CN105295910A - Method for preparing red light carbon dots by taking biomass as precursor - Google Patents
Method for preparing red light carbon dots by taking biomass as precursor Download PDFInfo
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Abstract
A method for preparing red light carbon dots by taking biomass as a precursor comprises the following steps: selecting a biomass material; shearing the biomass material into dices; putting the dices into a mortar; adding a mixed liquid of ethanol and water; grinding; taking out juice; carrying out centrifugation to remove precipitation and chips; adding the obtained solution I into a high-pressure reaction kettle; heating for reaction; putting a solution II obtained after the reaction into a dialysis bag for dialysis; dialyzing micromolecular carbon dots and the unreacted biomass mixed solution III; obtaining the required red light carbon dot solution. The method has the advantages that the toxicity is low; the biocompatibility is high; the cost is low; the preparation technology is simple; the environment is protected.
Description
Technical field
The present invention relates to a kind of take biomass as the method for precursor power ruddiness carbon point.
Background technology
Near-infrared fluorescent bio-imaging technology has the advantages such as dark penetration into tissue, the interference of low background fluorescence, the damage of minimum bio sample light and causes people to pay close attention to widely because of it.The more fluorescent material of current report is fluorescence dye, semiconductor-quantum-point and polymer quantum dot.But it all exists, and toxicity is large, poor biocompatibility, cost are high, the problem of complicated process of preparation and contaminate environment.And fluorescent carbon point is compared with traditional near-infrared light-emitting material, there is hypotoxicity, good biocompatibility and carbon source and enrich, make it become a dazzling star at biomedical sector.
At present, the method preparing fluorescent carbon point reported is a lot, is mainly divided into method and from bottom to top method from top to bottom.Method is large carbon skeleton structure deteriorate will be become little carbon skeleton structure in brief from top to bottom; And method is that organism is formed carbon point particle by dehydration carbonization from bottom to top.But, the fluorescence multidigit that the carbon point that these methods obtain at present is launched is in blue light or green wavelength (LeiY, WeihuaJ, LipengQ, etal.Onepotsynthesisofhighlyluminescentpolyethyleneglyco lanchoredcarbondotsfunctionalizedwithanuclearlocalizatio nsignalpeptideforcellnucleusimaging [J] .Nanoscale, 2015,7 (14): 6104-6113.); Preparation process is comparatively complicated and use poisonous chemical reagent for presoma or be etching agent (JiangKai, SunShan, ZhangLing, etal.Red, green, andblueluminescencebycarbondots:full-coloremissiontuning andmulticolorcellularimaging. [J] .AngewandteChemie, 2015,54 (18): 5360-5363. this section of documents take phenylenediamine as precursor power carbon point.Xiaoyun, Tan, Yunchao, Li, Xiaohong, Li, etal.Electrochemicalsynthesisofsmall-sizedredfluorescent graphenequantumdotsasabioimagingplatform. [J] .ChemicalCommunications, 2015,51 (13): 2544-2546. this section of documents adopt electrochemical method, uses K
2s
2o
8etching graphite prepares carbon point); And it is little about the report of ruddiness carbon point.Therefore, seek that toxicity is low, good biocompatibility, cost are low, preparation is simple and the novel method of environmental protection is prepared ruddiness carbon point and will be advanced the practical application of carbon point in bio-imaging.
Summary of the invention
The object of the invention is to solve prior art problem, provide that a kind of toxicity is low, good biocompatibility, cost are low, preparation technology is simple and environmental protection take biomass as the method for precursor power ruddiness carbon point.
For solving the problems of the technologies described above, technical scheme of the present invention is, the biological material selecting environmental protection is presoma, add the mixed solvent of second alcohol and water, milled processed in mortar, after the clear liquid of taking-up is centrifugal, puts into hydrothermal reaction kettle reacting by heating, terminate to be placed in dialysis tubing to dialyse, obtain ruddiness carbon point.
The present invention take biomass as the method for precursor power ruddiness carbon point, comprises the steps:
(1) choose biological material, cut into fritter, be placed in mortar, add the mixed solution of second alcohol and water, milled processed;
(2) juice is taken out, centrifugal removing precipitation and fragment;
(3) gained solution in step (2) is added in autoclave, reacting by heating;
(4) reacted solution is placed in dialysis tubing and dialyses, and gives micromolecular carbon point and unreacted biomass mixing solutions; Namely required ruddiness carbon point solution is obtained;
As ruddiness carbon point pressed powder need be obtained, freeze drying box lyophilize will be placed in, can obtain.
As step (1) biological material mainly selects green plants, as vegetables, leaf and green herbaceous plant.
Volume ratio as ethanol in step (1) and deionized water is (1-20): 1; Biological material: mixing solutions=8-12g:10-50ml; Milling time is t (5min≤m≤10min).
If the rotating speed of whizzer in step (2) is at 5000-12000r/min, centrifugal 5-15min;
If the selection range of temperature of reaction in step (3) is at 140-180 DEG C, the scope 4-8h in reaction times.When exceeding this scope, the carbonizing degree of carbon point and productive rate cannot be balanced.
If the selection range of dialysis tubing molecular weight cut-off in step (4) is at 3000-8000MW, dialysis 2-4 days.
Product after hydro-thermal, is placed in dialysis tubing, and the scope of molecular weight cut-off is 3000-8000MW, within the scope of this, be conducive to unreacted biomass solution to give, it is excessive that molecular weight cut-off crosses the carbon point particle diameter that conference makes to retain, scattering phenomenon is serious, is unfavorable for stable luminescence.
Freeze drier lyophilize need be adopted to obtain when obtaining pressed powder in step (6), avoid the destruction of causing luminescence center.
The even particle size distribution of the fluorescent carbon point that the present invention obtains, rich surface contains oxygen-containing functional group, multi-wavelength excitation, and maximum excitation wavelength lays respectively at 409nm, 511nm, 543nm, 616nm, optimum transmit wavelength is positioned at 685nm and 725nm, and entirety presents emission wavelength and do not rely on excitation wavelength.
Beneficial outcomes of the present invention is: 1. biomass presoma wide material sources; 2. the fluorescent carbon point prepared by present multiband excitation wavelength, and still have stronger excitation wavelength at 616nm, existing report is almost not in sight, and emission wavelength does not rely on excitation wavelength and offsets; 3. the optimum transmit wavelength of the fluorescent carbon point prepared by is 680nm, more moves near infrared region, still have obvious transmitting near 720-750nm than the emission wavelength of the ruddiness carbon point of existing report; 4. prepare ruddiness carbon point nontoxic, cost is low, the cycle is short, preparation technology is simple, environmental protection; 5. are the feasible novel methods preparing ruddiness carbon point of a kind of green, contribute to accelerating its paces in the application of near-infrared fluorescent bio-imaging.
Biomass are presoma is the novel method preparing ruddiness carbon point, and carbon source is mainly derived from the Nature, environmental protection.The solvent added in preparation process, is beneficial to biomass and becomes outside carbon, play modification on its surface, and biomass itself are rich carbon and rich nitrogen class material, has advantageous advantage preparing in ruddiness carbon point, does not need to carry out follow-up moditied processing to carbon point.
Accompanying drawing explanation
Fig. 1 take spinach as the fluorescence spectrum figure of biomass precursor power ruddiness carbon point;
Fig. 2 take spinach as the purple light spectrogram of biomass precursor power ruddiness carbon point;
Fig. 3 take spinach as the transmission electron microscope picture of biomass precursor power ruddiness carbon point;
Fig. 4 take trifolium as the fluorescence spectrum figure of biomass precursor power ruddiness carbon point;
Fig. 5 take Chinese parasol leaf as the fluorescence spectrum figure of biomass precursor power ruddiness carbon point.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.Every equivalence done according to the technology of the present invention content changes and retouching, all should be included within technology category of the present invention.
Embodiment 1:
One, the preparation of biomass presoma: select spinach to be biomass carbon source, get 10g the leaf of spinach and cut into fragment, be placed in the mixed solvent (volume ratio is 5:1) of 10ml second alcohol and water, grinding 5min, take out mixed solution in centrifuges with the 10min that works under 8000r/min rotating speed, get upper solution;
Two, hydrothermal carbonization: upper solution is placed in autoclave, at 150 DEG C of heating 8h, obtains carbon and orders mixed solution.
Three, dialyse: get the carbon reacting end in two steps and order mixed solution, be placed in dialysis tubing, dialysis tubing selects 3000MW, dialyses 3 days, obtains ruddiness carbon point solution;
Four, dry: in freeze drier, at-30 DEG C of pre-freeze 4h, follow procedure lyophilize 24h, obtains ruddiness carbon point pressed powder.
Adopt HoribaFluoromax-4 fluorescence spectrophotometer to carry out Fluorescent Characterization to prepared ruddiness carbon point, see Fig. 1.Fig. 1 presents multiband excitation wavelength, and emission wavelength does not rely on excitation wavelength.Maximum excitation wavelength is positioned at 409nm, 511nm, 543nm, 616nm, and optimum transmit wavelength is positioned at 685nm place, and has acromion to occur at 700-750nm.This phenomenon is not seen in existing report.And the present invention is positioned at 605nm than the optimum transmit of the report such as XiaoyunTanet. of existing report moves 80nm to long wave direction.
Uv-visible absorption spectroscopy utilizes SHIMADZUUV-3600 ultraviolet-visible spectrophotometer to test, and as shown in Figure 2, carbon point prepared by spinach all shows obvious absorption in 200-800nm region, and the absorption particularly in visible region also clearly; The carbon point that this feature is different from general preparation only has absorption at ultraviolet region.
Transmission electron microscope picture is as Fig. 3, and size is mainly distributed in 10-12nm.
Embodiment 2
One, the preparation of biomass presoma: select trifolium to be biomass carbon source, get 12g and cut into fragment, be placed in the mixed solvent (volume ratio is 10:1) of 50ml second alcohol and water, milled processed 10min, take out mixed solution in centrifuges with the 5min that works under 12000r/min rotating speed, get upper solution;
Two, hydrothermal carbonization: be placed in autoclave, at 160 DEG C of heating 8h.
Three, dialyse: get in two the carbon reacting end and order mixed solution, be placed in dialysis tubing, dialysis tubing selects 5000MW, dialyses 2 days, obtains ruddiness carbon point solution;
Four, dry: in freeze drier, at-30 DEG C of pre-freeze 4h, follow procedure lyophilize 24h, obtains ruddiness carbon point pressed powder.
Adopt HoribaFluoromax-4 fluorescence spectrophotometer to carry out Fluorescent Characterization to prepared ruddiness carbon point, see Fig. 4.There are two maximum excitation wavelengths, lay respectively at 425nm and 523nm, launch in multiband, and reach maximum in the intensity of the emission peak at 656nm place, be positioned at than the emission peak of the ruddiness carbon point of existing report and move 50nm to long wave direction.
Embodiment 3
One, the preparation of biomass presoma: select Chinese parasol leaf to be biomass carbon source, get 10g and cut into fragment, be placed in the mixed solvent (volume ratio is 20:1) of 20ml second alcohol and water, grinding 5min, take out mixed solution in centrifuges with the 15min that works under 5000r/min rotating speed, get upper solution;
Two, hydrothermal carbonization: be placed in autoclave, at 180 DEG C of heating 4h.
Three, dialyse: preparation process is identical with embodiment two;
Four, dry: method is identical with embodiment two.
When identical with the fluorometric investigation condition of embodiment 1,2, obtain fluorescence spectrum Fig. 5.Best excitation peak be positioned at 398nm and 502nm place, the optimum transmit wavelength of correspondence is positioned at 666nm place, and the fluorescence intensity in embodiment 3 is apparently higher than embodiment 2.May due to the otherness of O contained in Chinese parasol leaf and trifolium, N element amount, and in hydrothermal carbonization process, the surface imperfection of carbon point causes intensity that significantly change occurs.
Claims (9)
1. be a method for precursor power ruddiness carbon point with biomass, it is characterized in that comprising the steps:
(1) choose biological material, cut into fritter, be placed in mortar, add the mixed solution of second alcohol and water, milled processed;
(2) juice is taken out, centrifugal removing precipitation and fragment;
(3) gained solution in step (2) is added in autoclave, reacting by heating;
(4) reacted solution is placed in dialysis tubing and dialyses, and gives micromolecular carbon point and unreacted biomass mixing solutions; Namely required ruddiness carbon point solution is obtained.
2. a kind of as claimed in claim 1 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that ruddiness carbon point solution is placed in freeze drying box lyophilize, obtains ruddiness carbon point pressed powder.
3. a kind of as claimed in claim 1 or 2 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that step (1) biological material selects green plants.
4. a kind of as claimed in claim 3 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that green plants is vegetables, leaf or green herbaceous plant.
5. a kind of as claimed in claim 1 or 2 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that the volume ratio of ethanol and deionized water in step (1) is 1-20:1; Biological material: mixing solutions=8-12g:10-50ml; Milling time is for being more than or equal to 5min to being less than or equal to 10min.
6. a kind of as claimed in claim 1 or 2 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that the rotating speed of whizzer in step (2) is at 5000-12000r/min, centrifugal 5-15min.
7. a kind of as claimed in claim 1 or 2 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that in step (3), temperature of reaction is at 140-180 DEG C, reaction times 4-8h.
8. a kind of as claimed in claim 1 or 2 take biomass as the method for precursor power ruddiness carbon point, it is characterized in that in step (4), dialysis tubing molecular weight cut-off is at 3000-8000MW, dialysis 2-4 days.
9. a kind of as described in claim 18 one take biomass as the method for precursor power ruddiness carbon point, it is characterized in that the even particle size distribution preparing ruddiness carbon point, rich surface is containing oxygen-containing functional group, excitation wavelength lays respectively at 409nm, 511nm, 543nm, 616nm, and emission wavelength is positioned at 685nm and 725nm.
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| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106587008A (en) * | 2016-12-14 | 2017-04-26 | 江南大学 | Method for preparing nitrogen-sulfur-doped carbon dots from castanea mollissima peel |
| CN106892421A (en) * | 2017-03-01 | 2017-06-27 | 南京工业大学 | Preparation method of all-green red carbon quantum dots |
| CN108101023A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that multi-element doping carbon material is prepared using leek |
| CN108872171A (en) * | 2018-06-19 | 2018-11-23 | 江苏大学 | A kind of application of fluorescent carbon point and preparation method thereof and detection tetracycline |
| CN110054171A (en) * | 2019-04-25 | 2019-07-26 | 贺州学院 | A kind of preparation method of biomass near-infrared fluorescent carbon dots |
| CN110396406A (en) * | 2019-06-11 | 2019-11-01 | 华南农业大学 | A kind of chlorophyll carbon dots and preparation method thereof and the application in time detection label |
| CN110669515A (en) * | 2019-10-24 | 2020-01-10 | 吉林大学 | Two-photon near-infrared carbon dot with high brightness and ultra-narrow half-peak width and preparation method thereof |
| CN111977632A (en) * | 2019-05-22 | 2020-11-24 | 东北林业大学 | Green preparation method of spinach-based multicolor luminescent carbon quantum dots |
| CN112960665A (en) * | 2021-04-09 | 2021-06-15 | 山东农业大学 | Preparation method of red and blue light double-emission carbon dots and application of red and blue light double-emission carbon dots in plants |
| CN113265248A (en) * | 2021-06-11 | 2021-08-17 | 江南大学 | Orange red fluorescent carbon dot and preparation method thereof |
| CN114854402A (en) * | 2022-03-22 | 2022-08-05 | 桂林师范高等专科学校 | Preparation method of fluorescent nano material capable of promoting growth of cherokee rose group culture seedling |
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Cited By (14)
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| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106587008A (en) * | 2016-12-14 | 2017-04-26 | 江南大学 | Method for preparing nitrogen-sulfur-doped carbon dots from castanea mollissima peel |
| CN106892421A (en) * | 2017-03-01 | 2017-06-27 | 南京工业大学 | Preparation method of all-green red carbon quantum dots |
| CN108101023A (en) * | 2017-12-27 | 2018-06-01 | 重庆文理学院 | A kind of method that multi-element doping carbon material is prepared using leek |
| CN108872171A (en) * | 2018-06-19 | 2018-11-23 | 江苏大学 | A kind of application of fluorescent carbon point and preparation method thereof and detection tetracycline |
| CN110054171A (en) * | 2019-04-25 | 2019-07-26 | 贺州学院 | A kind of preparation method of biomass near-infrared fluorescent carbon dots |
| CN111977632A (en) * | 2019-05-22 | 2020-11-24 | 东北林业大学 | Green preparation method of spinach-based multicolor luminescent carbon quantum dots |
| CN110396406A (en) * | 2019-06-11 | 2019-11-01 | 华南农业大学 | A kind of chlorophyll carbon dots and preparation method thereof and the application in time detection label |
| CN110396406B (en) * | 2019-06-11 | 2021-10-19 | 华南农业大学 | Chlorophyll carbon dot, preparation method thereof and application thereof in time detection label |
| CN110669515A (en) * | 2019-10-24 | 2020-01-10 | 吉林大学 | Two-photon near-infrared carbon dot with high brightness and ultra-narrow half-peak width and preparation method thereof |
| CN110669515B (en) * | 2019-10-24 | 2021-07-27 | 吉林大学 | Two-photon near-infrared carbon dot with high brightness and ultra-narrow half-peak width and preparation method thereof |
| CN112960665A (en) * | 2021-04-09 | 2021-06-15 | 山东农业大学 | Preparation method of red and blue light double-emission carbon dots and application of red and blue light double-emission carbon dots in plants |
| CN113265248A (en) * | 2021-06-11 | 2021-08-17 | 江南大学 | Orange red fluorescent carbon dot and preparation method thereof |
| CN114854402A (en) * | 2022-03-22 | 2022-08-05 | 桂林师范高等专科学校 | Preparation method of fluorescent nano material capable of promoting growth of cherokee rose group culture seedling |
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