CN107384393A - Using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method - Google Patents
Using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method Download PDFInfo
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Abstract
The invention provides a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material, comprise the following steps：The preparation of glucose precursor solution；By volume 1~5:3 mixed glucose precursor solutions and concentrated phosphoric acid, obtain the first mixed solution；The first mixed solution obtained in S2 is heated, obtains brown solution；Brown solution in S3 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 is evaporated to obtain 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, green, the advantages of can largely preparing.
Description
Technical field
The invention belongs to fluorescent material preparing technical field, and in particular under a kind of temperate condition with glucose, concentrated phosphoric acid,
Ethylenediamine is the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material.
Background technology
In recent years, fluorescence carbon nanomaterial is because it there is good optical characteristics and cell hypotoxicity to cause research work
Persons' is widely studied.It has preferable photostability, and the presence of nontoxic secondary ion, suitable for detecting and showing for a long time
The experiment of track, had broad application prospects in biomarker and analysis detection etc..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.
The preparation method of carbon quantum dot mainly has two kinds at present：Method and from bottom to top method from top to bottom.Top-down conjunction
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 luminous, mainly including arc discharge, laser ablation, electrochemical oxidation, e-book radiation etc..This method often needs
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., fluorescent carbon quantum dot is directly synthesized by the suitable predecessor that is pyrolyzed or is carbonized, method includes：Combustion method, hydrothermal solution carbon
Change method, ultrasonic method etc., but used by this kind of method be all often non-renewable energy resources and need strict 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 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 advantages of at least will be described later.
It is a still further object of the present invention to provide it is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphorus
The preparation method of codope carbon quantum dot, it has carbon source abundant, cheap, and preparation process is simple, and preparation overall process is pollution-free, nothing
It is malicious, green, the advantages of can largely preparing.
In order to realize according to object of the present invention and further advantage, there is provided one kind is with glucose, concentrated phosphoric acid, second two
Amine is the preparation method of the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material, is comprised the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1~5:3 mixed glucose 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, the second mixed solution is obtained, filter second mixed solution, obtain filtrate；
S5, the dialysis filtrate, obtain dialyzate；
S6, dialyzate evaporated to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, be placed in when heating in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, rotary evaporation is carried out under 60 DEG C of constant temperature when evaporating in S6.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, glucose precursor solution and concentrated phosphoric acid volume ratio are 2 in S2:3.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, the volume ratio of brown solution and ethylenediamine is 5 in S4:1, and ethylenediamine will be added dropwise.
Preferably, it is described using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, in S1 the preparation of glucose precursor solution comprise the following steps：
Step 1: glucose that parts by weight are 50 parts, the complex enzyme that parts by weight are 0.2~0.5 part are placed in parts by weight and are
In 100~200 parts of magnetized water, it is ultrasonically treated, obtains the aqueous solution；Wherein, ultrasonic power is 200~600W, supersonic frequency
Rate is 50~100KHz, and ultrasonic time is 10~20min；It is 1 that the complex enzyme, which includes mass ratio,:0.2~0.8:0.5~1
Ribalgilase, carbohydrase and debranching enzyme mixture；
Step 2: by the aqueous solution in step 2 in power be 50~100W uviol lamps under irradiate 10~20min after be placed in
Temperature is in 30~40 DEG C of containers, and stink damp is passed through into container, and the pressure in holding container be 0.5~1Mpa, holding
Time is 5~10min；Then it is passed through ozone into reactor, the pressure in holding container is 1~1.5Mpa, and the retention time is
10~15min；Finally it is passed through nitrogen, the pressure in holding container is 1.5~2Mpa, and the retention time is 5~10min, is being stood
10~20min, the aqueous solution after being handled；
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, cools down and produces glucose precursor solution
The present invention comprises at least following beneficial effect：
1st, the present invention prepares water-soluble nitrogen phosphor codoping carbon quantum dot using gentle condition, and carbon source is abundant, cheap, system
Standby process is simple, and preparation overall process is pollution-free, nontoxic, green, can largely prepare.
2nd, the water-soluble nitrogen phosphor codoping carbon quantum dot that the present invention prepares has good water solubility, excitation-emission adjustable, glimmering
The advantages of light is stable, good biocompatibility, produced in biomarker, bio-sensing, fluorescence probe, anti-fake mark and immunochromatography
Product field has important application value.
3rd, water-soluble nitrogen phosphor codoping carbon quantum dot quantum yield prepared by the present invention can be more than 13%.
4th, the present invention is tried using glucose as presoma, and using biological complex enzyme as the activating agent of reaction and passivation
Agent, while ultraviolet light is used, and hydrogen sulfide gas and oxidizing gas ozone are passed through, the free radical of strong oxidizing property is produced,
The production cycle is shortened, industrial pollution will not be caused, and energy consumption is low, reduces production cost, and yield height is greatly improved, it is economical
Considerable benefit, and assisted microwave synthesis is reacted so that carbon quantum dot biological safety during preparation and use during the course of the reaction
Well, environmental and biological materials will not be damaged, reaction instrument is simple, and preparation process is convenient, is adapted to most of organic small
The carbonization of molecule, 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 the fluorescence excitation and fluorescent emission collection of illustrative plates of water-soluble nitrogen phosphor codoping carbon quantum dot prepared by the present invention；
Fig. 2 is fluorescent emission figure of the water-soluble nitrogen phosphor codoping carbon quantum dot of the invention prepared under different excitation wavelengths
Spectrum；
Fig. 3 is the fluorescence quantum yield figure of water-soluble nitrogen phosphor codoping carbon quantum dot prepared by embodiment 2.
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 more
The presence or addition of individual other elements or its combination.
Embodiment 1
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 2
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 2:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 3
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 3:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 4
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 4:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 5
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 5:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 6
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 5:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
Embodiment 7
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S1 the preparation of glucose precursor solution comprise the following steps：
Step 1: it is 100 parts that glucose that parts by weight are 50 parts, the complex enzyme that parts by weight are 0.2 part are placed in into parts by weight
Magnetized water in, be ultrasonically treated, obtain the aqueous solution；Wherein, ultrasonic power 200W, supersonic frequency 50KHz, when ultrasonic
Between be 10min；It is 1 that the complex enzyme, which includes mass ratio,:0.2:0.5 ribalgilase, carbohydrase and debranching enzyme mixture；
Step 2: in power it is to irradiate after 10min that to be placed in temperature be 30 DEG C under 50W uviol lamps by the aqueous solution in step 2
In container, and stink damp is passed through into container, the pressure in holding container is 0.5Mpa, retention time 5min；Then to
It is passed through ozone in reactor, the pressure in holding container is 1Mpa, retention time 10min；Finally it is passed through nitrogen, holding container
In pressure be 1.5Mpa, retention time 5min, standing 10min, the aqueous solution after being handled；
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, cool down and produce glucose precursor solution.
Embodiment 8
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S1 the preparation of glucose precursor solution comprise the following steps：
Step 1: it is 150 parts that glucose that parts by weight are 50 parts, the complex enzyme that parts by weight are 0.3 part are placed in into parts by weight
Magnetized water in, be ultrasonically treated, obtain the aqueous solution；Wherein, ultrasonic power 400W, supersonic frequency 80KHz, when ultrasonic
Between be 15min；It is 1 that the complex enzyme, which includes mass ratio,:0.5:0.7 ribalgilase, carbohydrase and debranching enzyme mixture；
Step 2: in power it is to irradiate after 15min that to be placed in temperature be 35 DEG C under 80W uviol lamps by the aqueous solution in step 2
In container, and stink damp is passed through into container, the pressure in holding container is 0.8Mpa, retention time 7min；Then to
It is passed through ozone in reactor, the pressure in holding container is 1.2Mpa, retention time 12min；Nitrogen is finally passed through, keeps holding
Pressure in device is 1.8Mpa, retention time 7min, is standing 15min, the aqueous solution after being handled；
Heated Step 3: the aqueous solution after the processing obtained in step 2 is placed in the micro-wave oven that power is 500W
8min, cool down and produce glucose precursor solution.
Embodiment 9
It is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method,
Comprise the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1:3 mixed glucose 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, it is molten to obtain brown
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 dialysis filtrate, obtain dialyzate；
Dialyzate evaporated under S6, constant temperature to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, it is placed in S3 in the insulating box that temperature is 80 DEG C, heat time 50min.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, rotary evaporation is carried out under 60 DEG C of constant temperature in S6.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, ethylenediamine will be added dropwise in S4.
It is described using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation side
Method, in S1 the preparation of glucose precursor solution comprise the following steps：
Step 1: it is 200 parts that glucose that parts by weight are 50 parts, the complex enzyme that parts by weight are 0.5 part are placed in into parts by weight
Magnetized water in, be ultrasonically treated, obtain the aqueous solution；Wherein, ultrasonic power 600W, supersonic frequency 100KHz, ultrasound
Time is 20min；It is 1 that the complex enzyme, which includes mass ratio,:0.8:1 ribalgilase, carbohydrase and debranching enzyme mixture；
Step 2: in power it is to irradiate after 20min that to be placed in temperature be 40 under 100W uviol lamps by the aqueous solution in step 2
In DEG C container, and stink damp is passed through into container, the pressure in holding container is 1Mpa, retention time 10min；Then to
It is passed through ozone in reactor, the pressure in holding container is 1.5Mpa, retention time 15min；Nitrogen is finally passed through, keeps holding
Pressure in device is 2Mpa, retention time 10min, is standing 20min, the aqueous solution after being handled；
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, cool down and produce glucose precursor solution.
Fig. 1 is the fluorescence excitation and fluorescent emission collection of illustrative plates of water-soluble nitrogen phosphor codoping carbon quantum dot prepared by the present invention.
Fig. 2 is fluorescent emission figure of the water-soluble nitrogen phosphor codoping carbon quantum dot of the invention prepared under different excitation wavelengths
Spectrum, wherein curve from top to bottom correspond to a~h respectively, and excitation wavelength corresponding to a~h curves be respectively 380nm, 390nm,
400nm、410nm、420nm、430nm、440nm、450nm。
First, immunochromatographiassays assays are tested
The water-soluble nitrogen phosphor codoping carbon quantum dot that the present invention is prepared can carry out immunochromatography point with antibody binding
Analysis.The fluorescent carbon quantum dot of antibody binding is more, and corresponding fluorescence intensity is stronger, can be carried out using the power of its fluorescence signal
Quantitative analysis.
The water-soluble nitrogen phosphor codoping carbon quantum dot that embodiment 2 is prepared now carries out following immunochromatographiassays assays examination
Test：
(1) under buffer solution system, two cyclohexyl diimines (DCC) or DIC (DIC) place are passed through
Reason can be crosslinked with streptavidin, then combine water-soluble nitrogen phosphor codoping carbon with the antibody binding of biotin labeling, acquisition
The antibody of quantum dot.
(2) immuno-chromatographic test paper strip includes sample application zone, conjugate release area, reaction zone and the suction zones set gradually；Institute
State the conjugate release pad that conjugate release area is combined with the antibody of water-soluble yellow fluorescence carbon quantum dot for coating；The reaction
To be divided into test section and control zone, the reaction zone is the antigen of test section coating and antibody binding, the anti-mouse of control zone coating in area
The solid support of IgG antibody.
(3) antibody for combining water-soluble nitrogen phosphor codoping carbon quantum dot is sprayed in conjugate release pad and obtains conjugate
Discharge area；
Antigen and dynamics are sprayed on the solid support of reaction zone, form test section respectively, control zone is obtained
Obtain reaction zone；
Being pasted onto on backing of mutually overlapping successively of sample application zone, conjugate release area, reaction zone and suction zones is produced.
Wherein, the antigen sprayed in immune chromatography reagent kit of the present invention on immuno-chromatographic test paper strip is directed to different detections
Thing can select the antigen being adapted with detectable substance.
2nd, anti-fake mark is tested
Water-soluble nitrogen phosphor codoping carbon quantum dot prepared by embodiment 2 is added in pure water, and preparation concentration is 2mg/mL water
Dissolubility nitrogen-phosphor codoping carbon quantum dot aqueous solution 2mL, it is mixed with 5mL polyvinyl alcohol (5.0wt%), by mixed solution
With on brush even spread to sheet glass, sheet glass is placed in 65 DEG C of baking ovens 1 hour afterwards, sheet glass is taken out and takes pictures, pass through
Contrast understands that sheet glass does not have any color under natural light, and the visible bright blue-fluorescence under 365nm uviol lamps, therefore
Carbon quantum dot can be used as anti-fake mark.
It is straight according to the straight slope of water-soluble nitrogen-phosphor codoping carbon quantum dot structure and quinine sulfate point structure in Fig. 3
The ratio of slope is multiplied by the quantum yield of quinine sulfate, and (quinine sulfate is standard volume, 54%) its quantum yield is can calculate
The fluorescence quantum yield for going out the carbon quantum dot of the present invention is 13%.
Embodiment 7,8,9 is similarly calculated to the fluorescence quantum yield of carbon quantum dot in the same way for respectively
13.4%th, 13.7%, 14.1%.
Comparative example 1
With embodiment 2, distinguish and ethylenediamine is being not added with reaction, the fluorescence of carbon quantum dot is calculated in the same way
Quantum yield is 11.2%.
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, it is of the invention and unlimited
In specific details and shown here as the legend with description.
Claims (8)
1. it is a kind of using glucose, concentrated phosphoric acid, ethylenediamine as the water-soluble nitrogen phosphor codoping carbon quantum dot of raw material preparation method, its
It is characterised by, comprises the following steps：
S1, glucose precursor solution preparation；
S2, by volume 1~5:3 mixed glucose 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, obtains filtrate；
S5, the dialysis filtrate, obtain dialyzate；
S6, dialyzate evaporated to obtain water-soluble nitrogen phosphor codoping carbon quantum dot.
2. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that it is heat time 50min in 80 DEG C of insulating box that temperature is placed in when being heated in S3.
3. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that in S6 evaporate when rotary evaporation is carried out under 60 DEG C of constant temperature.
4. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that the preparation of glucose precursor solution is that 1g glucose is dissolved in into 2mL ultra-pure waters in S1, standby.
5. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that glucose precursor solution and concentrated phosphoric acid volume ratio are 2 in S2:3.
6. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that in S5 dialysis be specially：Using the bag filter of shearing molecular weight 1000, dialyse 72 hours.
7. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that in S4 the volume ratio of brown solution and ethylenediamine be 5:1, and ethylenediamine will be added dropwise.
8. as claimed in claim 1 using glucose, concentrated phosphoric acid, ethylenediamine as raw material water-soluble nitrogen phosphor codoping carbon quantum dot
Preparation method, it is characterised in that the preparation of glucose precursor solution comprises the following steps in S1：
Step 1: by glucose that parts by weight are 50 parts, the complex enzyme that parts by weight are 0.2~0.5 part be placed in parts by weight be 100~
In 200 parts of magnetized water, it is ultrasonically treated, obtains the aqueous solution；Wherein, ultrasonic power is 200~600W, supersonic frequency 50
~100KHz, ultrasonic time are 10~20min；It is 1 that the complex enzyme, which includes mass ratio,:0.2~0.8:0.5~1 ribose core
Sour enzyme, carbohydrase and debranching enzyme mixture；
Step 2: by the aqueous solution in step 2 in power be 50~100W uviol lamps under irradiate 10~20min after be placed in temperature
For in 30~40 DEG C of containers, and stink damp is passed through into container, the pressure in holding container is 0.5~1Mpa, the retention time
For 5~10min；Then it is passed through ozone into reactor, the pressure in holding container is 1~1.5Mpa, the retention time is 10~
15min；Finally be passed through nitrogen, the pressure in holding container is 1.5~2Mpa, and the retention time is 5~10min, stand 10~
20min, the aqueous solution after being handled；
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, cool down and produce glucose precursor solution.
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| CN113201336A (en) * | 2021-05-19 | 2021-08-03 | 扬州大学 | Preparation method based on nitrogen-phosphorus doped carbon quantum dots and application of preparation method in rapid detection of tartrazine |
| CN113736456A (en) * | 2021-09-10 | 2021-12-03 | 四川大学 | Tumor targeting nanoprobe based on folic acid coupled carbon quantum dots and preparation method thereof |
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