CN110776654B - 芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和应用 - Google Patents

芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和应用 Download PDF

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CN110776654B
CN110776654B CN201911100979.9A CN201911100979A CN110776654B CN 110776654 B CN110776654 B CN 110776654B CN 201911100979 A CN201911100979 A CN 201911100979A CN 110776654 B CN110776654 B CN 110776654B
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贾红兵
王晶
林炎坤
尹清
张旭敏
宋万诚
李雪雨
陆少杰
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Abstract

本发明公开了一种芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和应用。所述的复合水凝胶是以芳纶纳米纤维和聚乙烯醇水凝胶为基质,并在酸性条件下原位聚合聚苯胺制得。在多种氢键的相互作用下,复合水凝胶的力学强度和韧性显著提升。同时,由于存在导电聚苯胺,本发明的复合水凝胶具有较高的灵敏度,并且在实际应用中能重复稳定的检测出电信号的变化。本发明的复合水凝胶具有高力学强度、高韧性和高灵敏度,适用于可穿戴式应变传感器领域。

Description

芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和 应用
技术领域
本发明属于聚合物复合材料制备技术领域,涉及一种芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和应用。
背景技术
应变传感材料是指以信号传导的形式将外界刺激(如拉伸、压缩等)转化为可传输的电信号来实现对外界刺激实时检测的功能材料。该类材料在人体临床诊断、健康监控评估、柔性触摸屏、柔性电子皮肤以及工业机器人等领域拥有极大的应用潜力。水凝胶是一种柔软和湿润聚合物,通过物理或者化学交联相互缠结形成三维空间网状结构的固体物质,不仅具有与生物组织相似的良好柔韧性,而且与传统的刚性聚合物材料相比,具有良好的拉伸性和恢复能力,是制备可穿戴或植入设备的理想选择。文献《J.Mater.Chem.C,2018,6,9200-9207》中将聚丙烯酸(PAA)和导电聚苯胺(PANI)复合制备了一类具有双重协同网络的极易拉伸和导电的水凝胶。该水凝胶可用于制造应变传感器,具有良好的灵敏度(GF=0.48~0.63)和宽广的感应范围(0~1130%),但是其最大拉伸强度仅为0.3MPa。因此,实现高强度,高韧性和高传感灵敏度是应变传感器发展的一个重要方向。
聚对苯二甲酰对苯二胺(PPTA)是一种高性能芳纶纤维(ANF),自七十年代以来其已作为一种轻质高强材料被广泛应用于军事领域。经溶液处理的ANF保留其宏观母体的高机械性能,可以作为高强度柔性导体和电池隔膜的构件。文献《Advanced Materials,2018,30(1):1703343-1703348》采用简单的溶剂交换法可以实现ANF纳米纤维的凝胶化,同时通过引入聚乙烯醇(PVA)与纳米纤维复合制备出的水凝胶材料在具有高持水量的同时,其拉伸模量、断裂伸长率、压缩强度分别可达9.1MPa、325%、26MPa。目前,对基于ANF纳米纤维水凝胶的研究相对缺乏,仍然主要集中于其优异的力学性能。
发明内容
本发明的目的在于提供一种芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶及其制备方法和应用。
实现本发明目的的技术解决方案为:
芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶(ANF/PVA/PANI)的制备方法,具体步骤如下:
(1)采用二甲基亚砜(DMSO)/KOH体系将PPTA纺丝纤维溶解制成芳纶纳米纤维溶液;
(2)将PVA溶解于DMSO中制成PVA溶液;
(3)将芳纶纳米纤维溶液与PVA溶液搅拌混合均匀,并将得到的混合溶液真空干燥除去多余的溶剂,控制固体含量为10~15%;
(4)将步骤(3)得到的混合体系浇铸在模具中,然后浸入水中,得到具有特定几何形状的ANF/PVA水凝胶;
(5)将ANF/PVA水凝胶浸泡在含有0.3~0.4M苯胺(ANI)的盐酸溶液中,冰水浴下浸渍24小时以上,然后加入预冷的含有过硫酸铵的盐酸水溶液,冰水浴下反应12~24h,反应结束后洗涤除去未反应的单体,得到ANF/PVA/PANI复合水凝胶。
进一步的,步骤(1)中,所述的芳纶纳米纤维溶液的浓度为10~20mg/mL,溶解时间为四周以上,溶解温度为室温。
进一步的,步骤(2)中,所述的PVA溶液的浓度为80~100mg/mL。PVA溶液的配制如下:将分子量为145000~165000的PVA置于DMSO中室温充分溶胀,然后在90~95℃的高温下溶解至完全透明,静置至气泡完全消失。
进一步的,步骤(3)中,所述的芳纶纳米纤维溶液和PVA溶液的质量比为1:5;搅拌混合温度为50~60℃,搅拌时间为4~6h;真空干燥为90~100℃。
进一步的,步骤(4)中,水中的浸渍时间为24h以上。
进一步的,步骤(5)中,所述的过硫酸铵的浓度0.1~0.15M,盐酸溶液的浓度为1~1.5M。
进一步的,步骤(5)中,洗涤方法为将ANF/PVA/PANI复合水凝胶放入水中,浸泡24h以上。
本发明与现有技术相比,其显著优点是:
(1)本发明将芳纶纳米纤维应用至水凝胶中,并将其与聚乙烯醇混合,实现了硬相和软相的完美结合,提高了水凝胶的机械性能。
(2)以芳纶纳米纤维和聚乙烯醇作为基质,并在其上原位聚合聚苯胺作为导电活性材料。同时,三元复合物存在的多种氢键作用,进一步提高了水凝胶的力学强度。
(3)本发明的ANF/PVA/PANI复合水凝胶具有导电性、高强度、高韧性和高应变灵敏度等优点,在大应变和小应变下都能重复多次检测出稳定的电信号,可以作为可穿戴式应变传感器,用于人体各关节的运动检测。
附图说明
图1是ANF/PVA/PANI复合水凝胶的制备流程示意图;
图2是ANF/PVA/PANI复合水凝胶的应力-应变曲线图;
图3是ANF/PVA/PANI复合水凝胶应变传感器的相对电阻变化率(ΔR/R0)与拉伸应变的关系曲线;
图4是ANF/PVA/PANI复合水凝胶应变传感器应用于监测人体脉搏和手指关节活动的相对电阻变化率(ΔR/R0)曲线。
具体实施方式
下面结合实施例和附图对本发明作进一步说明。
本发明的ANF/PVA/PANI复合水凝胶的制备流程示意图如图1所示。
下述实施例采用的PPTA为商业购买得到的凯夫拉纺丝纤维。
实施例1
称取1g凯夫拉纺丝纤维和1.5gKOH,加入DMSO,在室温下搅拌四周,得到20mg/mL的芳纶纳米纤维溶液。
称取5g分子量为145000~165000的聚乙烯醇,加入DMSO,室温充分溶胀,然后在90~95℃的高温下溶解至完全透明,静置至气泡完全消失,得到100mg/mL的PVA溶液。
将等体积的20mg/mL芳纶纳米纤维溶液和100mg/mL PVA溶液(质量比ANF:PVA=1:5),在60℃下搅拌混合,搅拌时间为4h;所得到的混合体系在真空干燥箱中干燥,除去多余的溶剂,控制固体含量在10%。
将上述混合体系浇铸在模具中,然后浸入水中溶剂交换24h,形成具有特定几何形状的ANF/PVA水凝胶。
将ANF/PVA水凝胶裁剪成尺寸为1×3cm2,并将其置于含有1.1mL苯胺的20mL浓度为1M的盐酸溶液中,在冰水浴条件下浸渍24h。将预冷的含有0.72g过硫酸铵的20mL浓度为1M的盐酸溶液倒入上述混合物中,在冰水浴条件下再浸渍24h,最后将ANF/PVA/PANI复合水凝胶在水中浸泡24h,洗涤得到ANF/PVA/PANI复合水凝胶。该ANF/PVA/PANI复合水凝胶的断裂伸长率为186%,拉伸强度为2.18MPa,ΔR/R0最高可达19。
实施例2
称取1g凯夫拉纺丝纤维和1.5g KOH,加入DMSO,在室温下搅拌四周,得到20mg/mL的芳纶纳米纤维溶液。
称取5g分子量为145000~165000的聚乙烯醇,加入DMSO,室温充分溶胀,然后在90~95℃的高温下溶解至完全透明,静置至气泡完全消失,得到100mg/mL的PVA溶液。
将等体积的20mg/mL芳纶纳米纤维溶液和100mg/mL PVA溶液(质量比ANF:PVA=1:5),在50℃下搅拌混合,搅拌时间为6h;所得到的混合体系在真空干燥箱中干燥,除去多余的溶剂,控制固体含量在15%。
将上述混合体系浇铸在模具中,然后浸入水中溶剂交换24h,形成具有特定几何形状的ANF/PVA水凝胶。
将ANF/PVA水凝胶裁剪成尺寸为1×3cm2,并将其置于含有1.48mL苯胺的20mL浓度为1M的盐酸溶液中,在冰水浴条件下浸渍24h。将预冷的含有0.72g过硫酸铵的20mL浓度为1M的盐酸溶液倒入上述混合物中,在冰水浴条件下下再浸渍24h,最后将ANF/PVA/PANI复合水凝胶在水中浸泡24h,洗涤得到ANF/PVA/PANI复合水凝胶。该ANF/PVA/PANI复合水凝胶的断裂伸长率为125%,拉伸强度为2.5MPa,ΔR/R0最高可达21。
对比例1
按照指定的各组分含量重复实施例1的方法,但在材料组成中不含有聚苯胺,且固体含量控制在8~10%。该水凝胶的断裂伸长率30%,拉伸强度为0.37MPa,无导电性。
对比例2
按照指定的各组分含量重复实施例1的方法,但在材料组成中不含有聚苯胺。该水凝胶的断裂伸长率55%,拉伸强度为1.1MPa,无导电性。
对比例3
按照指定的各组分含量重复实施例1的方法,但在材料组成中含有0.37mL苯胺。该复合水凝胶的断裂伸长率为76%,拉伸强度为1.62MPa,ΔR/R0最高可达5.7。
对比例4
按照指定的各组分含量重复实施例1的方法,但材料组成中用聚(4-苯乙烯磺酸盐)水凝胶代替芳纶纳米纤维和聚乙烯醇水凝胶。该水凝胶的断裂伸长率300%,拉伸强度为10kPa,ΔR/R0最高可达11。
表1为实施例1-2和对比例1-4的性能测试数据。
表1
Figure BDA0002269856880000051
本发明采用芳纶纳米纤维/聚乙烯醇水凝胶为基础,在其上原位聚合聚苯胺为导电网络制备了复合水凝胶应变传感器,这相比于其它类型的水凝胶传感器极大地提高了其拉伸强度、断裂伸长率和传感灵敏度,弥补了水凝胶应变传感器机械性弱这一方面的短板,达到了高机械性能和高灵敏度的统一。

Claims (10)

1.芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶的制备方法,其特征在于,具体步骤如下:
(1)采用DMSO/KOH体系将PPTA纺丝纤维溶解制成芳纶纳米纤维溶液;
(2)将PVA溶解于DMSO中制成PVA溶液;
(3)将芳纶纳米纤维溶液与PVA溶液搅拌混合均匀,并将得到的混合溶液真空干燥除去多余的溶剂,控制固体含量为10~15%;
(4)将步骤(3)得到的混合体系浇铸在模具中,然后浸入水中,得到具有特定几何形状的ANF/PVA水凝胶;
(5)将ANF/PVA水凝胶浸泡在含有0.3~0.4M苯胺的盐酸溶液中,冰水浴下浸渍24小时以上,然后加入预冷的含有过硫酸铵的盐酸水溶液,冰水浴下反应12~24h,反应结束后洗涤除去未反应的单体,得到ANF/PVA/PANI复合水凝胶。
2.根据权利要求1所述的制备方法,其特征在于,步骤(1)中,所述的芳纶纳米纤维溶液的浓度为10~20mg/mL,溶解时间为四周以上,溶解温度为室温。
3.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,所述的PVA溶液的浓度为80~100mg/mL。
4.根据权利要求1所述的制备方法,其特征在于,步骤(2)中,PVA溶液的配制如下:将分子量为145000~165000的PVA置于DMSO中室温充分溶胀,然后在90~95℃的高温下溶解至完全透明,静置至气泡完全消失。
5.根据权利要求1所述的制备方法,其特征在于,步骤(3)中,所述的芳纶纳米纤维溶液和PVA溶液的质量比为1:5;搅拌混合温度为50~60℃,搅拌时间为4~6h;真空干燥为90~100℃。
6.根据权利要求1所述的制备方法,其特征在于,步骤(4)中,水中的浸渍时间为24h以上。
7.根据权利要求1所述的制备方法,其特征在于,步骤(5)中,所述的过硫酸铵的浓度0.1~0.15M,盐酸溶液的浓度为1~1.5M。
8.根据权利要求1所述的制备方法,其特征在于,步骤(5)中,洗涤方法为将ANF/PVA/PANI复合水凝胶放入水中,浸泡24h以上。
9.根据权利要求1至8任一所述的制备方法制得的芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶。
10.根据权利要求9所述的芳纶纳米纤维/聚乙烯醇/聚苯胺复合水凝胶在制备应变传感器中的应用。
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