CN107312535B - 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 present invention provides the preparation methods that a kind of excitation-emission wavelength relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, comprising the following steps: the preparation of sucrose precursor solution；1~5:3 mixing sucrose precursor solution and concentrated phosphoric acid by volume obtain the first mixed solution；The first obtained mixed solution is heated, brown solution is obtained；Brown solution is placed under the conditions of ice-water bath 5:1~5 by volume and mixes brown solution and ethylenediamine, the second mixed solution is obtained, filters second mixed solution, obtain filtrate；It dialyses the filtrate, obtains dialyzate；Dialyzate is evaporated to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.The preparation method of water-soluble nitrogen phosphor codoping carbon quantum dot of the invention, abundant with carbon source, cheap, preparation process is simple, and preparation overall process is pollution-free, nontoxic, environmentally protective, the advantages of can largely preparing.
Description
Technical field
The invention belongs to the invention belongs to fluorescent material preparation technical fields, and in particular to a kind of excitation-emission wavelength dependence
The preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration.
Background technique
In recent years, fluorescence carbon nanomaterial is because it with good optical characteristics and cell hypotoxicity causes research work
The extensive research of persons.It has preferable photostability, and the presence of nontoxic secondary ion, suitable for detecting and showing for a long time
The experiment of track, biomarker and in terms of have broad application prospects.Carbon quantum dot (CQDs) shows
The excellent properties such as hydrophily, low cytotoxicity, chemistry and photostability make it in chemistry, biomedical, sensing is learned and photoelectron
Field has obtained extensive concern and application.
There are mainly two types of the preparation method of carbon quantum dot is current: method and from bottom to top method from top to bottom.Top-down conjunction
At method, i.e., the physical method of carbon nano-particle, then the side being passivated by polymer surfaces are prepared from biggish carbon structure peeling
Formula makes it effectively shine, and mainly includes arc discharge, laser ablation, electrochemical oxidation, e-book radiation etc..This method often needs
Stringent experiment condition and the special energy are wanted, it is at high cost, and also the carbon quantum yield obtained is relatively low.Synthesis from bottom to top
Method directly synthesizes fluorescent carbon quantum dot by pyrolysis or the suitable predecessor that is carbonized, method includes: combustion method, hydrothermal solution carbon
Change method, ultrasonic method etc., but be all often non-renewable energy resources used by such methods and need stringent post-processing, so
Also it is unfavorable for continuing simultaneously 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 anisotropic excellent and high quantum production rate carbon quantum dot and seems, to be even more important.
Summary of the invention
It is an object of the invention to solve the above problems, and provide the advantages of 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, abundant with carbon source, cheap, preparation process is simple, and preparation overall process is pollution-free, nontoxic, green
Environmental protection, the advantages of can largely preparing.
In order to realize these purposes and other advantages according to the present invention, a kind of excitation-emission wavelength dependence concentration is provided
Water-soluble nitrogen phosphor codoping carbon quantum dot preparation method, comprising the following steps:
The preparation of S1, sucrose precursor solution；
S2, by volume 1~5:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is heated, obtains brown solution；
S4, the brown solution in S3 is placed under the conditions of ice-water bath the mixing brown solution of 5:1~5 and second two by volume
Amine obtains the second mixed solution, filters second mixed solution, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
S6, dialyzate is evaporated to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method is placed in the insulating box that temperature is 80 DEG C, heating time 50min when heating in S3.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method carries out rotary evaporation when evaporating in S6 under 60 DEG C of constant temperature.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, the preparation of sucrose precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water in S1, spare.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, sucrose precursor solution and concentrated phosphoric acid volume ratio are 2:3 in S2.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method is dialysed in S5 specifically: using the bag filter of shearing molecular weight 1000, is dialysed 72 hours.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, the volume ratio of brown solution and ethylenediamine is 5:1 in S4, and ethylenediamine will be added dropwise.
Preferably, the excitation-emission wavelength relies on the preparation side of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, in S1 sucrose precursor solution preparation the following steps are included:
Step 1: by parts by weight be 10 parts sucrose, the silica gel that parts by weight are 5~10 parts, the people that parts by weight are 5~10 parts
It is uniform to make zeolite mixed grinding, 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
In the magnetized water that parts by weight are 30~40 parts, it is ultrasonically treated, obtains aqueous solution；Obtained aqueous solution is placed in electrodialysis to set
It is handled in standby, wherein the flow control of aqueous solution is in 2~2.5m3/ h, current density control are 70~75mA/cm2, until
The conductivity of aqueous solution is 10~20 μ s/cm, stopping processing, the aqueous solution that obtains that treated；Wherein, ultrasonic power be 200~
600W, supersonic frequency are 50~100KHz, and ultrasonic time is 10~20min；
Step 3: by treated obtained in step 2 aqueous solution is placed in power is in the micro-wave oven of 300~800W plus
5~10min of heat, it is cooling up to sucrose precursor solution.
The present invention is include at least the following beneficial effects:
1, the excitation-emission that the present invention prepares relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, using sucrose as carbon
Source, source carbon rich, cheap, preparation process is simple, and preparation overall process is pollution-free, nontoxic, environmentally protective, can largely prepare.
2, the water-soluble nitrogen phosphor codoping carbon quantum dot that the excitation-emission wavelength that the present invention prepares relies on concentration has water
The advantages of dissolubility is good, excitation-emission is adjustable, fluorescent stabilization, good biocompatibility, biomarker, bio-sensing, fluorescence probe,
Anti-fake mark and immunochromatography product scope have important application value.
3, sucrose precursor solution of the invention is by mixing sucrose with silica gel, artificial zeolite, and with and with ox blood it is pure
Albumen is to be placed in the electric field of electrodialysis plant after mixing is ultrasonic, the impurity in raw material can be enable to remove on the one hand to make
The standby carbon quantum dot for obtaining high-purity avoids the purification step of subsequent complexity, on the other hand can be electrically-degradable to raw material progress, makes original
The molecular weight distribution of material is relatively narrow, guarantees 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
It just, is a kind of method of green syt carbon quantum dot.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Detailed description of the invention
Fig. 1 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration of excitation-emission wavelength dependence concentration prepared by the present invention is
The fluorescence excitation of 1mg/mL and fluorescent emission map；
Fig. 2 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration of excitation-emission wavelength dependence concentration prepared by the present invention is
The fluorescence excitation of 5mg/mL and fluorescent emission map；
Fig. 3 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration of excitation-emission wavelength dependence concentration prepared by the present invention is
The fluorescence excitation of 10mg/mL and fluorescent emission map；
Fig. 4 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration of excitation-emission wavelength dependence concentration prepared by the present invention is
The fluorescence excitation of 15mg/mL and fluorescent emission map；
Fig. 5 is that the water-soluble nitrogen phosphor codoping carbon quantum dot concentration of excitation-emission wavelength dependence concentration prepared by the present invention is
The fluorescence excitation of 20mg/mL and fluorescent emission map.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings, to enable those skilled in the art referring to specification text
Word can be implemented accordingly.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or more
The presence or addition of a other elements or combinations thereof.
Embodiment 1
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 1:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:1 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
Embodiment 2
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 2:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:1 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The 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 preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 3:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:2 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
Embodiment 4
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 4:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:3 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
Embodiment 5
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 5:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:3 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
Embodiment 6
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 5:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:5 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water, spare.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
Embodiment 7
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 1:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:1 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution the following steps are included:
Step 1: by parts by weight be 10 parts sucrose, the silica gel that parts by weight are 5 parts, the artificial zeolite that parts by weight are 5 parts mix
It closes grinding uniformly, obtains 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 parts by weight
To be ultrasonically treated in 30 parts of magnetized water, aqueous solution is obtained；Obtained aqueous solution is placed in electrodialysis plant and is carried out
Processing, wherein the flow control of aqueous solution is in 2m3/ h, current density control are 70mA/cm2, until the conductivity of aqueous solution is 10
μ s/cm, stopping processing, the aqueous solution that obtains that treated；Wherein, ultrasonic power 200W, supersonic frequency 50KHz, when ultrasonic
Between be 10min；
Step 3: being heated in the micro-wave oven for being 300W by treated obtained in step 2 aqueous solution is placed in power
5min, it is cooling up to sucrose precursor solution.
Embodiment 8
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 1:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:1 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution the following steps are included:
Step 1: by parts by weight be 10 parts sucrose, the silica gel that parts by weight are 8 parts, the artificial zeolite that parts by weight are 8 parts mix
It closes grinding uniformly, obtains 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 weight
In the magnetized water that part is 35 parts, it is ultrasonically treated, obtains aqueous solution；Obtained aqueous solution is placed in electrodialysis plant and is carried out
Processing, wherein the flow control of aqueous solution is in 2.2m3/ h, current density control are 72mA/cm2, until the conductivity of aqueous solution is
15 μ s/cm, stopping processing, the aqueous solution that obtains that treated；Wherein, ultrasonic power 400W, supersonic frequency 80KHz, ultrasound
Time is 15min；
Step 3: being heated in the micro-wave oven for being 400W by treated obtained in step 2 aqueous solution is placed in power
8min, it is cooling up to sucrose precursor solution.
Embodiment 9
A kind of preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of excitation-emission wavelength dependence concentration, including it is following
Step:
The preparation of S1, sucrose precursor solution；
S2, by volume 1:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is stirred evenly, is placed in insulating box, is heated, it is molten obtains brown
Liquid is simultaneously cooled to room temperature；
S4, brown solution after cooling in S3 is placed in the brown solution of 5:1 mixing by volume and second under the conditions of ice-water bath
Diamines, and ultrapure water dilution is added, the second mixed solution is obtained, second mixed solution is filtered, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
Dialyzate is evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sets in S3
In the insulating box that temperature is 80 DEG C, heating time 50min.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S6 in
Rotary evaporation is carried out under 60 DEG C of constant temperature.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, in S5 thoroughly
Analysis specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, second in S4
Diamines will be added dropwise.
The excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, sugarcane in S1
The preparation of sugar precursor solution the following steps are included:
Step 1: by parts by weight be 10 parts sucrose, the silica gel that parts by weight are 10 parts, the artificial zeolite 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 parts by weight
To be ultrasonically treated in 30~40 parts of magnetized water, aqueous solution is obtained；By obtained aqueous solution be placed in electrodialysis plant into
Row processing, wherein the flow control of aqueous solution is in 2.5m3/ h, current density control are 75mA/cm2, until the conductivity of aqueous solution
For 20 μ s/cm, stopping processing, the aqueous solution that obtains that treated；Wherein, ultrasonic power 600W, supersonic frequency 100KHz surpass
The sound time is 20min；
Step 3: being heated in the micro-wave oven for being 800W by treated obtained in step 2 aqueous solution is placed in power
10min, it is cooling up to sucrose precursor solution.
Comparative example 1
With embodiment 2, the difference is that ethylenediamine is not added in reaction process.
One, 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
When for 1mg/mL, a length of 380nm of optimum excitation wave, best 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
When for 5mg/mL, a length of 420nm of optimum excitation wave, best 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
When for 10mg/mL, a length of 450nm of optimum excitation wave, best 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
When for 15mg/mL, a length of 480nm of optimum excitation wave, best 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
When for 20mg/mL, a length of 490nm of optimum excitation wave, best 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
When for 1mg/mL, a length of 400nm of optimum excitation wave, best 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
When for 1mg/mL, a length of 405nm of optimum excitation wave, best 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
When for 1mg/mL, a length of 410nm of optimum excitation wave, best 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
When for 1mg/mL, a length of 340nm of optimum excitation wave, best launch wavelength is 440nm.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and legend shown and described herein.
Claims (7)
1. a kind of excitation-emission wavelength relies on the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration, feature exists
In, comprising the following steps:
The preparation of S1, sucrose precursor solution；
S2, by volume 1~5:3 mixing sucrose precursor solution and concentrated phosphoric acid, obtain the first mixed solution；
S3, the first mixed solution obtained in S2 is heated, obtains brown solution；
S4, the brown solution in S3 is placed under the conditions of ice-water bath the mixing brown solution of 5:1~5 and ethylenediamine by volume, obtained
To the second mixed solution, second mixed solution is filtered, filtrate is obtained；
S5, the dialysis filtrate, obtain dialyzate；
S6, dialyzate is evaporated to obtain water-soluble nitrogen phosphor codoping carbon quantum dot；
In S1 sucrose precursor solution preparation the following steps are included:
Step 1: by parts by weight be 10 parts sucrose, the silica gel that parts by weight are 5~10 parts, parts by weight be 5~10 parts artificial boiling
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 weight
In the magnetized water that part is 30~40 parts, it is ultrasonically treated, obtains aqueous solution；Obtained aqueous solution is placed in electrodialysis plant
It is handled, wherein the flow control of aqueous solution is in 2~2.5m3/ h, current density control are 70~75mA/cm2, until water-soluble
The conductivity of liquid is 10~20 μ s/cm, stopping processing, the aqueous solution that obtains that treated；Wherein, ultrasonic power is 200~600W,
Supersonic frequency is 50~100KHz, and ultrasonic time is 10~20min；
Step 3: by treated obtained in step 2 aqueous solution is placed in power is heating 5 in the micro-wave oven of 300~800W~
10min, it is cooling up to sucrose precursor solution.
2. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that be placed in when being heated in S3 in the insulating box that temperature is 80 DEG C, heating time 50min.
3. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that rotary evaporation is carried out under 60 DEG C of constant temperature when evaporating in S6.
4. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that the preparation of sucrose precursor solution is that 1g sucrose is dissolved in 2mL ultrapure water in S1, spare.
5. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that sucrose precursor solution and concentrated phosphoric acid volume ratio are 2:3 in S2.
6. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that dialyse in S5 specifically: using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
7. the preparation side that excitation-emission wavelength as described in claim 1 relies on the water-soluble nitrogen phosphor codoping carbon quantum dot of concentration
Method, which is characterized in that the volume ratio of brown solution and ethylenediamine is 5:1 in S4, and ethylenediamine will be added dropwise.
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| CN108865132B (en) * | 2018-07-27 | 2021-11-16 | 中国科学院苏州生物医学工程技术研究所 | Fluorescent carbon quantum dot and preparation method and application thereof |
| CN109456761B (en) * | 2018-11-15 | 2022-01-28 | 山西大学 | Quantitative detection of vitamin B based on carbon quantum dot fluorescence quenching method12Fluorescent probe and preparation method and application thereof |
| CN111591975B (en) * | 2020-06-04 | 2022-03-01 | 山东丰益泰和科技有限公司 | Method for synthesizing carbon quantum dots based on diethylenetriamine penta (methylene phosphonic acid) |
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