CN103922300A - Preparation and application of bifluorescent carbon nanodots - Google Patents
Preparation and application of bifluorescent carbon nanodots Download PDFInfo
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Abstract
In allusion to preparation complexity and poor water solubility of an Al<3+> ratiometric fluorescent probe in the prior art, the invention provides a preparation method of bifluorescent carbon nanodots and an application of the prepared bifluorescent carbon nanodots used as an Al<3+> ratiometric fluorescent probe. According to the invention, a green product Avena nuda is used as a raw material to prepare the bifluorescent (347nm and 428nm) carbon nanodots with good resolution by a microwave method. The preparation method is simple and has low cost. The prepared bifluorescent carbon nanodots which are used as the Al<3+> ratiometric fluorescent probe have characteristics of good selectivity and high sensitivity, and can be used to rapidly detect the concentration of Al<3+> in an aqueous solution containing Al<3+>.
Description
Technical field
The present invention relates to nano material preparation and application, be specifically related to the preparation method of a kind of pair of fluorescent carbon nano dot, and two fluorescent carbon nano dots of preparation are as Al
3+the application of ratio fluorescent probe.
Background technology
Carbon nano dot is subject to the extensive concern of vast researcher as a kind of novel fluorescent carbon nano material.Compared with conventional semiconductors quantum dot, it has the plurality of advantages such as good water solubility, high, the easy functionalization of chemical stability, fast light bleaching, nontoxic, good biocompatibility, therefore has broad application prospects in the field such as biomarker and fluorescence imaging.
The preparation method of carbon nano dot is varied, substantially can be divided into laser lift-off graphite method, electrochemical oxidation process, arc discharge method, microwave process for synthesizing, chemical oxidization method, high temperature pyrolytic cracking (HTP) etc., main carbon source has Graphene, carbon nanotube, gac, small molecules organic compound etc.
At present, most of carbon nano dots are single fluorescence.From the angle of Application in Sensing, two fluorescent carbon nano dots of development distinguishing good (being greater than 80nm) are still subject to attention highly, because this carbon nano dot can utilize the intensity rate of the fluorescence peak that two distinguishings are good to be designed to ratio fluorescent probe.Compared with single fluorescence intensity probe, ratio fluorescent probe is by the fluorescence intensity at two different wave length places of measuring probe material, using its ratio as signal parameter, thereby measures target compound.Fluorescence ratio signal is not subject to the impact of intensity of light source fluctuation and instrumental sensitivity, and therefore ratio fluorescent probe can improve accuracy, sensitivity and the responding range of method.
In recent years, some Al
3+ratio fluorescent probe appears in the newspapers.Document (A naphthalimide – quinoline based probe for selective, fluorescence ratiometric sensing of trivalent ions, Shyamaprosad Goswami, Krishnendu Aich, Avijit Kumar Das, Abhishek Manna and Sangita Das, RSC Advances, 2013,3,2412), detect Al with naphthalimide-quinoline mixture
3+; Document (Design of a dual-signaling sensing system for fluorescent ratiometric detection of Al
3+ion based on the inner-filter effect, Yongxiang Wang, Limin Xiong, Fenghua Geng, Fuqiang Zhang and Maotian Xu, Analyst, 2011,136,4809), detect Al with alizarin red S and m-four (N-methyl-4-pyridyl) porphyrin durene sulfonate systems alone
3+; Document (A differentially selective sensor with fluorescence turn-on response to Zn
2+and dual-mode ratiometric response to Al
3+in aqueous media, Debabrata Maity and T.Govindaraju, Chem.Commun., 2012,48,1039 – 1041), detect Al with quinoline-tonka bean camphor mixture
3+; Document (Ratiometric fluorescence sensing and intracellular imaging of Al
3+ions driven by an intramolecular excimer formation of a pyrimidine – pyrene scaffold, Sudipta Das, Animesh Sahana, Arnab Banerjee, Sisir Lohar, Damir A.Safin, Maria G.Babashkina, Michael Bolte, Yann Garcia, Ipsit Hauli, Subhra Kanti Mukhopadhyay and Debasis Das, Dalton Trans., 2013,42,4757), detect Al with pyrimidine-pyrene mixture
3+.But, these Al
3+ratio fluorescent probe has the shortcoming of preparation complexity and poorly water-soluble.
Prior art does not also have the two fluorescent carbon nano dots Al simple as preparing, good water solubility using distinguishing good (being greater than 80nm)
3+ratio fluorescent probe.
Summary of the invention
The object of the invention is for existing Al
3+the preparation of ratio fluorescent probe is complicated, the problem of poorly water-soluble, provide the preparation method of a kind of pair of fluorescent carbon nano dot, and two fluorescent carbon nano dots prepared by the method is as Al
3+the application of ratio fluorescent probe.
The preparation method of a kind of pair of fluorescent carbon nano dot provided by the invention, comprises the steps:
(1) by naked oats at 200～600 DEG C of high temperature carbonizations;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by step (2) and mix 1:25～200 in mass ratio with water, react and obtain black dirty solution by microwave heating;
(4) black dirty solution is centrifugal with whizzer, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
The time of the described naked oats high temperature carbonization of step (1) is 0.5～4h.
The described microwave heating reaction times of step (3) is 6～16min.
The two fluorescent carbon nano dots of the present invention are as Al
3+the application of ratio fluorescent probe: carbon nano dot is dissolved in containing Al
3+phosphate buffer soln in, excitation wavelength is fixed between 250～310nm, under fixed temperature, it is carried out to fluorescence spectrum detection, measures 347nm and 428nm place fluorescence peak intensity, according to the ratio at two peaks, and then reaches Al
3+the detection of content.
Compared with prior art, beneficial effect of the present invention:
(1) the prepared carbon nano dot of the present invention uses naked oats as carbon precursor, and its raw material is cheap and easy to get, and preparation method is simple, can not place for a long time and can precipitate, and have no side effect.
(2) the prepared carbon nano dot of the present invention has two (>80nm) fluorescence peaks that distinguishing is good, can be used as ratio fluorescent probe in detecting Al
3+, eliminate systematic error and the background error of the instrument being caused by extraneous labile factor, its sensitivity is improved greatly.
(3) the prepared carbon nano dot of the present invention is as detecting Al
3+ratio fluorescent probe, to Al
3+the selectivity detecting is high, and favorable reproducibility is highly sensitive, and other metal ions are to Al
3+interference very little, can detect quickly and accurately Al in liquid to be measured
3+content.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of two fluorescent carbon nano dots of preparing of embodiment 1
Fig. 2 is two fluorescent carbon nano dot aqueous solution picture under fluorescent lamp, ultraviolet lamp (wavelength is 254nm and 365nm) irradiate respectively prepared by embodiment 1
Fig. 3 is two fluorescent carbon nano dots of the embodiment of the present invention 1 fluorescence emission spectrograms under different excitation wavelengths
Fig. 4 is the different concns Al that is dissolved with carbon nano dot in the embodiment of the present invention 7
3+the fluorescence emission spectrogram of phosphate buffer solution
Fig. 5 is the different concns Al that is dissolved with carbon nano dot in the embodiment of the present invention 7
3+phosphate buffer solution at 347nm and the fluorescence peak intensity rate (I of 428nm place
347/ I
428) with Al
3+the working curve of change in concentration
Fig. 6 is the fluorescence emission spectrogram that is dissolved with the phosphate buffer solution of the different metal ion of carbon nano dot in the embodiment of the present invention 8
Fig. 7 is dissolved with the phosphate buffer solution of different metal ion of carbon nano dot at 428nm and the fluorescence peak intensity rate (I of 347nm place in the embodiment of the present invention 8
428/ I
347) with the relation of metal ion
Embodiment
Following examples are further set forth content of the present invention, but the present invention is not limited to these embodiment.
Embodiment 1
The preparation of two fluorescent carbon nano dots:
(1) by 400 DEG C of high temperature carbonization 2h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 1g step (2) and mix with 80mL water, microwave heating reaction 12min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
The transmission electron microscope picture of two fluorescent carbon nano dots of preparation is shown in Fig. 1.
Two fluorescent carbon nano dot aqueous solution of the preparation respectively picture under fluorescent lamp, ultraviolet lamp (wavelength is 254nm and 365nm) irradiate are shown in Fig. 2, wherein 1 is the picture of the carbon nano dot aqueous solution under fluorescent lamp irradiates, color is colourless, 2 for wavelength be the picture under 254nm ultra violet lamp, color is blue, 3 for wavelength is the picture under 365nm ultra violet lamp, and color is cyanic colours.
The fluorescence spectrum figure of two fluorescent carbon nano dots of preparation under different excitation wavelengths is shown in Fig. 3, and wherein 1～6 is respectively that excitation wavelength is the fluorescence spectrum figure under 260nm, 270nm, 280nm, 290nm, 300nm and 310nm excite.
Embodiment 2
The preparation of two fluorescent carbon nano dots:
(1) by 300 DEG C of high temperature carbonization 3h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 1g step (2) and mix with 90mL water, microwave heating reaction 8min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
Embodiment 3
The preparation of two fluorescent carbon nano dots:
(1) by 200 DEG C of high temperature carbonization 4h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 1g step (2) and mix with 100mL water, microwave heating reaction 16min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
Embodiment 4
The preparation of two fluorescent carbon nano dots:
(1) by 500 DEG C of high temperature carbonization 1h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 0.5g step (2) and mix with 100mL water, microwave heating reaction 14min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
Embodiment 5
The preparation of two fluorescent carbon nano dots:
(1) by 600 DEG C of high temperature carbonization 0.5h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 0.5g step (2) and mix with 90mL water, microwave heating reaction 10min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
Embodiment 6
The preparation of two fluorescent carbon nano dots:
(1) by 350 DEG C of high temperature carbonization 2.5h of naked oats;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by 0.5g step (2) and mix with 80mL water, microwave heating reaction 6min obtains black dirty solution;
(4) use whizzer with the centrifugal 15-20min of 3500r/min rotating speed black dirty solution, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
Embodiment 7
Two fluorescent carbon nano dots of embodiment 1 are as detecting Al
3+the sensitivity experiment of ratio fluorescent probe:
With the 0.01molL of pH=5
-1phosphoric acid buffer and Al
2(SO
4)
3preparation is containing Al respectively
3+concentration is 0 μ molL
-1, 1 μ molL
-1, 2.5 μ molL
-1, 5 μ molL
-1, 10 μ molL
-1, 25 μ molL
-1, 50 μ molL
-1, 100 μ molL
-1, 150 μ molL
-1, 175 μ molL
-1, 200 μ molL
-1, 250 μ molL
-1with 300 μ molL
-1the aqueous solution, respectively 0.06mg carbon nano dot is dissolved into 3mL above-mentioned containing different concns Al
3+the aqueous solution in, fixing excitation wavelength is 310nm, at 20 DEG C, carries out fluorescence spectrum detection, measures 347nm and 428nm place fluorescence peak intensity, according to the ratio at two peaks, and then reaches Al
3+the detection of concentration.
Be dissolved with the different concns Al of carbon nano dot
3+the fluorescence emission spectrogram (see figure 4) of phosphate buffer solution: in figure, 1-13 is respectively Al
3+concentration is 0 μ molL
-1, 1 μ molL
-1, 2.5 μ molL
-1, 5 μ molL
-1, 10 μ molL
-1, 25 μ molL
-1, 50 μ molL
-1, 100 μ molL
-1, 150 μ molL
-1, 175 μ molL
-1, 200 μ molL
-1, 250 μ molL
-1with 300 μ molL
-1the fluorescence emission spectrogram of the phosphate buffer solution that is dissolved with carbon nano dot; As can be seen from the figure along with the increase of aluminium ion concentration, 347nm place fluorescence peak intensity is substantially constant, and 428nm place fluorescence peak intensity reduces gradually.
Be dissolved with the different concns Al of carbon nano dot
3+phosphate buffer solution at 347nm and the fluorescence peak intensity rate (I of 428nm place
347/ I
428) with Al
3+the working curve (see figure 5) of change in concentration: along with aluminium ion concentration is from 2.5 μ molL
-1be increased to 300 μ molL
-1, 347nm and the fluorescence peak intensity rate (I of 428nm place
347/ I
428) linear increasing.
Embodiment 8
Two fluorescent carbon nano dots of embodiment 1 are as detecting Al
3+the selectivity experiment of ratio fluorescent probe:
With the 0.01molL of pH=5
-1phosphoric acid buffer and Al
2(SO
4)
3, BaCl
2, CaCl
2, CdCl
2, Co (NO
3)
2, CuCl
2, Fe (NO
3)
3, HgCl
2, KCl, Mg (NO
3)
2, MnCl
2, NaCl, NiCl
2, Zn (NO
3)
2preparation is 300 μ molL containing different metal ionic concn respectively
-1solution, respectively 0.06mg carbon nano dot is dissolved into 3mL above-mentioned containing in the solution of different metal ion, fixing excitation wavelength is 310nm, at 20 DEG C, carry out fluorescence spectrum detection, measure 428nm and 347nm place fluorescence peak intensity, according to the ratio at two peaks, and then reach Al
3+optionally detect.In the phosphate buffer solution of the above-mentioned different metal ion that is dissolved with carbon nano dot, continue to add Al respectively
2(SO
4)
3, make Al
3+concentration is 300 μ molL
-1, fixing excitation wavelength is 310nm, at 20 DEG C, carries out fluorescence spectrum detection, measures 428nm and 347nm place fluorescence peak intensity, according to the ratio at two peaks, and then investigates different metal ion pair Al
3+optionally disturb.
Be dissolved with the fluorescence emission spectrogram (see figure 6) of the phosphate buffer solution of the different metal ion of carbon nano dot: Al
3+significantly quencher carbon nano dot 428nm place fluorescence peak, Cu
2+and Fe
3+simultaneously significantly quencher 347nm and 428nm place fluorescence peak, the fluorescence Spectra of other ion pair carbon nano dot has slight impact.
Be dissolved with the phosphate buffer solution of different metal ion of carbon nano dot at 428nm and the fluorescence peak intensity rate (I of 347nm place
428/ I
347) with metal ion be related to (see figure 7): in the phosphate buffer solution of different metal ion that is dissolved with carbon nano dot, only have Al
3+428nm and the fluorescence peak intensity rate (I of 347nm place
428/ I
347) significantly reduce, illustrate that carbon nano dot can optionally detect Al
3+.In the phosphate buffer solution of different metal ion that is dissolved with carbon nano dot, continue to add Al
3+, 428nm and the fluorescence peak intensity rate (I of 347nm place
428/ I
347) there is remarkable reduction, other ion pair Al is described
3+detection substantially do not disturb.
Claims (4)
1. a preparation method for two fluorescent carbon nano dots, is characterized in that, comprises the steps:
(1) by naked oats at 200～600 DEG C of high temperature carbonizations;
(2) by the product grind into powder after charing;
(3) get naked oats charing powder prepared by step (2) and mix 1:25～200 in mass ratio with water, react and obtain black dirty solution by microwave heating;
(4) black dirty solution is centrifugal with whizzer, remove black precipitate, obtain transparent supernatant liquor;
(5) by carrying out lyophilize under 50 DEG C of conditions of transparent supernatant liquor – to Powdered, obtain carbon nano dot.
2. the preparation method of a kind of pair of fluorescent carbon nano dot as claimed in claim 1, is characterized in that, the time of the described naked oats high temperature carbonization of step (1) is 0.5～4h.
3. the preparation method of a kind of pair of fluorescent carbon nano dot as claimed in claim 1, is characterized in that, the described microwave heating reaction times of step (3) is 6～16min.
4. two fluorescent carbon nano dots that as claimed in claim 1 prepared by method are as Al
3+the application of ratio fluorescent probe.
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| CN105092548A (en) * | 2015-07-14 | 2015-11-25 | 天津大学 | Method for detecting p-nitrophenol based on molecular imprinting ratio type fluorescent probe |
| CN109632752A (en) * | 2019-01-08 | 2019-04-16 | 苏州科技大学 | The method and detector of various metals ion are identified by fluorescent carbon point |
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| CN109632752A (en) * | 2019-01-08 | 2019-04-16 | 苏州科技大学 | The method and detector of various metals ion are identified by fluorescent carbon point |
| CN109632752B (en) * | 2019-01-08 | 2021-08-31 | 苏州科技大学 | Method and detector for identifying multiple metal ions through fluorescent carbon dots |
| CN109777405A (en) * | 2019-02-03 | 2019-05-21 | 山西大同大学 | A kind of red blue pair emits fluorescent carbon points and for detecting Al simultaneously3+And Cu2+The fluorescence analysis method of ion |
| CN109777405B (en) * | 2019-02-03 | 2022-02-08 | 山西大同大学 | Red-blue dual-emission fluorescent carbon dot and method for simultaneously detecting Al3+And Cu2+Method for fluorescence analysis of ions |
| CN115490224A (en) * | 2022-10-14 | 2022-12-20 | 山西大学 | Ratio type red fluorescent carbon dot and preparation method and application thereof |
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