CN107555416A - The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point - Google Patents
The method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point Download PDFInfo
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- CN107555416A CN107555416A CN201710667822.9A CN201710667822A CN107555416A CN 107555416 A CN107555416 A CN 107555416A CN 201710667822 A CN201710667822 A CN 201710667822A CN 107555416 A CN107555416 A CN 107555416A
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Abstract
The invention discloses a kind of method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point, belong to the synthesis technical field of functional fluorescence carbon point.Technical scheme main points are：Carbon source open country jujube is done and passivator tryptophan is dissolved in deionized water, stir and be placed in after being well mixed in autoclave and obtain brown color liquid in 150 210 DEG C of 12h of hydro-thermal reaction 3, obtained brown yellow solution is cooled to after room temperature again and uses the membrane filtration that aperture is 0.22 μm, so as to obtain N doping fluorescent carbon point.Synthetic route of the present invention is simple, side reaction is few and gross production rate is high, hydro-thermal method reaction condition is gentle, avoid and use toxic reagent, obtained N doping fluorescent carbon point can not only be directly used as the content of fluorescence probe detection material, and can be used for the research of biomarker and imaging, photocatalysis, optoelectronic device and biology sensor etc..
Description
Technical field
The invention belongs to the synthesis technical field of functional fluorescence carbon point, and in particular to a kind of hydro-thermal method synthesis N doping is glimmering
The method of light carbon point.
Background technology
Fluorescent carbon point is a kind of new carbon nanometer material after graphene, fullerene, CNT, carbon nano-fiber
Material, it draws by the features such as its hypotoxicity, good biocompatibility, higher chemical stability and excellent optical stability
The extensive concern of people is played.The many advantages of fluorescent carbon point make it in fluorescence sense, bio-imaging, photocatalysis, optoelectronic device
And the multiple fields such as pharmaceutical carrier have broad application prospects.The synthesis side of many fluorescent carbon points has been explored at present
Method, generally speaking, the synthetic method of fluorescent carbon point can be divided into method from top to bottom and from bottom to top method.From top to bottom method refer to by
Larger-size carbonaceous material is broken or dissociation turns into small molecule, mainly including arc discharge method, laser ablation and electrification
Method etc..On the contrary, method refers to that small molecule is reacted to greater particle size by pyrolysis or autohemagglutination from bottom to top
Material, such as microwave method, hydro-thermal method and ultrasonic method etc..Wherein hydro-thermal method is simple to operate, controllable mild condition is considered as system
The best approach of standby high fluorescent carbon point.In addition, the fluorescent carbon point obtained by different carbon sources can have the different characteristics of luminescences.Mesh
Before, some natural materials and chemicals have been successfully applied to the synthesis of fluorescent carbon point, but are much limited.Therefore, having must
Find a kind of green, dexterous and using inexpensive raw material as carbon source synthesis high-fluorescence quantum yield fluorescent carbon point method.
Fluorescent carbon point is the carbon nano-particles with fluorescent characteristic that particle diameter is less than 10nm, typically by substantial amounts of oxygen, hydrogen
Atom and SP2The carbon atom composition of hydridization, heteroatomic addition can effectively adjust the optical characteristics of fluorescent carbon point, including fluorescence
Carbon point surface state and electronics distribution etc..Not only its fluorescence intensity is very high for the fluorescent carbon point of doping nitrogen synthesized such as the present invention, and
And effectively increase fluorescence quantum yield.
The content of the invention
Present invention solves the technical problem that it there is provided a kind of method of hydro-thermal method synthetic nitrogen doping fluorescent carbon point, this method
It is dry as carbon source using natural wild jujube, using tryptophan as passivator, synthesize the fluorescent carbon point with high quantum production rate, this fluorescence
Nitrogen-atoms is adulterated in carbon point, effectively adjusts the optical characteristics of fluorescent carbon point.
The present invention is to solve above-mentioned technical problem to adopt the following technical scheme that, the side of hydro-thermal method synthetic nitrogen doping fluorescent carbon point
Method, it is characterised in that：Carbon source open country jujube is done and passivator tryptophan is dissolved in deionized water, stirs and is placed in height after well mixed
Brown color liquid is obtained in 150-210 DEG C of hydro-thermal reaction 3-12h in pressure reactor, then obtained brown yellow solution is cooled to room
Wen Houyong apertures are 0.22 μm of membrane filtration, so as to obtain N doping fluorescent carbon point.
Further preferably, hydrothermal temperature is preferably 170 DEG C, and the hydro-thermal reaction time is preferably 9h, carbon source open country jujube it is dry with
The mass ratio of passivator tryptophan is preferably 2:1.
Synthetic route of the present invention is simple, side reaction is few and gross production rate is high, and hydro-thermal method reaction condition is gentle, and avoiding use has
Malicious reagent, obtained N doping fluorescent carbon point can not only be directly used as the content of fluorescence probe detection material, and can use
In the research of biomarker and imaging, photocatalysis, optoelectronic device and biology sensor etc..
Brief description of the drawings
Fig. 1 is the FTIR spectrum figure of obtained N doping fluorescent carbon point under optimal conditions of the present invention；
Fig. 2 be under optimal conditions of the present invention obtained N doping fluorescent carbon point to the fluorescence response figure of different metal ions.
Embodiment
The above of the present invention is described in further details by the following examples, but this should not be interpreted as to this
The scope for inventing above-mentioned theme is only limitted to following embodiment, and all technologies realized based on the above of the present invention belong to this hair
Bright scope.
Embodiment 1
Take wild jujube to do 1.0g, tryptophan 0.5g and deionized water 10mL and be uniformly mixed respectively and be placed in 50mL autoclaves
In, 3h, 6h, 9h, 12h, 15h are reacted respectively in 170 DEG C and obtains brown yellow solution, then obtained brown yellow solution is cooled to room
Sepectrophotofluorometer is used in 100mL volumetric flasks by the membrane filtration that aperture is 0.22 μm, the filtrate constant volume of gained after temperature
（FP-6500 type XRFs, Japanese light splitting company）The fluorescence intensity of resulting solution is determined respectively, the results are shown in Table 1.
The influence that the hydrothermal temperature of table 1 synthesizes to fluorescent carbon point
| Reaction time（h） | 3 | 6 | 9 | 12 | 15 |
| Fluorescence intensity | 776 | 863 | 908 | 840 | 821 |
As shown in Table 1 with the extension in reaction time, hydro-thermal reaction gradually tends to be complete, when reacted between when being 9h, fluorescence is strong
Degree reaches maximum, therefore it is 9h to select optimal the hydro-thermal reaction time.
Embodiment 2
Take wild jujube to do 1.0g, tryptophan 0.5g and deionized water 10mL and be uniformly mixed respectively and be placed in 50mL autoclaves
In, brown yellow solution is obtained respectively at 150 DEG C, 170 DEG C, 190 DEG C and 210 DEG C hydro-thermal reaction 9h, then obtained brown color is molten
Liquid is cooled to after room temperature and uses fluorescence in 100mL volumetric flasks by the membrane filtration that aperture is 0.22 μm, the filtrate constant volume of gained
Spectrophotometer（FP-6500 type XRFs, Japanese light splitting company）The fluorescence intensity of resulting solution is determined respectively, as a result
It is shown in Table 2.
The influence that the hydrothermal temperature of table 2 synthesizes to fluorescent carbon point
| Reaction temperature（℃） | 150 | 170 | 190 | 210 |
| Fluorescence intensity | 878 | 934 | 908 | 896 |
As shown in Table 2 as the rise of hydrothermal temperature, the fluorescence intensity of the fluorescent carbon point of gained gradually strengthen, when reaction temperature
Spend for 170 DEG C when reach maximum, temperature declines on the contrary higher than the fluorescence intensity of 170 DEG C of resulting solutions, and this is due to rise temperature
Contribute to the carbonization of wild jujube, but too high temperature may cause coming off for carbon point surface group, influence the fluorescence of fluorescent carbon point
Intensity, therefore it is optimal hydrothermal temperature to select 170 DEG C.
Embodiment 3
Take wild jujube to do 1.0g, be separately added into tryptophan 0.3g, 0.4g, 0.5g, 0.6g and 0.7g, then plus deionized water 10mL is stirred
Mix to be well mixed and be placed in 50mL autoclaves obtaining brown yellow solution in 170 DEG C of hydro-thermal reaction 9h, then brown color is molten
Liquid is cooled to after room temperature and uses fluorescence in 100mL volumetric flasks by the membrane filtration that aperture is 0.22 μm, the filtrate constant volume of gained
Spectrophotometer（FP-6500 type XRFs, Japanese light splitting company）The fluorescence intensity of resulting solution is determined respectively, as a result
It is shown in Table 3.
The influence that the tryptophan dosage of table 3 synthesizes to fluorescent carbon point
| Tryptophan dosage（g） | 0.3 | 0.4 | 0.5 | 0.6 | 0.7 |
| Fluorescence intensity | 827 | 863 | 934 | 888 | 856 |
Understood by table 3 as the change of tryptophan dosage, fluorescence intensity constantly change.It is synthesized when addition is 0.5g
Fluorescent carbon point maximum intensity, therefore select 0.5g be optimal tryptophan dosage.
Embodiment 4
Wild jujube is taken to do 1.0g, then plus deionized water 10mL is uniformly mixed and is placed in 50mL autoclaves, in 170 DEG C
Hydro-thermal reaction 9h obtains brown yellow solution, then brown yellow solution is cooled to after room temperature by filter membrane mistake that aperture is 0.22 μm
Filter, the filtrate of gained（Without nitrogen-doped carbon point）Constant volume uses sepectrophotofluorometer in 100mL volumetric flasks（FP-6500 types are glimmering
Photothermal spectroscopic analyzer, Japanese light splitting company）The fluorescence intensity for determining resulting solution is 665, hence it is evident that less than N doping fluorescent carbon point.
Embodiment 5
1mM Ag has been investigated respectively+、Ba2+、Fe3+、Ca2+、K+、Cu2+、Cr3+、Mn2+、Li+、Mg2+、Pd2+、Al3+、Na+、Zn2+、
Pb2+、Cd2+、Co2+And Hg2+Shadow of totally 18 metal ion species to obtained N doping fluorescent carbon point fluorescence intensity under optimal conditions
Ring, as a result as shown in Figure 2.Only Hg2+Quenching degree to N doping fluorescent carbon point is larger, and other metal ions are to N doping
The influence of fluorescent carbon point fluorescence is little, illustrates N doping fluorescent carbon point to Hg2+Produce fluorescence response and it is selective preferably.
Embodiment above describes the general principle of the present invention, main features and advantages, the technical staff of the industry should
Understand, the present invention is not limited to the above embodiments, the original for simply illustrating the present invention described in above-described embodiment and specification
Reason, under the scope for not departing from the principle of the invention, various changes and modifications of the present invention are possible, and these changes and improvements are each fallen within
In the scope of protection of the invention.
Claims (2)
1. the method for hydro-thermal method synthetic nitrogen doping fluorescent carbon point, it is characterised in that：Carbon source open country jujube is dry molten with passivator tryptophan
In deionized water, stir and be placed in after well mixed in autoclave obtained in 150-210 DEG C of hydro-thermal reaction 3-12h it is pale brown
Color liquid, then it is 0.22 μm of membrane filtration that obtained brown yellow solution, which is cooled to after room temperature with aperture, is mixed so as to obtain nitrogen
Miscellaneous fluorescent carbon point.
2. the method for hydro-thermal method synthetic nitrogen doping fluorescent carbon point according to claim 1, it is characterised in that：Hydro-thermal reaction temperature
Degree is preferably 170 DEG C, and the hydro-thermal reaction time is preferably 9h, and the jujube dry mass ratio with passivator tryptophan in carbon source open country is preferably 2:1.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
| CN110272737A (en) * | 2019-07-11 | 2019-09-24 | 东北林业大学 | The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot |
| CN115124997A (en) * | 2022-08-09 | 2022-09-30 | 西北师范大学 | Preparation of carbon quantum dot fluorescent probe and application of carbon quantum dot fluorescent probe in detection of iron ions and cysteine |
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| CN104340965A (en) * | 2014-10-17 | 2015-02-11 | 中国科学技术大学 | Macroscopic preparation method of fluorescent carbon quantum dots |
| CN105366659A (en) * | 2015-12-14 | 2016-03-02 | 上海交通大学 | Method for hydro-thermal synthesis of carbon quantum dots based on fruits |
| CN105542762A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Preparation method of nitrogen-doped fluorescence carbon dots |
| CN105905884A (en) * | 2016-04-23 | 2016-08-31 | 哈尔滨师范大学 | Preparation method and application of fluorescence carbon quantum dots |
| CN106629657A (en) * | 2016-11-21 | 2017-05-10 | 辽宁大学 | Fluorescent carbon dots and preparation method and application thereof |
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| CN103834397A (en) * | 2014-03-11 | 2014-06-04 | 太原理工大学 | Method for preparing water-soluble fluorescent carbon dots |
| CN104340965A (en) * | 2014-10-17 | 2015-02-11 | 中国科学技术大学 | Macroscopic preparation method of fluorescent carbon quantum dots |
| CN105366659A (en) * | 2015-12-14 | 2016-03-02 | 上海交通大学 | Method for hydro-thermal synthesis of carbon quantum dots based on fruits |
| CN105542762A (en) * | 2015-12-28 | 2016-05-04 | 江南大学 | Preparation method of nitrogen-doped fluorescence carbon dots |
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| CN108483423A (en) * | 2018-04-08 | 2018-09-04 | 太原理工大学 | A kind of fast preparation method of right-handed chirality carbon dots |
| CN110272737A (en) * | 2019-07-11 | 2019-09-24 | 东北林业大学 | The preparation method of high yield pulp1 nitrogen sulphur self-luminous carbon nano dot |
| CN115124997A (en) * | 2022-08-09 | 2022-09-30 | 西北师范大学 | Preparation of carbon quantum dot fluorescent probe and application of carbon quantum dot fluorescent probe in detection of iron ions and cysteine |
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