CN110437830A - It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot - Google Patents
It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot Download PDFInfo
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Abstract
The invention discloses a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot, which is characterized in that is pre-processed using hydrochloric acid and potassium metaperiodate solution to buckwheat shell powder, obtains pretreatment buckwheat shell powder；Then, in with reaction kettle in polytetrafluoroethylene bushing, it is added by following composition mass percent, 1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 64 ~ 68%, pretreatment buckwheat shell powder: 24 ~ 28%, thioacetamide: 6 ~ 10%, temperature reacts 24 ~ 28h in 120 ± 2 DEG C of constant temperature, brown viscous transparency liquid is obtained, is crude product sulphur phosphor codoping carbon quantum dot；Sulphur phosphor codoping carbon quantum dot is purified to obtain using dialysis.The preparation method has environmentally protective, it is easy to operate, the features such as sulphur nitrogen boron codope carbon quantum dot composite material does not need secondary modification both and can have that fluorescence property stability is high, size is small and uniform, good biocompatibility, the quantum yield of sulphur phosphor codoping carbon quantum dot improves nearly 88%.
Description
Technical field
The invention belongs to nano luminescent material preparation technical fields, in particular to a kind of to be co-doped with by carbon source sulphur phosphorus of buckwheat shell
The preparation method and application of miscellaneous carbon quantum dot.
Background technique
For carbon quantum dot as a kind of emerging nano material, carbon quantum dot (C-Dots) has bio-compatibility good and nothing
Poison, the advantages that partial size is small, emission spectrum is adjustable, fluorescent stability is high and resistance to photobleaching, raw material is cheap in addition and abundance, easily
In the preparation and modification the features such as, make that its is prepared and application becomes one of the hot research field of analytical chemistry in recent years.However, mesh
The preceding research in relation to fluorescence C-Dots nano material is also in initial stage, and there are still some Scientific Research Problems urgently to be resolved, such as
The yield and fluorescence quantum yield (QY) of existing synthetic method are often relatively low, can not accurately control its lateral dimension and come to the surface
It learns, luminous mechanism is indefinite, fluorescence spectra is narrow etc..Therefore, there is also huge development spaces for the research field.
For carbon quantum dot in addition to itself having and being widely applied, the research based on carbon quantum dot composite material is also current hot spot
Project.Composite material is combined by two or more different materials, and every kind of composition material mutually cooperates with, and is not only sent out
Respective advantage is waved, new performance can be also possessed.Therefore, the research based on carbon quantum dot composite material is carbon quantum dot functionalization
An important topic.Carbon quantum dot is the nano material using carbon as skeleton structure, is that a kind of dispersion, size are less than 10nm
Spherical nano particle generally comprises Nano diamond, carbon particle and graphene quantum dot, and also referred to as carbon dots, carbon nano dot, carbon is received
Meter Jing.Similar with various metal quantum points, carbon quantum dot can issue bright fluorescence under light conditions.Carbon quantum dot is glimmering
Most important one kind in light carbon nanomaterial, it has unique small size property and superior photoluminescent property；Carbon quantum dot is glimmering
Bright position, stabilization, exciting light spectrum width, emission spectrum is narrow, and launch wavelength can by change material particle size and composition come
Regulation, unglazed bleaching phenomenon, certain carbon quantum dots are in addition, up-conversion fluorescence characteristic.In order to which synthesising biological compatibility is good, toxicity
Carbon quantum dot low, fluorescence is strong is selected organic naturally raw with promoting carbon quantum dot to be able to develop and apply in field of biomedicine
It is more desirable that object makees carbon source synthesis carbon quantum dot.
The advantages of other solvents that ionic liquid has are unable to reach has high thermal stability and chemical stability；Steam
Pressure is very small, non-volatile；It is easy to recycle and reuse；Conductivity is high；It is adjusted to inorganic in the characteristics of passing through zwitterion
The dissolubility of object, water, organic matter and polymer；To good solvability at all performances of big quantity of material, ionic liquid can be molten
Solve polymer substance, and it is nontoxic, non-volatile be also easy to recycle, this applies to ionic liquid and opens in plant cellulose research field
New direction has been warded off, while also having brought opportunity to fiber nano material industrial expansion.
Therefore the two big main problems that shortage of resources and environmental pollution have become the world today utilize natural reproducible
Resource, the inexorable trend of sustainable development will be become by developing environmentally friendly product and technology.Modern science thinks, " middle traditional Chinese medicines
Plant title block " it carries and releases: " buckwheat shell contains a large amount of rutin sophorin glucoside, the activity with vitamin, cellulose rich in goes back band
There is dentate abundant.Buckwheat shell be used as photocatalyst carrier have many advantages, such as it is renewable, degradable, environmentally friendly close friend, it is cheap, be
Important living resources will greatly improve the utilization efficiency of buckwheat shell.
The application is using buckwheat shell as carbon source, using thioacetamide as sulphur source, nitrogen source, with 1- ethyl -2,3- methylimidazole
Hexafluoro microcosmic salt is solvent and phosphorus source, prepares a kind of sulphur phosphor codoping carbon quantum dot composite material using without water-soluble dissolution method.
Summary of the invention
The purpose of the present invention is to provide a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot.
It is a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot, which is characterized in that this method has
Following processing step:
(1) buckwheat shell powder pre-processes: in the reactor, it is added by following composition mass percent, the hydrochloric acid solution of 3.0mol/L:
78 ~ 82%, potassium metaperiodate: 4 ~ 8%, dissolution adds buckwheat shell powder: 12 ~ 16%, the sum of each component is absolutely soaking at room temperature
8h, then 30min is boiled, it is washed with deionized after cooling to neutrality, is separated by solid-liquid separation, then be washed with deionized to neutrality, done
It is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, by following composition
Mass percent is added, 1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 64 ~ 68%, pretreatment buckwheat shell powder: and 24 ~ 28%, sulphur
For acetamide: 6 ~ 10%, the sum of each component is absolutely, to stir evenly, cover sealing cover, be placed in insulating box, temperature exists
120 ± 2 DEG C of constant temperature react 24 ~ 28h, obtain brown viscous transparency liquid, are crude product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
The buckwheat skin powder is that mature native buckwheat shelling obtains buckwheat shell through crushing, with 300 purposes in step (1)
Sieve obtains buckwheat shell powder.
The fluorescence quantum yield of prepared sulphur phosphor codoping carbon quantum dot is 34.26%, and quantum yield is high.In wavelength
Under the excitation wavelength of 435nm, the fluorescence (518 nm) that can succeed in sending up out.
The beneficial effects of the present invention are:
The application, as solvent and doping phosphorus source, dissolves day using 1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt ionic liquid
Right high molecular material buckwheat shell is carbon source, and the natural regeneration utilization of resources is environmentally protective, easy to operate, sulphur phosphor codoping carbon quantum
The features such as point does not need secondary modification both and can have that fluorescence property stability is high, size is small and uniform, good biocompatibility, sulphur
Phosphor codoping makes the fluorescence property (quantum yield) of carbon quantum dot can be improved nearly 88%.
Detailed description of the invention
Fig. 1 is the transmission electron microscope picture of sulphur phosphor codoping carbon quantum dot prepared by the application.
Fig. 2 is the fluorescence emission spectrogram of compound of various concentration sulphur phosphor codoping carbon quantum dot prepared by the application；
In figure curve be from top to bottom be that sulphur phosphor codoping carbon quantum dot concentration is respectively as follows: curve a:100, curve b:75, curve
C:40, (μm ol/L).
Specific embodiment
Embodiment 1
(1) buckwheat shell powder pre-processes: it in the reactor, is separately added into, the hydrochloric acid solution of 3.0mol/L: 80mL, and potassium metaperiodate:
6g, dissolution, adds buckwheat shell powder: 14g, soaking at room temperature 8h, then boil 30min, is washed with deionized after cooling to neutrality,
It is separated by solid-liquid separation, then is washed with deionized to neutrality, it is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 66g, pre-process buckwheat shell powder: 26g, thioacetamide: 8g is stirred evenly,
Sealing cover is covered, is placed in insulating box, temperature reacts 25h, obtain brown viscous transparency liquid, be thick in 120 ± 2 DEG C of constant temperature
Product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
Embodiment 2
(1) buckwheat shell powder pre-processes: it in the reactor, is separately added into, the hydrochloric acid solution of 3.0mol/L: 79mL, and potassium metaperiodate:
5g, dissolution, adds buckwheat shell powder: 16g, soaking at room temperature 8h, then boil 30min, is washed with deionized after cooling to neutrality,
It is separated by solid-liquid separation, then is washed with deionized to neutrality, it is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 67g, pre-process buckwheat shell powder: 27g, thioacetamide: 6g is stirred evenly,
Sealing cover is covered, is placed in insulating box, temperature reacts 26h, obtain brown viscous transparency liquid, be thick in 120 ± 2 DEG C of constant temperature
Product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
Embodiment 3
(1) buckwheat shell powder pre-processes: it in the reactor, is separately added into, the hydrochloric acid solution of 3.0mol/L: 78mL, and potassium metaperiodate:
7g, dissolution, adds buckwheat shell powder: 13g, soaking at room temperature 8h, then boil 30min, is washed with deionized after cooling to neutrality,
It is separated by solid-liquid separation, then is washed with deionized to neutrality, it is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 66g, pre-process buckwheat shell powder: 24g, thioacetamide: 10g is stirred evenly,
Sealing cover is covered, is placed in insulating box, temperature for 24 hours, obtains brown viscous transparency liquid, be thick in 120 ± 2 DEG C of constant temperature, reaction
Product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
Embodiment 4
(1) buckwheat shell powder pre-processes: it in the reactor, is separately added into, the hydrochloric acid solution of 3.0mol/L: 79mL, and potassium metaperiodate:
4g, dissolution, adds buckwheat shell powder: 15g, soaking at room temperature 8h, then boil 30min, is washed with deionized after cooling to neutrality,
It is separated by solid-liquid separation, then is washed with deionized to neutrality, it is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, being separately added into,
1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 65g, pre-process buckwheat shell powder: 28g, thioacetamide: 7g is stirred evenly,
Sealing cover is covered, is placed in insulating box, temperature reacts 28h, obtain brown viscous transparency liquid, be thick in 120 ± 2 DEG C of constant temperature
Product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
Embodiment 5
The measurement of sulphur phosphor codoping carbon quantum dot fluorescent yield: it has selected reference method: having selected dilute sulfuric acid for solvent, by quinine sulfate
It is dissolved in 0.1mol/LH2SO4In solution (solubility that quinine sulfate can be increased) formed quinine sulfate acid solution, then in
Carbon nano dot and quinine sulfate acid solution are measured in ultraviolet-uisible spectrophotometer in the absorbance of fixed excitation wave strong point.Finally
The fluorescence emission spectrogram of compound of carbon nano dot and quinine sulfate acid solution under given excitation wavelength is measured in Fluorescence Spectrometer, is obtained
To fluorescence integral area.Fluorescence quantum yield is calculated according to formula:
WhereinRepresent the quantum yield for the determinand being calculated；I be measure determinand fluorescence integral area (coupling it is glimmering
Luminous intensity), θ represents the refractive index of the solvent of sample to be tested substance.Represent the quantum yield of object of reference；Is representative measures
The fluorescence integral area (fluorescence intensity of coupling) of object of reference；δ represents the refractive index of the solvent of the object of reference measured, passes through survey
The carbon quantum dot undoped with sulphur nitrogen boron is measured under the excitation wavelength of 435nm, the quantum for the fluorescence (518 nm) that can be succeeded in sending up out
Yield is 18.22%, and the fluorescence quantum yield of sulphur nitrogen boron codope carbon quantum dot composite material is 34.26%, and quantum yield mentions
Height nearly 88%.
Claims (3)
1. a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot, which is characterized in that this method have with
Lower processing step:
(1) buckwheat shell powder pre-processes: in the reactor, it is added by following composition mass percent, the hydrochloric acid solution of 3.0mol/L:
78 ~ 82%, potassium metaperiodate: 4 ~ 8%, dissolution adds buckwheat shell powder: 12 ~ 16%, the sum of each component is absolutely soaking at room temperature
8h, then 30min is boiled, it is washed with deionized after cooling to neutrality, is separated by solid-liquid separation, then be washed with deionized to neutrality, done
It is dry, obtain pretreatment buckwheat shell powder；
(2) preparation of crude product sulphur phosphor codoping carbon quantum dot: in reaction kettle in polytetrafluoroethylene bushing, by following composition
Mass percent is added, 1- ethyl -2,3- methylimidazole hexafluoro microcosmic salt: 64 ~ 68%, pretreatment buckwheat shell powder: and 24 ~ 28%, sulphur
For acetamide: 6 ~ 10%, the sum of each component is absolutely, to stir evenly, cover sealing cover, be placed in insulating box, temperature exists
120 ± 2 DEG C of constant temperature react 24 ~ 28h, obtain brown viscous transparency liquid, are crude product sulphur phosphor codoping carbon quantum dot；
(3) preparation of sulphur phosphor codoping carbon quantum dot: the solution that step (2) obtains being injected into bag filter and is dialysed,
Molecular cut off is 800D, and dialysis time is for 24 hours, to change a water at interval of 2h；Dialysis product is evaporated, is concentrated
Solution；Concentrate solution carries out quick freeze, freeze-drying to powdered, acquisition sulphur phosphor codoping carbon quantum under the conditions of -20 DEG C
Point.
2. it is according to claim 1 a kind of using buckwheat shell as the preparation method of carbon source sulphur phosphor codoping carbon quantum dot, it is special
Sign is that buckwheat skin powder as described in step (1) is that mature native buckwheat shelling obtains buckwheat shell through crushing, with the sieve of 300 mesh
Son sieving, obtains buckwheat shell powder.
3. according to claim 1 a kind of using buckwheat shell as prepared by the preparation method of carbon source sulphur phosphor codoping carbon quantum dot
Sulphur phosphor codoping carbon quantum dot.
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| CN117402549A (en) * | 2023-10-16 | 2024-01-16 | 江苏众立生包装科技有限公司 | Method for synthesizing fluorescent anti-counterfeiting paint by using carbon quantum dot modified waterborne polyurethane with coconut shell as precursor |
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Application publication date: 20191112 |