CN109781677A - It is a kind of for detecting the preparation method of the carbon dots material of Hg2+ in different water bodys - Google Patents
It is a kind of for detecting the preparation method of the carbon dots material of Hg2+ in different water bodys Download PDFInfo
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- CN109781677A CN109781677A CN201711112805.5A CN201711112805A CN109781677A CN 109781677 A CN109781677 A CN 109781677A CN 201711112805 A CN201711112805 A CN 201711112805A CN 109781677 A CN109781677 A CN 109781677A
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Abstract
The present invention relates to one kind for detecting Hg in different water bodys2+Carbon dots material preparation method, this method specifically: by pyridine -2,6- dicarboxyl aqueous acid is put into autoclave, then a certain amount of ethylenediamine solution is added, reaction kettle is put into baking oven and carries out pyroreaction, after reaction filters gained reaction product, a certain amount of distilled water water is added into filtered product, mixed liquor is poured into bag filter, dialyses certain time in ultrapure water to remove the impurity in reaction product.The carbon dots of this method preparation have good fluorescence property, and to Hg2+It has good selectivity and specificity.
Description
Technical field
The invention belongs to carbon nanomaterial and heavy metal analysis technical fields, and in particular to one kind is for detecting different water
Hg in body2+Carbon dots material preparation method.
Background technique
Hg2+, since there is high application value and extensive purposes in industrial circle, while there is high physiology again
Toxicity, therefore, to detecting always without departing from the concern of people for Hg2+.It is shown according to data, due to the life of the mankind
Production activity, about 4700 tons of mercury is released to 187 in environment every year.Although 80% quilt in these mercury pollution artificially generated
It discharges into the atmosphere, 15% is released to land circle, and 5% into hydrosphere, but is recycled by water and the effects of biogenic deposit, mercury
The main influence object of pollution is water and aquatile.Therefore Hg in detection water environment2+Concentration carry out always people in recent years
The hot issue paid close attention to.Pass through the Hg of electrochemical method2+Generally selecting property of detection device and poor sensitivity, and many molecules are visited
There is the problems such as poorly water-soluble, synthesis cost is high in needle, more furthermore the nanometer Hg containing heavy metal again2+Sensing material is also easy to make
At the secondary pollution of use process, practical application is not utilized.Carbon fluorescence quantum is as a kind of nano fluorescent risen recently
Material has obtained extensive research in last decade.Compared to traditional semiconductor alloy fluorescence quantum or molecular probe, by
In generating a large amount of group, such as carboxyl, hydroxyl etc. in the synthesis process, thus with very outstanding water solubility and a variety of have
The dissolubility of solvent.In addition, bio-toxicity and bio-compatibility are all than traditional gold since main component is more carbon skeletons
Metal nanometer material has improvement largely, and not will cause secondary pollution.Simultaneously as carbon fluorescence quantum synthetic method
Simply, various, raw material are extensive, and fluorescence intensity is relatively high, are the novel Hg of design2+The only choosing of sensor.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of each process of system is simple, the carbon dots of preparation have good fluorescence
Performance, and to Hg2+Ten have good selectivity the preparation method with the carbon dots material of specificity.
To solve this technical problem, the technical solution that wood invention uses are as follows:
One kind is for detecting Hg in different water bodys2+Carbon dots material preparation method, specific steps are as follows: by pyridine -2,6-
Dicarboxylic acids is put into autoclave, and a certain amount of ethylenediamine is then added, and reaction kettle is put into baking oven and carries out pyroreaction,
Gained reaction product is filtered after reaction, a certain amount of distilled water is added into filtered product, mixed liquor is poured into
It analyses in bag, for certain time of dialysing in ultrapure water to remove the impurity in reaction product, centrifuging and taking supernatant obtains product.
Pyridine -2,6- dicarboxyl the aqueous acid and ethylenediamine solution molar ratio are 0.1-1M:0.1-5M.
It is 180 DEG C -250 DEG C that the reaction kettle, which is put into and carries out the reaction temperature of pyroreaction in baking oven, reaction time 3-6
Hour.
The aperture of filter paper used in the filtering carbon dots is 0.22 micron, and dialysis bag retention molecular weight is 1000-3500 dongle
, centrifugal rotational speed 3000g-15300g.
The present invention is by utilizing Hg2+Ligand pyridine -2,6- dicarboxylic acids and ethylenediamine as predecessor, pass through a step dry combustion method
Having arrived for method has preferable photoluminescent property and Hg2+The carbon dots of selectivity.By experiment find the carbon dots can to natural water, from
Hg in water and human urine2+It is measured, there is good application potential.
The present invention has the advantage that
1, the preparation method does not use strong acid and strong base or other chemical reagent with environmental pollution in operation, tool
There is the features such as safety and environmental protection, simple and easy, low in cost.
2, the carbon dots prepared through the invention have good physics, chemical stability, higher water solubility, biology poison
The low and good bio-compatibility of property, while a variety of organic solvents are dissolved in, and can be scattered in partial polymer, have
Potential biomedical applications value；
3, the carbon dots of invention preparation can detecte the Hg in natural water, tap water and human urine2+Ion, and examine
Rising limit is lower than national standard, has wide applicability.
Detailed description of the invention
Fig. 1 is the high power transmission electron microscope picture for the carbon dots that the method for the present invention is prepared.
Fig. 2 is the excitation and emission spectra figure of the solution for the carbon dots that the method for the present invention is prepared.
Fig. 3 be the excitation wavelength of carbon dots solution prepared of the present invention from 310nm to 400nm luminescence generated by light figure.
Fig. 4 is selectivity of the carbon dots solution of the invention prepared to metal ion
Fig. 5 is fluorescence intensity and Hg of the carbon dots of the invention prepared in different water bodys2+The linearity curve of ion
Specific embodiment
Above content of the invention is described in further details by the following examples, but this should not be interpreted as this hair
Bright to be limited only to following embodiment, all technologies realized based on the content of present invention are regarded as the scope of the present invention.
Embodiment 1
The ethylenediamine of the pyridine -2,6- dicarboxylic acids of 0.1M and 5M is mixed and is transferred to the ptfe autoclave of 25mL
In, 250 DEG C at a temperature of heat 4h.After reaction, 10mL ultrapure water is added into reaction solution to mix, mixed liquor is poured into
Molecular cut off is in 3500 dalton bag filters, and ultrapure water dialyses 48 hours to remove impurity in reaction product, after from
The heart takes supernatant to obtain carbon dots solution.
Prepared carbon dots, are scanned through transmission electron microscope, see Fig. 1, it can be seen that synthesized carbon dots are divided in water
It is good to dissipate property, pattern is circular granular, and partial size is within 5nm.The fluorescence excitation of the most sub- point of carbon and fluorescence emission spectrum such as Fig. 2,
It can be concluded that a length of 340nm of optimum excitation wave of the carbon dots of this experiment preparation, the emission spectra under maximum excitation wavelength from figure
The most strong emission peak of figure is at 420nm.See during the fluorescence exciting wavelength of the carbon dots gradually becomes 400nm from 310nm
Red shift occurs for the maximum emission peak of Fig. 3, the fluorescence emission spectrum of carbon dots.K+,Cu2+,Na+,Mg2+,Zn2+,Ca2+,Al3+,Cd2+,Ag+,Ni2+,Co2+,Fe3+,Hg2+Fig. 4 is shown in influence Deng 13 metal ion species to carbon dots fluorescence intensity, wherein only Hg2+It is most sub to carbon
Point has the broken effect of going out of apparent fluorescence, and influence sill of other metal ions to carbon dots fluorescence intensity is little.Prepared water
Dissolubility fluorescent carbon point is to Hg2+Ion has good selectivity, can be used as fluorescence probe to detect the Hg in water2+。
Embodiment 2
The ethylenediamine of the pyridine -2,6- dicarboxylic acids of 1M and 0.1M are mixed into the polytetrafluoroethyl-ne alkene reaction that amalgamation liquid is transferred to 25mL
In kettle, 200 DEG C at a temperature of heat 6h.After reaction, 20mL ultrapure water is added into reaction solution to mix, mixed liquor is fallen
Entering molecular cut off is in 1000 dalton bag filters, and ultrapure water dialyses 48 hours to remove impurity in reaction product, after
Centrifuging and taking supernatant obtains carbon dots solution, consistent with 1 product of embodiment through analysis products therefrom.
Embodiment 3
The ethylenediamine of the pyridine -2,6- dicarboxylic acids of 0.5M and 2.5M is mixed and is transferred to the polytetrafluoroethyl-ne alkene reaction of 25mL
In kettle, 180 DEG C at a temperature of heat 3h.After reaction, 15mL ultrapure water is added into reaction solution to mix, mixed liquor is fallen
Entering molecular cut off is in 3000 dalton bag filters, and ultrapure water dialyses 48 hours to remove impurity in reaction product, after
Centrifuging and taking supernatant obtains carbon dots solution.It is consistent with 1 product of embodiment through analysis products therefrom.
Embodiment 4
Carbon dots are dissolved in containing 1-8 μM of Hg2+Lake water in, change in fluorescence degree and Hg2+The relationship of concentration such as Fig. 5 A
Shown, standard variance 0.9994 illustrates the Hg that carbon dots can be used in quantitative detection lake water2+。
Embodiment 5
Carbon dots are dissolved in containing 1-8 μM of Hg2+Tap water in, change in fluorescence degree and Hg2+The relationship of concentration is as schemed
Shown in 5B, standard variance 0.99 illustrates the Hg that carbon dots can be used in quantitative detection tap water2+。
Embodiment 6
Carbon dots are dissolved in containing 1-8 μM of Hg2+Adult male urine in, change in fluorescence degree and Hg2+The pass of concentration
As shown in Figure 5 C, standard variance 0.9977 illustrates the Hg that carbon dots can be used in quantitative detection tap water for system2+。
Embodiment 7
Carbon dots are dissolved in containing 1-8 μM of Hg2+Adult male urine in, change in fluorescence degree and Hg2+The pass of concentration
As shown in Figure 5 D, standard variance 0.9997 illustrates the Hg that carbon dots can be used in quantitative detection tap water for system2+。
Find that the water body sample of the selection of carbon dots influences less selectivity and sensitivity in embodiment, embodiment 4-7 benefit
With gained carbon dots in embodiment respectively to the Hg in lake water, tap water and adult male and female urine sample2+It is tested, is found
All have good linear relationship.
Claims (4)
1. one kind is for detecting Hg in different water bodys2+Carbon dots material preparation method, it is characterised in that according to the following steps into
Row: pyridine -2,6- dicarboxyl aqueous acid being put into autoclave, a certain amount of ethylenediamine solution is then added, will be anti-
It answers kettle to be put into baking oven and carries out pyroreaction, after reaction filter gained reaction product, be added into filtered product
Distilled water pours into mixed liquor in bag filter, certain time of dialysing in ultrapure water to remove impurity in reaction product, from
The heart takes supernatant to obtain product.
2. according to claim 1 for detecting Hg in different water bodys2+Carbon dots material preparation method, it is characterised in that
The molar ratio of the pyridine -2,6- dicarboxylic acids and ethylenediamine is 0.1-1M:0.1-5M.
3. according to claim 1 for detecting Hg in different water bodys2+Carbon dots material preparation method, it is characterised in that
It is 180 DEG C -250 DEG C that the reaction kettle, which is put into and carries out the reaction temperature of pyroreaction in baking oven, and the reaction time is 3-6 hours.
4. according to claim 1 for detecting Hg in different water bodys2+Carbon dots material preparation method, it is characterised in that
The aperture for filtering filter paper used in carbon dots is 0.22 micron, and dialysis bag retention molecular weight is 1000-3500 dalton, centrifugal rotational speed
3000g-15300g。
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115975640A (en) * | 2023-02-08 | 2023-04-18 | 盐城工学院 | One-step synthesis nitrogen-doped carbon-based fluorescent nano probe and method for detecting silver ions by using same |
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