CN111452352B - 一种超弹性3d打印纳米纤维素复合材料及其制备方法 - Google Patents
一种超弹性3d打印纳米纤维素复合材料及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种超弹性3D打印纳米纤维素复合材料及其制备方法,包括以下步骤:将浓度为1.5~12wt%的纳米纤维素水溶液与无机纳米颗粒共混,经均质处理后进行3D打印成型,打印水凝胶经吸湿性盐浸渍,冷冻干燥成型,即得。本发明提供的抗疲劳、高弹性3D复合材料,在物质吸附、水收集、生物工程等方面具有广阔的应用前景。
Description
技术领域
本发明涉及3D打印材料技术领域,具体涉及一种超弹性3D打印纳米纤维素复合材料及其制备方法。
背景技术
纤维素广泛存在于植物及其加工物、海洋生物和细菌等。纳米纤维素因其独特的小尺寸效应、高比表面积、高杨氏模量、高机械强度以及高生物生物相容性等,使其在物理、化学、力学性能上与宏观物体显著不同。纳米纤维素还具有良好的蓬松三维网络结构,能促使聚合物基体和纳米纤维素达到机械结合,增强基体材料性能。因此,采用纳米纤维素作为主体材料或填充材料,符合高性能绿色复合材料的发展趋势。
纳米纤维素/无机纳米颗粒高性能复合材料成为制备功能材料的重要方法,随着3D打印技术的兴起,人们对材料的要求更加严格,目前,3D打印技术主要包括树脂复合材料、高分粉末材料、石蜡粉末材料、陶瓷粉末材料、木塑复合材料等。常规的3D打印方法依托高温熔融等方法,容易造成生物质碳化等问题,因此,直写成型打印方式具有一定的发展空间。而无机纳米颗粒水溶液由于极低的黏度和浓度,不能采用3D打印技术,因此,在3D打印技术领域开发纳米纤维素/无机纳米颗粒复合材料具有重要意义。
传统的纳米纤维素复合3D打印材料具有刚性特征,不具有弹性和抗疲劳性,而改性该材料力学性能的方法主要为硅烷气相沉积等化学修饰方法。这种方法成本较高,且不符合环保可持续发展的要求。因此,目前亟需提供具有高弹性抗疲劳的3D打印纳米纤维素/无机纳米颗粒复合材料。
发明内容
针对现有技术中存在的缺陷和不足,本发明提供了一种超弹性3D打印纳米纤维素复合材料及其制备方法。
本发明采用特定浓度纳米纤维素作为增稠剂,实现无机纳米颗粒的打印成型,并采用浸渍法使材料表面覆盖吸湿性盐,从而达到柔化复合物材料的目的,最终制备具有高弹性抗疲劳的3D打印纳米纤维素复合材料。
本发明的目的之一在于提供一种超弹性3D打印纳米纤维素复合材料的制备方法,包括以下步骤:将浓度为1.5~12wt%的纳米纤维素水溶液与无机纳米颗粒共混,经均质处理后进行3D打印成型,打印水凝胶经吸湿性盐浸渍,冷冻干燥成型,即得。
根据本发明的一些优选实施方式,包括以下步骤:
步骤1),直接配制或脱水处理形成浓度为1.5~12wt%的纳米纤维素水溶液;
步骤2),向步骤1)中的所述纳米纤维素水溶液中加入质量分数5~90%的无机纳米颗粒,进行高速均质,得打印墨水;
步骤3),将步骤2)中所制备的打印墨水进行3D打印成型,得成型样品;
步骤4),将步骤3)的所述成型样品置于0.1~2mol/L的吸湿性盐溶液中浸泡1min以上,然后进行干燥,即得。
根据本发明的一些优选实施方式,步骤1)中,所述纳米纤维素包括微晶纤维素、TEMPO氧化纤维素、羟甲基纤维素或酶解纳米纤维素,动物纳米纤维素或细菌纤维素中的一种或多种,优选为微晶纤维素或TEMPO氧化纤维素。
根据本发明的一些优选实施方式,步骤1)中,配制浓度为6~8wt%的微晶纳米纤维素或羟甲基纤维素的水溶液;和/或,对TEMPO纳米纤维素水溶液脱水处理形成浓度为2~3wt%的纳米纤维素水溶液。本发明中通过采用特定浓度纳米纤维素起到增稠的效果,从而增强水性聚氨酯的可打印性。
根据本发明的一些优选实施方式,步骤2)中,所述无机纳米颗粒的固含量为5~90%;和/或,所述无机纳米颗粒和纳米纤维素共混的固含质量比为1:19~9:1,优选为5:5~8:2。
根据本发明的一些优选实施方式,步骤2)中,所述无机纳米颗粒包含纳米粒子、纳米纤维、纳米薄膜、纳米块状和纳米晶中的一种或多种,优选为TiO2纳米颗粒,SiO2纳米颗粒,碳纳米管、石墨烯或纳米蒙脱土。
根据本发明的一些优选实施方式,步骤1)中,所述脱水处理为真空干燥去水、自然干燥去水、烘箱干燥去水或冷冻干燥去水。
根据本发明的一些优选实施方式,步骤3)中,3D打印成型为常温打印,打印速度为2~6mm/s,材料挤出速度为1~3mL/h,喷嘴口直径为0.2~0.6mm,优选的,打印速度为2.5mm/s,材料挤出速度为1.5mL/h,喷嘴口直径为0.41mm。
根据本发明的一些优选实施方式,步骤4)中,所述吸湿性盐溶液选自钙盐、镁盐、钠盐和铵盐中的一种或多种的盐溶液,浓度0.1~2mol/L,优选选自氯化钠、氯化钙、尿素、硝酸铵和氯化镁中的一种或多种的盐溶液,优选浓度为0.3~0.75mol/L。
根据本发明的一些优选实施方式,步骤4)中,所述吸湿性盐溶液浸泡时间为1~30min;优选5~10min。
本发明中通过采用吸湿性盐以特定浓度和工艺参数吸附到样品内部,能有效吸收水分,水分破坏纤维素氢键作用,起到柔化纤维的效果,从而增强复合材料的弹性。
根据本发明的一些优选实施方式,步骤4)中,所述干燥采用室温干燥、超临界干燥、冷冻干燥或溶液置换干燥,优选为液氮冷冻干燥。
根据本发明的一些优选实施方式,1)直接配制6wt%的微晶纳米纤维素或将低浓度TEMPO氧化纳米纤维素水溶液脱水至2.5wt%,加入无机纳米颗粒,无机纳米颗粒与纳米纤维素共混的固含质量比为1:19到9:1,共混后进行高速均质;2)在室温下直接用于3D打印成型,打印速度为2~6mm/s,材料挤出速度为1~3mL/h,喷嘴口直径为0.2~0.6mm;3)用浓度为0.3~0.75mol/L的吸湿性盐溶液滴加到成型样品上1min以上,或将打印水凝胶样品浸泡至以上浓度的吸湿性盐溶液中1min以上;4)样品取出后采用常温干燥、冷冻干燥、超临界干燥和溶剂置换干燥方式成型。
本发明另一目的在于提供一种超弹性3D打印纳米纤维素复合材料,由所述的方法制备得到。
本发明的有益效果至少在于:本发明提供的方法制备了具有高弹性抗疲劳的3D打印纳米纤维素/无机纳米颗粒复合材料,高弹性抗疲劳压缩性能优异使材料具有循环使用、节约成本的优势。本发明提供的抗疲劳、高弹性3D复合材料,在物质吸附、水收集、生物工程等方面具有广阔的应用前景。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚,下面对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例是本发明一部分实施例,而不是全部的实施例。本发明技术方案不局限于以下所列举具体实施方式,还包括各具体实施方式间的任意组合,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。
本发明中,实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件,或者按照产品说明书进行。所用仪器等未注明生产厂商者,均为可通过正规渠道商购买得到的常规产品。本发明中所用的化工原料均可在国内化工产品市场方便买到。
实施例1
本实施例提供超弹性3D打印纳米纤维素复合材料的制备方法,步骤如下:
步骤1)配制6wt%质量分数的微晶纳米纤维素溶液100克;
步骤2)在配制好的微晶纳米纤维素水溶液中加入TiO2纳米颗粒6克,采用高速均质机均质;
步骤3)在室温下直接用于3D打印成型,打印速度为2.5mm/s,材料挤出速度为1.5mL/h,喷嘴口直径为0.41mm;
步骤4)用浓度为0.5mol/L的氯化钙溶液滴加到成型样品上5min,样品取出后液氮冷冻干燥,置于40%的湿度环境中。
通过对实施例1制备的纳米纤维素/TiO2纳米颗粒复合物3D打印样品进行24次50%形变压缩测试,压缩速率为50mm/min,检测结果如下:24次压缩后,只有6%的压缩形变没有恢复,94%的压缩形变可恢复,可以看出,本实施例方法制备的纳米纤维素/TiO2纳米颗粒复合物3D打印样品具有优异的回弹性能和抗疲劳性能。
实施例2
本实施例提供超弹性3D打印纳米纤维素材料的制备方法,步骤如下:
步骤1)采用真空干燥方式使TEMPO氧化制备的纳米纤维素水溶液脱水至2.0wt%浓度,取100克;
步骤2)在脱水后的纳米纤维素水溶液中加入纳米蒙脱土18克,采用高速均质机均质;
步骤3)在室温下直接用于3D打印成型,打印速度为2.5mm/s,材料挤出速度为1.5mL/h,喷嘴口直径为0.41mm;
步骤4)用浓度为0.75mol/L的氯化钙溶液滴加到成型样品上30min,样品取出后液氮冷冻干燥,置于40%的湿度环境中。
对比例1
采用实施例2中的方法,不同之处仅在于步骤4)采用0.05mol/L的氯化钙溶液滴加到打印成型样品上。
实验例1
对以上实施例2和对比例1中的复合材料进行力学压缩测试,压缩形变为50%时,实施例2样品100%形变恢复,对比例1样品接近40%的压缩变形不可恢复,可以看出,低浓度吸湿性盐不能使材料具有回弹性能。
虽然,上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。
Claims (8)
1.一种超弹性3D打印纳米纤维素复合材料的制备方法,其特征在于,包括以下步骤:
步骤1),配制浓度为6~8wt%的微晶纳米纤维素或羟甲基纤维素的水溶液,或对TEMPO纳米纤维素水溶液脱水处理形成浓度为2~3wt%的纳米纤维素水溶液;所述纳米纤维素包括微晶纤维素、TEMPO氧化纤维素、羟甲基纤维素、酶解纳米纤维素、动物纳米纤维素、细菌纤维素中的一种或多种;所述脱水处理为真空干燥去水;
步骤2),向步骤1)中的所述纳米纤维素水溶液中加入质量分数5~90%的无机纳米颗粒,进行高速均质,得打印墨水;所述无机纳米颗粒为TiO2纳米颗粒、SiO2纳米颗粒、碳纳米管、石墨烯或纳米蒙脱土;
步骤3),将步骤2)中所制备的打印墨水进行3D打印成型,得成型样品;3D打印成型为常温打印,打印速度为2~6 mm/s,材料挤出速度为1~3 mL/h,喷嘴口直径为0.2~0.6 mm;
步骤4),将步骤3)的所述成型样品置于0.3~0.75mol/L的吸湿性盐溶液中浸泡1~30min,然后进行干燥,即得;所述吸湿性盐溶液选自氯化钠、氯化钙、尿素、硝酸铵和氯化镁中的一种或多种的盐溶液。
2.根据权利要求1所述的方法,其特征在于,步骤1)中,所述纳米纤维素为微晶纤维素或TEMPO氧化纤维素。
3.根据权利要求1所述的方法,其特征在于,步骤2)中,所述无机纳米颗粒的固含量为5~90%;和/或,所述无机纳米颗粒和纳米纤维素共混的固含质量比为1:19~9:1。
4.根据权利要求3所述的方法,其特征在于,所述无机纳米颗粒和纳米纤维素共混的固含质量比为5:5~8:2。
5.根据权利要求1所述的方法,其特征在于,步骤3)中,打印速度为2.5 mm/s,材料挤出速度为1.5 mL/h,喷嘴口直径为0.41 mm。
6.根据权利要求1所述的方法,其特征在于,步骤4)中,所述吸湿性盐溶液浸泡时间为5~10min;和/或,所述干燥采用室温干燥、超临界干燥、冷冻干燥或溶液置换干燥。
7.根据权利要求6所述的方法,其特征在于,步骤4)中,所述干燥为液氮冷冻干燥。
8.一种超弹性3D打印纳米纤维素复合材料,其特征在于,由权利要求1-7任一项所述的方法制备得到。
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