CN103265952A - Environmental-friendly synthesis method of fluorescent carbon dot with up-down conversion function - Google Patents
Environmental-friendly synthesis method of fluorescent carbon dot with up-down conversion function Download PDFInfo
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Abstract
The invention belongs to the field of preparation of fluorescent carbon dots, and discloses a synthesis method of the fluorescent carbon dot with an up-down conversion function. The method comprises the following steps of: adding chilli flakes into water and evenly mixing, thereby obtaining a mixture; transferring the mixture into a hydrothermal kettle, performing a hydrothermal treatment at 120 to 200 DEG C for 2 to 10 hours, and cooling and filtering, thereby obtaining a brown liquid; centrifuging the brown liquid for 10 to 20 minutes, thereby obtaining a supernatant; dialyzing the supernatant by using a dialysis bag with the flow interception volume of 3500; and collecting a dialysate after dialyzing for 10 to 30 hours, thereby obtaining the fluorescent carbon dot. By taking a cheap raw material as a carbon source and the water as a solvent, the method for synthesizing the fluorescent carbon dot with the up-down conversion function in an environmental-friendly manner has the effects that the process is simple; the pretreatment operation is not required; the process that the synthesis is assisted by a strong acid or a surface passivator is not required; the raw material is cheap and easy to obtain; the synthesis condition is moderate and controllable; the high fluorescence quantum yield is achieved; and the carbon dot is good in fluorescent bleaching resistance and stability.
Description
Technical field
The invention belongs to the preparation field of fluorescent carbon point, be specifically related to a kind of green synthesis method of carbon point.
Background technology
Fluorescent carbon point is as a kind of novel fluorescence nano material, owing to its good water-soluble, intrinsic unreactiveness, simple chemically modified, higher fast light bleaching, hypotoxicity and good biocompatibility make the carbon point be subjected to investigator's attention.A lot of method in recent years all is used to synthetic fluorescent carbon point such as electrochemical oxidation, hydro-thermal, acid heat solution, template preparation, microwave, ultrasonic, arc-over and laser-induced thermal etching etc.The non-feature of environmental protection of the costliness of most of its synthesis device of synthetic method and material, the complexity of operation, by product has limited its suitability for industrialized production and in the widespread use of every field.Wherein hydrothermal method is simple to operate, process is controlled, mild condition is acknowledged as best synthetic method.Utilizing in the method for hydrothermal synthesis of carbon point is to adopt the small molecules of carbon containing to be raw material mostly, perhaps adds some other materials in water-heat process, thereby changes the carbon point that thermal and hydric environment obtains better character such as acid, alkali, inorganic salt or organic solvent.Recently become the focus of research with green material as the synthetic fluorescent carbon point of carbon source, because be that the synthetic carbon point of carbon source has advantages such as low cost, environmental protection with the green material.At present, Lu and the member of seminar thereof use the shaddock skin to realize Hg as fluorescent probe as carbon source synthesizing blue fluorescent carbon point and with it
2+Sensitive Detection; Pyrolysis orange juice in alcohol solvent such as Sahu obtains the high strength fluorescent carbon point; It is 7.1% fluorescent carbon point that Zhou etc. have also obtained quantum yield by one step hydro thermal method by Watermelon rind.Yet the carbon that these green synthesis methods obtain is put auxiliary or organic solvents such as its lower fluorescence quantum yield and use inorganics; The unicity of its light and the susceptibility of pH etc. limited its widespread use in chemistry, environment, biology and life science, and the synthetic carbon point of these methods does not appear in the newspapers, and it possesses upper conversion function.
Up-conversion luminescence is based on two-photon or multiphoton process, luminescence center absorbs two or more photons in succession, reach luminous energy level through radiationless relaxation, produce short wavelength photons thereby transit to ground state, be about to the low frequency exciting light and convert high frequency emission light to.Near infrared light has also brought many advantages as its excitaton source, as darker light penetration depth, almost not damaged, biological tissue can luminous (no background fluorescences) etc. to biological tissue.Traditional up-conversion luminescent material mainly is based on rare earth ion doped gained micron or nanoparticle.But this up-conversion is based on rare earth metal, its building-up process complex operation, and the gained material granule was modified than big and synthetic the needs mostly afterwards, so had increased the Operating Complexity of using.Relative rare earth up-conversion, the carbon point with up-conversion fluorescence character is synthetic simple, and particle has only several nanometers, does not need the back to modify; The environmental protection of carbon point has littler toxicity simultaneously.Therefore, the up-conversion fluorescence of carbon point has wide application space.
The synthetic method of existing carbon point needs several steps operations such as pre-treatment mostly, use strong acid or surface passivation agent to assist synthesizes.Therefore, the apparatus expensive that its synthetic method is used, complicated operation, by-product contamination is serious; Synthetic carbon point stability of photoluminescence is poor, and optical property is subject to extraneous interference and luminous single.And be that the synthetic carbon point of carbon source hydro-thermal scarcely has last conversion character or its up-conversion fluorescence character is relatively poor with green cheap raw material at present, and yet there are no report based on the analytical applications of its up-conversion fluorescence.Therefore be necessary to seek a kind of simple, with the raw material of cheapness be carbon source synthesize have about the method for fluorescent carbon point of transition function.
Summary of the invention
At the deficiencies in the prior art, it is carbon source with the cheap raw material that the present invention aims to provide a kind of, is solvent with water, the green synthetic fluorescent carbon point of conversion character up and down that has.This method synthesis step is simple, does not need the pre-treatment operation, and it is synthetic not need to use strong acid or surface passivation agent to assist, and raw material is cheap and easy to get, and the synthesis condition gentleness is controlled, environmental protection, fluorescence quantum yield height, the anti-bleaching of light and good stability.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of have a up and down synthetic method of the fluorescent carbon point of transition function, and concrete steps are:
1) the capsicum sheet is added to the water, wherein the mass ratio of capsicum sheet and water is: capsicum sheet: water=1-8:1, evenly mix, and get mixture;
2) mixture is transferred in the water heating kettle, in 120 ℃-200 ℃ following hydro-thermal 2 h-10 h;
3) cooling is filtered, and obtains brown liquid, gets supernatant liquor after the centrifugal 10-20 of brown liquid minute, is the dialysis of 3500 dialysis tubings with the supernatant liquor interception, collects with the peritoneal effluent of dialysis after 10-30 hour, namely gets fluorescent carbon point.
The mass ratio of the described capsicum sheet of step 1) and water is preferably: the capsicum sheet: water=2-4:1.
Step 2) preferably at 170 ℃ of-190 ℃ of following hydro-thermal 4-6h.
Step 2) preferably at 180 ℃ of following hydro-thermal 5h.
Step 3) preferably is the dialysis of 3500 dialysis tubings with the supernatant liquor interception, collects with the peritoneal effluent of dialysis after 20 hours.
With respect to existing with the cheap raw material for for the method for carbon source hydrothermal synthesis of carbon point, present method does not adopt any additives and uses organic and inorganic reagent, only adopt capsicum and water as reactant, by optimizing the carbon point that recently obtains excellent properties of hydro-thermal time, hydrothermal temperature, raw material and water.It is the synthetic carbon point of carbon source mostly with the biomaterial that gained carbon puts that its fluorescence quantum yield and last conversion character be better than.
Use capsicum to have a fluorescent carbon point of conversion character up and down as carbon source is synthetic, down-conversion fluorescent wavelength-tunable it on can utilize it on down-conversion fluorescent character to the detection of hypochlorite realization dual signal.For example, use down-conversion fluorescent and detect hypochlorite in the tap water in the dual signal mode, increased reliability and the sensitivity of its detection.On it under down-conversion fluorescent spectrum and the ultraviolet lamp pictorial diagram see accompanying drawing 3-5.
Compared with prior art, advantage of the present invention is:
1, this method raw material is cheap and easy to get, preparation technology is simple, and the synthesis condition gentleness is controlled; Its building-up process is not used chemical additive and is produced pollutent, process environmental protection.
2, the prepared carbon point of this method does not need multistep purifying, separation, and carbon point fluorescence quantum yield height reaches 19.2%, is fit to large-scale industrial production.
3, prepared carbon point good water solubility and the good stability of this method, fast light whitening capacity is strong.At room temperature place some months or continuous light, it is luminous stable in high ion concentration and different pH environment, sees accompanying drawing 6-9.
4, the prepared carbon point of this method has very strong last down-conversion fluorescent, but dual signal detects the hypochlorite in the tap water, and its optic response character is seen accompanying drawing 10-11.
Description of drawings
Fig. 1 is the green synthetic fluorescent carbon point operational flowchart of conversion character up and down.
Fig. 2 is the transmission electron microscope photo of the stable fluorescent carbon point of the present invention's preparation.
Fig. 3 is that gained carbon of the present invention is put the down-conversion fluorescent spectrogram under the different excitation wavelengths.
Fig. 4 is that gained carbon of the present invention is put the up-conversion fluorescence spectrogram under the different excitation wavelengths.
Fig. 5 is the photo of stable fluorescent carbon nano-particles under ultra violet lamp of the present invention's preparation.
Gained carbon point change in fluorescence figure in Fig. 6 one month.
Fig. 7 gained carbon point change in fluorescence figure in different pH.
Fig. 8 gained carbon point change in fluorescence figure in different ionic strength solution.
Fig. 9 gained carbon point fluorescence time scan figure; This carbon point has very strong fast light bleaching.
Figure 10 for the fluorescent carbon point of the present invention preparation in phosphate buffer soln down-conversion fluorescent to the experimental result of clorox sensing; A is the fluorescence spectrum when not having hypochlorous acid to exist, the fluorescence spectrum when b exists for 0.4mmol hypochlorous acid.Show that hypochlorite is to this carbon point fluorescence response sensitivity.
Up-conversion fluorescence is to the experimental result of clorox sensing in phosphate buffer soln for the fluorescent carbon point that Figure 11 prepares for the present invention, and wherein a is the fluorescence spectrum when not having hypochlorous acid to exist, and b is the fluorescence spectrum under 0.4mmol hypochlorous acid exists.Up-conversion fluorescence has increased the reliability and the sensitivity that detect to the sensitivity response of hypochlorite.
Embodiment
The present invention is described further below in conjunction with embodiment.
Embodiment 1:
A kind of method for preparing the excellent properties fluorescent carbon point comprises following operating process, and synthetic route chart is seen Fig. 1:
Be carbon source with edible red pepper, water is solvent.The fresh chilli sheet that 4 g clean adds 1 g water, is transferred in the water heating kettle of 25 mL after evenly mixing, at 180 ℃ of following hydro-thermal 5 h.After being cooled to room temperature, discard big foreign material, obtain brown mixed solution, getting supernatant liquor behind centrifugal 15 min under 13 krpm.Be 3500 dialysis tubings dialysis 24 hours with the supernatant liquor interception, collect dialyzate.
The carbon point that makes is dispersed in the deionized water, obtain wavelength of transmitted light in the 400nm-600nm scope, quantum yield is 19.2% the upper and lower conversion character fluorescent carbon point that has.
Fig. 2 is the transmission electron microscope photo of the stable fluorescent carbon point of the present invention's preparation.Fig. 3 is that gained carbon of the present invention is put the down-conversion fluorescent spectrogram under the different excitation wavelengths.This carbon point down-conversion fluorescent maximum emission wavelength is at the 450nm place, its wavelength-tunable, and optical property is stable.Fig. 4 is that gained carbon of the present invention is put the up-conversion fluorescence spectrogram under the different excitation wavelengths; Its up-conversion fluorescence maximum emission peak is at the 470nm place, wavelength-tunable, and optical property is synchronized with down-conversion fluorescent.Fig. 5 is the photo (former figure be photochrome) of stable fluorescent carbon nano-particles under ultra violet lamp of the present invention's preparation.Gained carbon point change in fluorescence figure in Fig. 6 one month; This figure shows carbon point good water solubility, and gained carbon point fluorescence is not influenced by the medium material of air.Fig. 7 gained carbon point change in fluorescence figure in different pH; The fluorescence of this carbon point light intensity in different pH is stable, is suitable for the analytical applications of various soda acid systems.Fig. 8 gained carbon point change in fluorescence figure in different ionic strength solution; The anti-high ionic strength character of this fluorescence shows its potential application in bioanalysis.Fig. 9 gained carbon point fluorescence time scan figure, this carbon point has very strong fast light bleaching.
Figure 10 for the fluorescent carbon point of the present invention preparation in phosphate buffer soln down-conversion fluorescent to the experimental result of clorox sensing; A is the fluorescence spectrum when not having hypochlorous acid to exist, the fluorescence spectrum when b exists for 0.4mmol hypochlorous acid.Show that hypochlorite is to this carbon point fluorescence response sensitivity.Up-conversion fluorescence is to the experimental result of clorox sensing in phosphate buffer soln for the fluorescent carbon point that Figure 11 prepares for the present invention, and wherein a is the fluorescence spectrum when not having hypochlorous acid to exist, and b is the fluorescence spectrum under 0.4mmol hypochlorous acid exists.Up-conversion fluorescence has increased the reliability and the sensitivity that detect to the sensitivity response of hypochlorite.
Edible red pepper with maturation is carbon source, and water is solvent.Get the clean capsicum of 4g and shred back adding 1g water, be sealed in the water heating kettle in 180 ℃ of following hydro-thermal 2h.
Reaction finishes to take out still and is cooled to room temperature, filters out large particulate matter, gets its mixed solution centrifugal removing than the macroparticle material under 13krpm, and supernatant liquor is transferred in the beaker.Be 3500 dialysis tubings dialysis 24 hours with the supernatant liquor interception, collect dialyzate.Its fluorescence quantum yield is 14.8%.
Edible red pepper with maturation is carbon source, and water is solvent.Get the clean capsicum of 4g and shred back adding 1g water, be sealed in the water heating kettle in 140 ℃ of following hydro-thermal 5h.
Reaction finishes to take out still and is cooled to room temperature, filters out large particulate matter, gets its mixed solution centrifugal removing than the macroparticle material under 13krpm, and supernatant liquor is transferred in the beaker.Be 3500 dialysis tubings dialysis 24 hours with the supernatant liquor interception, collect dialyzate.Its fluorescence quantum yield is 15.6%.
Claims (5)
1. one kind has the synthetic method of the fluorescent carbon point of transition function up and down, it is characterized in that concrete steps are:
(1) the capsicum sheet is added to the water, wherein the mass ratio of capsicum sheet and water is: capsicum sheet: water=1-8:1, evenly mix, and get mixture;
(2) mixture is transferred in the water heating kettle, in 120 ℃-200 ℃ following hydro-thermal 2 h-10 h;
(3) cooling is filtered, and obtains brown liquid, gets supernatant liquor after the centrifugal 10-20 of brown liquid minute, is the dialysis of 3500 dialysis tubings with the supernatant liquor interception, collects the peritoneal effluent of dialysis after 10-30 hour, namely gets fluorescent carbon point.
2. have a up and down synthetic method of the fluorescent carbon point of transition function according to claim 1 is described, it is characterized in that the mass ratio of the described capsicum sheet of step 1) and water is: capsicum sheet: water=2-4:1.
3. describedly have a up and down synthetic method of the fluorescent carbon point of transition function according to claim 1 or 2, it is characterized in that step 2) be at 170 ℃ of-190 ℃ of following hydro-thermal 4-6 h.
4. have a up and down synthetic method of the fluorescent carbon point of transition function according to claim 3 is described, it is characterized in that step 2) be at 180 ℃ of following hydro-thermal 5h.
5. describedly have a up and down synthetic method of the fluorescent carbon point of transition function according to claim 1 or 2, it is characterized in that step 3) is the dialysis of 3500 dialysis tubings with the supernatant liquor interception, collect with the peritoneal effluent after dialysing 20 hours.
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| CN103833004A (en) * | 2014-02-28 | 2014-06-04 | 东北林业大学 | Method for preparing water-soluble fluorescent carbon nanoparticle dots |
| CN103911151A (en) * | 2014-04-14 | 2014-07-09 | 河南师范大学 | Sulfur phosphorus nitrogen co-doped carbon point with adjustable fluorescence property and preparation method of sulfur phosphorus nitrogen co-doped carbon point |
| CN104263366A (en) * | 2014-09-09 | 2015-01-07 | 中国科学院宁波材料技术与工程研究所 | Red-light emission fluorescent carbon dot with up and down conversion function and preparation method of red-light emission fluorescent carbon dot |
| CN104403664A (en) * | 2014-11-07 | 2015-03-11 | 山西大学 | Preparation method of green fluorescent carbon spot and application of green fluorescent carbon spot in cell imaging |
| CN104535549A (en) * | 2014-12-30 | 2015-04-22 | 广西师范大学 | Preparation and application of fluorescent carbon dot nanoprobe for detecting free chlorine in water |
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| CN105399078A (en) * | 2015-12-28 | 2016-03-16 | 江南大学 | Method for preparing fluorescent carbon dots on basis of shaddock |
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| CN110482527A (en) * | 2019-08-29 | 2019-11-22 | 临沂大学 | A kind of fast preparation method for converting double fluorescent carbon points up and down |
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| CN102703070A (en) * | 2012-06-01 | 2012-10-03 | 河南师范大学 | Preparation method of stable fluorescent carbon |
| CN102994080A (en) * | 2012-12-07 | 2013-03-27 | 上海大学 | Method for preparing fluoresent carbon nanoparticles |
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- 2013-05-22 CN CN201310191704.7A patent/CN103265952B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102703070A (en) * | 2012-06-01 | 2012-10-03 | 河南师范大学 | Preparation method of stable fluorescent carbon |
| CN102994080A (en) * | 2012-12-07 | 2013-03-27 | 上海大学 | Method for preparing fluoresent carbon nanoparticles |
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| CN103833004A (en) * | 2014-02-28 | 2014-06-04 | 东北林业大学 | Method for preparing water-soluble fluorescent carbon nanoparticle dots |
| CN103911151A (en) * | 2014-04-14 | 2014-07-09 | 河南师范大学 | Sulfur phosphorus nitrogen co-doped carbon point with adjustable fluorescence property and preparation method of sulfur phosphorus nitrogen co-doped carbon point |
| CN103911151B (en) * | 2014-04-14 | 2015-12-09 | 河南师范大学 | Nitrogen co-doped carbon point of the sulphur phosphorus that a kind of fluorescence property is adjustable and preparation method thereof |
| CN104263366A (en) * | 2014-09-09 | 2015-01-07 | 中国科学院宁波材料技术与工程研究所 | Red-light emission fluorescent carbon dot with up and down conversion function and preparation method of red-light emission fluorescent carbon dot |
| CN104403664A (en) * | 2014-11-07 | 2015-03-11 | 山西大学 | Preparation method of green fluorescent carbon spot and application of green fluorescent carbon spot in cell imaging |
| CN104535549B (en) * | 2014-12-30 | 2017-06-16 | 广西师范大学 | The preparation and its application of the fluorescent carbon point nano-probe of free chlorine in a kind of detection water |
| CN104535549A (en) * | 2014-12-30 | 2015-04-22 | 广西师范大学 | Preparation and application of fluorescent carbon dot nanoprobe for detecting free chlorine in water |
| CN104629760A (en) * | 2015-02-09 | 2015-05-20 | 浙江师范大学 | Preparation method of carbon quantum dots for detecting Hg<2+> and Fe<3+> in water |
| CN104789217A (en) * | 2015-04-28 | 2015-07-22 | 安徽大学 | Amphipathy carbon quantum dot and preparation method thereof |
| CN104927847A (en) * | 2015-05-25 | 2015-09-23 | 浙江师范大学 | Preparation method for carbon quantum dot material for detecting Cu<2+> |
| CN104987861A (en) * | 2015-06-23 | 2015-10-21 | 沈阳大学 | Method for preparing carbon dots with up-down conversion luminescence characteristic from maize straw |
| CN105419792A (en) * | 2015-12-28 | 2016-03-23 | 江南大学 | Preparation method of carbon dots soluble in water phase and organic phase |
| CN105399078A (en) * | 2015-12-28 | 2016-03-16 | 江南大学 | Method for preparing fluorescent carbon dots on basis of shaddock |
| CN105969348A (en) * | 2016-05-23 | 2016-09-28 | 中国科学院长春光学精密机械与物理研究所 | Carbon nano-point fluorescent powder, preparation method and LED lamp bead |
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| CN110482527A (en) * | 2019-08-29 | 2019-11-22 | 临沂大学 | A kind of fast preparation method for converting double fluorescent carbon points up and down |
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