CN114015045B - 一种荧光聚合物、Fe3+检测试纸及其制备方法与应用 - Google Patents
一种荧光聚合物、Fe3+检测试纸及其制备方法与应用 Download PDFInfo
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Abstract
本发明公开了一种荧光聚合物及其制备方法,该荧光聚合物引入三氟甲基,能够提高聚合物的光、热稳定性,有利于金属离子检测方面荧光响应的提高,使其具有较好的荧光‑金属离子响应性,可用于金属离子的荧光检测,同时该聚合物具有良好的可溶解性,便于加工应用。将合成得到的荧光聚合物配制成溶液,通过浸渍法制备得到金属Fe3+检测试纸,该试纸对金属Fe3+具有荧光增强响应性,还具有便携、灵敏度高和检测操作简单等优势,将待测溶液滴于试纸,就能够快速、简便地进行金属Fe3+的检测。
Description
技术领域
本发明属于荧光检测领域,更具体地,涉及一种荧光聚合物、Fe3+检测试纸及其制备方法与应用。
背景技术
铁本身不具有毒性,但当摄入过量或误服过量的铁制剂时也可能导致铁中毒。铁过量会损伤细胞的基本成分,例如脂肪酸、蛋白质、核酸等,导致其他微量元素失衡,特别是钙、镁的需求量。饮用水中含铁过多,可引起食欲不振、呕吐、腹泻、胃肠道紊乱、排便失常等症状。在生活上,铁离子能在白色织物或用水器皿、卫生器具上留下黄斑,同时还容易使铁细菌繁殖,堵塞管道。因此,对水体铁离子的检测是有必要的。
对于铁离子的检测,邻菲啰啉法、磺基水杨酸法和硫氰酸钾比色法是较为常用的几种方法,但操作过程繁琐,而仪器分析法所使用的仪器较为昂贵。荧光检测技术以其灵敏度高和动态响应范围广的优势被逐渐研究成为一种新型的检测方式。
发明内容
本发明的目的是针对以上不足,提供一种荧光聚合物及其制备方法,该荧光聚合物具有良好的可溶解性,便于加工应用,且具有较好的荧光-金属离子响应性,可用于Fe3+荧光检测。
本发明是另一个目的在于提供一种金属Fe3+离子检测试纸,该试纸具有便携性,遇金属Fe3+发生荧光增强,能够快速、简便地检测金属Fe3+离子。
为实现上述目的,本发明是通过以下技术方案实现的:
一种荧光聚合物,其结构式为:
优选的,所述重复结构单元n为60~120。
上述荧光聚合物的合成路线如下:
上述荧光聚合物的制备方法,包括以下步骤:
将二胺单体和六氟苯酐单体混入有机溶剂中,加入催化剂,在室温下搅拌25~40分钟;
将反应液温度调整至170~200℃,继续反应10~12小时;
待反应结束后,将反应液洗涤,沉降,然后真空干燥,得到目标荧光聚合物。
优选的,所述二胺单体的结构式为
所述六氟苯酐单体的结构式为
优选的,所述二胺单体和六氟苯酐的摩尔比为1:1~1:4,进一步优选为1:3。
优选的,所述有机溶剂的用量为所述二胺单体与六氟苯酐总质量的6~12倍;所述催化剂的用量为所述有机溶剂质量的1%~3%。
优选的,所述有机溶剂为间甲酚;所述催化剂为异喹啉。
优选的,室温下采用磁力搅拌,搅拌时间为30分钟;再将反应液温度调整至190℃,温度调整后的反应时间为12小时。
优选的,所述洗涤,沉降,真空干燥的具体步骤为:待反应结束后,将反应液倒于200~300mL无水乙醇中,沉降结束后,得到目标聚合物;将聚合物在120~150℃条件下真空干燥8~12小时,以确保样品完全干燥。
进一步优选的,所述无水乙醇为250mL,真空干燥温度为120℃,干燥时间为10小时。
本发明还提供了上述荧光聚合物在Fe3+荧光检测中的应用,即用于制备Fe3+检测试纸。
一种Fe3+检测试纸,是通过上述荧光聚合物制备得到的,其采用的基底为滤纸。
上述Fe3+检测试纸的制备方法,包括以下步骤:
将荧光聚合物和有机溶剂混合,震荡至荧光聚合物充分溶解,配制得到荧光聚合物溶液;
将滤纸浸渍于荧光聚合物溶液中5~10分钟后,取出,在70~100℃下真空烘干1~3小时,得到金属Fe3+检测试纸。
优选的,所述有机溶剂为N,N-二甲基乙酰胺,N,N-二甲基甲酰胺,二氯甲烷,三氯甲烷,四氢呋喃中一种。
优选的,所述荧光聚合物溶液的浓度为8wt%~15wt%。
与现有技术相比,本发明的有益效果为:
(1)本发明合成的荧光聚合物,在聚合物结构中引入三氟甲基,能够提高聚合物的光、热稳定性,有利于金属离子检测方面荧光响应的提高,使其具有较好的荧光-金属离子响应性,可用于金属离子的荧光检测,同时该聚合物具有良好的可溶解性,便于加工应用。
(2)本发明采用所述荧光聚合物制备的金属Fe3+检测试纸,具有便携、灵敏度高和检测操作简单等优势,遇金属Fe3+发生荧光增强,能够快速、简便地检测金属Fe3+离子。
附图说明
图1为实施例1所制备的荧光聚合物的核磁氢谱图;
图2为图1中的局部放大图。
图3为实施例2中金属Fe3+检测试纸的SEM表面图;
图4为实施例3中金属Fe3+吸附前后试纸的荧光光谱及紫外光照射下的对比图。
具体实施方式
下面将结合附图和具体实施例更详细地描述本发明的优选实施方式。
以下实施例中所用到的二胺单体:参照专利202011492069.2制备得到。
六氟苯酐单体为市售,购于TCI公司。
实施例1
一种荧光聚合物,其结构式如下:
其中,n=60~120。
上述荧光聚合物的合成路线如下:
上述荧光聚合物的制备方法如下:
在三口烧瓶中,加入5mmol二胺单体和5mmol六氟苯酐单体,加入48mL甲酚作溶剂,0.1503g异喹啉为催化剂,在室温下磁力搅拌30分钟,然后将反应液温度调整至190℃,继续反应12小时。待反应结束后,将反应液倒于250mL无水乙醇中,沉降结束反应,进一步过滤,洗涤。最后将聚合物在120℃条件下真空干燥10小时,得到目标聚合物。图1和图2是目标聚合物的核磁氢谱图,从图中可看出合成得到的聚合物各吸收峰的积分值与所设计的结构式中质子数完全一致。
实施例2
一种Fe3+检测试纸的制备,制备过程如下:
称取1.041g实施例1所述荧光聚合物与10mL N,N-二甲基乙酰胺混合,震荡至聚合物充分溶解,配制得到10wt%的荧光聚合物溶液。将滤纸浸渍于聚合物溶液中5分钟后,取出固定于支撑架上,在80℃下烘干2小时,得到金属Fe3+检测试纸。
如图3所示,制备得到的检测试纸表面平整且具有大量的孔隙,这是干燥过程中溶剂挥所形成,这些孔隙能够使待测液体充分渗透到试纸中,有利于对液体中的金属离子进行吸附。
实施例3
金属Fe3+检测试纸的应用,测试过程如下:
配制5×10-6mol/L含Fe3+的溶液,将溶液滴于检测试纸,等待60s后在紫外光照射下与空白试纸进行对照。
如图4所示,检测试纸在吸附Fe3+前的荧光发射光谱在603nm处显示最大荧光发射峰,吸附Fe3+后,荧光最大发射峰红移至630nm处,试纸在吸附Fe3+后荧光强度增强,对比紫外光照下普通滤纸和吸附前后的试纸,检测试纸呈现出黄色荧光,且吸附Fe3+后的试纸有明显的荧光增强现象,说明本发明制备的检测试纸遇金属Fe3+有荧光增强的响应性,能够检测到水体中的Fe3+。
以上已经描述了本发明的各实施例,上述说明是示例性的,并非穷尽性的,并且也不限于所披露的各实施例。在不偏离所说明的各实施例的范围和技术原理的情况下,对于本技术领域的普通技术人员来说许多修改和变更都是显而易见的,这些修改和变更也应视为本发明的保护范围。
Claims (7)
1.一种荧光聚合物在Fe3+荧光检测中的应用,其特征在于,所述荧光聚合物的结构式为:
;
所述结构式中重复结构单元n为60~120。
2.根据权利要求1所述的荧光聚合物在Fe3+荧光检测中的应用,其特征在于,所述荧光聚合物的制备方法包括以下步骤:
将二胺单体和六氟苯酐单体混入有机溶剂中,加入催化剂,在室温下搅拌25~40分钟;
将反应液温度调整至170~200℃,继续反应10~12 小时;
待反应结束后,将反应液洗涤,沉降,然后真空干燥,得到目标荧光聚合物。
3.根据权利要求2所述的荧光聚合物在Fe3+荧光检测中的应用,其特征在于,所述二胺单体和六氟苯酐的摩尔比为1:1~1:4,所述有机溶剂的用量为所述二胺单体与六氟苯酐总质量的6~12倍;所述催化剂的用量为所述有机溶剂质量的1%~3%。
4.一种Fe3+检测试纸,其特征在于,是由权利要求1所述的荧光聚合物制备得到的,所述荧光聚合物的结构式为:
,所述结构式中重复结构单元n为60~120;
所述Fe3+检测试纸的制备方法包括以下步骤:
将荧光聚合物和有机溶剂混合,震荡至荧光聚合物充分溶解,配制得到荧光聚合物溶液;
将滤纸浸渍于荧光聚合物溶液中5~10 分钟后,取出,在70-100 ℃下真空烘干1~3 小时,得到金属Fe3+检测试纸。
5.根据权利要求4所述的Fe3+检测试纸,其特征在于,所述有机溶剂为N,N-二甲基乙酰胺,N,N-二甲基甲酰胺,二氯甲烷,三氯甲烷,四氢呋喃中一种。
6. 根据权利要求4所述的Fe3+检测试纸,其特征在于,所述荧光聚合物溶液的浓度为8wt%~15 wt%。
7.一种权利要求4所述的Fe3+检测试纸在Fe3+的荧光检测中的应用。
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