CN107383427A - 一种碳纳米管复合二氧化硅‑二氧化钛材料的改性方法 - Google Patents
一种碳纳米管复合二氧化硅‑二氧化钛材料的改性方法 Download PDFInfo
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Abstract
本发明提供的是一种碳纳米管复合二氧化硅‑二氧化钛材料的改性方法,具体步骤是:取碳纳米管@二氧化硅‑二氧化钛MWCNTs@ SiO2‑TiO2纳米材料加入乙醇溶液,然后加γ‑(2,3‑环氧丙氧) 丙基三甲氧基硅烷KH‑560,超声分散后加热回流,冷却至室温,过滤,用去离子水洗涤,在真空烘箱中干燥,得改性碳纳米管@二氧化硅‑二氧化钛纳米材料。用该改性方法改性的碳纳米管复合二氧化硅‑二氧化钛材料能很好地改善热塑性聚氨酯弹性体的力学性能和耐热性,同时改性剂能够与聚氨酯中的氨酯基发生作用,促进了有机与无机之间的交联,提高无机材料在复合材料中的分散性。
Description
技术领域
本发明涉及一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,属于中间体材料制备的技术领域。
背景技术
碳纳米管(CNTs)具有极高的强度、韧性和弹性模量,主要分多壁碳纳米管或单壁碳纳米管。单壁碳纳米管是由单层圆柱型石墨层构成,直径分布范围小、缺陷少,具有较高的均一性;多壁碳纳米管具有多层结构,层层之间很容易成为陷阱中心而捕获各种缺陷,因而多壁管的管壁上通常不满小洞的缺陷。将CNTs作为复合材料增强体,可表现出良好的轻度、弹性、抗疲劳性能等,这有利于复合材料的发展。此外,碳纳米管具有优异的力学性能、电学性能、热稳定性和非线性光学性能,是目前制备功能复合材料理想的填料。二氧化硅和二氧化钛具有良好的化学稳定性、热稳定性、无毒等优良性能,且制备方法简单成熟并廉价易得,广泛用于改性聚氨酯弹性体。纳米二氧化硅尺寸小、比表面积大、能耐高温,二氧化硅能够改善热塑性聚氨酯的机械强度、延伸率、耐磨性能以及耐老化性能。二氧化钛不仅明显改善聚氨酯的力学性能,对弹性体的耐热性也有一定的提高,而且,加入二氧化钛后的弹性体还具有耐腐性以及抗菌性。
对制备的纳米材料用γ-缩水甘油醚氧丙基三甲氧基硅烷偶联剂改性,使制备的纳米材料与聚氨酯之间形成化学键,不是简单的物理共混,对复合材料性能提高具有重要作用。
发明内容
技术问题:本发明的目的是提供一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,用该改性方法改性的碳纳米管复合二氧化硅-二氧化钛材料能很好地改善热塑性聚氨酯弹性体的力学性能和耐热性,同时改性剂能够与聚氨酯中的氨酯基发生作用,促进了有机与无机之间的交联,提高无机材料在复合材料中的分散性。
技术方案:本发明的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法为:取碳纳米管@二氧化硅-二氧化钛MWCNTs@ SiO2-TiO2纳米材料加入乙醇溶液,然后加γ-(2,3-环氧丙氧) 丙基三甲氧基硅烷KH-560,超声分散后加热回流,冷却至室温,过滤,用去离子水洗涤,在真空烘箱中干燥,得改性碳纳米管@二氧化硅-二氧化钛纳米材料。(改性MWCNTs@SiO2-TiO2纳米材料)
其中,
所述的取碳纳米管@二氧化硅-二氧化钛MWCNTs@ SiO2-TiO2纳米材料加入乙醇溶液,其温度条件是25 ℃。
所述的超声分散,其时间为1-2小时。
所述的加热回流,其时间为4-5小时。
所述的用去离子水洗涤,其洗涤次数为三次或三次以上。
所述的在真空烘箱中干燥,其干燥温度为60℃-65℃,干燥时间为24小时以上。
有益效果:该改性方法工艺简单,可靠性高,使用该改性方法改性的碳纳米管复合二氧化硅-二氧化钛材料能很好地改善热塑性聚氨酯弹性体的力学性能和耐热性,使改性后的热塑性聚氨酯复合材料具有CNTs、SiO2和TiO2三种材料的独特性能,能很好地改善热塑性聚氨酯弹性体的力学性能和耐热性,同时该改性方法改性的碳纳米管复合二氧化硅-二氧化钛材料能够与聚氨酯中的氨酯基发生作用,促进了有机与无机之间的交联,提高无机材料在复合材料中的分散性。
具体实施方式
25 ℃下,将0.5 g 多壁碳纳米管(MWCNTs)加入到砂芯酸化器中,将砂芯酸化器悬空置于含有2.5 mL(质量分数65 wt.%)硝酸的100 mL密闭反应釜中,然后升温至160 ℃,酸化4 h。反应结束冷却至室温,除去硝酸溶液,用去离子水洗涤至中性,60 ℃真空烘箱干燥后得到酸化碳纳米管。然后取0.1 g 酸化碳纳米管加入到反应器中,并加入5 mL乙醇和5mL水,超声分散1 h。用质量分数为25 wt.%~28 wt.%的氨水调节pH至9.0~10.0,用恒压滴液漏斗向反应体系中在1 h内滴加含有1 mL正硅酸四乙酯和1 mL钛酸正丁酯的60 mL乙醇混合溶液,反应8 h。过滤,用50 mL乙醇洗涤三次,然后用50 mL去离子水洗涤三次,在60 ℃真空烘箱中干燥24 h,得碳纳米管@二氧化硅-二氧化钛纳米材料(MWCNTs@SiO2-TiO2纳米材料);
25 ℃下,取0.1 g MWCNTs@ SiO2-TiO2纳米材料加入20 mL乙醇溶液,然后加1 mL γ-(2,3-环氧丙氧) 丙基三甲氧基硅烷(KH-560),超声分散1 h后加热回流4 h,冷却至室温,过滤,用50 mL去离子水洗涤三次,在60 ℃真空烘箱中干燥24 h,得改性碳纳米管@二氧化硅-二氧化钛纳米材料(改性MWCNTs@SiO2-TiO2纳米材料)。
Claims (6)
1.一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于,
取碳纳米管@二氧化硅-二氧化钛MWCNTs@ SiO2-TiO2纳米材料加入乙醇溶液,然后加γ-(2,3-环氧丙氧) 丙基三甲氧基硅烷KH-560,超声分散后加热回流,冷却至室温,过滤,用去离子水洗涤,在真空烘箱中干燥,得改性碳纳米管@二氧化硅-二氧化钛纳米材料。
2.根据权利要求书1所述的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于所述的取碳纳米管@二氧化硅-二氧化钛MWCNTs@ SiO2-TiO2纳米材料加入乙醇溶液,其温度条件是25 ℃。
3.根据权利要求书1所述的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于所述的超声分散,其时间为1-2小时。
4.根据权利要求书1所述的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于所述的加热回流,其时间为4-5小时。
5.根据权利要求书1所述的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于所述的用去离子水洗涤,其洗涤次数为三次或三次以上。
6.根据权利要求书1所述的一种碳纳米管复合二氧化硅-二氧化钛材料的改性方法,其特征在于所述的在真空烘箱中干燥,其干燥温度为60℃-65℃,干燥时间为24小时以上。
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CN114907687B (zh) * | 2022-05-27 | 2023-03-31 | 福州大学 | 用于mjr3d打印的二氧化硅包裹碳纳米管增强尼龙12复合材料及其制备方法和应用 |
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