CN107603608A - A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source - Google Patents
A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source Download PDFInfo
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Abstract
A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, belongs to fluorescent carbon point preparation field.By dried gynostemma pentaphylla powder, uniformly mix, be transferred in reactor with deionized water, water-soluble good fluorescent carbon point is made by hydro-thermal method；Dry gynostemma pentaphylla is either directly made to the fluorescent carbon point of good water solubility and launch wavelength length using calcination method.The method have the advantages that：Using natural biomass gynostemma pentaphylla as carbon source, wide material sources, cheap and easy to get, method is simple and easy, safe ready, green, toxic chemical need not be added, it can be achieved that simple extensive synthesizing water-solubility is good, fluorescent carbon point of good light stability, fluorescence intensity is high, launch wavelength is grown, and excitation wavelength is in 460 nm, most strong launch wavelength is in 530 nm or so, the effective influence for avoiding organism autofluorescence, it is contemplated that this carbon point shows wide application potential in cell imaging, biomarker, biology sensor and metal ion detection etc..
Description
Technical field
The invention belongs to fluorescent carbon point preparation field, and in particular to a kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source
Method.
Background technology
Carbon rich content in nature, existence form are polynary.In recent years, as the development of nanometer technology, carbon are received
Rice material family goes from strength to strength, mainly comprising fullerene, CNT, graphene etc..Fluorescent carbon point (Carbon dots,
CDs) it is fluorescent carbon nano-particles of the particle diameter less than 10 nm, as a kind of new fluorescence carbon nanomaterial, relative to a huge sum of money
Belong to quantum dot and traditional organic dyestuff, with toxicity is low, chemical stability is high, anti-light Bleachability strong, good biocompatibility, appearance
It is easily-synthesized, the advantages that excitation wavelength determines its emission wavelength characteristics, therefore has attracted researchers widely to pay close attention to.Carbon point is not only
The fields such as bio-imaging, drug transport, bio-sensing and fluorescence labeling are widely applied to, and in photocatalysis and photoelectric energy
Equipment aspect has potential application prospect.Isolated and purified accidentally from single-walled carbon nanotube using electrophoresis first from Xu in 2004 etc.
Since obtaining fluorescent carbon point, the correlative study of carbon point is also more and more, and at present, the primary synthetic methods of carbon point are different according to carbon source
Two classes can be divided into：One kind is method from top to bottom, refers to that the method that big carbon structure passes through physically or chemically forms nano-scale
Fluorescent carbon point, including arc discharge, laser ablation and electrochemical oxidation process；Another kind is method from bottom to top, is referred to small
Molecule is that presoma polymerize to form nano level carbon particle, including hydro-thermal method, microwave method, ultrasonic method and high temperature pyrolytic cracking (HTP).But
The carbon source of these method selections is usually artificial synthesized carbon compound, adds poisonous chemical reagent, and synthesis step is cumbersome,
Reaction condition is difficult to control.Therefore, Recent study person always search for carbon source that is green, inexpensive, being readily available
To prepare carbon point, someone utilizes natural biomass, such as orange juice, grape juice, bananas juice, grass, coffee etc. to be used as carbon at present
Successfully prepare fluorescent carbon point in source.But the launch wavelength of the fluorescent carbon point prepared by these raw materials is shorter, it is deep in vivo to influence it
The optical imaging effect of layer tissue, and low yield, it is not easy to realize large-scale production.Gynostemma pentaphylla is widespread in nature,
And each organ in body can be effectively protected, be able to can also not only be eliminated certainly with anti-aging, antifatigue, radioresistance
By base and improve nervous function, regulation human endocrine activity.At present, the launch wavelength of most of fluorescent carbon points is in
Ultraviolet light or short-wavelength visible light area, the penetrability of these light is poor, produces autofluorescence, interference images effect in vivo
Fruit.
The content of the invention
The invention aims to overcome complicated existing fluorescent carbon point synthesis, organism autofluorescence and raw material limitation to be present
The problem of property, there is provided a kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, this method pass through water using gynostemma pentaphylla as carbon source
Hot method or calcination method prepare the fluorescent carbon point of good water solubility, good light stability and launch wavelength length, realize simple extensive system
Standby, method is green, and cost is cheap.
To achieve the above object, the technical scheme that the present invention takes is as follows：
A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, methods described are hydro-thermal method, and specific preparation process is as follows：
Step 1：Dry gynostemma pentaphylla powder is uniformly mixed with deionized water, is transferred to the polytetrafluoro of high-pressure hydrothermal reaction kettle
In ethene liner, the reaction temperature of reactor is 160 ~ 200 DEG C, and the reaction time is 1 ~ 24 h, naturally cools to room temperature, its
In, the w/v of gynostemma pentaphylla and deionized water is 1g：5 ~ 20 mL；
Step 2：The reaction product that step 1 is obtained centrifuges 20 ~ 30 min, and centrifugation rate is 12000 r/min, through filter membrane
Filtering, then after being dialysed with bag filter, obtain fluorescent carbon point solution, the solution is freeze-dried under the conditions of -20 DEG C ~ -60 DEG C
48 ~ 72 h, that is, obtain fluorescent carbon point powder.
A kind of method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, methods described are calcination method, and specific preparation process is such as
Under：
Step 1：Dried gynostemma pentaphylla powder is passed through protection when 200 ~ 600 DEG C of h of temperature lower calcination 2 ~ 10, calcining
Gas；
Step 2：Deionized water is added into the gynostemma pentaphylla after calcining, forms suspension, persistently stirs 40 ~ 96 h or 700W
Micro-wave oven in microwave heat 3 ~ 30 min, wherein, the mass volume ratio of gynostemma pentaphylla and deionized water is 1g：40~200mL；
Step 3：Suspension is centrifuged into 20 ~ 30 min, centrifugation rate is 12000 r/min, through membrane filtration, obtains fluorescence
Carbon dots solution, the solution is freeze-dried 48 ~ 72 h under the conditions of -20 DEG C ~ -60 DEG C, obtains fluorescent carbon point powder.
It is of the invention to be relative to the beneficial effect of prior art：It is wide as carbon source, source using natural biomass gynostemma pentaphylla
It is general, cheap and easy to get, method is simple and easy, safe ready, green, without adding toxic chemical, it is possible to achieve simple
Extensive synthesizing water-solubility is good, good light stability fluorescent carbon point, and fluorescence intensity is high, launch wavelength length, and excitation wavelength exists
During 460 nm, most strong launch wavelength effectively avoids the influence of organism autofluorescence, it is contemplated that this carbon point exists in 530 nm or so
Cell imaging, biomarker, biology sensor and metal ion detection etc. show wide application potential.
Brief description of the drawings
Fig. 1 is fluorescence spectra of the fluorescent carbon point of the preparation of embodiment 1 under different excitation wavelengths；
Fig. 2 is the HRTEM figures of fluorescent carbon point prepared by embodiment 2；
Fig. 3 is fluorescence spectra of the fluorescent carbon point of the preparation of embodiment 2 under different excitation wavelengths；
Fig. 4 is fluorescent carbon point material object digital photograph prepared by embodiment 2；
Fig. 5 is the uv absorption spectra of fluorescent carbon point prepared by embodiment 3.
Embodiment
Technical scheme is further described with reference to the accompanying drawings and examples, but is not limited thereto,
It is every technical solution of the present invention to be modified or equivalent substitution, all should without departing from the scope of technical solution of the present invention
Cover among protection scope of the present invention.
Embodiment one：What present embodiment was recorded is a kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source
Method, methods described are hydro-thermal method, and specific preparation process is as follows：
Step 1：Dry gynostemma pentaphylla powder is uniformly mixed with deionized water, is transferred to the polytetrafluoro of high-pressure hydrothermal reaction kettle
In ethene liner, the reaction temperature of reactor is 160 ~ 200 DEG C, and the reaction time is 1 ~ 24 h, naturally cools to room temperature, its
In, the w/v of gynostemma pentaphylla and deionized water is 1g：5 ~ 20 mL；
Step 2：The reaction product that step 1 is obtained centrifuges 20 ~ 30 min, and centrifugation rate is 12000 r/min, through filter membrane
Filtering, then after being dialysed with bag filter, obtain fluorescent carbon point solution, the solution is freeze-dried under the conditions of -20 DEG C ~ -60 DEG C
48 ~ 72 h, that is, obtain fluorescent carbon point powder.
Embodiment two：A kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source described in embodiment one
Method, in step 2, the aperture of the filter membrane is 0.22 μm.
Embodiment three：A kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source described in embodiment one
Method, in step 2, the molecular cut off of the bag filter is 1000 ~ 3500Da, and dialysis time is 48 ~ 72 h.
Embodiment four：What present embodiment was recorded is a kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source
Method, methods described are calcination method, and specific preparation process is as follows：
Step 1：Dried gynostemma pentaphylla powder is passed through protection when 200 ~ 600 DEG C of h of temperature lower calcination 2 ~ 10, calcining
Gas；
Step 2：Deionized water is added into the gynostemma pentaphylla after calcining, forms suspension, persistently stirs 40 ~ 96 h or 700W
Micro-wave oven in microwave heat 3 ~ 30 min, wherein, the mass volume ratio of gynostemma pentaphylla and deionized water is 1g：40~200mL；
Step 3：Suspension is centrifuged into 20 ~ 30 min, centrifugation rate is 12000 r/min, through membrane filtration, obtains fluorescence
Carbon dots solution, the solution is freeze-dried 48 ~ 72 h under the conditions of -20 DEG C ~ -60 DEG C, obtains fluorescent carbon point powder.
Embodiment five：A kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source described in embodiment four
Method, in step 1, the protection gas is N2、H2、NH3Or one kind in Ar.
Embodiment six：A kind of side that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source described in embodiment four
Method, in step 3, the aperture of the filter membrane is 0.22 μm.
Embodiment 1：
Take the dried g of gynostemma pentaphylla 4 and 20 mL deionized waters uniformly to mix respectively, be transferred to poly- the four of high-pressure hydrothermal reaction kettle
In PVF liner, 3 h are reacted at 200 DEG C, after naturally cool to room temperature.Reacted brown color liquid is placed in centrifuge
20 min are centrifuged in 12000 r/min centrifugation rate, then the filtering with microporous membrane that via hole diameter is 0.22 μm, gained filtrate are used
Bag filter 72 h of dialysis that molecular cut off is 1000 Da, obtain carbon dots solution, are saved in 4 DEG C of refrigerators.- 20 DEG C ~-
48 h are freeze-dried under the conditions of 60 DEG C, that is, obtain fluorescent carbon point powder.
Fluorescence property test is carried out to the water-soluble fluorescent carbon point prepared in the present embodiment with sepectrophotofluorometer, obtained
Fig. 1, as can be seen from Figure 1 as excitation wavelength increases, Red Shift Phenomena occurs for the absorption maximum summit of emission spectrum, and embodiment is set out
Penetrating spectrum has excitation wavelength dependency characteristic.When excitation wavelength is 340 nm, maximum emission wavelength is 425 nm.
Embodiment 2：
Dried gynostemma pentaphylla is taken to calcine 10 h at 200 DEG C, in N2Under protection, black solid is obtained, treats natural cooling.Take
Black solid after 600 mg calcinings, adds 20 mL deionized waters, forms suspension, persistently stirs 48h, suspension is placed in
Centrifuge centrifuges 20 min in 12000 r/min centrifugation rate, then the filtering with microporous membrane that via hole diameter is 0.22 μm, obtains
Carbon dots solution, it is saved in 4 DEG C of refrigerators.48 h are freeze-dried under the conditions of -20 DEG C ~ -60 DEG C, that is, obtain fluorescent carbon point powder
End.
Electron-microscope scanning is carried out to the water-soluble fluorescent carbon point prepared in the present embodiment with transmission electron microscope, obtains Fig. 2,
Figure it is seen that the carbon point of this method synthesis is the homogeneous spheroidal particle for having good dispersion.Use sepectrophotofluorometer
Fluorescence property test is carried out to the water-soluble fluorescent carbon point prepared in the present embodiment, Fig. 3 is obtained, as can be seen from Figure 3 with sharp
Wavelength increase is sent out, Red Shift Phenomena occurs for the absorption maximum summit of emission spectrum, and embodying emission spectrum has excitation wavelength dependence
Characteristic.When excitation wavelength is 460 nm, maximum emission wavelength is 530 nm.Fig. 4 be prepared in the present embodiment it is water-soluble glimmering
The digital photograph of light carbon point product.
Embodiment 3：
Dried gynostemma pentaphylla is taken to calcine 10 h at 200 DEG C, in N2Under protection, black solid is obtained, treats natural cooling.Take
Black solid after 100 mg calcinings, adds 10 mL deionized waters, and after being well mixed, it is micro- to be positioned over the family expenses that power is 700W
6 min are heated in ripple stove, obtained burned black shape solid is dissolved in 10 mL deionized waters, are being placed in centrifuge in 12000 r/
Min centrifugation rate centrifuges 30 min, then the filtering with microporous membrane that via hole diameter is 0.22 μm, obtains carbon dots solution, is saved in 4
In DEG C refrigerator.48 h are freeze-dried under the conditions of -20 DEG C ~ -60 DEG C, that is, obtain fluorescent carbon point powder.
Ultra-violet absorption spectrum survey is carried out to the water-soluble fluorescent carbon point of the preparation in the present embodiment with ultraviolet specrophotometer
Examination, obtained ultra-violet absorption spectrum is as shown in figure 5, it can be seen that the fluorescent carbon point solution of this method synthesis is 250
There is a weak absorbing peak at nm, this is as caused by π-π * transition of phenyl ring sp2 hydridization.
Claims (6)
- A kind of 1. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, it is characterised in that：Methods described is hydro-thermal method, specific system Standby step is as follows：Step 1：Dry gynostemma pentaphylla powder is uniformly mixed with deionized water, is transferred to the polytetrafluoro of high-pressure hydrothermal reaction kettle In ethene liner, the reaction temperature of reactor is 160 ~ 200 DEG C, and the reaction time is 1 ~ 24 h, naturally cools to room temperature, its In, the w/v of gynostemma pentaphylla and deionized water is 1g：5 ~ 20 mL；Step 2：The reaction product that step 1 is obtained centrifuges 20 ~ 30 min, and centrifugation rate is 12000 r/min, through filter membrane Filtering, then after being dialysed with bag filter, obtain fluorescent carbon point solution, the solution is freeze-dried under the conditions of -20 DEG C ~ -60 DEG C 48 ~ 72 h, that is, obtain fluorescent carbon point powder.
- A kind of 2. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source according to claim 1, it is characterised in that：Step In two, the aperture of the filter membrane is 0.22 μm.
- A kind of 3. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source according to claim 1, it is characterised in that：Step In two, the molecular cut off of the bag filter is 1000 ~ 3500Da, and dialysis time is 48 ~ 72 h.
- A kind of 4. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source, it is characterised in that：Methods described is calcination method, specific system Standby step is as follows：Step 1：Dried gynostemma pentaphylla powder is passed through protection when 200 ~ 600 DEG C of h of temperature lower calcination 2 ~ 10, calcining Gas；Step 2：Deionized water is added into the gynostemma pentaphylla after calcining, forms suspension, persistently stirs 40 ~ 96 h or 700W Micro-wave oven in microwave heat 3 ~ 30 min, wherein, the mass volume ratio of gynostemma pentaphylla and deionized water is 1g：40~200mL；Step 3：Suspension is centrifuged into 20 ~ 30 min, centrifugation rate is 12000 r/min, through membrane filtration, obtains fluorescence Carbon dots solution, the solution is freeze-dried 48 ~ 72 h under the conditions of -20 DEG C ~ -60 DEG C, obtains fluorescent carbon point powder.
- A kind of 5. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source according to claim 4, it is characterised in that：Step In one, the protection gas is N2、H2、NH3Or one kind in Ar.
- A kind of 6. method that fluorescent carbon point is prepared using gynostemma pentaphylla as carbon source according to claim 4, it is characterised in that：Step In three, the aperture of the filter membrane is 0.22 μm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747397A (en) * | 2020-06-30 | 2020-10-09 | 山西大学 | Preparation method and application of grape carbon quantum dots |
| CN113148981A (en) * | 2021-05-28 | 2021-07-23 | 沈阳大学 | Novel green environment-friendly dragon fruit carbon dots prepared by hydrothermal method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
| CN104927845A (en) * | 2015-06-09 | 2015-09-23 | 山西大学 | Color-tunable fluorescence carbon dot, and preparation method and application thereof |
| CN106190118A (en) * | 2016-07-20 | 2016-12-07 | 四川文理学院 | Radix Scrophulariae method preparing fluorescent carbon quantum dot and products thereof and application |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102745669A (en) * | 2012-07-18 | 2012-10-24 | 中国人民解放军军事医学科学院卫生装备研究所 | Method for preparing photoluminescence carbon quantum dot |
| CN104927845A (en) * | 2015-06-09 | 2015-09-23 | 山西大学 | Color-tunable fluorescence carbon dot, and preparation method and application thereof |
| CN106190118A (en) * | 2016-07-20 | 2016-12-07 | 四川文理学院 | Radix Scrophulariae method preparing fluorescent carbon quantum dot and products thereof and application |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111747397A (en) * | 2020-06-30 | 2020-10-09 | 山西大学 | Preparation method and application of grape carbon quantum dots |
| CN113148981A (en) * | 2021-05-28 | 2021-07-23 | 沈阳大学 | Novel green environment-friendly dragon fruit carbon dots prepared by hydrothermal method |
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