CN107312535A - Excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration - Google Patents
Excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration Download PDFInfo
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Abstract
The preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration is relied on the invention provides a kind of excitation-emission wavelength, is comprised the following steps：The preparation of sucrose precursor solution；By volume 1~5:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；By the first obtained mixed solution heating, brown solution is obtained；Brown solution is placed under the conditions of ice-water bath by volume 5:1~5 mixing brown solution and ethylenediamine, obtain the second mixed solution, filter second mixed solution, obtain filtrate；Dialyse the filtrate, obtain dialyzate；Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot.The preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of the present invention, it has carbon source abundant, cheap, and preparation process is simple, and preparation overall process is pollution-free, nontoxic, environmental protection, the advantage that can largely prepare.
Description
Technical field
The invention belongs to the invention belongs to fluorescent material preparing technical field, and in particular to a kind of excitation-emission wavelength is relied on
The preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration.
Background technology
In recent years, fluorescence carbon nanomaterial there is good optical characteristics and cell hypotoxicity to cause research work because of it
Persons' is widely studied.It has preferable photostability, and the presence of nontoxic secondary ion, it is adaptable to detects and shows for a long time
The experiment of track, has broad application prospects in terms of biomarker and analysis detection.Carbon quantum dot (CQDs) shows
The excellent properties such as hydrophily, low cytotoxicity, chemistry and photostability, make it be learned and photoelectron in chemistry, biomedical, sensing
Field has obtained extensive concern and application.
The preparation method of carbon quantum dot mainly has two kinds at present：Method and from bottom to top method from top to bottom.It is top-down to close
Into method, i.e., the physical method of carbon nano-particle, then the side being passivated by polymer surfaces are prepared from larger carbon structure peeling
Formula makes it effectively light, mainly including arc discharge, laser ablation, electrochemical oxidation, e-book radiation etc..This method is often needed
Strict experiment condition and the special energy are wanted, cost is high, and the carbon quantum productivity ratio obtained is relatively low.Synthesis from bottom to top
Method, i.e., directly synthesize fluorescent carbon quantum dot, method includes by the suitable predecessor that is pyrolyzed or is carbonized：Combustion method, hydrothermal solution carbon
Change method, ultrasonic method etc., but this kind of method used be all often non-renewable energy resources and need strict post-processing, so
Also it is unfavorable for continuing and large-scale production fluorescent carbon quantum dot.Therefore, cheap and easy to get, Nantural non-toxic raw material is found, using simple
Effective method, which quickly prepares excellent and high quantum production rate the carbon quantum dot of the opposite sex and seemed, to be even more important.
The content of the invention
It is an object of the invention to solve the above problems, and provide the advantage that at least will be described later.
It is a still further object of the present invention to provide the water-soluble nitrogen phosphor codoping carbon that a kind of excitation-emission wavelength relies on concentration
The preparation method of quantum dot, it has carbon source abundant, cheap, and preparation process is simple, and preparation overall process is pollution-free, nontoxic, green
Environmental protection, the advantage that can largely prepare.
Concentration is relied on there is provided a kind of excitation-emission wavelength according to object of the present invention and further advantage in order to realize
Water-soluble nitrogen phosphor codoping carbon quantum dot preparation method, comprise the following steps：
S1, sucrose precursor solution preparation；
S2, by volume 1~5:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, by the first mixed solution obtained in S2 heat, obtain brown solution；
S4, the brown solution in S3 is placed under the conditions of ice-water bath to by volume 5:1~5 mixing brown solution and second two
Amine, obtains the second mixed solution, filters second mixed solution, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
S6, by dialyzate evaporation obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
It is placed in when being heated in method, S3 in the insulating box that temperature is 80 DEG C, the heat time is 50min.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
In carrying out rotary evaporation under 60 DEG C of constant temperature when being evaporated in method, S6.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
The preparation of sucrose precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters in method, S1, standby.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Sucrose precursor solution and concentrated phosphoric acid volume ratio are 2 in method, S2:3.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Dialysis is specially in method, S5：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
The volume ratio of brown solution and ethylenediamine is 5 in method, S4:1, and ethylenediamine will be added dropwise.
Preferably, described excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
The preparation of sucrose precursor solution comprises the following steps in method, S1：
Step 1: by sucrose, the silica gel that parts by weight are 5~10 parts, the people that parts by weight are 5~10 parts that parts by weight are 10 parts
Make zeolite mixed grinding uniform, obtain the first mixture；
Step 2: the first mixture that parts by weight are 5~10 parts, the bovine serum albumin(BSA) that parts by weight are 1~2 part are placed in
Parts by weight are ultrasonically treated in 30~40 parts of magnetized water, to carry out, and obtain the aqueous solution；The obtained aqueous solution is placed in into electrodialysis to set
Handled for middle, wherein the flow of the aqueous solution is controlled in 2~2.5m3/ h, current density control is 70~75mA/cm2, until
The electrical conductivity of the aqueous solution is 10~20 μ s/cm, stopping processing, the aqueous solution after being handled；Wherein, ultrasonic power be 200~
600W, supersonic frequency is 50~100KHz, and ultrasonic time is 10~20min；
Add Step 3: the aqueous solution after the processing obtained in step 2 is placed in the micro-wave oven that power is 300~800W
5~10min of heat, cooling produces sucrose precursor solution.
The present invention at least includes following beneficial effect：
1st, the excitation-emission that the present invention is prepared relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, using sucrose as carbon
Source, its carbon rich of originating, cheap, preparation process is simple, prepares that overall process is pollution-free, nontoxic, environmental protection, can largely prepare.
2nd, the water-soluble nitrogen phosphor codoping carbon quantum dot for the excitation-emission wavelength dependence concentration that the present invention is prepared has water
Dissolubility is good, excitation-emission is adjustable, the advantage of fluorescent stabilization, good biocompatibility, biomarker, bio-sensing, fluorescence probe,
Anti-fake mark and immunochromatography product scope have important application value.
3rd, sucrose precursor solution of the invention is by the way that sucrose is mixed with silica gel, artificial zeolite, and with and with ox blood it is pure
On the one hand albumen can enable the impurity in raw material remove to make to be placed in the electric field of electrodialysis plant after mixing ultrasound
The standby carbon quantum dot for obtaining high-purity avoids the purification step of follow-up complexity, on the other hand can be electrically-degradable to raw material progress, makes original
The molecular weight distribution of material is narrower, it is ensured that the uniformity of final quantum point particle；Then assisted microwave synthesis, and it is silica gel in raw material, artificial
Zeolite can largely absorb microwave energy, and compared with former method, the reaction time is short, and reaction instrument is simple, preparation process side
Just, it is a kind of method of green syt carbon quantum dot.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings
Fig. 1 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration that excitation-emission wavelength prepared by the present invention relies on concentration is
1mg/mL fluorescence excitation and fluorescent emission collection of illustrative plates；
Fig. 2 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration that excitation-emission wavelength prepared by the present invention relies on concentration is
5mg/mL fluorescence excitation and fluorescent emission collection of illustrative plates；
Fig. 3 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration that excitation-emission wavelength prepared by the present invention relies on concentration is
10mg/mL fluorescence excitation and fluorescent emission collection of illustrative plates；
Fig. 4 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration that excitation-emission wavelength prepared by the present invention relies on concentration is
15mg/mL fluorescence excitation and fluorescent emission collection of illustrative plates；
Fig. 5 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration that excitation-emission wavelength prepared by the present invention relies on concentration is
20mg/mL fluorescence excitation and fluorescent emission collection of illustrative plates.
Embodiment
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or many
The presence or addition of individual other elements or its combination.
Embodiment 1
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 1:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:1 mixing brown solution and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Embodiment 2
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 2:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:1 mixing brown solution and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4 second two
Amine will be added dropwise.
Embodiment 3
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 3:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:2 mixing brown solutions and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Embodiment 4
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 4:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:3 mixing brown solutions and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Embodiment 5
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 5:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:3 mixing brown solutions and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Embodiment 6
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 5:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:5 mixing brown solutions and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters, standby.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Embodiment 7
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 1:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:1 mixing brown solution and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution comprises the following steps：
Step 1: the sucrose, the silica gel that parts by weight are 5 parts, the artificial zeolite that parts by weight are 5 parts that parts by weight are 10 parts are mixed
Close grinding uniform, obtain the first mixture；
Step 2: the first mixture that parts by weight are 5 parts, the bovine serum albumin(BSA) that parts by weight are 1 part are placed in into parts by weight
It is ultrasonically treated in 30 parts of magnetized water, to carry out, obtain the aqueous solution；The obtained aqueous solution is placed in electrodialysis plant and located
The flow of reason, the wherein aqueous solution is controlled in 2m3/ h, current density control is 70mA/cm2, until the electrical conductivity of the aqueous solution is 10 μ
S/cm, stopping processing, the aqueous solution after being handled；Wherein, ultrasonic power is 200W, and supersonic frequency is 50KHz, ultrasonic time
For 10min；
Heated Step 3: the aqueous solution after the processing obtained in step 2 is placed in the micro-wave oven that power is 300W
5min, cooling produces sucrose precursor solution.
Embodiment 8
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 1:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:1 mixing brown solution and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution comprises the following steps：
Step 1: the sucrose, the silica gel that parts by weight are 8 parts, the artificial zeolite that parts by weight are 8 parts that parts by weight are 10 parts are mixed
Close grinding uniform, obtain the first mixture；
Step 2: the first mixture that parts by weight are 8 parts, the bovine serum albumin(BSA) that parts by weight are 1.5 parts are placed in into weight
Part is ultrasonically treated in 35 parts of magnetized water, to carry out, and obtains the aqueous solution；The obtained aqueous solution is placed in electrodialysis plant and carried out
The flow of processing, the wherein aqueous solution is controlled in 2.2m3/ h, current density control is 72mA/cm2, until the electrical conductivity of the aqueous solution is
15 μ s/cm, stopping processing, the aqueous solution after being handled；Wherein, ultrasonic power is 400W, and supersonic frequency is 80KHz, ultrasound
Time is 15min；
Heated Step 3: the aqueous solution after the processing obtained in step 2 is placed in the micro-wave oven that power is 400W
8min, cooling produces sucrose precursor solution.
Embodiment 9
A kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, including following
Step：
S1, sucrose precursor solution preparation；
S2, by volume 1:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 stirred, be placed in insulating box, heated, obtain brown molten
Liquid is simultaneously cooled to room temperature；
S4, the brown solution after being cooled down in S3 is placed under the conditions of ice-water bath by volume 5:1 mixing brown solution and second
Diamines, and ultra-pure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the filtrate of dialysing, obtain dialyzate；
Dialyzate evaporation is obtained into water-soluble nitrogen phosphor codoping carbon quantum dot under S6, constant temperature.
Described excitation-emission wavelength is relied on to be put in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S3
In temperature in 80 DEG C of insulating box, the heat time is 50min.
Described excitation-emission wavelength rely in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
Described excitation-emission wavelength is relied in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S5 thoroughly
Analysis is specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Described excitation-emission wavelength relies on second in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S4
Diamines will be added dropwise.
Described excitation-emission wavelength relies on sugarcane in the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, S1
The preparation of sugar precursor solution comprises the following steps：
Step 1: by sucrose, the silica gel that parts by weight are 10 parts, the artificial zeolite that parts by weight are 10 parts that parts by weight are 10 parts
Mixed grinding is uniform, obtains the first mixture；
Step 2: the first mixture that parts by weight are 10 parts, the bovine serum albumin(BSA) that parts by weight are 2 parts are placed in into parts by weight
It is ultrasonically treated in 30~40 parts of magnetized water, to carry out, obtain the aqueous solution；The obtained aqueous solution is placed in electrodialysis plant
Row processing, the wherein flow of the aqueous solution are controlled in 2.5m3/ h, current density control is 75mA/cm2, until the electrical conductivity of the aqueous solution
For 20 μ s/cm, stopping processing, the aqueous solution after being handled；Wherein, ultrasonic power is 600W, and supersonic frequency is 100KHz, is surpassed
The sound time is 20min；
Heated Step 3: the aqueous solution after the processing obtained in step 2 is placed in the micro-wave oven that power is 800W
10min, cooling produces sucrose precursor solution.
Comparative example 1
Be the same as Example 2, difference is in course of reaction to be not added with ethylenediamine.
First, excitation-emission wavelength relies on concentration experiment
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 2 relies on concentration is made into concentration
During for 1mg/mL, a length of 380nm of optimum excitation wave, optimal launch wavelength is 480nm, as shown in Figure 1.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 2 relies on concentration is made into concentration
During for 5mg/mL, a length of 420nm of optimum excitation wave, optimal launch wavelength is 520nm, as shown in Figure 2.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 2 relies on concentration is made into concentration
During for 10mg/mL, a length of 450nm of optimum excitation wave, optimal launch wavelength is 540nm, as shown in Figure 3.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 2 relies on concentration is made into concentration
During for 15mg/mL, a length of 480nm of optimum excitation wave, optimal launch wavelength is 560nm, as shown in Figure 4.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 2 relies on concentration is made into concentration
During for 20mg/mL, a length of 490nm of optimum excitation wave, optimal launch wavelength is 580nm, as shown in Figure 5.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 7 relies on concentration is made into concentration
During for 1mg/mL, a length of 400nm of optimum excitation wave, optimal launch wavelength is 500nm.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 8 relies on concentration is made into concentration
During for 1mg/mL, a length of 405nm of optimum excitation wave, optimal launch wavelength is 510nm.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by embodiment 9 relies on concentration is made into concentration
During for 1mg/mL, a length of 410nm of optimum excitation wave, optimal launch wavelength is 520nm.
The water-soluble nitrogen phosphor codoping carbon quantum dot that excitation-emission wavelength prepared by comparative example 1 relies on concentration is made into concentration
During for 1mg/mL, a length of 340nm of optimum excitation wave, optimal launch wavelength is 440nm.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the legend with description.
Claims (8)
1. a kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, its feature exists
In comprising the following steps：
S1, sucrose precursor solution preparation；
S2, by volume 1~5:3 mixing sucrose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；
S3, by the first mixed solution obtained in S2 heat, obtain brown solution；
S4, the brown solution in S3 is placed under the conditions of ice-water bath to by volume 5:1~5 mixing brown solution and ethylenediamine, are obtained
To the second mixed solution, second mixed solution is filtered, filtrate is obtained；
S5, the filtrate of dialysing, obtain dialyzate；
S6, by dialyzate evaporation obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
2. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that be placed in when being heated in S3 in the insulating box that temperature is 80 DEG C, the heat time is 50min.
3. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that in carrying out rotary evaporation under 60 DEG C of constant temperature when being evaporated in S6.
4. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that the preparation of sucrose precursor solution is that 1g sucrose is dissolved in into 2mL ultra-pure waters in S1, standby.
5. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that sucrose precursor solution and concentrated phosphoric acid volume ratio are 2 in S2:3.
6. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that dialysis is specially in S5：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
7. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that the volume ratio of brown solution and ethylenediamine is 5 in S4:1, and ethylenediamine will be added dropwise.
8. excitation-emission wavelength as claimed in claim 1 relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, it is characterised in that the preparation of sucrose precursor solution comprises the following steps in S1：
Step 1: by the sucrose that parts by weight are 10 parts, the silica gel that parts by weight are 5~10 parts, the artificial boiling that parts by weight are 5~10 parts
Stone mixed grinding is uniform, obtains the first mixture；
Step 2: the first mixture that parts by weight are 5~10 parts, the bovine serum albumin(BSA) that parts by weight are 1~2 part are placed in into weight
Part is ultrasonically treated in 30~40 parts of magnetized water, to carry out, and obtains the aqueous solution；The obtained aqueous solution is placed in electrodialysis plant
Handled, wherein the flow of the aqueous solution is controlled in 2~2.5m3/ h, current density control is 70~75mA/cm2, Zhi Daoshui
The electrical conductivity of solution is 10~20 μ s/cm, stopping processing, the aqueous solution after being handled；Wherein, ultrasonic power be 200~
600W, supersonic frequency is 50~100KHz, and ultrasonic time is 10~20min；
Step 3: by the aqueous solution after the processing obtained in step 2 be placed in power be 300~800W micro-wave oven in heating 5~
10min, cooling produces sucrose precursor solution.
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