CN110358533A - A kind of preparation method and application of nitrogen-sulfur doping green fluorescent carbon dots - Google Patents

A kind of preparation method and application of nitrogen-sulfur doping green fluorescent carbon dots Download PDF

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Publication number
CN110358533A
CN110358533A CN201810305179.XA CN201810305179A CN110358533A CN 110358533 A CN110358533 A CN 110358533A CN 201810305179 A CN201810305179 A CN 201810305179A CN 110358533 A CN110358533 A CN 110358533A
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triethanolamine
green fluorescent
carbon dots
fluorescent carbon
solvent
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钟元
胡栩华
陈永华
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Huzhou Kevin Micro Technology Co Ltd
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Huzhou Kevin Micro Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y20/00Nanooptics, e.g. quantum optics or photonic crystals
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64Fluorescence; Phosphorescence
    • G01N21/6486Measuring fluorescence of biological material, e.g. DNA, RNA, cells

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Abstract

The present invention relates to a kind of using triethanolamine as the preparation method of solvent nitrogen-sulfur doping green fluorescent carbon dots.The method provided by the invention for preparing green fluorescent carbon dots as solvent using triethanolamine is: (1) under room temperature; taurine is dissolved in triethanolamine; above-mentioned solution is transferred in reaction kettle by ultrasonic disperse, the solution that isothermal reaction certain time obtains at a certain temperature;(2) after being dried, ethanol washing is added, filtering obtains solution, rotates to get green fluorescent carbon dots solid is arrived;It (3) is for the first time carbon source preparation green fluorescent carbon dots by solvent taurine of triethanolamine, easy to operate, raw material is easy to get and cheap, and reaction condition can mildly regulate and control in the present invention.On the other hand, raw material contains a large amount of N, O, S, without adding dopant that can directly obtain nitrogen-sulfur doping green fluorescent carbon dots, fluorescent carbon point cytotoxicity obtained is low, good biocompatibility, fluorescence intensity is high, fluorescent stability is good, which can be used for metal ion detection, biomarker and Biological imaging etc..

Description

A kind of preparation method and application of nitrogen-sulfur doping green fluorescent carbon dots
Technical field
The present invention relates to directly prepare nitrogen-sulfur doping green fluorescent carbon dots method from taurine using triethanolamine as solvent And application, belong to the technical field for preparing the carbon dots that shine.
Background technique
Triethanolamine is a kind of common weakly alkaline organic complexing agent or solvent, is had a wide range of applications.Taurine is again Claim 2-aminoethanesulfonic acid, there is good physiological function, be a kind of amino acid necessary to body, in pharmaceuticals industry and food row It is widely used in industry.On the other hand, taurine contains a large amount of N, O, S, can obtain preferable fluorescence property by doping.It is at present Taurine is not only prepared into using triethanolamine as solvent the report of green fluorescent carbon dots.
Carbon dots (Carbon dots, CDs) have been constantly subjected to the favor of researcher since 2004 find for the first time.In recent years Come, fluorescent carbon point is most popular one of carbon nanomaterial after fullerene, carbon nanotube and graphene.This nano material Certain disadvantages of traditional quantum dot are overcome, not only there is excellent optical property and small size property, but also have good Biocompatibility, it is easy to accomplish it is surface-functionalized, it is carried in biochemical sensitive, imaging analysis, environment measuring, photocatalysis technology and drug The fields such as body have good application potential.
Summary of the invention
In the present invention, nitrogen-sulfur doping green fluorescent carbon dots are prepared as carbon source using triethanolamine as solvent taurine for the first time. The green fluorescent carbon dots cytotoxicity of preparation is low, good biocompatibility, easy to operate, and raw material is easy to get and cheap, reacts item Part can mildly regulate and control.The fluorescent carbon point can be used for metal ion detection, biomarker and Biological imaging etc..
For this purpose, the present invention relates to a kind of using triethanolamine as solvent nitrogen-sulfur doping green fluorescent carbon dots preparation method, packet It includes:
(1) under room temperature, taurine is dissolved in triethanolamine, ultrasonic disperse, above-mentioned solution is transferred to reaction In kettle;(2) solution that isothermal reaction certain time obtains at a certain temperature;(3) after being dried, ethyl alcohol is added and washes It washs, filters, obtain solution, rotate to get green fluorescent carbon dots solid is arrived.
The concentration of taurine solution is 0.2-0.4mol/L in the step (1);The ultrasonic disperse time is 10-15min;Instead Answering kettle is autoclave.
Reaction temperature is 150 DEG C -175 DEG C in the step (2);Reaction time is 8-10 hours.
The means being dried in the step (3) are freeze-drying.
Fluorescence detection should be carried out in the detection darkroom in Fluorescence Spectrometer in described, launch wavelength range 300-600nm swashs Hair and transmite slit 2nm.
Beneficial effect
In the present invention, nitrogen-sulphur is prepared using taurine as carbon source using triethanolamine as solvent for the first time and mixes green fluorescent carbon dots. Gained fluorescent carbon point cytotoxicity of the invention is low, good biocompatibility, fluorescence intensity is high, fluorescent stability is good, easy to operate, former Material is easy to get and cheap, and reaction condition can mildly regulate and control, which can be used for metal ion detection, biomarker and life Object image etc..
Detailed description of the invention
Fig. 1 is the nitrogen-sulfur doping green fluorescent carbon dots of the invention prepared by solvent of triethanolamine in different excitation wavelengths Under fluorescence pattern;
Fig. 2 is the nitrogen-sulfur doping fluorescent carbon point fluorescent emission spectrogram prepared under different solvents in case one;
Fig. 3 is nitrogen-sulfur doping green fluorescent carbon dots appearance and outdoor scene prepared in case one by solvent of triethanolamine Figure;
Fig. 4 is nitrogen-sulfur doping green fluorescent carbon dots powder high-resolution-ration transmission electric-lens figure in case two;
Fig. 5 is nitrogen-sulfur doping green fluorescent carbon dots cell toxicity data figure in case three;
Fig. 6 is nitrogen-influence of the sulfur doping green fluorescent carbon dots to cellular morphology in case three.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited Range.
Case study on implementation one,
Using taurine as carbon source, under room temperature, 0.5g taurine is dissolved separately in 10mL ethyl alcohol, diethylene glycol list In butyl ether, toluene, chloroform, tetraethyl orthosilicate, distilled water and triethanolamine, ultrasonic disperse 10min is transferred to autoclave In, the constant temperature 8h at 170 DEG C, rear natural cooling is dried using freeze drier, and ethanol wash is added afterwards, it filters, Solution is obtained, revolving obtains nitrogen-sulfur doping green fluorescent carbon dots (N-S/CDs) solid.It can be obtained by fluophotometer, with three second Hydramine is that yellowish-brown is presented in the carbon dots solution under natural light of N-S/CDs made from solvent, by changing excitation wavelength, corresponding hair Ejected wave length can also occur to change accordingly, and very big Red Shift Phenomena occurs, has the characteristics that apparent excitation wavelength dependence.It is different The N-S/CDs that solvent is prepared most hyperfluorescence emission peak has certain difference, the N-S/CDs prepared using triethanolamine as solvent Fluorescence intensity is most strong and what nitrogen-sulfur doping fluorescent carbon point for only prepare using triethanolamine as solvent was sent out is green light, so change Reaction dissolvent has strong influence to preparation N-S/CDs.Therefore we can be by changing reaction dissolvent to N-S/CDs fluorescence It is modified to carry out selectivity.
Case study on implementation two,
Using triethanolamine as solvent, using taurine as carbon source, under room temperature, 0.5g taurine is dissolved in 10mL tri- In ethanol amine, ultrasonic disperse 10min is transferred in autoclave, the constant temperature 10h at 160 DEG C, rear natural cooling, and utilization is cold Lyophilizer is dried, and ethanol wash is added afterwards, filtering, obtains solution, and revolving obtains nitrogen-sulfur doping green fluorescence carbon Point (N-S/CDs) solid.Prepared fluorescent carbon point good dispersion, nothing in triethanolamine can be obtained by high-resolution-ration transmission electric-lens The phenomenon that reunion, appearance almost spherical, and particle diameter distribution is more uniform, in 4.0nm, surface has more clear average grain diameter Clear lattice fringe structure, spacing of lattice 0.21nm.This lesser fluorescent carbon point of partial size can easily enter thin Born of the same parents, make its bio-imaging and in terms of have a wide range of applications.
Case study on implementation three,
Using triethanolamine as solvent, using taurine as carbon source, under room temperature, 0.35g taurine is dissolved in 10mL In triethanolamine, ultrasonic disperse 10min is transferred in autoclave, the constant temperature 9h at 165 DEG C, rear natural cooling, and utilization is cold Lyophilizer is dried, and ethanol wash is added afterwards, filtering, obtains solution, and revolving obtains nitrogen-sulfur doping green fluorescence carbon Point (N-S/CDs) solid.Carbon dots powder cytotoxicity test is carried out, is found when N-S/CDs is at concentrations up to 150 μ g/mL, carefully Born of the same parents' survival rate is still greater than 90%;It is found that cellular morphology in influence experiment of the N-S/CDs solution of various concentration to cellular morphology Very nearly the same with cell (d) form of control group, cell is substantially all presentation shuttle shape, illustrates N-S/CDs solution to the shape of cell State influences smaller.Combination cell toxicity test data further illustrate N-S/CDs cytotoxicity very little, with traditional fluorescence Marker is compared, and N-S/CDs is nontoxic under quite high concentration.

Claims (5)

1. a kind of using triethanolamine as the preparation of solvent nitrogen-sulfur doping green fluorescent carbon dots, which is characterized in that it is with triethanolamine It for solvent, is prepared: (1) under room temperature, taurine being dissolved in triethanolamine, ultrasonic disperse using following methods, Above-mentioned solution is transferred in reaction kettle;(2) isothermal reaction certain time at a certain temperature, obtained solution;(3) it is done After dry processing, ethanol washing is added, filtering obtains solution, rotates to get green fluorescent carbon dots solid is arrived.
2. a kind of using triethanolamine as the preparation of solvent green fluorescent carbon dots according to claim 1, it is characterised in that: used Solvent is the pure triethanolamine of chemistry.
3. a kind of using triethanolamine as the preparation of solvent green fluorescent carbon dots according to claim 1, it is characterised in that: gained Carbon dots wavelength of transmitted light is mainly between 450nm-550nm.
4. a kind of using triethanolamine as the preparation of solvent green fluorescent carbon dots according to claim 1, it is characterised in that: ox sulphur The concentration of acid solution is 0.2-0.4mol/L.
5. a kind of using triethanolamine as the preparation of solvent green fluorescent carbon dots according to claim 1, it is characterised in that: ultrasound Jitter time is 10-15min;The temperature of reaction is 150 DEG C -175 DEG C;The time of reaction is 8-10h.
CN201810305179.XA 2018-04-09 2018-04-09 A kind of preparation method and application of nitrogen-sulfur doping green fluorescent carbon dots Pending CN110358533A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111849475A (en) * 2020-08-25 2020-10-30 中南民族大学 Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111849475A (en) * 2020-08-25 2020-10-30 中南民族大学 Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof
CN111849475B (en) * 2020-08-25 2022-05-24 中南民族大学 Nitrogen and sulfur co-doped carbon dot and preparation method and application thereof

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Application publication date: 20191022