CN108084997A - The preparation method of N doping fluorescent carbon quantum dots - Google Patents
The preparation method of N doping fluorescent carbon quantum dots Download PDFInfo
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- CN108084997A CN108084997A CN201711455410.5A CN201711455410A CN108084997A CN 108084997 A CN108084997 A CN 108084997A CN 201711455410 A CN201711455410 A CN 201711455410A CN 108084997 A CN108084997 A CN 108084997A
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Abstract
The invention discloses the preparation methods of N doping fluorescent carbon quantum dots, specifically include following steps：A, raw material is organized as with animal flesh, the animal flesh cut into slices is put into preheated oven, 10 min of baking, 30 min；B, after meat cooling, meat is removed and is impregnated with organic solvent, carbon quantum dot is extracted by magnetic agitation；C, filtered with cloth funnel, remove the visible foreign in solution；D, using Rotary Evaporators, organic solvent is removed, is redissolved with distilled water；E, extracted and centrifuged with organic solvent, further removed the lipid impurities in carbon quantum dot solution, take supernatant, obtain the carbon quantum dot aqueous solution of higher degree；F, above-mentioned carbon quantum dot aqueous solution bag filter is purified；H, bag filter external environment solution is taken, after vacuum freeze drying, obtains the carbon quantum dot powder of high-purity.Raw material of the present invention easily obtains, and recovery rate is high, and impurity is few, and synthesis technology is simple, and the carbon quantum dot grain size of acquisition is small and uniform, can be used in biological fluorescent labelling.
Description
Technical field
The invention belongs to technical field of nanometer material preparation more particularly to a kind of preparation sides of N doping fluorescents carbon quantum dot
Method.
Background technology
In the prior art, carbon quantum dot (CQDs, C-dots or CDs) is a kind of new carbon nanomaterial, and size exists
10 below nm have good water solubility, chemical inertness, hypotoxicity, are easy to functionalization and anti-light Bleachability, photostability etc.
Excellent properties, are a glittering stars in carbon nanometer family, and carbon quantum dot is that researcher in 2004 is net using electrophoresis
Change a kind of Novel Carbon Nanomaterials found for the first time during separating single-wall carbon nanotubes, Sun etc. was closed in 2006 by laser ablation
Into fluorescence carbon nanomaterial, and be named as carbon quantum dot, in the past few years, the synthesis of CQDs, property, using etc.
Aspect all achieves huge progress, and compared with traditional semiconductor-quantum-point and organic dyestuff, the CQDs that shines has high water-soluble
Property, extensive chemical stability, the functionalization that is easy to, anti-light Bleachability and excellent biological nature, good biocompatibility, in life
Object medicine (bio-imaging, bio-sensing, drug delivery etc.) has potential application prospect, meanwhile, CQDs has excellent photoelectricity
Property can not only be used as electron donor but also can be used as electron acceptor, this causes it to have in fields such as photoelectron, catalysis and sensings
It is widely applied value；At past several years, had been achieved with for the research of the synthesis of carbon quantum dot, property and application etc.
Certain progress, compared with the traditional semiconductor-quantum-point and organic dyestuff, fluorescent carbon quantum dot good water solubility, chemical stabilization
Property it is high, easy function dough, anti-light bleaching power is strong, and carbon quantum dot has excellent biological nature such as hypotoxicity, good biology
Compatibility, these properties make them have the potentiality applied to bio-imaging, bio-sensing etc..
At present, it is for from top to bottom and Self-absorption Correction Factor respectively there are mainly two types of the preparation methods of carbon quantum dot：From upper
The preparation method under and generally requires stringent reaction condition, to the more demanding of experiment material and instrument, causes the cost of material
It is high, it is impossible to which that large-scale production, application range is narrow, and the synthetic method from bottom to top predecessor being suitble to that then needs to be pyrolyzed or be carbonized is straight
Carbon quantum dot is bonded into, carbon quantum dot is prepared with biological raw material, there is raw material easily to obtain, nontoxic, reaction condition is simple, if
It is standby to require low, the advantages that quantum yield is high, it is the effective way of carbon quantum dot prepare with scale.
The content of the invention
The object of the present invention is to provide a kind of preparation methods of N doping fluorescents carbon quantum dot.
Present invention technical solution used for the above purpose is：A kind of preparation side of N doping fluorescents carbon quantum dot
Method specifically includes following steps：
A, raw material is organized as with animal flesh, the animal flesh cut into slices is put into preheated oven, be baked 10 min -30
min；
B, after meat cooling, meat is removed and is impregnated with organic solvent, and passes through magnetic agitation and extracts carbon quantum dot；
C, filtered with cloth funnel, remove the visible foreign in solution；
D, using Rotary Evaporators, organic solvent is removed, and is redissolved with distilled water；
E, extracted and centrifuged with organic solvent, further remove carbon quantum dot solution in lipid impurities, take supernatant, obtain compared with
The carbon quantum dot aqueous solution of high-purity；
F, above-mentioned carbon quantum dot aqueous solution bag filter is purified；
H, bag filter external environment solution is taken, after vacuum freeze drying, obtains the carbon quantum dot powder of high-purity.
Animal flesh used is organized as terrestrial mammal in the step A, including being not limited to mutton, beef, chicken, pig
Meat, the flesh of fish or duck.
Oven temperature is at 200 DEG C -350 DEG C in the step A.
Organic solvent is one or more of ethyl alcohol, methanol, ether or ethyl acetate in the step B.
The ratio of the organic solvent and meat is 1:50-1:20.
Rotary evaporation condition is that temperature is in the step D：50 DEG C -65 DEG C, rotating speed is 50 rpm -80 rpm.
Organic solvent is one or more of dichloromethane, chloroform or ethyl acetate in the step E.
The ratio of the carbon quantum dot solution and organic solvent is 1:1-1:10.
Centrifugal condition is 4000 rpm -10000 rpm, 10-30 min in the step E.
Bag filter molecular cut off is 1000 Da -3500 Da in the step F, and dialysis time is in 72 h -96 h.
Sublimation drying is in 96 h -120 h in the step H.
A kind of preparation method of N doping fluorescents carbon quantum dot of the present invention, raw material easily obtain, and recovery rate is high, and impurity is few, synthesis
Simple for process, low to the requirement of operating personnel's operational capacity, the carbon quantum dot grain size of acquisition is small and uniform, can be used in bioluminescence
Mark.
Description of the drawings
Fig. 1 is the transmission that a kind of preparation method embodiment one of N doping fluorescents carbon quantum dot of the present invention prepares carbon quantum dot
Electromicroscopic photograph.
Fig. 2 is the transmission that a kind of preparation method embodiment two of N doping fluorescents carbon quantum dot of the present invention prepares carbon quantum dot
Electromicroscopic photograph.
Fig. 3 is the transmission that a kind of preparation method embodiment three of N doping fluorescents carbon quantum dot of the present invention prepares carbon quantum dot
Electromicroscopic photograph.
Fig. 4 is the transmission that a kind of preparation method example IV of N doping fluorescents carbon quantum dot of the present invention prepares carbon quantum dot
Electromicroscopic photograph.
Fig. 5 is that a kind of preparation method example IV of N doping fluorescents carbon quantum dot of the present invention prepares carbon quantum dot for thin
The confocal microscope photo of born of the same parents' mark.
Specific embodiment
As shown in Figures 1 to 5, the preparation method of N doping fluorescents carbon quantum dot, specifically includes following steps：A, with animal
Meat tissue is raw material, the animal flesh cut into slices is put into preheated oven, is baked 10 min -30 min, animal used
Meat tissue is terrestrial mammal, and including being not limited to mutton, beef, chicken, pork, the flesh of fish, duck etc., oven temperature exists
200oC - 350oC；B, after meat cooling, meat is removed and is impregnated with organic solvent, and carbon quantum dot is extracted by magnetic agitation,
Organic solvent is one or more of ethyl alcohol, methanol, ether, ethyl acetate, and the ratio of organic solvent and meat is 1:50-1:
20；C, filtered with cloth funnel, remove the visible foreign in solution；D, using Rotary Evaporators, organic solvent is removed, and with steaming
Distilled water is redissolved, and rotary evaporation condition is that temperature is：50 oC - 65 oC, rotating speed is 50 rpm -80 rpm；E, organic solvent is used
It extracts and centrifuges, further remove the lipid impurities in carbon quantum dot solution, take supernatant, obtain the carbon quantum dot of higher degree
Aqueous solution, organic solvent is dichloromethane, chloroform, one or more of ethyl acetate, carbon quantum dot solution and organic solvent
Ratio be 1:1-1:10, centrifugal condition is 4000 rpm -10000 rpm, 10-30 min；F, by above-mentioned carbon quantum dot water
Solution bag filter purifies, and bag filter molecular cut off is 1000 Da -3500 Da, and dialysis time is in 72 h -96 h；H, take
Bag filter external environment solution after vacuum freeze drying, obtains the carbon quantum dot powder of high-purity, sublimation drying is in 96 h
- 120 h。
Embodiment one, prepares nano-particle：Raw material is mutton, and quality puts the mutton cut into slices without special requirement
Enter preheated 250 oCIn oven, 30 min are baked, after meat cooling, meat is removed and uses absolute ethyl alcohol（Meat：Absolute ethyl alcohol=1:
20）24 h are impregnated, and passing through magnetic agitation makes carbon quantum dot fully be extracted, and obtains the alcoholic solution with carbon dots, uses cloth
Formula funnel filters, and removes the visible foreign in solution, using Rotary Evaporators, removes ethyl alcohol, and is redissolved with distilled water, uses dichloro
Methane extracts（Above-mentioned solution：Dichloromethane=1:4）, and centrifuge, the lipid impurities in carbon quantum dot solution are further removed, are taken
Supernatant obtains the carbon quantum dot aqueous solution of higher degree.Above-mentioned carbon quantum dot solution is put into molecular cut off as 3500 Da
Bag filter in, at room temperature 2000 mL distill water environment under dialyse 3 days, take bag filter external environment solution, done through vacuum refrigeration
After dry, the carbon quantum dot powder of high-purity is obtained.
Embodiment two, prepares nano-particle：Raw material is mutton, and quality puts the mutton cut into slices without special requirement
Enter preheated 200 oCIn oven, 30 min are baked, after meat cooling, meat is removed and uses absolute ethyl alcohol（Meat：Absolute ethyl alcohol=1:
20）24 h are impregnated, and passing through magnetic agitation makes carbon quantum dot fully be extracted, and obtains the alcoholic solution with carbon dots, uses cloth
Formula funnel filters, and removes the visible foreign in solution, using Rotary Evaporators, removes ethyl alcohol, and is redissolved with distilled water, uses dichloro
Methane extracts（Above-mentioned solution：Dichloromethane=1:4）, and centrifuge, the lipid impurities in carbon quantum dot solution are further removed, are taken
Supernatant obtains the carbon quantum dot aqueous solution of higher degree, and above-mentioned carbon quantum dot solution is put into molecular cut off for 3500 Da
Bag filter in, at room temperature 2000 mL distill water environment under dialyse 3 days, take bag filter external environment solution, done through vacuum refrigeration
After dry, the carbon quantum dot powder of high-purity is obtained.
Embodiment three prepares nano-particle, and raw material is mutton, and quality puts the mutton cut into slices without special requirement
Enter preheated 300 oCIn oven, 30 min are baked, after meat cooling, meat is removed and uses absolute ethyl alcohol（Meat：Absolute ethyl alcohol=1:
20）24 h are impregnated, and passing through magnetic agitation makes carbon quantum dot fully be extracted, and obtains the alcoholic solution with carbon dots, uses cloth
Formula funnel filters, and removes the visible foreign in solution, using Rotary Evaporators, removes ethyl alcohol, and is redissolved with distilled water, uses dichloro
Methane extracts（Above-mentioned solution：Dichloromethane=1:4）, and centrifuge, the lipid impurities in carbon quantum dot solution are further removed, are taken
Supernatant obtains the carbon quantum dot aqueous solution of higher degree, and above-mentioned carbon quantum dot solution is put into molecular cut off for 3500 Da
Bag filter in, at room temperature 2000 mL distill water environment under dialyse 3 days, take bag filter external environment solution, done through vacuum refrigeration
After dry, the carbon quantum dot powder of high-purity is obtained.
Example IV prepares nano-particle：Raw material is mutton, and quality puts the mutton cut into slices without special requirement
Enter preheated 350 oCIn oven, 30 min are baked, after meat cooling, meat is removed and uses absolute ethyl alcohol（Meat：Absolute ethyl alcohol=1:
20）24 h are impregnated, and passing through magnetic agitation makes carbon quantum dot fully be extracted, and obtains the alcoholic solution with carbon dots, uses cloth
Formula funnel filters, and removes the visible foreign in solution, using Rotary Evaporators, removes ethyl alcohol, and is redissolved with distilled water, uses dichloro
Methane extracts（Above-mentioned solution：Dichloromethane=1:4）, and centrifuge, the lipid impurities in carbon quantum dot solution are further removed, are taken
Supernatant obtains the carbon quantum dot aqueous solution of higher degree, and above-mentioned carbon quantum dot solution is put into molecular cut off for 3500 Da
Bag filter in, at room temperature 2000 mL distill water environment under dialyse 3 days, take bag filter external environment solution, done through vacuum refrigeration
After dry, the carbon quantum dot powder of high-purity is obtained, it is burnt in copolymerization after 7 h of culture medium incubated cell containing carbon quantum dot
MIcrosope image display transmitting is predominantly located at that HepG2 is intracellular, further, since unique red-shifted emission phenomenon, thin positioned at HepG2
Carbon quantum dot in born of the same parents sends multicolor fluorescence when 405,458 and 488 nm are excited respectively.
Claims (11)
1. a kind of preparation method of N doping fluorescents carbon quantum dot, which is characterized in that specifically include following steps：
A, raw material is organized as with animal flesh, the animal flesh cut into slices is put into preheated oven, be baked 10 min -30
min；
B, after meat cooling, meat is removed and is impregnated with organic solvent, and passes through magnetic agitation and extracts carbon quantum dot；
C, filtered with cloth funnel, remove the visible foreign in solution；
D, using Rotary Evaporators, organic solvent is removed, and is redissolved with distilled water；
E, extracted and centrifuged with organic solvent, further remove carbon quantum dot solution in lipid impurities, take supernatant, obtain compared with
The carbon quantum dot aqueous solution of high-purity；
F, above-mentioned carbon quantum dot aqueous solution bag filter is purified；
H, bag filter external environment solution is taken, after vacuum freeze drying, obtains the carbon quantum dot powder of high-purity.
2. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step A
In animal flesh used be organized as terrestrial mammal, including being not limited to mutton, beef, chicken, pork, the flesh of fish or duck.
3. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step A
Middle oven temperature is at 200 DEG C -350 DEG C.
4. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step B
Middle organic solvent is one or more of ethyl alcohol, methanol, ether or ethyl acetate.
5. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 4, it is characterised in that：It is described organic
The ratio of solvent and meat is 1:50-1:20.
6. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step D
Middle rotary evaporation condition is that temperature is：50 DEG C -65 DEG C, rotating speed is 50 rpm -80 rpm.
7. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step E
Middle organic solvent is one or more of dichloromethane, chloroform or ethyl acetate.
8. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 7, it is characterised in that：The carbon amounts
The ratio of son point solution and organic solvent is 1:1-1:10.
9. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step E
Middle centrifugal condition is 4000 rpm -10000 rpm, 10-30 min.
10. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step
Bag filter molecular cut off is 1000 Da -3500 Da in F, and dialysis time is in 72 h -96 h.
11. a kind of preparation method of N doping fluorescents carbon quantum dot according to claim 1, it is characterised in that：The step
Sublimation drying is in 96 h -120 h in H.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108529594A (en) * | 2018-06-22 | 2018-09-14 | 大连工业大学 | The preparation method of fluorescent carbon nano-particles from roast chicken |
| CN108587617A (en) * | 2018-06-22 | 2018-09-28 | 大连工业大学 | The preparation method of carbon nano-particles in roasting Spanish mackerel |
| CN108929683A (en) * | 2018-07-28 | 2018-12-04 | 大连工业大学 | The preparation method of food-borne nanoparticle |
| CN108998009A (en) * | 2018-06-22 | 2018-12-14 | 大连工业大学 | The fluorescent carbon point preparation method of roast chicken and the method for utilizing the fluorescent carbon point probe in detecting seralbumin concentration from roast chicken |
| CN109852386A (en) * | 2019-01-08 | 2019-06-07 | 大连工业大学 | A method of extracting fluorescent carbon quantum dot from canned fish |
| CN110627036A (en) * | 2018-06-22 | 2019-12-31 | 北京中医药大学 | Preparation and application of dragon bone carbon quantum dots (nano particles/nano particles) |
| CN115368890A (en) * | 2022-03-30 | 2022-11-22 | 天津万象恒远科技有限公司 | Chicken skeleton carbon quantum dot and synthesis method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106978160A (en) * | 2017-02-27 | 2017-07-25 | 大连工业大学 | Nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof |
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2017
- 2017-12-28 CN CN201711455410.5A patent/CN108084997A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106978160A (en) * | 2017-02-27 | 2017-07-25 | 大连工业大学 | Nitrogen sulfur doping carbon namo fluorescence probe environment-friendly preparation method thereof |
Cited By (10)
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| CN108529594A (en) * | 2018-06-22 | 2018-09-14 | 大连工业大学 | The preparation method of fluorescent carbon nano-particles from roast chicken |
| CN108587617A (en) * | 2018-06-22 | 2018-09-28 | 大连工业大学 | The preparation method of carbon nano-particles in roasting Spanish mackerel |
| CN108998009A (en) * | 2018-06-22 | 2018-12-14 | 大连工业大学 | The fluorescent carbon point preparation method of roast chicken and the method for utilizing the fluorescent carbon point probe in detecting seralbumin concentration from roast chicken |
| CN110627036A (en) * | 2018-06-22 | 2019-12-31 | 北京中医药大学 | Preparation and application of dragon bone carbon quantum dots (nano particles/nano particles) |
| CN108998009B (en) * | 2018-06-22 | 2021-04-09 | 大连工业大学 | Preparation method of fluorescent carbon dots of roasted chicken and method for detecting serum albumin concentration by using fluorescent carbon dot probe from roasted chicken |
| CN110627036B (en) * | 2018-06-22 | 2021-12-17 | 北京中医药大学 | Preparation and application of dragon bone carbon quantum dots (nano particles/nano particles) |
| CN108929683A (en) * | 2018-07-28 | 2018-12-04 | 大连工业大学 | The preparation method of food-borne nanoparticle |
| CN109852386A (en) * | 2019-01-08 | 2019-06-07 | 大连工业大学 | A method of extracting fluorescent carbon quantum dot from canned fish |
| CN115368890A (en) * | 2022-03-30 | 2022-11-22 | 天津万象恒远科技有限公司 | Chicken skeleton carbon quantum dot and synthesis method and application thereof |
| CN115368890B (en) * | 2022-03-30 | 2023-06-16 | 天津万象恒远科技有限公司 | Chicken skeleton carbon quantum dot and synthesis method and application thereof |
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Application publication date: 20180529 |