CN109135738A - A kind of N doping carbon dots and its synthetic method and application based on waste tobacco stem - Google Patents
A kind of N doping carbon dots and its synthetic method and application based on waste tobacco stem Download PDFInfo
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- CN109135738A CN109135738A CN201811101083.8A CN201811101083A CN109135738A CN 109135738 A CN109135738 A CN 109135738A CN 201811101083 A CN201811101083 A CN 201811101083A CN 109135738 A CN109135738 A CN 109135738A
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Abstract
The synthetic method that the present invention provides a kind of N doping carbon dots based on waste tobacco stem takes water as a solvent using waste tobacco stem as carbon source and carries out hydro-thermal reaction in reaction kettle, prepares after reaction through filtering, dialysis, concentration, drying.The N doping carbon dots surface is rich in functional groups such as carboxyl and amino, about 4.7 nm of average grain diameter, it is water-soluble good, under ultraviolet excitation can emitting bright fluorescence, and the fluorescent emission behavior that there is excitation to rely on, it can be used as fluorescence probe applied to bio-imaging etc..
Description
Technical field
The invention belongs to carbon dots synthesis technical fields, and in particular to a kind of N doping carbon dots and its conjunction based on waste tobacco stem
At methods and applications, this method is synthesized for the first time using the waste tobacco stem in production of cigarettes as carbon source using one step hydro thermal method preparation
The N doping carbon dots of good luminescence property.
Background technique
Offal is the by-product of cigarette industry, accounts for about the 25% ~ 30% of leaf weight.Cell wall substance content is higher in offal, main
It to include cellulose, hemicellulose, pectic substance and lignin, in addition there are plurality of active ingredients such as nicotine, Salanesol, green originals
Acid, protein and amino acid etc. have very high utility value.But it is limited by the prior art, it is domestic at present to have number every year
100000 tons of offal is discarded, and also results in the great wasting of resources while polluting environment.Therefore, develop new technology, open up
The higher value application approach of wide offal becomes the new research hotspot of tobacco business.
Carbon dots are at least one a kind of dimensions below l0 nm and the c-based nanomaterial with photoluminescent property.
Since the raw material resources of carbon dots are abundant, and there is excellent chemical inertness, high-biocompatibility, good water-soluble, transmitting
The advantages that spectrum is adjustable and anti-light bleaching, in recent years in bio-imaging, biological medicine, chemical sensitisation, photocatalysis and photoelectricity
Device etc. shows wide application prospect.Natural biomass materials protein rich in, carbohydrate and fat etc. are
For preparing the ideal green presoma of carbon dots.And carbon dots obtained prepares using different carbon source, due to surface texture with
Fluorescence property is different, has different application potentials in basic research field.Carbohydrate rich in, albumen in offal
Matter and amino acid, it is possible to provide to prepare carbon dots, the more active function groups contained can also increase carbon dots for carbon source and nitrogen source
Reactivity, while a kind of new approach is provided for the recycling of offal.There has been no prepare nitrogen about using waste tobacco stem at present
Adulterate the relevant report of carbon dots.
Summary of the invention
The N doping carbon dots based on waste tobacco stem that it is an object of that present invention to provide a kind of, with the label rejected in production of cigarettes
Stalk is carbon source, the N doping carbon dots of good luminescence property has been prepared using one step hydro thermal method, improve waste tobacco stem has
Utilization rate is imitated, is reduced resource waste simultaneously.
The present invention also provides the synthetic method of the N doping carbon dots of above-mentioned waste tobacco stem and its as fluorescence probe in life
The application of object imaging aspect.
The present invention adopts the following technical scheme:
A kind of synthetic method of the N doping carbon dots based on waste tobacco stem takes water as a solvent using waste tobacco stem as carbon source in anti-
Answer and carry out hydro-thermal reaction in kettle, after reaction through filtering, dialysis, be concentrated, be drying to obtain.
The synthetic method of the above-mentioned N doping carbon dots based on waste tobacco stem comprising following steps:
1) will clean, after dry offal powder is mixed with distilled water in reaction kettle under the conditions of 190-210 DEG C hydro-thermal reaction
5-15 hours；
2) after reaction, cooled to room temperature is filtered with filter paper；Gained filtrate is 100-500 Da with molecular cut off
Dialysis membrane dialyse at least 48 hours, obtain carbon dots solution；
3) carbon dots solution obtains brown carbon dots powder through concentrated by rotary evaporation, freeze-drying.
Specifically, in order to obtain preferable hydro-thermal reaction effect, in step 1), to add by solid-liquid ratio 0.5-2g:10 mL
Entering offal powder and distilled water is advisable.
It is further preferred that in step 2, the qualitative filter paper that filter paper used is 15 ~ 20 μm, in order to preferably remove degranulation
Phase sediment；Dialysis membrane is dialysed 72 hours.
The present invention provides the N doping carbon dots synthesized using above-mentioned synthetic method.
Application the present invention also provides N doping carbon dots as fluorescence probe in terms of bio-imaging.
To reduce the wasting of resources, the effective rate of utilization of waste tobacco stem is improved, the present invention is obstructed with the label rejected in production of cigarettes
For carbon source, N doping carbon dots are prepared using one step hydro thermal method, and it is excellent by optimum synthesis condition to have obtained luminescent properties
Good N doping carbon dots.Compared to the prior art, beneficial effects of the present invention are as follows:
1) present invention realizes that the N doping of carbon dots and amino surface are modified through one step hydro thermal method using waste tobacco stem as carbon source.Through trying
Issue after examination and approval existing: N doping carbon dots of the present invention have excellent water solubility and luminescent properties, can emitting bright under ultraviolet excitation
Blue-fluorescence, and the fluorescent emission behavior for having excitation to rely on, maximum excitation and launch wavelength are respectively 330 nm and 440 nm, amount
Sub- yield 7.4% can be used as fluorescence probe applied to bio-imaging etc.；
2) synthetic method process of the present invention is mild, environmentally friendly, easy to operate, opens new approach for the comprehensive utilization of offal.
Detailed description of the invention
Fig. 1 is the high-resolution-ration transmission electric-lens photo (left side) and grain size distribution (right side) of carbon dots；
Fig. 2 is infrared absorption spectrum (left side) and x-ray photoelectron spectroscopy (right side) of carbon dots；
(excitation wavelength is 330 nm to the ultraviolet-visible absorption spectroscopy and fluorescence emission spectrum that Fig. 3 is carbon dots；Embedded figure is carbon dots water
Picture of the solution under natural light (left side) and ultraviolet lamp (right side) irradiation)；
The three-dimensional fluorescence spectrum figure (left side) and the fluorescent emission spectrogram (right side) under 330 ~ 400 nm excitation wavelengths that Fig. 4 is carbon dots.
Specific embodiment
Technical solution of the present invention is further discussed in detail with reference to embodiments, but protection scope of the present invention
It is not limited thereto.
In following embodiments, major experimental instrument used is listed below:
BSA22AS type single-deck electronic balance (Beijing Sai Duolisi Instrument Ltd.), DHG-9030A type electric heating constant temperature air blast are dry
Dry case (the upper macro experimental facilities Co., Ltd of Nereid), RE52CS type Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant), freezing are dry
Dry machine (Beijing Bo Yikang laboratory apparatus Co., Ltd), F-7000 sepectrophotofluorometer (Hitachi Ltd), U-3900 is ultraviolet
Visible spectrophotometer (Hitachi Ltd), Nicolet-6700 type infrared spectrometer (Thermo Scientific),
250 photoelectron spectrograph of ESCALAB (Thermo Scientific), JEM-2100F type field emission electron transmission electron microscope
(JEOL), Hamamatsu Quantaurus-QY absolute fluorescence quantum yield spectrometer (Hamamatsu Photonics).
Embodiment 1
A kind of synthetic method of the N doping carbon dots based on waste tobacco stem comprising following steps:
1) offal for taking cut tobacco winnowing process to reject is lyophilized, grind into powder after cleaning；
2) 0.5 g offal powder is weighed, the hydro-thermal reaction of 25 mL polytetrafluoroethyllining linings is transferred to after 10 mL distilled water of addition
In kettle, the hydro-thermal reaction 10 hours under the conditions of 200 DEG C；
3) after reaction, cooled to room temperature is filtered with 15 ~ 20 μm of qualitative filter papers；Gained filtrate is with molecular cut off
The dialysis membrane of 100-500 Da is dialysed 72 hours, and carbon dots solution is obtained；
3) carbon dots solution obtains brown N doping carbon dots powder after concentrated by rotary evaporation, freeze drier freeze-drying.
The structure and performance characterization of carbon dots.
(1) high-resolution-ration transmission electric-lens characterize:
Fig. 1 is the high-resolution-ration transmission electric-lens photo (left side) and grain size distribution (right side) of carbon dots.As shown in Figure 1, using discarded label stalk
Preparation gained N doping carbon dots are spherical in evenly dispersed standard, and do not observe apparent lattice fringe, are amorphous structure；Grain
Diameter is distributed in 2 ~ 8 nm, is symmetrically distributed in narrow, and it is about 4.7 nm that average grain diameter, which is calculated, by statistics.
(2) infrared absorption spectrum and x-ray photoelectron spectroscopy:
Fig. 2 is infrared absorption spectrum (left side) and x-ray photoelectron spectroscopy (right side) of carbon dots.From x-ray photoelectron spectroscopy: carbon
Carbon rich in, three kinds of nitrogen, oxygen elements in point, the nitrogen and oxygen element of high level mean that prepared sample is rich in oxygen
, the carbon dots of N doping.In infrared absorption spectrum, 3375 cm-1With 3265 cm-1The absorption peak at place be respectively belonging to-OH and-
NH2Symmetrical stretching vibration peak；2920 cm-1With 2855 cm-1The peak at place is the asymmetric and symmetric stretching vibration peak of C-H；
1600 cm-1The flexural vibrations peak that place is N-H；1680 cm-1With 1120 cm-1It is the stretching vibration peak of C=O and C-O respectively；
1295 cm-1With 1395 cm-1It is the stretching vibration peak of C-N and C=N respectively.Illustrate the carbon dots surface-OH ,-NH rich in2
With the functional groups such as-COOH, it is made to have excellent water dispersible.
(3) optical characterisation of carbon dots:
(excitation wavelength is 330 nm to the ultraviolet-visible absorption spectroscopy and fluorescence emission spectrum that Fig. 3 is carbon dots；Embedded figure is carbon dots water
Picture of the solution under natural light (left side) and ultraviolet lamp (right side) irradiation).As shown in figure 3, in carbon dots structure conjugated double bond π-π *
Transition absorption and carbonyl group and pyridine nitrogen in the transition absorption of n- π * cause the UV absorption within the scope of 240 ~ 290 nm.
Under ultraviolet light irradiation, carbon dots aqueous solution issues bright blue-fluorescence；When excitation wavelength is 330 nm, the fluorescent emission of carbon dots
Maximum intensity, emission peak are located at 440 nm, and measurement quantum yield is about 7.4%.
(4) fluorescence property of carbon dots:
The three-dimensional fluorescence spectrum figure (left side) and the fluorescent emission spectrogram (right side) under 330 ~ 400 nm excitation wavelengths that Fig. 4 is carbon dots.Fig. 4
In three-dimensional fluorescence spectrum and the emission spectrum under different excitation wavelengths show: as excitation wavelength is moved to by 330 nm
400 nm, maximum emission wavelength is from 440 nm red shifts to 500 nm, and fluorescence intensity gradually decreases.The partial size of prepared carbon dots is big
It is small to be unevenly distributed, and surface energy defect sites are more, result in this phenomenon that changing dependent on excitation wavelength, while this
The emission characteristics relied on is excited to provide theoretical foundation for the polychrome imaging of carbon dots.
Embodiment 2
A kind of synthetic method of the N doping carbon dots based on waste tobacco stem comprising following steps:
1) will clean, after dry offal powder is mixed with distilled water by solid-liquid ratio 1g:10 mL in reaction kettle in 190 DEG C of items
Hydro-thermal reaction 12 hours under part；
2) after reaction, cooled to room temperature is filtered with 15 ~ 20 μm of qualitative filter papers；Gained filtrate is with molecular cut off
The dialysis membrane of 100-500 Da is dialysed 72 hours, and carbon dots solution is obtained；
3) carbon dots solution obtains brown carbon dots powder through concentrated by rotary evaporation, freeze drier freeze-drying.
Embodiment 3
A kind of synthetic method of the N doping carbon dots based on waste tobacco stem comprising following steps:
1) will clean, after dry offal powder is mixed with distilled water by solid-liquid ratio 2g:10 mL in reaction kettle in 210 DEG C of items
Hydro-thermal reaction 6 hours under part；
2) after reaction, cooled to room temperature is filtered with 15 ~ 20 μm of qualitative filter papers；Gained filtrate is with molecular cut off
The dialysis membrane of 100-500 Da is dialysed 72 hours, and carbon dots solution is obtained；
3) carbon dots solution obtains brown carbon dots powder through concentrated by rotary evaporation, freeze drier freeze-drying.
To sum up, the present invention is obstructed with the discarded label rejected in production of cigarettes for carbon source, and nitrogen is prepared by one step hydro thermal method
Carbon dots are adulterated, rich in functional groups such as carboxyl and amino, water solubility is good on the N doping carbon dots surface, can send out under ultraviolet excitation
Bright blue-fluorescence, and the fluorescent emission behavior that there is excitation to rely on are penetrated, can be used as fluorescence probe applied to bio-imaging etc.
Aspect.In the synthesis process, environmentally protective, easy to operate without adding other reagents, and be effectively utilized in cigarette processing process
By-product, be the high value of offal using providing a kind of new approach.
It should be noted last that: technical solution of the present invention that the above embodiments are only illustrative and not limiting is any right
The equivalent replacement and do not depart from the modification of spirit and scope of the invention or locally replace that the present invention carries out, should all cover in this hair
Within bright protective scope of the claims.
Claims (6)
1. a kind of synthetic method of the N doping carbon dots based on waste tobacco stem, which is characterized in that using waste tobacco stem as carbon source, with water
Hydro-thermal reaction is carried out in reaction kettle for solvent, after reaction through filtering, dialysis, be concentrated, be drying to obtain.
2. the synthetic method of the N doping carbon dots based on waste tobacco stem according to claim 1, which is characterized in that including such as
Lower step:
1) will clean, after dry offal powder is mixed with distilled water in reaction kettle under the conditions of 190-210 DEG C hydro-thermal reaction
6-12 hours；
2) after reaction, cooled to room temperature is filtered with filter paper；Gained filtrate is 100-500 Da with molecular cut off
Dialysis membrane dialyse at least 48 hours, obtain carbon dots solution；
3) carbon dots solution through concentrated by rotary evaporation, be freeze-dried to obtain the final product.
3. the synthetic method of the N doping carbon dots based on waste tobacco stem according to claim 2, which is characterized in that step 1)
In, offal powder and distilled water is added by solid-liquid ratio 0.5-2g:10 mL.
4. the synthetic method of the N doping carbon dots based on waste tobacco stem according to claim 2, which is characterized in that step 2
In, filter paper used is 15 ~ 20 μm of qualitative filter paper；Dialysis membrane is dialysed 72 hours.
5. the N doping carbon dots synthesized using any synthetic method of Claims 1-4.
6. application of the N doping carbon dots as fluorescence probe in terms of bio-imaging described in claim 5.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109929550A (en) * | 2019-04-16 | 2019-06-25 | 山西大学 | A kind of N doping blue-fluorescence carbon quantum dot and its preparation method and application |
| CN110054171A (en) * | 2019-04-25 | 2019-07-26 | 贺州学院 | A kind of preparation method of biomass near-infrared fluorescent carbon dots |
| CN110104629A (en) * | 2019-05-20 | 2019-08-09 | 河南师范大学 | The method for synthesizing fluorescent carbon point as raw material one step hydro thermal method using wild gleditsia sinensis |
| CN110155984A (en) * | 2019-06-12 | 2019-08-23 | 浙江科技学院 | Using soybean slag as the method and application of raw material hydro-thermal method synthesising biological matter fluorescent carbon point |
| CN113148979A (en) * | 2021-02-05 | 2021-07-23 | 贵州省烟草科学研究院 | Method for preparing carbon dots with different colors under same wavelength by using tobacco waste and application |
| CN113287782A (en) * | 2021-02-01 | 2021-08-24 | 云南中烟工业有限责任公司 | Carboxylated carbon-based adsorbent for cigarette filter tip and preparation method and application thereof |
| CN114137048A (en) * | 2021-06-28 | 2022-03-04 | 中北大学 | Preparation method and application of nitrogen-doped graphene quantum dots with sunflower pectin as carbon source |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109929550A (en) * | 2019-04-16 | 2019-06-25 | 山西大学 | A kind of N doping blue-fluorescence carbon quantum dot and its preparation method and application |
| CN110054171A (en) * | 2019-04-25 | 2019-07-26 | 贺州学院 | A kind of preparation method of biomass near-infrared fluorescent carbon dots |
| CN110104629A (en) * | 2019-05-20 | 2019-08-09 | 河南师范大学 | The method for synthesizing fluorescent carbon point as raw material one step hydro thermal method using wild gleditsia sinensis |
| CN110155984A (en) * | 2019-06-12 | 2019-08-23 | 浙江科技学院 | Using soybean slag as the method and application of raw material hydro-thermal method synthesising biological matter fluorescent carbon point |
| CN113287782A (en) * | 2021-02-01 | 2021-08-24 | 云南中烟工业有限责任公司 | Carboxylated carbon-based adsorbent for cigarette filter tip and preparation method and application thereof |
| CN113148979A (en) * | 2021-02-05 | 2021-07-23 | 贵州省烟草科学研究院 | Method for preparing carbon dots with different colors under same wavelength by using tobacco waste and application |
| CN114137048A (en) * | 2021-06-28 | 2022-03-04 | 中北大学 | Preparation method and application of nitrogen-doped graphene quantum dots with sunflower pectin as carbon source |
| CN114137048B (en) * | 2021-06-28 | 2024-03-12 | 中北大学 | Preparation method and application of nitrogen-doped graphene quantum dot with sunflower pectin as carbon source |
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