CN105542760A - Preparation method of nitrogen- and sulfur-doped fluorescence carbon dots - Google Patents
Preparation method of nitrogen- and sulfur-doped fluorescence carbon dots Download PDFInfo
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Abstract
The invention discloses a preparation method of nitrogen- and sulfur-doped fluorescence carbon dots. The fluorescence carbon dots are prepared by a hydrothermal method adopting grapefruit juice as a precursor and an N- and S-containing compound as a passivator. The method comprises the following steps: adding the grapefruit juice together with ammonium sulfate, ammonium persulfate, thioacetamide and ammonium sulfide respectively into a reaction kettle and heating for several hours; and centrifuging the reaction liquid, filtering with a filtering membrane and dialyzing to obtain an aqueous solution of carbon dots. According to the preparation method disclosed by the invention, the adopted grapefruit juice comes from natural resources and is easily available; and the doped nitrogen and sulfur are good for enhancing the fluorescence property. The method has the advantages of simple preparation process and controllable conditions and is green and environmentally friendly.
Description
Technical field
The invention belongs to technical field of nano material, relate to one using GRAPEFRUIT EXTRACT as carbon source, adopt hydrothermal method to prepare the method for carbon point.
Background technology
Carbon point is the class Novel Carbon Nanomaterials that development in recent years is got up.After Xu in 2004 etc. adopt electrophoretic method to obtain carbon point from Single Walled Carbon Nanotube separation and purification first, the research about carbon point receives increasing concern.The grain diameter of carbon point is less than 10nm usually, has the optical property that fluorescence intensity is high, good light stability, resistance to photobleaching etc. are excellent.Because carbon point forms primarily of carbon, not containing metallic element, and its surface is containing the water soluble functional group such as hydroxyl and carboxyl, therefore carbon point has hypotoxicity and good water-soluble, thus make carbon point have desirable biocompatibility, have a wide range of applications in cell marking, cell imaging etc.
The preparation method of carbon point can be divided into " from top to bottom " and " from bottom to top " two kinds of methods substantially." from top to bottom " method is that macroscopical carbon structure material is prepared carbon point, as arc process, laser irradiation, electrochemical oxidation process, chemical oxidization method etc. by the method for fracture, pulverizing." from bottom to top " method is as precursor synthesis carbon point using organic molecule.The method comprises high temperature pyrolytic cracking (HTP), hydrothermal method, microwave method and supersonic method etc.Although develop the preparation method of numerous carbon point at present, often there is the shortcomings such as raw materials cost is high, conversion unit is expensive, severe reaction conditions, reaction process are loaded down with trivial details in these methods.Therefore, need to find a kind of cheaper starting materials and be easy to get, preparation process is simple, the carbon point preparation method of environmental protection.
Shaddock is a kind of common fruit, and its output is high, cheap and easy to get, and is rich in carbon and oxygen element, for the carbon point preparing high optical property provides possibility.While being presoma with natural resources, adding compound that is nitrogenous, sulphur can effectively strengthening its fluorescence property.Fructus Citri grandis juice as presoma, respectively using ammonium sulfate, ammonium persulphate, thioacetyl ammonium, ammonium sulfide as passivator, is prepared fluorescent carbon point by the present invention.The method method for making has the features such as simple to operate, environmental protection, is applicable to scale operation.
Summary of the invention
Content of the present invention is to provide that a kind of raw material is easy to get, preparation method's environmental protection, carbon point preparation method simple to operate.For achieving the above object, the fluorescent carbon point preparation method of a kind of nitrogen that adulterates provided by the invention, sulphur take Fructus Citri grandis juice as presoma, and nitrogenous, sulphur compound, as passivator, prepares carbon point by hydrothermal method.The invention provides following technical scheme:
(1) put into wall-breaking machine broken wall after being cut into pieces by shaddock and become Fructus Citri grandis juice, centrifugal, get supernatant liquor;
(2) GRAPEFRUIT EXTRACT and passivator that is nitrogenous, sulphur are added in reactor by a certain percentage react certain hour at a certain temperature;
(3) reaction solution is centrifugal, through membrane filtration, more namely obtain carbon point solution with after dialysis tubing dialysis.
Wherein, in described step (1), the rotating speed of wall-breaking machine is 45000r/min, and centrifugal rotating speed is 8000r/min, and centrifugation time is 10min.
Wherein, containing N passivator in described step (2) is ammonium sulfate, ammonium persulphate, thioacetyl ammonium, ammonium sulfide.
Wherein, in described step (2), the temperature of reaction of GRAPEFRUIT EXTRACT in reactor is 140-200 DEG C, and the reaction times is 8-24h.
Wherein, in described step (3), centrifugal rotating speed is 12000r/min, and the time is 20min.
Wherein, in described step (3), the molecular weight cut-off of dialysis tubing is 3500Mw, and dialysis time is 48h.
Compared with prior art, the beneficial effect that the present invention realizes: the present invention take Fructus Citri grandis juice as presoma, and nitrogenous, sulphur compound is that carbon point prepared by passivator, its preparation method is simple, environmental protection.Carbon point good water solubility prepared by the present invention, good in optical property, is applicable to the fluorescent mark of cell.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture that embodiment 2 prepares carbon point
Embodiment
Embodiment 1
Shaddock wall-breaking machine (45000r/min, 10min) is broken into pulpous state, and centrifugal (8000r/min, 10min) gets supernatant liquor.Get 10mL supernatant liquor and 1.2g ammonium sulfate together to add in reactor react 6h in 160 DEG C.Just reaction solution first centrifugal (10000r/min, 20min) with the membrane filtration using 0.22 μm after removing solid macrobead again.Gained solution molecular weight cut-off is the dialysis tubing dialysis 48h of 3500Da, finally obtains carbon point solution.
Embodiment 2
Shaddock wall-breaking machine (45000r/min, 10min) is broken into pulpous state, and centrifugal (8000r/min, 10min) gets supernatant liquor.Get 10mL supernatant liquor and 1.6g ammonium persulphate together to add in reactor react 18h in 180 DEG C.Just reaction solution first centrifugal (10000r/min, 20min) with the membrane filtration using 0.22 μm after removing solid macrobead again.Gained solution molecular weight cut-off is the dialysis tubing dialysis 48h of 3500Da, finally obtains carbon point solution.
Embodiment 3
Shaddock wall-breaking machine (45000r/min, 10min) is broken into pulpous state, and centrifugal (8000r/min, 10min) gets supernatant liquor.Get 10mL supernatant liquor and 1.6g thioacetyl ammonium together to add in reactor react 24h in 160 DEG C.Just reaction solution first centrifugal (10000r/min, 20min) with the membrane filtration using 0.22 μm after removing solid macrobead again.Gained solution molecular weight cut-off is the dialysis tubing dialysis 48h of 3500Da, finally obtains carbon point solution.
Embodiment 4
Shaddock wall-breaking machine (45000r/min, 10min) is broken into pulpous state, and centrifugal (8000r/min, 10min) gets supernatant liquor.Get 10mL supernatant liquor and 1.8g ammonium sulfide together to add in reactor react 15h in 180 DEG C.Just reaction solution first centrifugal (10000r/min, 20min) with the membrane filtration using 0.22 μm after removing solid macrobead again.Gained solution molecular weight cut-off is the dialysis tubing dialysis 48h of 3500Da, finally obtains carbon point solution.
Claims (6)
1. adulterate the fluorescent carbon point preparation method of nitrogen, sulphur, it is characterized in that comprising the steps:
(1) put into wall-breaking machine broken wall after being cut into pieces by shaddock and become Fructus Citri grandis juice, centrifugal, get supernatant liquor;
(2) GRAPEFRUIT EXTRACT and passivator that is nitrogenous, sulphur are added in reactor by a certain percentage react certain hour at a certain temperature;
(3) reaction solution is centrifugal, through membrane filtration, more namely obtain carbon point solution with after dialysis tubing dialysis.
2. the fluorescent carbon point preparation method of doping nitrogen according to claim 1, sulphur, is characterized in that, the rotating speed of the wall-breaking machine described in step (1) is 45000r/min, and centrifugal rotating speed is 8000r/min, and centrifugation time is 10min.
3. the fluorescent carbon point preparation method of doping nitrogen according to claim 1, sulphur, is characterized in that, described in step (2) is ammonium sulfate, ammonium persulphate, thioacetyl ammonium, ammonium sulfide containing N passivator.
4. the fluorescent carbon point preparation method of doping nitrogen according to claim 1, sulphur, is characterized in that, the temperature of reaction described in step (2) is 160-220 DEG C, and the reaction times is 6-24h.
5. the fluorescent carbon point preparation method of doping nitrogen according to claim 1, sulphur, is characterized in that, the centrifugal rotating speed described in step (3) is 12000r/min, and the time is 20min.
6. the fluorescent carbon point preparation method of doping nitrogen according to claim 1, sulphur, is characterized in that, the molecular weight cut-off of the dialysis tubing described in step (3) is 3500Da, and dialysis time is 48h.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165267A (en) * | 2018-01-05 | 2018-06-15 | 山西大学 | A kind of switching mode pH fluorescence probes and its preparation method and application |
| CN109904007A (en) * | 2019-02-15 | 2019-06-18 | 上海应用技术大学 | A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material |
| WO2021207807A3 (en) * | 2020-01-31 | 2022-02-17 | Fundação Universidade De Brasilia | Photosynthesis stimulator based on hybrid carbon nanoparticles, related production method and related use as nanobiostimulants and nanofertilizers in agricultural crops |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108165267A (en) * | 2018-01-05 | 2018-06-15 | 山西大学 | A kind of switching mode pH fluorescence probes and its preparation method and application |
| CN108165267B (en) * | 2018-01-05 | 2020-09-29 | 山西大学 | Switch type pH fluorescent probe and preparation method and application thereof |
| CN109904007A (en) * | 2019-02-15 | 2019-06-18 | 上海应用技术大学 | A kind of preparation method of spongy nitrogen sulphur codope porous carbon electrode material |
| WO2021207807A3 (en) * | 2020-01-31 | 2022-02-17 | Fundação Universidade De Brasilia | Photosynthesis stimulator based on hybrid carbon nanoparticles, related production method and related use as nanobiostimulants and nanofertilizers in agricultural crops |
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