CN106698393A - Method for synthesizing water-soluble carbon quantum dots from orange peels - Google Patents

Method for synthesizing water-soluble carbon quantum dots from orange peels Download PDF

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Publication number
CN106698393A
CN106698393A CN201611103828.5A CN201611103828A CN106698393A CN 106698393 A CN106698393 A CN 106698393A CN 201611103828 A CN201611103828 A CN 201611103828A CN 106698393 A CN106698393 A CN 106698393A
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Prior art keywords
orange peel
carbon quantum
water
quantum dot
treatment
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CN201611103828.5A
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Chinese (zh)
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黄珊
肖琦
杨二利
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Guangxi Teachers College
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Guangxi Teachers College
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09KMATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K11/00Luminescent, e.g. electroluminescent, chemiluminescent materials
    • C09K11/08Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
    • C09K11/65Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/60Optical properties, e.g. expressed in CIELAB-values

Abstract

The invention discloses a method for synthesizing water-soluble carbon quantum dots from orange peels. The method comprises the following steps: 1) pre-treating the orange peels; 2) mixing de-ionized water and glycerol according to the volume ratio of (2 to 5) to 1, so as to obtain a mixed solution for later use; 3) adding the pre-treated orange peels into the mixed solution obtained by the step 2) and stirring; enabling the mixed solution to react for 12h at 160 DEG C, so as to obtain a brown solution; 4) filtering the brown solution to obtain filtrate; 5) dialyzing the filtrate; 6) evaporating dislysate under a constant-temperature condition, so as to obtain the water-soluble carbon quantum dots. The water-soluble carbon quantum dots prepared by the method disclosed by the invention have the advantages of good water solubility, stable fluorescence, good biocompatibility, no pollution and no toxin and have an important application value in the aspects of biomarkers, biological sensing, fluorescent probes and the like.

Description

The method of orange peel synthesizing water-solubility carbon quantum dot
Technical field
The invention belongs to fluorescent material preparing technical field, and in particular to a kind of orange peel synthesizing water-solubility carbon quantum dot Method.
Background technology
Semiconductor-quantum-point (Quantum dots, QDs) has good optics, electricity and optical and electrical properties because of it, The research fields such as biomarker, biomedicine and opto-electronic device have a wide range of applications.But conventional semiconductor quantum Point will necessarily introduce heavy metal element during preparation, have potentially hazardous property to environment and human health, therefore open Send out nontoxic, it is environmentally friendly, and with the novel fluorescence nano material similar with semiconductor-quantum-point turn into everybody pay close attention to Jiao Point.
Arbitrarily abandoned by people do not know before the value of orange peel, with scientists constantly grinding to it Study carefully, its value is also increasingly paid much attention to by people.From orange peel in terms of food, feed, medicine and environment Exploitation overview can see, currently the research of orange peel is also rested on the basis of simple application, how to be entered One step is upgraded, the scientific and technological content that reinforcement is utilized, and is increased operation rate, and reaches industrial operation, is all problem demanding prompt solution.And Orange peel is developed without research more many.Therefore, make great efforts to improve the correct understanding that people are worth orange peel, fill Divide more economical with great scientific research and practical value for the mankind bring using orange peel.Meanwhile, its effective utilization will For scientific research provides new thinking, so can environmental protection can turn waste into wealth again and bring certain economic benefit.
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 method of orange peel synthesizing water-solubility carbon quantum dot, including following step Suddenly:
1) orange peel pre-treatment;
2) by volume 2~5:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specifically It is rotary evaporation;Constant temperature, is 60 DEG C of constant temperature.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the pre-treatment includes:Cleaning, solarization Dry, crushing.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the step 2) in volume ratio be 3: 1。
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing The bag filter of molecular weight 1000, dialyses 48 hours.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, leaked using core Bucket is filtered.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the Water-soluble carbon quantum dot application In cell marking, fluorescence probe, anti-fake mark and immunochromatography product scope.
Preferably, the method for described orange peel synthesizing water-solubility carbon quantum dot, the pre-treatment is specially:By orange Skin is crushed, by weight 1:1 mixing orange peel and magnetized water, in the lower 55 DEG C of boiling 3h of nitrogen atmosphere, is added thereto to cellulose Enzyme, the cellulase weight is the 3% of the orange peel weight, is well mixed, and 30 DEG C of holding 60min, filtering obtains filter residue; High-pressure extrusion to filter residue water content is less than 8% again;Filter residue is placed in carries out calcination treatment in stove, then natural cooling, calcination process Nitrogen is passed through toward stove until filter residue cooling, to be nitrogen atmosphere in ensureing calcination process and cooling procedure stove, obtains final product premenstrual The orange peel for the treatment of.
The present invention at least includes following beneficial effect:
1. the present invention directly carries out the preparation of Water-soluble carbon quantum dot using microwave method, and carbon source is abundant, cheap, and it is right to be conducive to The recycling of discarded object, preparation process is simple, and preparation overall process is pollution-free, nontoxic, environmental protection, can largely prepare.
2. the Water-soluble carbon quantum dot that the present invention is prepared has good water solubility, fluorescent stabilization, good biocompatibility, without dirt Dye, nontoxic advantage, have important application value at aspects such as biomarker, bio-sensing and fluorescence probes.
3. the Water-soluble carbon quantum dot quantum yield that prepared by the present invention is high, and up to 93.2%.
Further advantage of the invention, target and feature embody 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 carbon quantum dot of the invention;
Fig. 2 is the quantum yield figure of Water-soluble carbon quantum dot prepared by embodiment 2.
Specific 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 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) orange peel pre-treatment;
2) by volume 2:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the pre-treatment includes:Clean, dry, crush.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 2) in volume ratio be 3:1.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
Embodiment 2
1) orange peel pre-treatment;
2) by volume 3:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the pre-treatment includes:Clean, dry, crush.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 2) in volume ratio be 3:1.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
Embodiment 3
1) orange peel pre-treatment;
2) by volume 5:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the pre-treatment includes:Clean, dry, crush.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
Embodiment 4
1) orange peel pre-treatment;
2) by volume 2:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The pre-treatment is specially:Orange peel is crushed, by weight 1:1 mixing orange peel and magnetized water, in blanket of nitrogen Lower 55 DEG C of boiling 3h are enclosed, cellulase is added thereto to, the cellulase weight is the 3% of the orange peel weight, mixed Uniformly, 30 DEG C of holding 60min, filtering, obtain filter residue;High-pressure extrusion to filter residue water content is less than 8% again for mixing;Filter residue is placed in stove In carry out calcination treatment, then natural cooling, calcination process toward being passed through nitrogen in stove until filter residue is cooled down, with ensure calcination process and Nitrogen atmosphere is in cooling procedure stove, is obtained final product through the orange peel of pre-treatment.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 2) in volume ratio be 3:1.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
Embodiment 5
1) orange peel pre-treatment;
2) by volume 3:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The pre-treatment is specially:Orange peel is crushed, by weight 1:1 mixing orange peel and magnetized water, in blanket of nitrogen Lower 55 DEG C of boiling 3h are enclosed, cellulase is added thereto to, the cellulase weight is the 3% of the orange peel weight, mixed Uniformly, 30 DEG C of holding 60min, filtering, obtain filter residue;High-pressure extrusion to filter residue water content is less than 8% again for mixing;Filter residue is placed in stove In carry out calcination treatment, then natural cooling, calcination process toward being passed through nitrogen in stove until filter residue is cooled down, with ensure calcination process and Nitrogen atmosphere is in cooling procedure stove, is obtained final product through the orange peel of pre-treatment.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 2) in volume ratio be 3:1.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
Embodiment 6
1) orange peel pre-treatment;
2) by volume 5:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;It is placed in 160 DEG C, 12h is reacted, obtain brown solution;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 6) in, evaporation, specially rotation are steamed Hair;Constant temperature, is 60 DEG C of constant temperature.
The pre-treatment is specially:Orange peel is crushed, by weight 1:1 mixing orange peel and magnetized water, in blanket of nitrogen Lower 55 DEG C of boiling 3h are enclosed, cellulase is added thereto to, the cellulase weight is the 3% of the orange peel weight, mixed Uniformly, 30 DEG C of holding 60min, filtering, obtain filter residue;High-pressure extrusion to filter residue water content is less than 8% again for mixing;Filter residue is placed in stove In carry out calcination treatment, then natural cooling, calcination process toward being passed through nitrogen in stove until filter residue is cooled down, with ensure calcination process and Nitrogen atmosphere is in cooling procedure stove, is obtained final product through the orange peel of pre-treatment.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the dialysis, specially using shearing molecular weight 1000 bag filter, dialyses 48 hours.
The method of described orange peel synthesizing water-solubility carbon quantum dot, the step 4) in, carried out using sand core funnel Filter.
First, immunochromatographiassays assays experiment
The Water-soluble carbon quantum dot that the present invention is prepared can be combined with antibody and carry out immunochromatographiassays assays.Antibody is combined Fluorescent carbon quantum dot it is more, corresponding fluorescence intensity is stronger, and quantitative analysis can be carried out using the power of its fluorescence signal.
Following immunochromatographiassays assays experiment is carried out to the Water-soluble carbon quantum dot that embodiment 2 is prepared now:
(1) under buffer solution system, by two cyclohexyl diimines (DCC) or DIC (DIC) place Reason can be crosslinked with streptavidin, then be combined with the antibody of biotin labeling, obtain and combine the anti-of Water-soluble carbon quantum dot Body.
(2) immuno-chromatographic test paper strip includes the sample application zone, conjugate release area, reaction zone and the suction zones that set gradually;Institute State the conjugate release pad that conjugate release area is the antibody that coating is combined with Water-soluble carbon quantum dot;The reaction zone is to be divided into Test section and control zone, the reaction zone are antigen, the control zone coating dynamics that test section coating is combined with antibody Solid support.
(3) antibody for combining Water-soluble carbon quantum dot is sprayed in conjugate release pad and obtains conjugate release 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 being sprayed on immuno-chromatographic test paper strip in immune chromatography reagent kit of the present invention is directed to different detections Thing can select the antigen being adapted with detectable substance.
2nd, anti-fake mark experiment
Water-soluble carbon quantum dot prepared by embodiment 2 is added in pure water, and preparation concentration is 2mg/mL water-soluble carbon quantum Point aqueous solution 2mL, it is mixed with 5mL polyvinyl alcohol (5.0wt%), by mixed solution brush even spread to glass On piece, sheet glass is placed in 1 hour in 65 DEG C of baking ovens afterwards, takes out sheet glass and take pictures, understand that sheet glass is in nature by contrast There is no any color under light, and the visible bright green fluorescence under 365nm uviol lamps, therefore Water-soluble carbon quantum dot can be used as preventing Puppet mark.
According to the straight slope of Water-soluble carbon quantum dot structure in Fig. 2 and the ratio of the quinine sulfate point straight slope of structure Be multiplied by quinine sulfate quantum yield (quinine sulfate is standard volume, its quantum yield for 54%) can calculate it is of the invention Quantum yield is 93.2%.
Although embodiment of the present invention is disclosed as above, it is not restricted to listed in specification and implementation method With, it can be applied to various suitable the field of the invention completely, for those skilled in the art, can be easily Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited In specific details and shown here as the legend with description.

Claims (8)

1. a kind of method of orange peel synthesizing water-solubility carbon quantum dot, it is characterised in that comprise the following steps:
1) orange peel pre-treatment;
2) by volume 2~5:1 mixing deionized water and glycerine, obtains mixed solution standby;
3) orange peel that obtains pre-treatment adds the step 2) in the mixed solution that obtains, stirring;160 DEG C are placed in, instead 12h is answered, brown solution is obtained;
4) brown solution is filtered, filtrate is obtained;
5) the dialysis filtrate;
6) dialyzate evaporation is obtained into Water-soluble carbon quantum dot under constant temperature.
2. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the step 6) In, evaporation, specially rotary evaporation;Constant temperature, is 60 DEG C of constant temperature.
3. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the pre-treatment bag Include:Clean, dry, crush.
4. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the step 2) in Volume ratio is 3:1.
5. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the dialysis, tool Body is the bag filter using shearing molecular weight 1000, is dialysed 48 hours.
6. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the step 4) In, filtered using sand core funnel.
7. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the water-soluble carbon Quantum dot is applied to cell marking, fluorescence probe, anti-fake mark and immunochromatography product scope.
8. the method for orange peel synthesizing water-solubility carbon quantum dot as claimed in claim 1, it is characterised in that the pre-treatment tool Body is:Orange peel is crushed, by weight 1:1 mixing orange peel and magnetized water, in the lower 55 DEG C of boiling 3h of nitrogen atmosphere, thereto Cellulase is added, the cellulase weight is the 3% of the orange peel weight, be well mixed, 30 DEG C of holding 60min, mistake Filter, obtains filter residue;High-pressure extrusion to filter residue water content is less than 8% again;Filter residue is placed in carries out calcination treatment in stove, then naturally cold But, calcination process is toward nitrogen is passed through in stove until filter residue is cooled down, to be blanket of nitrogen in ensureing calcination process and cooling procedure stove Enclose, obtain final product through the orange peel of pre-treatment.
CN201611103828.5A 2016-12-05 2016-12-05 Method for synthesizing water-soluble carbon quantum dots from orange peels Pending CN106698393A (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN107446578A (en) * 2017-07-20 2017-12-08 中国科学院理化技术研究所 A kind of nitrogen-doped carbon quanta point material and its preparation method and application
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
CN112552904A (en) * 2020-12-17 2021-03-26 中国标准化研究院 Novel fluorescent carbon quantum dot material and synthesis method and application thereof

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CN104560036A (en) * 2014-12-30 2015-04-29 中国农业科学院农产品加工研究所 Carbon quantum dot fluorescence-labeled material adopting honey as carbon source, as well as preparation method and application thereof
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107446578A (en) * 2017-07-20 2017-12-08 中国科学院理化技术研究所 A kind of nitrogen-doped carbon quanta point material and its preparation method and application
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
CN112552904A (en) * 2020-12-17 2021-03-26 中国标准化研究院 Novel fluorescent carbon quantum dot material and synthesis method and application thereof

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