CN114940725B - 一种仿贻贝微凝胶、其制备方法及应用 - Google Patents
一种仿贻贝微凝胶、其制备方法及应用 Download PDFInfo
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Abstract
本发明属于功能高分子材料技术领域,具体涉及一种仿贻贝微凝胶、其制备方法及其应用制备导电导磁水凝胶的方法。该方法是在加热条件下,以含有仿贻贝结构的微凝胶和纳米四氧化三铁(Fe3O4)为引发体系,引发导电聚合物单体聚合,制备出导电导磁水凝胶。本发明采用仿贻贝微凝胶和纳米Fe3O4为引发体系,有效避免了磁性纳米粒子在导电水凝胶中分散不均的问题,使其在柔性生物可穿戴器件领域有更好的应用价值。
Description
技术领域
本发明涉及属于功能高分子材料技术领域,具体涉及一种仿贻贝微凝胶、其制备方法及应用。
背景技术
近年来,导电水凝胶传感器由于其具有较好的导电性、高韧性和生物相容性广泛应用于柔性可穿戴生物器件中,对人体进行生理监测。
传统导电水凝胶通常由引入导电聚合物、导电颗粒和导电离子来制备,具有优良的物理、化学性质、生物相容性、导电性和多重刺激响应性。然而,在临床应用中人体生理监测时,通常同时有多台机器检测,导致导电水凝胶传感器相互出现信号干扰,从而影响信号的转换,使得信号输出数据失真。磁性通常具有抗信号干扰的特性,同时具有导电性和导磁性的水凝胶作为柔性可穿戴器件能很好的解决信号干扰的问题。然而在水凝胶中加入导磁性物质,最常见的如纳米Fe3O4,其分散性较差,达不到抗信号干扰的目的,因此亟需一种能够提高纳米Fe3O4在水凝胶中分散的物质。
发明内容
本发明的目的是针对现有技术的不足,从而提供一种仿贻贝微凝胶、其制备方法及应用。
为了实现上述目的,本发明所采用的技术方案为:
一种仿贻贝微凝胶,它是由多巴胺甲基丙烯酰胺形成的邻苯二酚结构的聚合物微球,所述微凝胶的粒径为300~800nm。
一种所述微凝胶的制备方法,所述微凝胶由多巴胺甲基丙烯酰胺和丙烯酰胺类化合物在光引发剂作用下通过微乳液聚合方式制备而成。反应中采用的多巴胺甲基丙烯酰胺为已公开的化合物,可以市购,也可以采用以下方法制备:以多巴胺盐酸盐、甲基丙烯酸酐、碳酸氢钠、十水合四硼酸钠等为原料,通过酰胺化反应,制备多巴胺甲基丙烯酰胺(DMA),在制备过程中,原料十水合四硼酸钠:碳酸氢钠:多巴胺盐酸盐的质量比为2-3:1:1~2,甲基丙烯酸酐:四氢呋喃的体积比为1:4~6,反应时要让溶液的pH保持在8以上,反应结束后,为了将DMA沉淀出来,调节溶液pH需小于2。
微凝胶制备时以光引发剂如VA-086,在氮气和紫外光照射的条件下,得到高分子链,再以交联剂如N,N,-亚甲基双丙烯酰胺交联,制得仿贻贝微凝胶。其中,溶剂由正己烷和表面活性剂司班80、吐温80组成,它们的体积比为69~71:0.3~0.5:0.1。表面活性剂也可选用司班20、司班83、吐温60。需要注意的是表面活性剂过量可能会降低油相分散和增溶力可能破乳。停止通氮气之后,继续搅拌,并在使反应瓶保持封闭状态在365 nm紫外灯下照射,直至反应瓶中的液体呈现乳液状。
作为技术方案的进一步改进,所述丙烯酰胺类化合物为N,N-亚甲基双丙烯酰胺、N-(2-羟乙基)丙烯酰胺和N-异丙基丙烯酰胺中的一种或多种。
一种用于导电导磁水凝胶的引发剂组合物,它由所述微凝胶和纳米Fe3O4组成,所述微凝胶和纳米Fe3O4的质量比为1~2:1。
一种导电导磁水凝胶组合物,它包括权利要求4所述的引发剂组合物、导电聚合物单体和交联剂。其中引发剂组合物在导电导磁水凝胶组合物中量保证有效引发和导磁性即可,交联剂在导电导磁水凝胶组合物中量保证聚合物有效交联得到三维结构凝胶即可,其中优选微凝胶、纳米Fe3O4和导电聚合物单体的质量比为1-2:1:1.8-20。
作为技术方案的进一步改进,所述导电聚合物单体为丙烯酸钠、N-乙烯基吡咯烷酮、4-苯乙烯磺酸钠盐中的一种或多种。
作为技术方案的进一步改进,所述弹性聚合物单体为丙烯酰胺,交联剂为聚乙二醇双丙烯酸酯(PEGDA)。
作为技术方案的进一步改进,它还包括烯烃类弹性聚合物单体。其中的弹性聚合物单体用于改善水凝胶的力学性能,当单独使用的导电聚合物单体聚合、交联后得到水凝胶具有足够的力学强度,也可单独使用导电聚合物单体。烯烃类弹性聚合物单体可选用丙烯酰胺、丙烯酸、乙烯醇、乙二醇双丙烯酸酯等。
作为技术方案的进一步改进,烯烃类弹性聚合物单体和导电聚合物单体的质量比为3:0~4。
本发明还公开一种根据所述组合物制备水凝胶的方法,在80~95℃加热条件下所述引发剂组合物引发所述导电聚合物单体聚合或者所述烯烃类弹性聚合物单体和导电聚合物单体聚合然后交联制备得到。低于该加热温度,无法成胶或凝胶有缺口;高于该温度范围,同样无法成胶。
本发明还公开一种所述制备方法制备的导电导磁水凝胶。
本发明相对现有技术具有突出的实质性特点和显著的进步,具体的说,本发明的仿贻贝微凝胶粒径小,可以和纳米Fe3O4搭配使用作为引发剂,使得纳米磁性粒子在水凝胶中分散均匀,制得的导电倒磁水凝胶导磁强度满足抗干扰需求,作为柔性可穿戴器件能很好的解决信号干扰的问题。
具体实施方式
下面通过具体实施方式,对本发明的技术方案做进一步的详细描述。
各实施例中和对比例中所用多巴胺甲基丙烯酰胺(DMA)以下列方法制备:
(1)称取十水硼酸钠20 g、碳酸氢钠8 g置于500mL反应瓶中,加入200mL三蒸水,通氮气30分钟,形成碱性溶液。在氮气流下,加入10 g多巴胺盐酸盐,并滴加溶解在50mL四氢呋喃中的9.5mL甲基丙烯酸酐。调节完pH后,通氮气24 h。
(2)将反应液用乙酸乙酯洗涤2次,取下层水相。然后用浓盐酸处理溶液调节溶液pH使得pH<2析出固体。再用乙酸乙酯洗3次,取上层有机相,向有机相中加入无水硫酸镁,吸水干燥,过滤得滤液。将所得液体用旋转蒸发仪进行旋蒸,得灰色固体即为多巴胺甲基丙烯酰胺(DMA)。
实施例1
(1)仿贻贝微凝胶制备:取DMA 0.1001 g、N,N,-亚甲基双丙烯酰胺0.0444 g、光引发剂(VA-086)0.0536 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:将反应液倒入烧杯,加入200mL丙酮等待固体析出,待固体析出后去上清,然后依次按照异丙醇、丙酮、异丙醇、0.01M磷酸缓冲盐溶液(1xPBS)的顺序进行离心得仿贻贝微凝胶,其中离心转速为8000 r/s,时间为4 min。用ZEN3600激光粒度仪测得仿贻贝微凝胶粒径为375 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶28 mg、丙烯酰胺0.1194 g、丙烯酸钠0.0395 g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3 h(温度为85℃),制得以丙烯酰胺和丙烯酸钠(质量比为3.02:1)的共聚物的导电导磁水凝胶。
实施例2
(1)仿贻贝微凝胶制备:取DMA 0.1100 g、N,N,-亚甲基双丙烯酰胺0.0502 g、光引发剂(VA-086)0.0576 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1得仿贻贝微凝胶粒径为512 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶22mg、丙烯酰胺0.1045 g、丙烯酸钠0.0592 g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以丙烯酰胺和丙烯酸钠(质量比为1.77:1)的共聚物的导电导磁水凝胶。
实施例3
(1)仿贻贝微凝胶制备:取DMA 0.1024 g、N,N,-亚甲基双丙烯酰胺0.0435 g、光引发剂(VA-086)0.0525 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1得仿贻贝微凝胶粒径为414 nm。其中离心机内芯型号为F0850,转速为8000 r/s,时间为4 min。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶30mg、丙烯酰胺0.0895g、丙烯酸钠0.079 g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以丙烯酰胺和丙烯酸钠(质量比为1.13:1)的共聚物的导电导磁水凝胶。
实施例4
(1)仿贻贝微凝胶制备:取DMA 0.1203 g、N,N,-亚甲基双丙烯酰胺0.0525 g、光引发剂(VA-086)0.0666 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1得仿贻贝微凝胶粒径为632 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶24mg、丙烯酰胺0.0746g、丙烯酸钠0.0987 g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以丙烯酰胺和丙烯酸钠(质量比为0.76:1)的共聚物的导电导磁水凝胶。
实施例5
(1)仿贻贝微凝胶制备:取DMA 0.1135 g、N,N,-亚甲基双丙烯酰胺0.0474 g、光引发剂(VA-086)0.0546 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为579 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶20mg、N-乙烯基吡咯烷酮179.02μL,丙烯酰胺0.0298g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以N-乙烯基吡咯烷酮和丙烯酰胺(质量比为6.27:1)的共聚物的导电导磁水凝胶。
实施例6
(1)仿贻贝微凝胶制备:取DMA 0.1206 g、N,N,-亚甲基双丙烯酰胺0.0515 g、光引发剂(VA-086)0.0673 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为654 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶30mg、N-乙烯基吡咯烷酮156.64μL,丙烯酰胺0.0448g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以N-乙烯基吡咯烷酮和丙烯酰胺(质量比为3.65:1)的共聚物的导电导磁水凝胶。
实施例7
(1)仿贻贝微凝胶制备:取DMA 0.1223 g、N,N,-亚甲基双丙烯酰胺0.0544 g、光引发剂(VA-086)0.069 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为705 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶26mg、N-乙烯基吡咯烷酮134.26μL,丙烯酰胺0.0597g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以N-乙烯基吡咯烷酮和丙烯酰胺(质量比为2.35:1)的共聚物的导电导磁水凝胶。
实施例8
(1)仿贻贝微凝胶制备:取DMA 0.1231 g、N,N,-亚甲基双丙烯酰胺0.0555 g、光引发剂(VA-086)0.071 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为714 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶31mg、N-乙烯基吡咯烷酮111.89μL,丙烯酰胺0.0746g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以N-乙烯基吡咯烷酮和丙烯酰胺(质量比为1.56:1)的共聚物的导电导磁水凝胶。
实施例9
(1)仿贻贝微凝胶制备:取DMA 0.1174 g、N,N,-亚甲基双丙烯酰胺0.0526 g、光引发剂(VA-086)0.0682 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为678 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶29mg、4-苯乙烯磺酸钠0.4g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),制得以4-苯乙烯磺酸钠聚合的导电导磁水凝胶。
对比例1
(1)仿贻贝微凝胶制备:取DMA 0.0986 g、N,N,-亚甲基双丙烯酰胺0.0414 g、光引发剂(VA-086)0.0517 g、N-(2-羟乙基)丙烯酰胺(HEAA)464 μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为315 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶25mg、丙烯酰胺0.3g、交联剂PEGDA30mg和 1xPBS 1mL,混合均匀,加入纳米Fe3O420mg,搅拌混合1 min,放入烘箱3 h(温度为85℃),制得聚丙烯酰胺导电导磁水凝胶。
对比例2
(1)仿贻贝微凝胶制备:取DMA 0.1174 g、N,N,-亚甲基双丙烯酰胺0.0526 g、光引发剂(VA-086)0.0682 g、N-(2-羟乙基)丙烯酰胺(HEAA)464μL、三蒸水2.5mL、二甲亚砜(DMSO)1.98mL为原料制得的溶液逐滴加入已通30 min氮气的溶剂中,即体积比为70:0.5:0.1的正己烷、司班80、吐温80,在365 nm紫外光下反应4 h以上。
(2)仿贻贝微凝胶后处理:操作同实施例1,得仿贻贝微凝胶粒径为678 nm。
(3)导电导磁水凝胶制备:取仿贻贝微凝胶15mg、4-苯乙烯磺酸钠0.4g、交联剂PEGDA 30mg和1xPBS 2mL混合均匀,再加入纳米Fe3O4 20mg,室温搅拌混合1min,放入烘箱3h(温度为85℃),未成胶,反应失败。
检测实施例1-9和对比例1制得的水凝胶的性能,检测结果如表1所示。
其中压缩强度采用通用机械试验机(CMT4304型, 中国SNAS试验机有限公司)测定,压缩测试:压缩速率为5 mm/min,触发力为0.5 N,形变设置为50%, 温度25℃,相对湿度65%±5%。
电导率采用CHI700E电化学工作站测定,LCR利用LCR测试仪IM3523测定,电导率测试:首先将样品制备成长、宽、厚分别为 40 mm,10 mm,3 mm 的长方形样条,通过四电极交流阻抗法在 0.1-1×105Hz 的频率范围内对水凝胶进行测试,测量期间电化学工作站的电压设置为 0.1 V,并根据测得的电阻值计算得到水凝胶的电导率。
最大饱和磁度采用3100系列振动样品磁强计测定,最大饱和磁度测试:测试过程中使用的磁场大小设置为最大磁场H=O.8T,增场步距为4(oe),其中仪器的最高灵敏度为5×10-5emu。
表1制得的水凝胶的性能列表
由表1数据可以看出,三种导电聚合物单体都赋予了水凝胶导电性能,并且随着导电聚合物单体含量的增加,水凝胶的导电能力也越来越好。其中导电性能最佳的是单体丙烯酰胺:丙烯酸钠,当质量比为1:1.3时,导电率高达3.71S▪cm-1。实施例制得的水凝胶具有相当的压缩强度,适用于制备柔性可穿戴器件。
最后应当说明的是:以上实施例仅用以说明本发明的技术方案而非对其限制;尽管参照较佳实施例对本发明进行了详细的说明,所属领域的普通技术人员应当理解,依然可以对本发明的具体实施方式进行修改或者对部分技术特征进行等同替换;而不脱离本发明技术方案的精神,其均应涵盖在本发明请求保护的技术方案范围当中。
Claims (8)
1.一种仿贻贝微凝胶,其特征在于,它是由多巴胺甲基丙烯酰胺形成的具有邻苯二酚结构的聚合物微球,所述微凝胶的粒径为300-800nm;所述微凝胶由多巴胺甲基丙烯酰胺和丙烯酰胺类化合物在光引发剂作用下通过微乳液聚合法制备而成;所述丙烯酰胺类化合物为N,N-亚甲基双丙烯酰胺、N-(2-羟乙基)丙烯酰胺、N-异丙基丙烯酰胺中的一种或多种。
2.一种用于制备导电导磁水凝胶的引发剂组合物,其特征在于,它由权利要求1所述微凝胶和纳米Fe3O4组成,所述微凝胶和纳米Fe3O4的质量比为1~2:1。
3.一种导电导磁水凝胶组合物,其特征在于,它包括权利要求2所述的引发剂组合物、导电聚合物单体和交联剂。
4.根据权利要求3所述的导电导磁水凝胶组合物,其特征在于,所述导电聚合物单体为丙烯酸钠、N-乙烯基吡咯烷酮和4-苯乙烯磺酸钠盐中的一种或多种。
5.根据权利要求4所述的导电导磁水凝胶组合物,其特征在于,它还包括烯烃类弹性聚合物单体。
6.根据权利要求5所述的导电导磁水凝胶组合物,其特征在于,烯烃类弹性聚合物单体和导电聚合物单体的质量比为3:0~4。
7.根据权利要求5所述的导电导磁水凝胶组合物,其特征在于,所述烯烃类弹性聚合物单体为丙烯酰胺,所述交联剂为聚乙二醇双丙烯酸酯PEGDA。
8.一种根据权利要求3-7任一项所述组合物制备水凝胶的方法,其特征在于,在80~95℃加热条件下,所述引发剂组合物引发所述导电聚合物单体聚合或者引发所述烯烃类弹性聚合物单体和导电聚合物单体聚合,然后交联制备得到。
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CN106866994A (zh) * | 2017-02-27 | 2017-06-20 | 江南大学 | 一种聚苯胺基自修复导电水凝胶的制备方法 |
JP2018070894A (ja) * | 2017-12-22 | 2018-05-10 | 東レ株式会社 | 導電性ハイドロゲル |
CN108371728A (zh) * | 2018-03-09 | 2018-08-07 | 西南交通大学 | 一种用于组织修复的仿贻贝接触抗菌水凝胶的制备方法 |
CN111995777A (zh) * | 2019-05-31 | 2020-11-27 | 中国科学院青岛生物能源与过程研究所 | 一种强粘附性、高机械强度的pegda-贻贝粘附蛋白-胶原蛋白复合水凝胶的制备方法 |
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CN106866994A (zh) * | 2017-02-27 | 2017-06-20 | 江南大学 | 一种聚苯胺基自修复导电水凝胶的制备方法 |
JP2018070894A (ja) * | 2017-12-22 | 2018-05-10 | 東レ株式会社 | 導電性ハイドロゲル |
CN108371728A (zh) * | 2018-03-09 | 2018-08-07 | 西南交通大学 | 一种用于组织修复的仿贻贝接触抗菌水凝胶的制备方法 |
CN111995777A (zh) * | 2019-05-31 | 2020-11-27 | 中国科学院青岛生物能源与过程研究所 | 一种强粘附性、高机械强度的pegda-贻贝粘附蛋白-胶原蛋白复合水凝胶的制备方法 |
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