CN104964955A - Production method and application of fluorescence gel film for detecting mercury ions - Google Patents
Production method and application of fluorescence gel film for detecting mercury ions Download PDFInfo
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- CN104964955A CN104964955A CN201510274216.1A CN201510274216A CN104964955A CN 104964955 A CN104964955 A CN 104964955A CN 201510274216 A CN201510274216 A CN 201510274216A CN 104964955 A CN104964955 A CN 104964955A
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Abstract
The invention discloses a production method of a fluorescence gel film for detecting mercury ions. The method comprises the following steps: grafting a fluorescence carbon dot to polyvinylamine through a covalent bond, carrying out cross-linking copolymerization on fluorescence carbon dot-grafted polyvinylamine and an acrylamide monomer, and placing the obtained material in a die to produce the fluorescence gel film. The fluorescence gel film has the advantages of good water solubility, simple manufacturing, low production cost, high mercury ion concentration detection sensitivity and simple operation; and the fluorescence gel film used in the mercury ion detection can be repeatedly used after ethylene diamine tetraacetic acid treatment, so the fluorescence gel film also has the advantages of environmental protection and use cost reduction.
Description
Technical field
The invention belongs to material preparation and environment ion detection technique field, more particularly, the present invention relates to a kind of preparation method of the fluorescence gel film for detecting mercury ion, and the application that this fluorescence gel film detects mercury ion in water.
Background technology
The environmental pollution caused due to the urbanization that increases fast and industrialization is becoming increasingly rampant, heavy metal causes pollution serious all the more, in heavy metal ion, dimercurion has higher toxicity, it can enrichment in vivo, and be finally absorbed by the body through food chain, thus cause a series of serious disease of the mankind, constitute a serious threat to ecologic environment and human health, the detection of the mercury ion in aquatic ecosystem has become a very important problem of environmental area.
Along with the development of science and technology, the method for ion detection is on the increase, and mainly contains Atomic absorption/emission spectrometry, Auger electron spectroscopy, inductively coupled plasma mass spectrometry, polarography, electrochemical method be applied to ion detection.But these method costs are higher, and testing process is loaded down with trivial details.Detection method based on fluorescence demonstrates the unique advantages such as highly sensitive, simple to operate and response time is short, many by adopting organic molecule, polymkeric substance, metal nanometer cluster and semiconductor-quantum-point etc. to be in the news for the detection of mercury ion based on the method for fluorescence at present.But the building-up process of these fluorescent materials is complicated, and cost is high, poorly water-soluble, limit the practical application of these fluorescent materials in water environment.Therefore, develop that to can be used for the fluorescent nano material of mercury ion detecting in water environment significant.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above and/or defect, and the advantage will illustrated at least is below provided.
A further object of the invention is to provide a kind of fluorescence gel film for detecting mercury ion, by fluorescent carbon point is grafted on polyvinylamine with covalent bond with fixing fluorescent carbon point, again itself and acrylamide monomer are placed in mould are made by copolymerzation with cross-linking, the fluorescence gel film obtained can detect the concentration of mercury ion in water, can also, by reusing after ethylenediamine tetraacetic acid process, detect sensitive.
In order to realize, according to these objects of the present invention and other advantage, providing a kind of technical scheme:
For detecting a preparation method for the fluorescence gel film of mercury ion, fluorescent carbon point being grafted on polyvinylamine with covalent bond, being then placed in mould with acrylamide monomer by copolymerzation with cross-linking and making fluorescence gel film.
Present invention also offers a kind of scheme, a kind of preparation method of the fluorescence gel film for detecting mercury ion, comprises the following steps:
1) get 5-10mL fluorescent carbon point solution and be placed in container, add coupling agent under magnetic stirring, and regulate pH to 4.5, lucifuge reaction 20min, wherein, the volume ratio of fluorescent carbon point solution and coupling agent is 1: 0.8-1, and the concentration of described fluorescent carbon point solution is 0.5g/L;
2) in step 1) add 0.1-0.3g polyvinylamine hydrochloride, lucifuge reaction 12h under magnetic stirring in the mixed solution that obtains;
3) in step 2) add the dilution of 20mL deionized water in the mixed solution that obtains, add 1.7-1.9g acrylamide monomer and 0.002gN, N under magnetic stirring '-methylene-bisacrylamide, obtain clear solution after stirring 15min;
4) in described clear solution, 0.02-0.03g initiating agent and 18-22 μ LN is added, N, N ', N '-tetramethylethylenediamine, stirs, and obtains gel solution;
5) described gel solution is poured in mould, after continuing reacting drying, obtain fluorescence gel film.
Preferably, the preparation method of the described fluorescence gel film for detecting mercury ion, described coupling agent is the potpourri of EDC and NHS, and the mol ratio of EDC and NHS is 10: 1.
Preferably, the preparation method of the described fluorescence gel film for detecting mercury ion, described initiating agent is potassium persulfate or ammonium persulfate.
Preferably, the preparation method of the described fluorescence gel film for detecting mercury ion, step 5) in the temperature of reaction be 40 DEG C, the time is 24h.
Preferably, the application of the described fluorescence gel film for detecting mercury ion, described fluorescence gel film is to the detection of the ion concentration of mercury in aqueous solution.
The present invention at least comprises following beneficial effect:
1) fluorescence gel film of the present invention has good water solubility, make simple, production cost is low, detect the advantage that ion concentration of mercury is highly sensitive, simple to operate, and fluorescence gel film of the present invention is after detection mercury ion, can reuse with after ethylenediamine tetraacetic acid process, both environmental protection again reduced use cost.
2) under the first pH environment being suitable for of the present invention, activating coupling agent makes its activity the highest, add polyvinylamine hydrochloride again to make it to carry out cross-linking reaction with fluorescent carbon point, improve the percent grafting of fluorescent carbon point, in addition, the percent grafting using polyvinylamine hydrochloride ratio polyvinylamine and fluorescent carbon point to react is high, further increase the percent grafting of fluorescent carbon point, thus increase the sensing range of mercury ion in gel film;
3) the present invention adds N, and N '-methylene-bisacrylamide, initiating agent, TEMED, with make acrylamide carry out gel film that free radical polymerization obtains cross-linked structure, improve the thin film strength of fluorescence gel.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Accompanying drawing explanation
Fig. 1 is the infrared spectrum of fluorescent carbon point and polyvinylamine-g-fluorescent carbon point of the present invention;
Fig. 2 is that fluorescence gel film of the present invention excites the lower fluorescence emission spectrogram to ion concentration of mercury response in 300nm excitation wavelength;
Fig. 3 is fluorescence gel film of the present invention linear relationship chart based on fluorescence intensity and ion concentration of mercury under 422nm excitation wavelength excites.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, can implement according to this with reference to instructions word to make those skilled in the art.
Should be appreciated that used hereinly such as " to have ", other element one or more do not allotted in " comprising " and " comprising " term or the existence of its combination or interpolation.
Embodiment 1
For detecting a preparation method for the fluorescence gel film of mercury ion, comprise the following steps:
1) get 5mL fluorescent carbon point solution and be placed in container, the concentration of described fluorescent carbon point solution is 0.5g/L, adds 5mL coupling agent under magnetic stirring, and regulates pH to 4.5, lucifuge reaction 20min;
2) in step 1) add 0.1g polyvinylamine hydrochloride, lucifuge reaction 12h under magnetic stirring in the mixed solution that obtains;
3) in step 2) add the dilution of 20mL deionized water in the mixed solution that obtains, add 1.7g acrylamide monomer and 0.002gN, N under magnetic stirring '-methylene-bisacrylamide, obtain clear solution after stirring 15min;
4) in described clear solution, 0.02g initiating agent and 18 μ LN are added, N, N ', N '-tetramethylethylenediamine, stirs, and obtains gel solution;
5) described gel solution is poured in mould, after continuing reacting drying, obtain fluorescence gel film.
Wherein, described coupling agent is the potpourri of EDC and NHS, and the mol ratio of EDC and NHS is 10: 1.
Wherein, described initiating agent is potassium persulfate.
Wherein, step 5) in the temperature of reaction be 40 DEG C, the time is 24h.
Embodiment 2
For detecting a preparation method for the fluorescence gel film of mercury ion, comprise the following steps:
1) get 10mL fluorescent carbon point solution and be placed in container, the concentration of described fluorescent carbon point solution is 0.5g/L, adds 8mL coupling agent under magnetic stirring, and regulates pH to 4.5, lucifuge reaction 20min;
2) in step 1) add 0.2g polyvinylamine hydrochloride, lucifuge reaction 12h under magnetic stirring in the mixed solution that obtains;
3) in step 2) add the dilution of 20mL deionized water in the mixed solution that obtains, add 1.8g acrylamide monomer and 0.002gN, N under magnetic stirring '-methylene-bisacrylamide, obtain clear solution after stirring 15min;
4) in described clear solution, 0.03g initiating agent and 20 μ LN are added, N, N ', N '-tetramethylethylenediamine, stirs, and obtains gel solution;
5) described gel solution is poured in mould, after continuing reacting drying, obtain fluorescence gel film.
Wherein, described coupling agent is the potpourri of EDC and NHS, and the mol ratio of EDC and NHS is 10: 1.
Wherein, described initiating agent is ammonium persulfate.
Wherein, step 5) in the temperature of reaction be 40 DEG C, the time is 24h.
Claims (6)
1. for detecting a preparation method for the fluorescence gel film of mercury ion, it is characterized in that, fluorescent carbon point is grafted on polyvinylamine with covalent bond, be then placed in mould with acrylamide monomer make fluorescence gel film by copolymerzation with cross-linking.
2. as claimed in claim 1 for detecting a preparation method for the fluorescence gel film of mercury ion, it is characterized in that, comprise the following steps:
1) get 5-10mL fluorescent carbon point solution and be placed in container, add coupling agent under magnetic stirring, and regulate pH to 4.5, lucifuge reaction 20min, wherein, the volume ratio of fluorescent carbon point solution and coupling agent is 1: 0.8-1, and the concentration of described fluorescent carbon point solution is 0.5g/L;
2) in step 1) add 0.1-0.3g polyvinylamine hydrochloride, lucifuge reaction 12h under magnetic stirring in the mixed solution that obtains;
3) in step 2) add the dilution of 20mL deionized water in the mixed solution that obtains, add 1.7-1.9g acrylamide monomer and 0.002gN, N under magnetic stirring '-methylene-bisacrylamide, obtain clear solution after stirring 15min;
4) in described clear solution, 0.02-0.03g initiating agent and 18-22 μ LN is added, N, N ', N '-tetramethylethylenediamine, stirs, and obtains gel solution;
5) described gel solution is poured in mould, after continuing reacting drying, obtain fluorescence gel film.
3. as claimed in claim 2 for detecting the preparation method of the fluorescence gel film of mercury ion, it is characterized in that, described coupling agent is the potpourri of EDC and NHS, and the mol ratio of EDC and NHS is 10: 1.
4. as claimed in claim 3 for detecting the preparation method of the fluorescence gel film of mercury ion, it is characterized in that, described initiating agent is potassium persulfate or ammonium persulfate.
5. as claimed in claim 4 for detecting the preparation method of the fluorescence gel film of mercury ion, to it is characterized in that, step 5) in the temperature of reaction be 40 DEG C, the time is 24h.
6. as claimed in claim 5 for detecting the application of the fluorescence gel film of mercury ion, it is characterized in that, described fluorescence gel film is to the detection of the ion concentration of mercury in aqueous solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112697757A (en) * | 2020-12-10 | 2021-04-23 | 浙江理工大学 | Preparation method of fluorescent sensor for Cr (VI) instant detection and product thereof |
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| US20120238035A1 (en) * | 2011-03-18 | 2012-09-20 | Geddes Chris D | Multicolor microwave-accelerated metal-enhanced fluorescence (m-mamef) |
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| CN102964608A (en) * | 2012-11-15 | 2013-03-13 | 中北大学 | Preparation method of carbon quantum dot containing calcium alginate gel for detecting copper ions |
| US20140224641A1 (en) * | 2011-03-18 | 2014-08-14 | Chris D. Geddes | Metal-enhanced photoluminescence from carbon nanodots |
| CN104610964A (en) * | 2015-01-08 | 2015-05-13 | 中国科学院大学 | Preparation method of wavelength adjustable fluorescent carbon dot and application of fluorescent carbon dot in mercury ion detection |
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| US20120238035A1 (en) * | 2011-03-18 | 2012-09-20 | Geddes Chris D | Multicolor microwave-accelerated metal-enhanced fluorescence (m-mamef) |
| US20140224641A1 (en) * | 2011-03-18 | 2014-08-14 | Chris D. Geddes | Metal-enhanced photoluminescence from carbon nanodots |
| CN102702546A (en) * | 2012-05-10 | 2012-10-03 | 陕西师范大学 | Preparation method of perylene bisimide cholesterol polymer gel fluorescent sensing film, and application thereof |
| CN102964608A (en) * | 2012-11-15 | 2013-03-13 | 中北大学 | Preparation method of carbon quantum dot containing calcium alginate gel for detecting copper ions |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112697757A (en) * | 2020-12-10 | 2021-04-23 | 浙江理工大学 | Preparation method of fluorescent sensor for Cr (VI) instant detection and product thereof |
| CN112697757B (en) * | 2020-12-10 | 2024-05-03 | 浙江理工大学 | Preparation method of fluorescence sensor for instant detection of Cr (VI) and product thereof |
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