CN106832991A - 一种碳纳米管增强轻质木塑复合材料的制备方法 - Google Patents
一种碳纳米管增强轻质木塑复合材料的制备方法 Download PDFInfo
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Abstract
一种碳纳米管增强轻质木塑复合材料的制备方法,以质量百分比计其原料组成:30‑70%塑料基体、30‑70%植物粉末、0.5‑3%碳纳米管、3‑8%偶联剂、0.1‑1%发泡剂、0.1‑1%增容剂、1‑3%润滑剂、2~4%增韧剂、0.01~0.1%过氧化物及其它功能助剂。通过偶联剂、分散剂、润滑剂等助剂将少量碳纳米管分散在基体相和木粉与塑料的界面两相中及介质空隙内,加入适量发泡剂实现微发泡处理,以降低复合材料密度,赋予木塑复合材料轻质高强优良特性。所制备木塑复合材料不仅具有无毒、耐水、安全、价廉等优点,而且具有质轻、高强度、防静电等优良特性,扩大了木塑复合材料使用环境及应用范围,具有广阔的经济前景和社会效益。
Description
技术领域
本发明涉及一种碳纳米管增强轻质木塑复合材料的制备方法,具体属于高分子复合材料技术领域。
背景技术
随着人类社会的进步,生态环保型材料越来越受到人们的青睐,使得木塑复合材料应运而生,木塑复合材料是以植物纤维为主要原料,经适当活化处理使其与各种塑料树脂按一定比例混合并添加相关助剂,再经混炼、高温、加工成型等工序制成的一种新型复合材料。木塑复合材料是一种应用广泛、性能好、附加值高的新型环境友好材料,代表着现代材料的工业发展方向之一。目前,木塑复合材料应用范围越来越广,如包装行业、建筑行业、园林庭院、铁路轨枕、汽车内装饰件等,其中有些领域对木塑复合材料的性能指标,特别在耐拉伸、抗弯曲、耐冲击、质轻、无毒、耐水等方面提出了更高的要求。因此,具有高强度、质轻特性的木塑复合材料是目前研制开发的重要方向。
已有的木塑复合材料制备技术中,如专利公开号为CN 102942798 A、CN103333390A、论文“碳纳米管增强聚丙烯基木塑复合材料的研究”、“第二届中国林业学术大会—S11木材及生物质资源高效增值利用与木材安全论文集”等。利用纳米二氧化硅、纳米碳酸钙、纳米纤维、碳纳米管和木纤维及塑料复合,制备出高模量、高强度纳米木塑复合材料,虽然能满足力学性能要求,但其密度偏高,通常为木材密度的2~3 倍,自重较高,产品的安装费用相对较高,无法满足实际要求,因此,其应用范围受到很大的限制。鉴如此,本发明就是制备出一种碳纳米管增强轻质木塑复合材料的制备方法,开发的碳纳米管增强轻质木塑复合材料具有质轻、高强度、防静电等优良特性。
发明内容
为实现上述发明目的,本发明一种碳纳米管增强轻质木塑复合材料的制备方法包括以下步骤:
(1) 按质量百分比计,称取各组成:
30%-70%的塑料基材、30%-70%的植物粉末、0.5%-3%的碳纳米管、3%-8%的偶联剂、0.1%-1%的发泡剂、0.1%-1%的增容剂、1%-3%的润滑剂、2%-4%的增韧剂、0.01%-0.1%的过氧化物。
(2)偶联剂乙醇溶液的配制
按质量百分比计,所配置的偶联剂乙醇溶液中偶联剂20%、乙醇70%、水10%。
(3)植物粉末的干燥
将植物粉末在105℃下干燥10h以上,直至其中水分的质量百分数<2%。
(4)碳纳米管活化处理
将碳纳米管、植物粉末、偶联剂乙醇溶液加入混合机中,在温度60~80℃和转速200~300rpm的范围内搅拌20分钟,其后将混合物料维持在100℃下干燥10h,得到碳纳米管和植物纤维粉末的活化预混物。
(5)物料的混炼
混炼温度控制在150~220℃,将塑料基材塑化5-15分钟后再加入活化预混物、发泡剂、增容剂、润滑剂、增韧剂、过氧化物,继续混炼20-30分钟,得到高温混炼物料。
(6)木塑复合材料的成型
上述高温混炼物料经热压或挤出成型,得到木塑复合材料;所述的热压成型工艺条件:在10.0MPa压力和180±10℃的温度下,热压10-20分钟;所述的挤出成型工艺条件:挤出温度170~200℃,螺杆转速200-300 rpm/min。
所述的碳纳米管为单壁碳纳米管、双壁碳纳米管、多壁碳纳米管、短切碳纳米管、羟基化碳纳米管或羧基化碳纳米管中的一种或几种的组合,且碳纳米管的直径均在2~50nm,长度均在5~30μm;发泡剂为小苏打、偶氮二甲酰胺、偶氮二异丁腈中的至少一种;植物粉末的颗粒粒度范围50~200目;塑料基材为聚丙烯、聚乙烯、聚氯乙烯和聚苯乙烯中的一种或几种的组合。
所述的偶联剂为钛酸酯偶联剂、硅烷偶联剂中的至少一种。
所述的润滑剂为硬脂酸及其盐、聚乙烯蜡、石蜡或氧化聚乙烯蜡。
所述的过氧化物为过氧化二异丙苯、过氧化苯甲酰、叔丁基过氧化氢或过氧化苯甲酸叔丁酯中的至少一种。
所述的增容剂为顺丁烯二酸酐、异氰酸酯、邻苯二甲酸酐、聚亚甲基聚苯基异氰酸酯中的至少一种。
所述的增韧剂为热塑性弹性体增韧剂。
所述的热塑性弹性体增韧剂为SBS、SEBS、POE、TPO、TPV中的至少一种。
本发明的有益效果:本发明制备方法采用偶联剂、增容剂、分散剂、润滑剂等助剂将少量碳纳米管分散在基体相和木粉与塑料的界面两相中及介质空隙内,共混物熔融时可产生双逾渗效应,有利于应力的传递转移,从而大幅度提高复合材料的力学性能,再通过通过实现微发泡处理,降低木塑材料的密度,赋予木塑复合材料轻质高强度的优良特性。另外,碳纳米管本身是良好导电材料,能将材料表面的静电荷迅速泄漏走,降低体积电阻率和表面电阻率,具有防静电性能。可见,所制备木塑复合材料强度高不仅具有普通木塑复合材料无毒、耐水、安全、价廉等优点,而且具有质轻、高强度、防静电等优良特性,可最大限度地扩大木塑复合材料的使用环境及应用范围,具有广阔的经济前景和社会效益。
具体实施方式
下面结合实施范例对本发明进行具体的描述,需要指出的是,所列举的实施范例只用于对本发明进行进一步的说明,不能理解为对本发明保护范围的限制。
一种碳纳米管增强轻质木塑复合材料,其是由以下质量百分比的原料组成范围:30-70%的塑料基体、30-70%的植物粉末、0.5-3%的碳纳米管、3-8%的偶联剂、0.1-1%的发泡剂、0.1-1%的增容剂、1-3%的润滑剂、2~4%的增韧剂、0.01~0.1%的过氧化物等。另外,根据需要还可以添加其他功能助剂,如抗氧剂、阻燃剂、颜料、防菌剂一种或几种的组合。
实施例1
碳纳米管增强轻质PP木塑复合材料的制备步骤:
(1)原料制备:将80目松木粉末置于干燥箱中,在105℃下干燥10h以上,直至水质量分数<2%备用;取50份经干燥的松木粉,1.5份羟基化碳纳米管(平均直径:20nm,平均长度:8μm)、2份聚乙二醇300,3份的KH-570硅烷偶联剂乙醇溶液(偶联剂质量含量为20%,乙醇质量含量为70%,水质量含量为10%)加入混合机中,设置温度在80~100℃范围内,转速设置在200~300rpm范围内,混合搅拌20分钟后将物料置于干燥箱或干燥室中在100℃下,干燥10h,得到活化处理的碳纳米管预处理物料粉末;
(2)混合处理:将混炼机升温至190℃,然后加入35份聚丙稀塑料,塑化8分钟, 再将上述全部碳纳米管预处理物料粉末、0.5份偶氮二甲酰胺,2份POE弹性体、2份硬脂酸、2份顺丁烯二酸酐、2份过氧化二异丙苯加入混炼机中,混合15分钟得到高温炼物料;
(3)材料成型:将上述混合处理高温混炼木塑熔体由运输管道送到单螺杆挤出机中,挤出机温度优选为170~200℃,混合物料经熔融挤出得到复合材料,再经真空定型台定型、冷却、牵引、切割工艺后得到碳纳米管增强轻质PP木塑复合板材。
碳纳米管增强轻质PP木塑复合板材经性能测试:静曲强度为22.3MPa,甲醛含量0.2mg/L,含水率0.8%,尺寸稳定性0.81%,邵氏硬度82HD,抗弯弹性模量2511MPa,板面握钉力1673N,能满足检验标准GB18580-2001及GBT24137-2009的要求。
实施例2
碳纳米管增强轻质PE木塑复合材料的制备步骤:
(1)原料制备:将50目杨木粉末置于干燥室中,在105℃下干燥10h以上,直至水质量分数<2%备用;取45份经干燥的杨木粉,1.5份羧基化碳纳米管(平均直径:30nm,平均长度:12μm),2份聚乙二醇300,3份的KH-550硅烷偶联剂乙醇溶液(偶联剂质量含量为20%,乙醇质量含量为70%,水质量含量为10%)加入混合机中,设置温度在80~100℃范围内,转速设置在200~300rpm范围内,混合搅拌20分钟后将物料置于干燥箱或干燥室中在100℃下,干燥10h,得到活化处理的碳纳米管预处理物料粉末;
(2)混合处理:将混炼机升温至180℃,然后加入40份高密度聚乙稀塑料,塑化8分钟,再将上述全部碳纳米管预处理物料粉末、0.5份偶氮二异丁腈,2份POE弹性体、2份聚乙烯蜡、2份异氰酸酯、2份过氧化苯甲酰加入混炼机中,混合15分钟得到高温炼物料;
(3)材料成型:将上述高温混炼处理的物料转移到平板硫化机的模具中,在模具内表面涂上脱模剂,在压力为10.0MPa下热压10分钟,热压温度为180℃,最后冷却定型,得到碳纳米管增强轻质PE木塑复合板材;
碳纳米管增强轻质PE木塑复合板材经性能测试:静曲强度为25.6MPa,甲醛含量0.1mg/L,含水率0.76%,尺寸稳定性0.85%,邵氏硬度79HD,抗弯弹性模量2651MPa,板面握钉力1858N,能满足检验标准GB18580-2001及GBT24137-2009的要求。
实施例3
碳纳米管增强轻质PVC竹塑复合材料的制备步骤:
(1)原料制备:将100目竹粉末置于干燥箱或干燥室中,在105℃下干燥10h以上,直至水质量分数<2%备用;取40份经干燥的竹木粉,1.0份短切碳纳米管(平均直径:15nm,平均长度:15μm)、2份聚乙二醇300,4份JTW-101钛酸酯偶联剂乙醇溶液(偶联剂质量含量为20%,乙醇质量含量为70%,水质量含量为8%)加入混合机中,设置温度在80~100℃范围内,转速设置在200~300rpm范围内,混合搅拌20分钟后将物料置于干燥箱或干燥室中在110℃下,干燥10h,得到活化处理的碳纳米管预处理物料粉末;
(2)混合处理:将混炼机升温至175℃,然后加入45份高密度聚乙稀塑料,塑化8分钟,再将上述全部碳纳米管预处理物料粉末、0.5份偶氮二甲酰胺,2份POE弹性体、2份石蜡、2份顺丁烯二酸酐、1.5份过氧化二异丙苯加入混炼机中,混合15分钟得到高温炼物料;
(3)材料成:将上述高温混炼处理的物料转移到平板硫化机的模具中,在模具内表面涂上脱模剂,在压力为10.0MPa下热压10分钟,热压温度为180℃,最后冷却定型,得到碳纳米管增强轻质PE木塑复合板材;
纳米管增强轻质PE木塑复合板材经性能测试:静曲强度为24.5MPa,甲醛含量0.2mg/L,含水率0.87%,尺寸稳定性0.79%,邵氏硬度85HD,抗弯弹性模量2583MPa,板面握钉力1723N,能满足检验标准GB18580-2001及GBT24137-2009的要求。
Claims (7)
1.一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的制备方法包括以下步骤:
(1)按质量百分比计,称取各组成:
30%-70%的塑料基材、30%-70%的植物粉末、0.5%-3%的碳纳米管、3%-8%的偶联剂、0.1%-1%的发泡剂、0.1%-1%的增容剂、1%-3%的润滑剂、2%-4%的增韧剂、0.01%-0.1%的过氧化物;
(2) 偶联剂乙醇溶液的配制
按质量百分比计,所配置的偶联剂乙醇溶液中偶联剂20%、乙醇70%、水10%;
(3) 植物粉末的干燥
将植物粉末在105℃下干燥10h以上,直至其中水分的质量百分数<2%;
(4) 碳纳米管活化处理
将碳纳米管、植物粉末、偶联剂乙醇溶液加入混合机中,在温度60~80℃和转速200~300rpm的范围内搅拌20分钟,其后将混合物料维持在100℃下干燥10h,得到碳纳米管和植物纤维粉末的活化预混物;
(5) 物料的混炼
混炼温度控制在150~220℃,将塑料基材塑化5-15分钟后再加入活化预混物、发泡剂、增容剂、润滑剂、增韧剂、过氧化物,继续混炼20-30分钟,得到高温混炼物料;
(6) 木塑复合材料的成型
上述高温混炼物料经热压或挤出成型,得到木塑复合材料;所述的热压成型工艺条件:在10.0MPa压力和180±10℃的温度下,热压10-20分钟;所述的挤出成型工艺条件:挤出温度170~200℃,螺杆转速200-300 rpm/min;
所述的碳纳米管为单壁碳纳米管、双壁碳纳米管、多壁碳纳米管、短切碳纳米管、羟基化碳纳米管或羧基化碳纳米管中的一种或几种的组合,且碳纳米管的直径均在2~50nm,长度均在5~30μm;发泡剂为小苏打、偶氮二甲酰胺、偶氮二异丁腈中的至少一种;植物粉末的颗粒粒度范围50~200目;塑料基材为聚丙烯、聚乙烯、聚氯乙烯和聚苯乙烯中的一种或几种的组合。
2.根据权利要求1所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的偶联剂为钛酸酯偶联剂、硅烷偶联剂中的至少一种。
3.根据权利要求1所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的润滑剂为硬脂酸及其盐、聚乙烯蜡、石蜡或氧化聚乙烯蜡。
4.根据权利要求1所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的过氧化物为过氧化二异丙苯、过氧化苯甲酰、叔丁基过氧化氢或过氧化苯甲酸叔丁酯中的至少一种。
5.根据权利要求1所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的增容剂为顺丁烯二酸酐、异氰酸酯、邻苯二甲酸酐、聚亚甲基聚苯基异氰酸酯中的至少一种。
6.根据权利要求1所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的增韧剂为热塑性弹性体增韧剂。
7.根据权利要求6所述的一种碳纳米管增强轻质木塑复合材料的制备方法,其特征在于:所述的热塑性弹性体增韧剂为SBS、SEBS、POE、TPO、TPV中的至少一种。
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