,将天然纤维自身进行炭化处理,用活化剂进行活化处理,将改性后的天然纤维与高分子材料通过熔融共混复合;在高密度聚乙烯/鸡毛纤维(HDPE/FF)复合材料中添加活化改性后的炭化FF,改性后的复合材料不仅保留了HDPE/FF原有的优良的特性,还很好的增强了复合材料的韧性;使得复合材料的实际产业化生产提供了可能;并研究了非等温结晶动力学和驰豫行为,为蛋白质类再生天然纤维/高分子复合材料的生产提供了理论依据。
Description
技术领域
本发明属于高分子复合材料领域,尤其是在蛋白质类再生天然纤维/高分子复合材料中加入炭化天然纤维来增强复合材料的力学性能。
背景技术
纤维增强高分子复合材料指的是由增强体(再生天然纤维)、基体(树脂)、以及二者之间界面所组成的复合体系。增强体起骨架支撑的作用,基体起到连接的作用,而界面用于传递载荷。而再生天然纤维最常用来作增强的是木纤维和禽类毛纤维等。而用于做基体的树脂一般要求熔点比较低,方便加工。普遍用的是高密度聚乙烯(HDPE)、聚苯乙烯(PS)、聚氯乙烯(PVC)等热塑性塑料。
纤维增强聚合物树脂材料不仅有增强纤维的优点,同时有树脂具有的性质,主要特征是:力学强度高于一般树脂、无天然纤维材料制品常见缺陷、加工方式范围宽泛、绿色环保可回收再利用等等。
虽然再生天然纤维/高分子树脂复合材料的优点很多,但是相关的研究进展仍处在探索阶段还不成熟,再加上天然纤维与高分子树脂之间存在一些技术难题亟待解决。
(1)天然纤维与高分子树脂之间的界面问题。植物纤维中含有纤维素、果胶,动物纤维中多为氨基酸、油脂等极性物质,而选用的高分子树脂多为非极性物质,其界面难以相容,二者之间存在清晰明显的界面,界面结合力弱,制品容易出现力学缺陷。
(2)天然纤维内部存在强的作用力,不容易在基体内分散均匀。
偶联处理FF是处理天然纤维最为基本的方法,偶联剂其分子结构特殊,既有与聚合物中碳长链相连的部分,也有与无机填料相连的部分,由于HDPE是非极性的,而FF还有大量极性基团是极性的,极性不相容。FF与HDPE界面结合不好,通过偶联剂的桥联作用改善了这一情况。
同时,树脂与填料之间的界面结合力增强,使复合材料的刚性得到提高,但是,复合材料的抗冲击强度往往会有所下降,普遍使用的方法是加入增韧剂来提高复合材料的韧性。
聚合物增韧一般是天然纤维/高分子复合材料的重点研究内容,最早采用弹性体来增韧聚合物,但是在提高复合材料韧性的同时,复合材料的刚性、强度发生大幅度下降。采用无机刚性粒子代替橡胶的增韧体系,虽然保证了复合材料的强度,但是由于无机粒子的加入影响了天然纤维在基质内的分散,以及会破坏天然纤维与树脂之间的界面结合从而影响增韧效果,固研究无机粒子在树脂间的分散程度与无机粒子的比表面积、表面极性、无机粒子与树脂之间的界面作用等因素有关。因此,要提高复合材料的韧性,要求无机填料与树脂之间的表面能、极性要匹配,树脂的粘度也要变小。
炭化FF经过活化改性后,其比表面积大幅提高,FF形成中孔多孔结构,经过活化剂的活化,其孔通道进一步拓宽,已广泛应用于离子吸附领域。
发明内容
本发明在保证HDPE/FF复合材料刚性的基础上,添加炭化FF以改善复合材料的韧性,提供一种用于添加炭化FF的HDPE/FF复合材料及其制备方法。
本发明的目的是通过以下技术方案实现的:
一种添加炭化FF的HDPE/FF复合材料,其组分及重量分数为:
而且,所述的偶联剂为硅烷偶联剂或铝酸酯偶联剂或钛酸酯偶联剂。
而且,所述硅烷偶联剂为KH570,0.8-2份;所述的铝酸酯偶联剂为DLL-411A,0.06-0.12份;所述的钛酸酯偶联剂为NDZ-201,0.06-0.12份。
而且,所述的FF为50旦的鸡毛纤维。
一种添加炭化FF的HDPE/FF复合材料的制备方法,步骤如下:
(1)用偶联剂处理FF;
(2)将炭化FF活化处理;
(3)将步骤(1)偶联剂处理的FF与HDPE与步骤(2)活化处理的炭化FF在开炼机中混合;
(4)将共混物进行破碎,注塑成样。
而且,所述的炭化FF的制备方法为:
(1)将FF在马弗炉中加热18-24h,温度为210-230℃;
(2)将加热后的炭化FF继续在马弗炉中高温烧结2-3h,温度为400-450℃;
(3)将烧结后的炭化FF在微波炉中微波加热1.5-2h,温度调节为高温大火。
而且,所述的炭化FF的活化处理的方法为:将炭化FF浸泡于浓度为10-30%的柠檬酸溶液中,浸泡20-24h,以微波为热源进行加热,冷却后水洗,酸洗2-3次,干燥得活化处理后的炭化FF。
而且,步骤(1)所述的用偶联剂处理的FF的方法为:配置85-95wt%的乙醇水溶液,将硅烷偶联剂KH570倒入乙醇溶液中磁力搅拌1.5-2h,超声震荡0.5-1h,将FF用乙醇溶液浸泡1-2h,在60-80℃的温度条件下,水浴加热且不断搅拌,将处理后的硅烷偶联剂KH570溶液逐滴滴加至盛有FF的乙醇水溶液中,搅拌0.5-1h,取出浆液中的FF,在60-70℃的真空烘箱中烘干备用。
而且,步骤(1)所述的用偶联剂处理的FF的方法为:配置85-95wt%的乙醇水溶液,将铝酸酯偶联剂DL-411A或钛酸酯偶联剂NDZ-201倒入乙醇溶液中磁力搅拌1.5-2h,超声震荡0.5-1h,将FF用乙醇溶液浸泡1-2h,将处理后的铝酸酯偶联剂DL-411A或钛酸酯偶联剂NDZ-201溶液逐滴滴加至盛有FF的乙醇水溶液中,搅拌0.5-1h,取出浆液中的FF,在60-70℃的真空烘箱中烘干备用。
而且,步骤(3)所述的在开炼机中混合,设置开炼机前辊温度为125-135℃,开炼机后辊温度为120-130℃;步骤(4)所述的注塑条件为:注塑温度为料筒温度从加料口到喷嘴方向依次为:170℃、175℃、175℃、170℃,注塑压力为50MPa,模具温度为50℃。
本发明的优点和积极效果是:
1.本发明在HDPE/FF体系中添加增韧剂炭化FF,在保证复合材料的强度的基础上,改善了复合材料的韧性。
2本发明所用的增韧剂为FF自身进行物理改性得到的炭化FF,对HDPE与FF两相界面的结合无负面影响,并没有影响硅烷偶联剂对FF的偶联效果,其分散效果没有受到影响。
附图说明
图1为HDPE复合材料断面SEM图;
图2为HDPE/FF复合材料断面SEM图;
图3为HDPE/FF复合材料断面SEM图(KH570用量为FF10wt%处理FF);
图4为HDPE/FF复合材料断面SEM图(DL-411-A用量为FF1wt%处理FF);
图5为HDPE/FF复合材料断面SEM图(NDZ-201用量为FF1wt%处理FF)。
图6为HDPE/FF复合材料断面SEM图(KH570用量为FF10wt%处理FF);
图7为HDPE/FF复合材料断面SEM图(KH570用量为FF10wt%处理FF基础上添加20份炭化FF);
图8为HDPE/FF复合材料断面SEM图(KH570用量为FF10wt%处理FF基础上添加20份浓度为25%柠檬酸改性的炭化FF)。
图9为KH570用量对材料抗拉伸强度的影响曲线图;
图10为KH570用量对材料抗冲击强度的影响曲线图;
图11为KH570用量对材料弯曲强度的影响曲线图;
图12为KH570用量对材料熔融指数的影响曲线图;
图13为DL-411-A用量对材料抗拉伸强度的影响曲线图;
图14为DL-411-A用量对材料抗冲击强度的影响曲线图;
图15为DL-411-A用量对材料弯曲强度的影响曲线图;
图16为DL-411-A用量对材料熔融指数的影响曲线图;
图17为NDZ-201量对材料抗拉伸强度的影响曲线图;
图18为NDZ-201用量对材料抗冲击强度的影响曲线图;
图19为NDZ-201用量对材料弯曲强度的影响曲线图;
图20为NDZ-201用量对材料熔融指数的影响曲线图;
图21为碳化FF用量对材料拉伸强度的影响曲线图;
图22为碳化FF用量对材料缺口冲击强度的影响曲线图;
图23为碳化FF用量对材料弯曲强度的影响曲线图。
具体实施方式
下面结合实施例,对本发明进一步说明;下述实施例是说明性的,不是限定性的,不能以下述实施例来限定本发明的保护范围。
实施例1:
一种添加炭化FF的HDPE/FF复合材料,其配方为:
一种添加炭化FF的HDPE/FF复合材料的制备方法,其制备方法的步骤是:
(1)配置90wt%的乙醇水溶液,将KH570倒入乙醇溶液中磁力搅拌1h,超声震荡2h。将FF用乙醇浸泡1h,60-80℃的条件下水浴加热且不断搅拌,将处理后的KH570溶液逐滴滴加到盛有FF的乙醇浆液中,搅拌2h,取出浆液中的FF,在70℃的烘箱中烘干备用。
(2)将20gFF在马弗炉中加热26h,温度为215℃;将加热后的炭化FF在马弗炉中高温烧结2h,温度为400℃;将炭化FF在微波炉中微波加热2h,温度调节为大火。将炭化FF浸泡于浓度为25%的柠檬酸溶液中,浸泡24h后,以微波为热源进行加热,冷却后,酸洗、水洗2~3次,干燥得改性的炭化FF。
(3)将偶联处理的FF和HDPE以20:100比例与改性过的炭化FF在开炼机中混合,前辊温度为120℃,后辊温度为115℃。
(4)将共混物进行破碎,注塑成样。注塑温度为料筒温度(从加料口到喷嘴方向):170℃、175℃、175℃、170℃,注塑压力50MPa,模具温度为50℃。
实施例2:
一种添加炭化FF的HDPE/FF复合材料,其配方为:
一种添加炭化FF的HDPE/FF复合材料的制备方法,其制备方法的步骤是:
(1)配置90wt%的乙醇水溶液,将DL-411A倒入乙醇溶液中磁力搅拌1h,超声震荡2h。将FF用乙醇浸泡1h,将处理后的DL-411A溶液逐滴滴加到盛有FF的乙醇浆液中,搅拌2h,取出浆液中的FF,在70℃的烘箱中烘干备用。
(2)将20gFF在马弗炉中加热26h,温度为215℃;将加热后的炭化FF在马弗炉中高温烧结2h,温度为400℃;将炭化FF在微波炉中微波加热2h,温度调节为大火。将炭化FF浸泡于浓度为10-30%的柠檬酸溶液中,浸泡24h后,以微波为热源进行加热,冷却后,酸洗、水洗2~3次,干燥得改性的炭化FF。
(3)将偶联处理的FF和HDPE以20:100比例与改性过的炭化FF在开炼机中混合,前辊温度为120℃,后辊温度为115℃。
(4)将共混物进行破碎,注塑成样。注塑温度为料筒温度(从加料口到喷嘴方向):170℃、175℃、175℃、170℃,注塑压力50MPa,模具温度为50℃。
实施例3:
一种添加炭化FF的HDPE/FF复合材料,其配方为:
一种添加炭化FF的HDPE/FF复合材料的制备方法,其制备方法的步骤是:
(1)配置90wt%的乙醇水溶液,将NDZ-201倒入乙醇溶液中磁力搅拌1h,超声震荡2h。将FF用乙醇浸泡1h,将处理后的NDZ-201溶液逐滴滴加到盛有FF的乙醇浆液中,搅拌2h,取出浆液中的FF,在70℃的烘箱中烘干备用。
(2)将20gFF在马弗炉中加热26h,温度为215℃;将加热后的炭化FF在马弗炉中高温烧结2h,温度为400℃;将炭化FF在微波炉中微波加热2h,温度调节为大火。将炭化FF浸泡于浓度为10-30%的柠檬酸溶液中,浸泡24h后,以微波为热源进行加热,冷却后,酸洗、水洗2~3次,干燥得改性的炭化FF。
(3)将偶联处理的FF和HDPE以20:100比例与改性过的炭化FF在开炼机中混合,前辊温度为120℃,后辊温度为115℃。
(4)将共混物进行破碎,注塑成样。注塑温度为料筒温度(从加料口到喷嘴方向):170℃、175℃、175℃、170℃,注塑压力50MPa,模具温度为50℃。
表1 Jeziorny修正后的Avrami方程参数
(a)HDPE纯料;
(b)HDPE/FF复合材料;
(c)HDPE/FF复合材料(添加FF10wt%KH570);
(d)HDPE/FF复合材料(添加FF1wt%DL-411-A);
(e)HDPE/FF复合材料(添加FF1wt%NDZ-201)。
表2界面处理对HDPE/FF复合体系的力学性能以及驰豫行为的影响
(a)HDPE纯料;
(b)HDPE/FF复合材料;
(c)HDPE/FF复合材料(添加FF10wt%KH570);
(d)HDPE/FF复合材料(添加FF1wt%DL-411-A);
(e)HDPE/FF复合材料(添加FF1wt%NDZ-201);
表3 Jeziorny修正后的Avrami方程参数
(a)HDPE纯料;
(c)HDPE/FF复合材料(添加FF10wt%KH570);
(l)HDPE/FF复合材料(在添加FF10wt%KH570基础上添加20份炭化FF);
(m)HDPE/FF复合材料(在添加FF10wt%KH570基础上添加20份经过柠檬酸处理的炭化FF);
添加炭化FF的HDPE/FF复合材料的驰豫行为及力学性能数据
表4炭化处理对HDPE/FF复合体系的力学性能以及驰豫行为的影响
(a)HDPE纯料;
(b)HDPE/FF复合材料;
(c)HDPE/FF复合材料(添加FF10wt%KH570);
(d)HDPE/FF复合材料(在添加FF10wt%KH570基础上添加20份炭化FF);
(e)HDPE/FF复合材料(在添加FF10wt%KH570基础上添加20份经过柠檬酸处理的炭化FF)。
Claims (10)
1.一种添加炭化FF的HDPE/FF复合材料,其组分及重量分数为:
2.根据权利1所述的添加炭化FF的HDPE/FF复合材料,其特征在于:所述的偶联剂为硅烷偶联剂或铝酸酯偶联剂或钛酸酯偶联剂。
3.根据权利2所述的添加炭化FF的HDPE/FF复合材料,其特征在于:所述硅烷偶联剂为KH570,0.8-2份;所述的铝酸酯偶联剂为DLL-411A,0.06-0.12份;所述的钛酸酯偶联剂为NDZ-201,0.06-0.12份。
4.根据权利1所述的添加炭化FF的HDPE/FF复合材料,其特征在于:所述的FF为50旦的鸡毛纤维。
5.根据权利1所述的添加炭化FF的HDPE/FF复合材料的制备方法,其特征在于:步骤如下:
(1)用偶联剂处理FF;
(2)将炭化FF活化处理;
(3)将步骤(1)偶联剂处理的FF与HDPE与步骤(2)活化处理的炭化FF在开炼机中混合;
(4)将共混物进行破碎,注塑成样。
6.根据权利要求5所述的制备方法:其特征在于:所述的炭化FF的制备方法为:
(1)将FF在马弗炉中加热18-24h,温度为210-230℃;
(2)将加热后的炭化FF继续在马弗炉中高温烧结2-3h,温度为400-450℃;
(3)将烧结后的炭化FF在微波炉中微波加热1.5-2h,温度调节为高温大火。
7.根据权利要求5或6所述的制备方法:其特征在于:所述的炭化FF的活化处理的方法为:将炭化FF浸泡于浓度为10-30%的柠檬酸溶液中,浸泡20-24h,以微波为热源进行加热,冷却后水洗,酸洗2-3次,干燥得活化处理后的炭化FF。
8.根据权利要求5所述的制备方法,其特征在于:步骤(1)所述的用偶联剂处理的FF的方法为:配置85-95wt%的乙醇水溶液,将硅烷偶联剂KH570倒入乙醇溶液中磁力搅拌1.5-2h,超声震荡0.5-1h,将FF用乙醇溶液浸泡1-2h,在60-80℃的温度条件下,水浴加热且不断搅拌,将处理后的硅烷偶联剂KH570溶液逐滴滴加至盛有FF的乙醇水溶液中,搅拌0.5-1h,取出浆液中的FF,在60-70℃的真空烘箱中烘干备用。
9.根据权利要求5所述的制备方法,其特征在于:步骤(1)所述的用偶联剂处理的FF的方法为:配置85-95wt%的乙醇水溶液,将铝酸酯偶联剂DL-411A或钛酸酯偶联剂NDZ-201倒入乙醇溶液中磁力搅拌1.5-2h,超声震荡0.5-1h,将FF用乙醇溶液浸泡1-2h,将处理后的铝酸酯偶联剂DL-411A或钛酸酯偶联剂NDZ-201溶液逐滴滴加至盛有FF的乙醇水溶液中,搅拌0.5-1h,取出浆液中的FF,在60-70℃的真空烘箱中烘干备用。
10.根据权利要求5所述的制备方法:其特征在于:步骤(3)所述的在开炼机中混合,设置开炼机前辊温度为125-135℃,开炼机后辊温度为120-130℃;步骤(4)所述的注塑条件为:注塑温度为料筒温度从加料口到喷嘴方向依次为:170℃、175℃、175℃、170℃,注塑压力为50MPa,模具温度为50℃。
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