CN112831060A - 一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法 - Google Patents

一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法 Download PDF

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CN112831060A
CN112831060A CN202011618056.5A CN202011618056A CN112831060A CN 112831060 A CN112831060 A CN 112831060A CN 202011618056 A CN202011618056 A CN 202011618056A CN 112831060 A CN112831060 A CN 112831060A
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从怀萍
李政
秦海利
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Hefei University of Technology
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Abstract

本发明公开了一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，先是采用取向冷冻形成多孔结构的银纳米线‑聚合物水凝胶基底，然后用光引发剂907改性水凝胶基底的银纳米线壁，最后引入油性前体溶液进行紫外光聚。同时，两种亲水和油性穿插网络的协同作用，使得本发明制备的有机水凝胶具有优异的耐低温性、耐低温性、抗油溶胀性。

Description

一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备 方法
技术领域
本发明涉及一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，为银纳米线-聚合物水凝胶基底与油性凝胶网络构建的有机水凝胶，属于功能材料领域。
背景技术
水凝胶顾名思义是由亲水性聚合物在水相中形成的三维网络结构。由于含有高达80％-90％的含水量，相似的理化性质赋予了其在人体组织，生物医学等有着极大的应用潜力。越来越多的科学家在水凝胶的合成与应用上投入了大量的精力，从而促进了水凝胶领域的发展。然而，水凝胶由于其单一的组分，高含水量使其对环境有着高度的敏感性，随着外界环境的改变，如温度，湿度，酸碱性等，其结构和性能会发生极大的改变，使其原有的性能发生明显的衰减或者失去其原有的性能，从而限制了水凝胶材料的进一步应用。
随着材料领域的发展，有机水凝胶一词被提了出来，将有机与无机结合起来，二者协同从而赋予了凝胶材料更优异的性能。有机水凝胶的制备方法目前主流上是：1、添加无机盐；2、二元溶剂；3、穿插网络；4、离子凝胶；5、与弹性体结合的核壳结构。基于此，本发明通过以一种抗疲劳银纳米线-聚合物水凝胶为基底，通过银硫配位键将具有更高油溶胀性的甲基丙烯酸月桂酯与更好机械性能的甲基丙烯酸丁酯引入形成穿插网络的三维结构有机水凝胶，从而赋予了其在一些极端环境中压力传感的应用。
发明内容
本发明提供了一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，以赋予该压力传感器耐低温、抗疲劳、抗油膨胀性能。
本发明耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，首先通过取向冷冻银纳米线-聚合物的方法形成均质有序的多孔三维网络结构；然后通过银硫配位键引入油性穿插网络。通过二重穿插网络的协同作用，本发明有机水凝胶具有优异的抗疲劳性，耐低温，抗油溶胀性等。
本发明耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，包括如下步骤：
步骤1：合成银纳米线。首先将5.86g Mw＝40000的聚乙烯吡咯烷酮加入190ml的丙三醇溶液中，搅拌均匀后于微波中加热10min使聚乙烯吡咯烷酮完全溶解；然后降温到室温，倒入250ml的三颈烧瓶中，再依次向其中加入1.58g硝酸银、10ml丙三醇以及配制好的0.5ml去离子水59mg氯化钠的混合溶液，随后20min升温到210℃，同时控制搅拌速率为50rpm；待反应完成后，倒入500ml的烧杯中，加入等体积的去离子水，降温后离心两次，分散定容。
步骤1中，所得银纳米线的长度是5-10μm，直径是50-80nm。
步骤2：取30mg/mL银纳米线5mL，在冰浴的条件下依次加入质量13％-16％银纳米线分散液的单体丙烯酰胺，0.02％-0.06％银纳米线分散液的交联剂亚甲基双丙烯酰胺，0.2％-0.6％银纳米线分散液的引发剂过二硫酸钾，催化剂四甲基乙二胺并300rpm搅拌；然后通过液氮调节冷冻盘温度为-100℃，放入模具，滴加水凝胶基底前体溶液，待冻结之后于-20℃环境中保存一夜，取出解冻即所获得的银纳米线-聚合物水凝胶基底。
步骤3：配制油性前体溶液；将单体、交联剂和引发剂依次加入溶剂中，超声分散均匀后置于真空干燥箱除去溶解的氧气和多余气泡即可。
步骤3中，所述溶剂为乙醇，其含量为油性前体溶液质量的30％-35％。
步骤3中，所述单体为甲基丙烯酸丁酯和甲基丙烯酸月桂酯，体积比为1:1；所述单体的添加质量为油性前体溶液质量的62％-68％。
步骤3中，所述交联剂为二甲基丙烯酸乙二醇酯，添加质量为油性前体溶液质量的0.03％-0.08％。
步骤3中，所述引发剂为光引发剂907，添加质量为油性前体溶液质量的0.2％-0.6％。
步骤4：氮气保护下，将步骤2所获得的银纳米线-聚合物水凝胶基底浸泡于步骤3所获得的油性前体溶液中24-36小时。
步骤5：将经步骤4浸泡后的水凝胶基底于紫外灯下光照40-60分钟，取出后即得有机水凝胶。
不同浓度的银纳米线具有不同的电导率，在取向冷冻的过程中会产生不同的网络结构，对于30mg/ml的银纳米线溶液浓度会产生更加均质的网络结构，从而具有更优异的性能。
本发明的有益效果体现在：
本发明在制备有机水凝胶压力传感器时，采用银硫配位键的穿插网络协同作用制备方法，首先是通过取向冷冻银纳米线-聚合物形成均质有序多孔水凝胶基底；随后浸泡油性前体溶液引入银硫配位键的穿插网络。因此，通过二重网络的协同作用，本发明有机水凝胶压力传感器在较低的温度、油性环境中表现出优异的抗疲劳性与较高的灵敏性。
综上，本发明提供了一种全新的耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法。本发明方法为有机水凝胶材料合成及特殊性能方面提供了全新的思路与理论基础。同时，也为有机水凝胶在适应极端环境的压力传感方面提供了重要的支持。
附图说明
图1是本发明所制备的银纳米线的投射电子显微镜照片。从图1中可以看出本发明制备的银纳米线溶液分散均匀。
图2是本发明所制备的银纳米线-聚合物水凝胶基底的扫描电子显微镜照片。从图2中可以看出该水凝胶基底均质的多孔结构，有利于二元穿插网络的形成。
图3是本发明所制备的有机水凝胶在液氮营造的-50℃下灯泡演示图。从图3中可以看出本发明制备的有机水凝胶具有优异的耐低温性能。
图4是本发明所制备的有机水凝胶在石油醚中超长时间压缩循环图。从图4中可以看出本发明制备的有机水凝胶具有优异的抗疲劳性和抗油溶胀性能。
图5是本发明所制备的有机水凝胶在石油醚中的电阻变化图。从图5中可以看出本发明制备的有机水凝胶具有优异的压力感知灵敏性。
具体实施方式
以下实施例详细的说明了本发明。本发明所使用的试剂原料及设备均为市售产品，可通过市场购买。
实施例1：
1、首先将5.86g Mw＝40000的聚乙烯吡咯烷酮加入190ml的丙三醇溶液中，搅拌均匀于微波中加热10min使聚乙烯吡咯烷酮完全溶解。然后降温到室温，倒入250ml的三颈烧瓶中，再依次向其中加入1.58g的硝酸银，然后加入10ml丙三醇，配制好的0.5ml去离子水59mg氯化钠的混合溶液，随20min升温到210℃，同时控制搅拌速率为50rpm。待反应完成后，倒入500ml的烧杯中，加入等体积的去离子水，待降温后6000rpm,10min离心两次，分散定容。
2、取30mg/ml银纳米线5mL，在冰浴的条件下依次加入质量13％-16％银纳米线分散液的单体丙烯酰胺，0.02％-0.06％银纳米线分散液的交联剂亚甲基双丙烯酰胺，0.2％-0.6％银纳米线分散液的引发剂过二硫酸钾，催化剂四甲基乙二胺并300rpm搅拌；然后通过液氮调节冷冻盘温度为-100℃，放入模具，滴加水凝胶基底前体溶液，待冻结之后于-20℃环境中保存一夜，取出解冻即所获得的银纳米线-聚合物水凝胶基底。
3、配制油性前体溶液，将总质量的62％-68％甲基丙烯酸丁酯与甲基丙烯酸月桂酯按照体积比1:1，总质量的0.02％-0.06％二甲基丙烯酸乙二醇酯，总质量的0.2％-0.6％光引发剂907依次加入到无水乙醇中，超声5-10分钟，待均质分散并在真空干燥箱除去溶解的氧气和多余气泡即可。
4、将步骤2所得到的的银纳米线-聚合物水凝胶基底缓慢放入步骤3所得到的的油性前体溶液中，浸泡24小时，过程均在氮气保护下进行。
5、将步骤4所得到的浸泡好的水凝胶基底于紫外灯下光照40-60分钟，取出即所获得的抗疲劳、耐低温、抗油溶胀有机水凝胶。
实施例2：
1、首先将5.86g Mw＝40000的聚乙烯吡咯烷酮加入190ml的丙三醇溶液中，搅拌均匀于微波中加热10min使聚乙烯吡咯烷酮完全溶解。然后降温到室温，倒入250ml的三颈烧瓶中，再依次向其中加入1.58g的硝酸银，然后加入10ml丙三醇，配制好的0.5ml去离子水59mg氯化钠的混合溶液，随20min升温到210℃，同时控制搅拌速率为50rpm。待反应完成后，倒入500ml的烧杯中，加入等体积的去离子水，待降温后6000rpm,10min离心两次，分散定容。
2、取25mg/mL银纳米线5mL，在冰浴的条件下依次加入质量15％银纳米线分散液的单体丙烯酰胺，0.02％-0.06％银纳米线分散液的交联剂亚甲基双丙烯酰胺，0.2％-0.6％银纳米线分散液的引发剂过二硫酸钾，催化剂四甲基乙二胺并300rpm搅拌；然后通过液氮调节冷冻盘温度为-100℃，放入模具，滴加水凝胶基底前体溶液，待冻结之后于-20℃环境中保存一夜，取出解冻即所获得的银纳米线—聚合物水凝胶基底。
3、配制油性前体溶液，将总质量的62％-68％甲基丙烯酸丁酯与甲基丙烯酸月桂酯按照体积比1:1，总质量的0.03％-0.08％二甲基丙烯酸乙二醇酯，总质量的0.2％-0.6％光引发剂907依次加入到无水乙醇中，超声5-10分钟，待均质分散并在真空干燥箱除去溶解的氧气和多余气泡即可。
4、将步骤2所得到的的银纳米线-聚合物水凝胶基底缓慢放入步骤3所得到的的油性前体溶液中，浸泡24-36小时，过程均在氮气保护下进行。
5、将步骤4所得到的浸泡好的水凝胶基底于紫外灯下光照40-60分钟，取出即所获得的抗疲劳、耐低温、抗油溶胀有机水凝胶。
实施例3：
1、首先将5.86g Mw＝40000的聚乙烯吡咯烷酮加入190ml的丙三醇溶液中，搅拌均匀于微波中加热10min使聚乙烯吡咯烷酮完全溶解。然后降温到室温，倒入250ml的三颈烧瓶中，再依次向其中加入1.58g的硝酸银，然后加入10ml丙三醇，配制好的0.5ml去离子水59mg氯化钠的混合溶液，随20min升温到210℃，同时控制搅拌速率为50rpm。待反应完成后，倒入500ml的烧杯中，加入等体积的去离子水，待降温后6000rpm,10min离心两次，分散定容。
2、取35mg/ml银纳米线5mL，在冰浴的条件下依次加入质量13％-16％银纳米线分散液的单体丙烯酰胺，0.02％-0.06％银纳米线分散液的交联剂亚甲基双丙烯酰胺，0.2％-0.6％银纳米线分散液的引发剂过二硫酸钾，催化剂四甲基乙二胺并300rpm搅拌；然后通过液氮调节冷冻盘温度为-100℃，放入模具，滴加水凝胶基底前体溶液，待冻结之后于-20℃环境中保存一夜，取出解冻即所获得的银纳米线-聚合物水凝胶基底。
3、配制油性前体溶液，将总质量的62％-68％甲基丙烯酸丁酯与甲基丙烯酸月桂酯按照体积比1:1，总质量的0.03％-0.08％二甲基丙烯酸乙二醇酯，总质量的0.2％-0.6％光引发剂907依次加入到无水乙醇中，超声5-10分钟，待均质分散并在真空干燥箱除去溶解的氧气和多余气泡即可。
4、将步骤2所得到的的银纳米线-聚合物水凝胶基底缓慢放入步骤3所得到的的油性前体溶液中，浸泡24-36小时，过程均在氮气保护下进行。
5、将步骤4所得到的浸泡好的水凝胶基底于紫外灯下光照40-60分钟，取出即所获得的抗疲劳、耐低温、抗油溶胀有机水凝胶。
本发明在制备纳米复合水凝胶时，采用的是基于银硫配位键构建穿插网络形成二元网络有机水凝胶，由于二元网络的协同作用，使该有机水凝胶具有优异的抗疲劳，抗疲劳，抗油溶胀性。同时，因为具有优良的导电性和压敏性，本发明制备的有机水凝胶在低温，复杂的油性环境中有着极大的传感应用空间。

Claims (7)

1.一种耐低温、抗疲劳、抗油溶胀有机水凝胶压力传感器的制备方法，其特征在于：
首先通过取向冷冻银纳米线-聚合物的方法形成均质有序的多孔三维网络结构；然后通过银硫配位键引入油性穿插网络，通过二重穿插网络的协同作用，赋予有机水凝胶优异的抗疲劳性、耐低温以及抗油溶胀性能。
2.根据权利要求1所述的制备方法，其特征在于包括如下步骤：
步骤1：合成银纳米线；
步骤2：在冰浴的条件下向银纳米线中依次加入单体丙烯酰胺、交联剂亚甲基双丙烯酰胺、引发剂过二硫酸钾以及催化剂四甲基乙二胺，通过取向冷冻形成多孔结构的银纳米线-聚合物水凝胶基底；
步骤3：将单体、交联剂和引发剂依次加入溶剂中，超声分散均匀后置于真空干燥箱除去溶解的氧气和多余气泡，获得油性前体溶液；
步骤4：氮气保护下，将步骤2所获得的银纳米线-聚合物水凝胶基底浸泡于步骤3所获得的油性前体溶液中24-36小时；
步骤5：将经步骤4浸泡后的水凝胶基底于紫外灯下光照40-60分钟，取出后即得有机水凝胶。
3.根据权利要求2所述的制备方法，其特征在于：
步骤1中，所得银纳米线的长度是5-10μm，直径是50-80nm。
4.根据权利要求2所述的制备方法，其特征在于：
步骤3中，所述溶剂为乙醇，其含量为油性前体溶液质量的30％-35％。
5.根据权利要求2所述的制备方法，其特征在于：
步骤3中，所述单体为甲基丙烯酸丁酯和甲基丙烯酸月桂酯，体积比为1:1；所述单体的添加质量为油性前体溶液质量的62％-68％。
6.根据权利要求2所述的制备方法，其特征在于：
步骤3中，所述交联剂为二甲基丙烯酸乙二醇酯，添加质量为油性前体溶液质量的0.03％-0.08％。
7.根据权利要求2所述的制备方法，其特征在于：
步骤3中，所述引发剂为光引发剂907，添加质量为油性前体溶液质量的0.2％-0.6％。
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