CN106634981A - Method for preparing water-soluble yellow fluorescent carbon quantum dot by taking bagasse as raw material - Google Patents
Method for preparing water-soluble yellow fluorescent carbon quantum dot by taking bagasse as raw material Download PDFInfo
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Abstract
The invention discloses a method for preparing a water-soluble yellow fluorescent carbon quantum dot by taking bagasse as a raw material. The method comprises the following steps of 1) performing bagasse pretreatment; 2) mixing ultrapure water and glycerol according to the volume ratio of (2-5):1 to obtain a mixed solution for later use; 3) adding the bagasse obtained through pretreatment into the mixed solution obtained in the step 2) to obtain a mixed solution, stirring, putting the mixed solution under a microwave environment and performing microwave treatment to obtain a brown solution; 4) filtering the brown solution to obtain filtrate; 5) dialyzing the filtrate to obtain dialysate; and 6) evaporating the dialysate under the condition of constant temperature to obtain the water-soluble yellow fluorescent carbon quantum dot. The water-soluble yellow fluorescent carbon quantum dot prepared by the method has the advantages of high water solubility, fluorescence stability, high biocompatibility, no pollution and no toxin, and has an important application value in the fields of biomarkers, biosensing, fluorescence probes, anti-fake markers and immunochromatography products.
Description
Technical field
The invention belongs to fluorescent material preparing technical field, and in particular to a kind of water solublity yellow with bagasse as raw material
The preparation method of fluorescent carbon quantum dot.
Background technology
In recent years, fluorescence carbon nanomaterial because of it there is good optical characteristics and cell hypotoxicity to cause research work
Persons' is widely studied.It has preferable light stability, and the presence of nontoxic secondary ion, it is adaptable to detects for a long time and shows
The experiment of track, has broad application prospects at the aspect such as biomarker and analysis detection.Carbon quantum dot (CQDs) presents
The excellent properties such as hydrophilic, low cytotoxicity, chemistry and light stability so as to learn and photoelectron in chemistry, biomedical, sensing
Field has obtained extensive concern and application.
The preparation method of carbon quantum dot mainly has at present two kinds: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..The method is often needed
Strict experiment condition and the special energy, high cost are wanted, and the carbon quantum productivity ratio for obtaining is relatively low.Synthesis from bottom to top
Method, i.e., be directly synthesized fluorescent carbon quantum dot by the suitable predecessor that is pyrolyzed or is carbonized, and method includes:Combustion method, hydrothermal solution carbon
Change method, ultrasonic method etc., but this kind of method adopted be all often non-renewable energy resources and need strict later stage to process, 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
Effectively method quickly prepares excellent and high quantum production rate the carbon quantum dot of the opposite sex and seems and is even more important.
The content of the invention
It is an object of the invention to solve at least the above, and provide the advantage that at least will be described later.
It is a still further object of the present invention to provide a kind of water solublity yellow fluorescence carbon quantum dot with bagasse as raw material
Preparation method, comprises the following steps:
1) bagasse pre-treatment;
2) by volume 2~5:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Step 3) in, under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature
For 180 DEG C, reaction power is 200W, and the response time is 30min.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Step 6) in, evaporation, specially rotary evaporation.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Pre-treatment includes:Desaccharide, washing, drying.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Step 2) in volume ratio be 5:1.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Dialysis, specially using the bag filter of shearing molecular weight 1000, dialyses 48 hours.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Step 4) in, filtered using sand core funnel.
Preferably, the preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, described
Pre-treatment is specially:Bagasse is crushed, by weight 1:1 mixing bagasse and magnetized water, in the lower 55 DEG C of steaming and decoctings of nitrogen atmosphere
3h, is added thereto to cellulase, and the cellulase weight is the 3% of the bagasse weight, mix homogeneously, 30 DEG C of holdings
60min, filters, and obtains filtering residue;Again high-pressure extrusion is less than 8% to filtering residue water content;Filtering residue is placed in stove carries out calcination process, then
Natural cooling, calcination process is passed through nitrogen toward stove and cools down up to filtering residue, to be in ensureing calcination process and cooling procedure stove
Nitrogen atmosphere, obtains final product the bagasse of premenstrual process.
The present invention at least includes following beneficial effect:
1. the present invention directly carries out the preparation of water solublity yellow fluorescence carbon quantum dot using microwave method, and carbon source is abundant, cheap,
Be conducive to the recycling to garbage, preparation process is simple, preparation overall process is pollution-free, nontoxic, environmental protection, can be a large amount of
Prepare.
2. the water solublity yellow fluorescence carbon quantum dot that the present invention is prepared has good water solubility, fluorescent stabilization, bio-compatible
Good, pollution-free, the nontoxic advantage of property, in biomarker, bio-sensing, fluorescent probe, anti-fake mark and immunochromatography product
Field has important using value.
3. the water solublity yellow fluorescence carbon quantum dot quantum yield that prepared by the present invention is high, and up to 92.3%.
The further advantage of the present invention, target and feature embody part by description below, and part will also be by this
The research of invention and practice and be understood by the person skilled in the art.
Description of the drawings
Fig. 1 is the fluorescence excitation and fluorescent emission collection of illustrative plates of water solublity yellow fluorescence carbon quantum dot prepared by the present invention;
Fig. 2 is fluorescent emission figure of the water solublity yellow fluorescence carbon quantum dot of present invention preparation under different excitation wavelengths
Spectrum;
Fig. 3 is the quantum yield figure of water solublity yellow fluorescence carbon quantum dot prepared by embodiment 2.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is described in further detail, to make those skilled in the art with reference to description text
Word can be implemented according to this.
It should be appreciated that it is used herein such as " have ", "comprising" and " including " term do not allot one or many
The presence or addition of individual other elements or its combination.
Embodiment 1
1) bagasse pre-treatment;
2) by volume 2:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment bag
Include:Desaccharide, washing, drying.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
Embodiment 2
1) bagasse pre-treatment;
2) by volume 3:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment bag
Include:Desaccharide, washing, drying.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
Embodiment 3
1) bagasse pre-treatment;
2) by volume 5:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment bag
Include:Desaccharide, washing, drying.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
Embodiment 4
1) bagasse pre-treatment;
2) by volume 2:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment is concrete
For:Bagasse is crushed, by weight 1:1 mixing bagasse and magnetized water, in the lower 55 DEG C of steaming and decocting 3h of nitrogen atmosphere, add thereto
Enter cellulase, the cellulase weight is the 3% of the bagasse weight, and mix homogeneously, 30 DEG C of holding 60min are filtered,
Obtain filtering residue;Again high-pressure extrusion is less than 8% to filtering residue water content for mixing;Filtering residue is placed in stove carries out calcination process, then naturally cold
But, calcination process is passed through nitrogen toward stove and cools down up to filtering residue, to be blanket of nitrogen in ensureing calcination process and cooling procedure stove
Enclose, obtain final product the bagasse of premenstrual process.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
Embodiment 5
1) bagasse pre-treatment;
2) by volume 3:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment is concrete
For:Bagasse is crushed, by weight 1:1 mixing bagasse and magnetized water, in the lower 55 DEG C of steaming and decocting 3h of nitrogen atmosphere, add thereto
Enter cellulase, the cellulase weight is the 3% of the bagasse weight, and mix homogeneously, 30 DEG C of holding 60min are filtered,
Obtain filtering residue;Again high-pressure extrusion is less than 8% to filtering residue water content for mixing;Filtering residue is placed in stove carries out calcination process, then naturally cold
But, calcination process is passed through nitrogen toward stove and cools down up to filtering residue, to be blanket of nitrogen in ensureing calcination process and cooling procedure stove
Enclose, obtain final product the bagasse of premenstrual process.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
Embodiment 6
1) bagasse pre-treatment;
2) by volume 5:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave
Under environment, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 3) in,
Under being placed in microwave environment, microwave treatment institute is carried out, specially:In being placed in the reaction tube of microwave synthesizer, and temperature is 180 DEG C,
Reaction power is 200W, and the response time is 30min.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the step 6) in,
Evaporation, specially rotary evaporation.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the pre-treatment is concrete
For:Bagasse is crushed, by weight 1:1 mixing bagasse and magnetized water, in the lower 55 DEG C of steaming and decocting 3h of nitrogen atmosphere, add thereto
Enter cellulase, the cellulase weight is the 3% of the bagasse weight, and mix homogeneously, 30 DEG C of holding 60min are filtered,
Obtain filtering residue;Again high-pressure extrusion is less than 8% to filtering residue water content;Filtering residue is placed in stove carries out calcination process, then natural cooling, burns
Burning process is passed through nitrogen toward stove and cools down up to filtering residue, to be nitrogen atmosphere in ensureing calcination process and cooling procedure stove, i.e.,
Obtain the bagasse of premenstrual process.
The preparation method of the described water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, the dialysis, specifically
It is the bag filter using shearing molecular weight 1000, dialyses 48 hours.
First, immunochromatographiassays assays test
The water solublity yellow fluorescence carbon quantum dot that the present invention is prepared can carry out immunochromatographiassays assays with antibodies.
The fluorescent carbon quantum dot of antibodies is more, and corresponding fluorescence intensity is stronger, and it is fixed to be carried out using the power of its fluorescence signal
Amount analysis.
The water solublity yellow fluorescence carbon quantum dot for preparing to embodiment 2 now carries out following immunochromatographiassays assays examination
Test:
(1) under buffer solution system, by two cyclohexyl diimines (DCC) or DIC (DIC) place
Reason can be crosslinked with streptavidin, then with the antibodies of biotin labeling, obtain and combine water solublity yellow fluorescence carbon amounts
The antibody of son point.
(2) immuno-chromatographic test paper strip includes sample application zone, conjugate release area, reaction zone and the suction zones for setting gradually;Institute
State the conjugate release pad that conjugate release area is the antibody that coating is combined with water solublity yellow fluorescence carbon quantum dot;The reaction
To be divided into test section and control zone, the reaction zone is that test section coating is coated with anti-Mus with the antigen of antibodies, control zone in area
The solid support of IgG antibody.
(3) acquisition conjugate in conjugate release pad will be sprayed on reference to the antibody of water solublity yellow fluorescence carbon quantum dot to release
Put area;
Antigen and dynamics are sprayed on the solid support of reaction zone, test section, control zone are formed respectively and 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 obtained final product.
Wherein, the antigen for spraying on immuno-chromatographic test paper strip in immune chromatography reagent kit of the present invention is for different detections
Thing can select the antigen being adapted with detectable substance.
2nd, anti-fake mark test
Water solublity yellow fluorescence carbon quantum dot prepared by embodiment 2 is added in pure water, and it is that 2mg/mL is water-soluble to prepare concentration
Property yellow fluorescence carbon quantum dot aqueous solution 2mL, it is mixed with 5mL polyvinyl alcohol (5.0wt%), by mixed solution brush
Sub- even spread is afterwards placed in sheet glass 1 hour in 65 DEG C of baking ovens on sheet glass, takes out sheet glass and takes pictures, through contrast
Understand, sheet glass under natural light without any color, and under 365nm uviol lamps visible bright yellow fluorescence, therefore carbon amounts
Son point can be used as anti-fake mark.
It is straight tiltedly according to the straight slope of water solublity yellow fluorescence carbon quantum dot structure in Fig. 3 and quinine sulfate point structure
The ratio of rate is multiplied by the quantum yield of quinine sulfate, and (quinine sulfate is standard volume, and 54%) its quantum yield can to calculate
The quantum yield of the present invention is 92.3%.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in description and embodiment
With, it can be applied to completely various suitable the field of the invention, for those skilled in the art, can be easily
Other modification is realized, therefore under the general concept 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 (9)
1. a kind of preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material, it is characterised in that include with
Lower step:
1) bagasse pre-treatment;
2) by volume 2~5:1 mixing ultra-pure water and glycerol, obtain mixed solution standby;
3) bagasse that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in microwave environment
Under, microwave treatment is carried out, obtain brown solution;
4) brown solution is filtered, obtains filtrate;
5) the dialysis filtrate, obtains dialysis solution;
6) dialysis solution evaporation is obtained into water solublity yellow fluorescence carbon quantum dot under constant temperature.
2. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the step 3) in, under being placed in microwave environment, microwave treatment institute is carried out, specially:It is placed in the reaction of microwave synthesizer
Guan Zhong, and temperature is 180 DEG C, reaction power is 200W, and the response time is 30min.
3. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the step 6) in, evaporation, specially rotary evaporation;Constant temperature, is 60 DEG C of constant temperature.
4. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the pre-treatment includes:Desaccharide, washing, drying.
5. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the step 2) in volume ratio be 5:1.
6. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the dialysis, specially using the bag filter of shearing molecular weight 1000, is dialysed 48 hours.
7. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the step 4) in, filtered using sand core funnel.
8. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the water solublity yellow fluorescence carbon quantum dot be applied to biomarker, bio-sensing, fluorescent probe, anti-fake mark with
And immunochromatography product scope.
9. the preparation method of the water solublity yellow fluorescence carbon quantum dot with bagasse as raw material as claimed in claim 1, it is special
Levy and be, the pre-treatment is specially:Bagasse is crushed, by weight 1:1 mixing bagasse and magnetized water, in nitrogen atmosphere
Lower 55 DEG C of steaming and decocting 3h, are added thereto to cellulase, and the cellulase weight is the 3% of the bagasse weight, and mixing is equal
Even, 30 DEG C of holding 60min are filtered, and obtain filtering residue;Again high-pressure extrusion is less than 8% to filtering residue water content;Filtering residue is placed in stove to be carried out
Calcination is processed, then natural cooling, and nitrogen is passed through toward stove for calcination process until filtering residue is cooled down, to ensure calcination process and cooled
Nitrogen atmosphere is in journey stove, the bagasse of premenstrual process is obtained final product.
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CN108562564A (en) * | 2018-03-29 | 2018-09-21 | 青岛大学 | A kind of carbon quantum dot and preparation method and application for the detection of dextrase activity |
CN108975309A (en) * | 2018-09-03 | 2018-12-11 | 南京林业大学 | The method and its application of Water-soluble carbon quantum dot and fluorescent ink are prepared using cyanobacteria |
CN112142036A (en) * | 2020-09-30 | 2020-12-29 | 广州医科大学附属第三医院 | Carbon nanodot and preparation method and application thereof |
CN115231551A (en) * | 2022-09-05 | 2022-10-25 | 云南师范大学 | Method for preparing carbon quantum dots by using dimethyl phthalate |
CN115380005A (en) * | 2020-01-31 | 2022-11-22 | 巴西利亚大学基金会 | Photosynthetic stimulators based on hybrid carbon nanoparticles, related production method and related use as nanostimulants and nanofertilizers in crops |
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