CN105295910B - A kind of method that feux rouges carbon point is prepared using biomass as presoma - Google Patents
A kind of method that feux rouges carbon point is prepared using biomass as presoma Download PDFInfo
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Abstract
It is a kind of using biomass as presoma prepare feux rouges carbon point method be choose biological material, cut into fritter, be placed in mortar, add second alcohol and water mixed liquor, milled processed, take out juice, be centrifuged off precipitation and fragment；Resulting solution is added in autoclave, heating response；Reacted solution, which is placed in bag filter, dialyses, and gives the carbon point of small molecule and unreacted biomass mixed solution；Obtain required feux rouges carbon dots solution.The present invention have toxicity is low, good biocompatibility, cost is low, preparation technology is simple and it is green the advantages of.
Description
Technical field
The present invention relates to a kind of method that feux rouges carbon point is prepared using biomass as presoma.
Background technology
Near-infrared fluorescent bio-imaging technology has deep penetration into tissue, the interference of low background fluorescence, minimum bio because of it
The advantages that sample light injury, causes people widely to pay close attention to.It is fluorescent dye, semiconductor amount to report more fluorescent material at present
Son point and macromolecule quantum dot.But it is present, and toxicity is big, poor biocompatibility, cost are high, preparation technology is complicated and dirty
The problem of contaminating environment.And fluorescent carbon point has hypotoxicity, good biocompatibility compared with traditional near-infrared light-emitting material
Enriched with carbon source, it is turned into a dazzling star in biomedical sector.
At present, the method for preparing fluorescent carbon point reported is a lot, is broadly divided into method from top to bottom and from bottom to top method.From
It is upper and laxative remedy is big carbon skeleton structure to be broken to small carbon skeleton structure in brief；And method is to pass through organic matter from bottom to top
Dehydration carbonization forms carbon point particle.But the fluorescence for the carbon point transmitting that these methods obtain at present is located at blue light or green glow more
Region (Lei Y, Weihua J, Lipeng Q, et al. One pot synthesis of highly
luminescent polyethylene glycol anchored carbon dots functionalized with a
nuclear localization signal peptide for cell nucleus imaging[J]. Nanoscale,
2015, 7(14):6104-6113.)；Preparation process is complex and is presoma using poisonous chemical reagent or is quarter
Lose agent (Jiang Kai, Sun Shan, Zhang Ling, et al. Red, green, and blue
luminescence by carbon dots: full-color emission tuning and multicolor
cellular imaging.[J]. AngewandteChemie, 2015, 54(18):5360-5363. this document is with benzene
Diamines is that presoma prepares carbon point.Xiaoyun, Tan, Yunchao, Li, Xiaohong, Li, et al.
Electrochemical synthesis of small-sized red fluorescent graphene quantum
dots as a bioimaging platform.[J]. Chemical Communications, 2015, 51(13):
2544-2546. this documents are the methods using electrochemistry, use K2S2O8Graphite is etched to prepare carbon point)；And on feux rouges carbon
The report of point is seldom.Therefore, seek that low toxicity, good biocompatibility, cost are low, preparation is simple and green
New method prepare feux rouges carbon point and will promote practical application of the carbon point in terms of bio-imaging.
The content of the invention
Present invention aim to address prior art problem, there is provided a kind of toxicity is low, good biocompatibility, cost are low, system
Standby technique is simple and the green method that feux rouges carbon point is prepared using biomass as presoma.
In order to solve the above technical problems, the technical scheme is that, green biological material is selected as forerunner
Body, the mixed solvent of second alcohol and water is added, the milled processed in mortar, after the clear liquid centrifugation of taking-up, is put into hydrothermal reaction kettle
Heating response, it is placed in bag filter and dialyses after terminating, obtains feux rouges carbon point.
The method that the present invention prepares feux rouges carbon point using biomass as presoma, comprises the following steps：
(1) selection biological material, cuts into fritter, is placed in mortar, the mixed liquor of addition second alcohol and water, at grinding
Reason；
(2) juice is taken out, is centrifuged off precipitation and fragment；
(3) by step（2）Middle resulting solution is added in autoclave, heating response；
(4) reacted solution, which is placed in bag filter, dialyses, and gives the carbon point of small molecule and unreacted biomass
Mixed solution；Obtain required feux rouges carbon dots solution；
As feux rouges carbon point solid powder need to be obtained, it is placed on being freeze-dried in freeze drying box, you can obtain.
Such as step（1）Biological material mainly selects green plants, such as vegetables, leaf and green herbaceous plant.
Such as step（1）The volume ratio of middle ethanol and deionized water is（1-20）:1；Biological material：Mixed solution=8-12
g：10-50 ml；Milling time is t (5min≤m≤10 min).
Such as step（2）The rotating speed of middle centrifuge is in 5000-12000 r/min, centrifugation 5-15 min；
Such as step（3）The selection range of middle reaction temperature is at 140-180 DEG C, the scope 4-8 h in reaction time.Beyond this model
When enclosing, the carbonizing degree and yield of carbon point can not be balanced.
If the selection range of bag filter molecular cut off in step (4) is in 3000-8000 MW, dialysis 2-4 days.
Product after hydro-thermal, is placed in bag filter, and the scope of molecular cut off is 3000-8000 MW, within this range,
Be advantageous to give unreacted biomass solution, molecular cut off crosses conference and make it that the carbon point particle diameter of retention is excessive, scattering
Phenomenon is serious, is unfavorable for stable luminescence.
It need to be freeze-dried to obtain using freeze drier when obtaining solid powder in step (6), avoid causing the centre of luminescence
Destruction.
The particle diameter distribution for the fluorescent carbon point that the present invention obtains is uniform, and surface is rich in oxygen-containing functional group, multi-wavelength excitation, most preferably
For excitation wavelength respectively positioned at 409 nm, 511 nm, 543 nm, 616 nm, optimal launch wavelength is located at 685 nm and 725 nm, whole
Launch wavelength is presented independent of excitation wavelength in body.
The present invention beneficial outcomes be：1. biomass presoma wide material sources；2. the presentation of fluorescent carbon point prepared by is more
Wave band excitation wavelength, and still have stronger excitation wavelength in 616 nm, existing report is not almost seen, and launch wavelength is disobeyed
Rely and shifted in excitation wavelength；3. the optimal launch wavelength of fluorescent carbon point prepared by is 680nm, than the feux rouges of existing report
The launch wavelength of carbon point more moves near infrared region, still there is obvious transmitting near 720-750nm；4. prepare feux rouges carbon point
It is nontoxic, cost is low, the cycle is short, preparation technology is simple, green；5. it is a kind of feasible new side for preparing feux rouges carbon point of green
Method, help speed up its paces in the application of near-infrared fluorescent bio-imaging.
Biomass is that presoma is the new method for preparing feux rouges carbon point, and carbon source is mainly derived from the Nature, green.System
The solvent added during standby, beneficial to biomass into outside carbon, modification is played on its surface, and biomass is rich carbon in itself
With rich nitrogen class material, there is advantageous advantage in terms of feux rouges carbon point is prepared, it is not necessary to which carbon point is carried out at follow-up modification
Reason.
Brief description of the drawings
Fig. 1 is the fluorescence spectra that feux rouges carbon point is prepared using spinach as biomass presoma；
Fig. 2 is the purple light spectrogram that feux rouges carbon point is prepared using spinach as biomass presoma；
Fig. 3 is the transmission electron microscope picture that feux rouges carbon point is prepared using spinach as biomass presoma；
Fig. 4 is the fluorescence spectra that feux rouges carbon point is prepared using clover as biomass presoma；
Fig. 5 is the fluorescence spectra that feux rouges carbon point is prepared using Chinese parasol leaf as biomass presoma.
Embodiment
Technical solution of the present invention is not limited to the embodiment of act set forth below, in addition to each embodiment it
Between any combination.Every equivalence changes done according to the technology of the present invention content and retouching, should be included in the skill of the present invention
Within art category.
Embodiment 1：
First, the preparation of biomass presoma：It is biomass carbon source to select spinach, takes 10g the leaf of spinach to be sheared and fragmentates,
It is placed in the in the mixed solvent of 10ml second alcohol and waters（Volume ratio is 5:1）, grind 5 min, take out mixed liquor in centrifuge with
Work 10min under 8000r/min rotating speeds, takes upper solution；
2nd, hydrothermal carbonization：Upper solution is placed in autoclave, 8 h is heated at 150 DEG C, obtains carbon and order mixed liquor.
3rd, dialyse：Take the carbon for reacting end in two steps to order mixed liquor, be placed in bag filter, bag filter selection
3000MW, dialyse 3 days, obtain feux rouges carbon dots solution；
4th, dry：In freeze drier, in -30 DEG C of pre-freeze 4h, 24h is dried by Slow-rate freezing, produces feux rouges carbon solid point
Body powder.
Fluorescent Characterization is carried out to prepared feux rouges carbon point using Horiba Fluoromax-4 XRFs, sees Fig. 1.
Multiband excitation wavelength is presented in Fig. 1, and launch wavelength is independent of excitation wavelength.Maximum excitation wavelength be located at 409nm, 511nm,
543nm, 616nm, optimal launch wavelength are located at 685nm, and have acromion appearance in 700-750nm.Do not seen in existing report
To this phenomenon.And optimal transmitting of the present invention than reports such as the Xiaoyun Tan et. of existing report is located at 605nm to long wave side
To mobile 80nm.
Uv-visible absorption spectroscopy is tested using SHIMADZU UV-3600 ultraviolet-visible spectrophotometers, such as Fig. 2
Shown, carbon point prepared by spinach all shows significantly to absorb in 200-800 nm regions, particularly in visible region
Absorb also clearly；The carbon point that the feature is different from being typically prepared only has absorption in ultraviolet region.
Transmission electron microscope picture such as Fig. 3, size are mainly distributed on 10-12 nm.
Embodiment 2
First, the preparation of biomass presoma：It is biomass carbon source to select clover, takes 12g to be sheared and fragmentates, is placed in
The in the mixed solvent of 50ml second alcohol and waters（Volume ratio is 10:1）, milled processed 10min, take out mixed liquor in centrifuge with
Work 5min under 12000r/min rotating speeds, takes upper solution；
2nd, hydrothermal carbonization：It is placed in autoclave, 8 h is heated at 160 DEG C.
3rd, dialyse：Take the carbon for reacting end in two to order mixed liquor, be placed in bag filter, bag filter selection 5000
MW, dialyse 2 days, obtain feux rouges carbon dots solution；
4th, dry：In freeze drier, in -30 DEG C of pre-freeze 4h, 24h is dried by Slow-rate freezing, produces feux rouges carbon solid point
Body powder.
Fluorescent Characterization is carried out to prepared feux rouges carbon point using Horiba Fluoromax-4 XRFs, sees Fig. 4.
There are two maximum excitation wavelengths, respectively positioned at 425nm and 523nm, launch in multiband, and the emission peak at 656 nm is strong
Degree reaches maximum, and the emission peak than the feux rouges carbon point of existing report is located to long wave direction movement 50nm.
Embodiment 3
First, the preparation of biomass presoma：It is biomass carbon source to select Chinese parasol leaf, takes 10g to be sheared and fragmentates, puts
In the in the mixed solvent of 20ml second alcohol and waters（Volume ratio is 20:1）, grind 5min, take out mixed liquor in centrifuge with
Work 15min under 5000r/min rotating speeds, takes upper solution；
2nd, hydrothermal carbonization：It is placed in autoclave, 4 h is heated at 180 DEG C.
3rd, dialyse：Preparation process is identical with embodiment two；
4th, dry：Method is identical with embodiment two.
In the case of the fluorometric investigation condition identical of embodiment 1,2, fluorescence spectrum Fig. 5 is obtained.The position of optimal excitation peak
At 398 nm and 502 nm, corresponding optimal launch wavelength is located at 666nm, and the fluorescence intensity in embodiment 3 is substantially high
In embodiment 2.May be due to contained O in Chinese parasol leaf and clover, the otherness of N element amount, and in hydrothermal carbonization process
In, the surface defect of carbon point causes intensity that obvious change occurs.
Claims (4)
- A kind of 1. method that feux rouges carbon point is prepared using biomass as presoma, it is characterised in that comprise the following steps：(1) biological material is chosen, fritter is cut into, is placed in mortar, adds the mixed liquor of second alcohol and water, milled processed；(2) juice is taken out, is centrifuged off precipitation and fragment；(3) by step（2）Middle resulting solution is added in autoclave, heating response；(4) reacted solution, which is placed in bag filter, dialyses, and gives carbon point and the mixing of unreacted biomass of small molecule Solution；Obtain required feux rouges carbon dots solution；（5）Feux rouges carbon dots solution, which is placed in freeze drying box, to be freeze-dried, and obtains feux rouges carbon point solid powder；Step（1）Biological material selects green plants；Step（1）The volume ratio of middle ethanol and deionized water is 1-20:1；Biological material：Mixed solution=8-12 g：10-50 ml；Milling time is extremely to be less than or equal to 10 min more than or equal to 5min；Step（2）The rotating speed of middle centrifuge is in 5000-12000 r/min, centrifugation 5-15 min；Step（3）Middle reaction temperature is at 140-180 DEG C, reaction time 4-8h.
- A kind of 2. method that feux rouges carbon point is prepared using biomass as presoma as claimed in claim 1, it is characterised in that green Plant is vegetables, leaf or green herbaceous plant.
- A kind of 3. method that feux rouges carbon point is prepared using biomass as presoma as claimed in claim 1, it is characterised in that step (4) bag filter molecular cut off is in 3000-8000 MW, dialysis 2-4 days in.
- 4. a kind of method that feux rouges carbon point is prepared using biomass as presoma as described in claim any one of 1-3, its feature It is that the particle diameter distribution for preparing feux rouges carbon point is uniform, surface is rich in oxygen-containing functional group, and excitation wavelength is respectively positioned at 409 nm, 511 Nm, 543 nm, 616 nm, launch wavelength are located at 685 nm and 725 nm.
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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 |
| 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 |
| 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 |
| CN113265248B (en) * | 2021-06-11 | 2022-04-26 | 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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