CN106916589A - A kind of method that fluorescent carbon point is prepared by waste material longan shell - Google Patents
A kind of method that fluorescent carbon point is prepared by waste material longan shell Download PDFInfo
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- CN106916589A CN106916589A CN201511005048.2A CN201511005048A CN106916589A CN 106916589 A CN106916589 A CN 106916589A CN 201511005048 A CN201511005048 A CN 201511005048A CN 106916589 A CN106916589 A CN 106916589A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a kind of method that fluorescent carbon point is prepared by waste material longan shell, belong to nanometer material science field, the present invention prepares the carbon point of fluorescent brightness high by high temperature pyrolytic cracking (HTP) using the longan shell that reclaims as carbon source.The method can both ensure with natural products as materials safety it is nontoxic the characteristics of, it is also possible to solve the problems, such as twice laid, and follow-up purification process is simple and convenient, it is not necessary to using being centrifuged and dialysis step, solve the problems, such as that the purifying of carbon point is cumbersome.Preparation method environmental protection, the carbon point fluorescent stabilization of preparation is not allowed degradable, has potential application value in terms of fluorescence imaging, phosphor pattern making.
Description
Technical field
The present invention relates to nanometer material science field, and in particular to by high temperature pyrolytic cracking (HTP), fluorescent carbon point is prepared by waste material longan shell
Method, the fluorescent carbon point fluorescence intensity of preparation is high, can apply to fluorescence imaging and fluorescent staining field.
Background technology
Carbon quantum dot be after after the carbon family member such as CNT, carbon nano rod, diamond, fullerene, discovery with excellent
The carbon nanomaterial of performance.Fluorescent carbon point has that photoluminescent property is stable, nontoxic, preparation method simple, low cost, bio-compatible
Property it is good the advantages of, obtained more and more extensive concern in fields such as bioanalysis, photocatalysis and optics, be expected to turn into new
A generation replaces the fluorescent material of organic fluorescence reagent and inorganic heavy metal nano material.
At present, the synthesis of fluorescent carbon point mainly uses hydro-thermal method and microwave method.Hydro-thermal method is mainly limited by reaction yield is low, microwave
Method can only be directed to relatively more special reactant, and the general microwave method of natural materials carbon source prepares difficult.High temperature pyrolytic cracking (HTP) is due to simple
Convenient, general carbon source is not limited by method, therefore is also a kind of conventional carbon point preparation method.Using natural materials as carbon
Both natural environmental-protective is nontoxic in source, and cost is again low, wherein it is a new bright spot that carbon point is prepared using the waste material in life, for working as
Modern environmental protection, can both solve waste disposal problem, it is also possible to make full use of waste, play the maximum value of waste.Vidhi
Carbon point is prepared Deng by litchi rind Hydrothermal Synthesiss, method is simply green non-poisonous, realize twice laid (Green synthesis of
Fluorescent carbon nanoparticles from Lychee (Litchi chinensis) plant.Vidhi Chaudhary, Anil
Kumar Bhowmick.Korean J.Chem.Eng., 2015,32 (8), 1707-1711).Also had been reported that in document with orange peel and
The method that pomelo peel prepares carbon point, but had not been reported with the method that longan shell prepares carbon point.Patent of the present invention is with longan shell as former
Material prepares carbon point by high temperature pyrolytic cracking (HTP).Longan shell is the crust of longan pulp, and many kernel peeling factories are big as waste material
Amount is discarded, and not only waste of materials but also environment has been polluted.If the longan shell that will be reclaimed can both ensure with natural as carbon source
The characteristics of product is nontoxic materials safety, it is also possible to solve the problems, such as twice laid, it may be said that be to kill two birds with one stone.And synthetic method
Environmental protection, subsequent purification treatment is simple, and fluorescent stabilization is not allowed degradable, has in terms of fluorescence imaging, fluorescent optical sensor latent
Application value.
The content of the invention
The purpose of the present invention is directed to the problem that current carbon point preparation cost is high, post processing is cumbersome, the waste produced in being lived using people
Used as carbon source, by high temperature pyrolysis reaction, by simple second alcohol and water extracting and washing, filtering with microporous membrane removes big longan shell
Granule foreign, obtains fluorescence property Stable Carbon point.
1. a kind of method that fluorescent carbon point is prepared by waste material longan shell, it is characterized in that：Using longan shell as carbon source, by after crushing
High temperature pyrolysis reaction is carried out, the nano-sized carbon point of high fluorescent is obtained.The carbon point of preparation is nontoxic, and pollution-free, preparation cost is low,
Twice laid is realized, can be used for the fields such as fluorescence imaging.The described method comprises the following steps：
(1) longan shell homogenizer is ground into superfines；
(2) superfines that will be crushed is added in Muffle furnace, and 350~460 DEG C of high-temperature heating reacts 1~5 hour；
(3) powder is ground into after being cooled to room temperature, is extracted with absolute ethyl alcohol, be filtrated to get brown color liquid；
(4) the brown color liquid that will be obtained boils off solvent, the powder for obtaining after with deionized water dissolving, by 0.22um's
Filtering with microporous membrane, you can obtain carbon dots solution.
2. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (1)
Described in longan shell be common longan pulp crust, can be obtained by waste recovery.Homogenizer is power rotating speed 40000
Wall-breaking machine more than rpm, powder is thinner, is more conducive to improving fluorescent brightness.
3. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (2)
Described in Muffle furnace heating-up temperature between 350~460 DEG C, the heat time is between 1~5 hour.
4. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (3)
Described in be filtered into the filtering with microporous membrane of 0.22um, remove the impurity of bulky grain.
5. a kind of method that fluorescent carbon point is prepared by waste material longan shell, it is characterized in that：Step heats vapo(u)rizing temperature described in (4)
Below 60 DEG C, using decompression rotary evaporation method.Extracting and washing step (3) and step (4) can be repeated, with
Obtain pure carbon point product.
6. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：The carbon point of preparation
With high brightness fluorescent luminosity, the fields such as fluorescence imaging are can apply to.
The advantage of the invention is that longan shell is life waste material, if can fully recycle, it has in terms of bioluminescence imaging
There is potential application value.And preparation method and subsequent purification treatment is simple, low cost, it is that a kind of simple to prepare safety non-toxic glimmering
The method of light reagent.
Brief description of the drawings
The fluorescence imaging picture of accompanying drawing carbon dots solution
Specific embodiment
Implementation below specifically further elucidates the content of invention, but is not limited to these embodiments.
The preparation of fluorescent carbon point：
Embodiment 1
(1) superfines will be ground into high speed broken wall mixer after longan shell cleaning, drying；
(2) 5 grams of superfines are weighed to be added in Muffle furnace, 400 DEG C is heated to and is reacted 1 hour；
(3) sample after (2) have been reacted grinds to form fine powder after being cooled to room temperature, is stirred 24 hours after adding absolute ethyl alcohol,
0.22um filtering with microporous membrane is used, brown color liquid is obtained；
(4) the brown color liquid for obtaining obtains powder by decompression rotary evaporation after removing solvent.The powder for obtaining spend again from
Sub- water is stirred 24 hours, then uses 0.22um filtering with microporous membrane, obtains carbon dots solution.
Embodiment 2
(1) superfines will be ground into high speed broken wall mixer after longan shell cleaning, drying；
(2) 5 grams of superfines are weighed to be added in Muffle furnace, 400 DEG C is heated to and is reacted 2 hours；
(3) sample after (2) have been reacted grinds to form fine powder after being cooled to room temperature, is stirred 24 hours after adding absolute ethyl alcohol,
0.22um filtering with microporous membrane is used, brown color liquid is obtained；
(4) the brown color liquid for obtaining obtains powder by decompression rotary evaporation after removing solvent.The powder for obtaining spend again from
Sub- water is stirred 24 hours, then uses 0.22um filtering with microporous membrane, obtains carbon dots solution.
Reaction time is different, and carbonizing degree is different, and the reaction time is more long, and carbonizing degree is stronger, and the reaction time is shorter, and be carbonized journey
Degree is weaker.Select suitable carbonization time most important to the yield impact that reacts, it is preferred anti-in 400 DEG C of heating-up temperature
It is 2 hours between seasonable.
Embodiment 3
(1) superfines will be ground into high speed broken wall mixer after longan shell cleaning, drying；
(2) 5 grams of superfines are weighed to be added in Muffle furnace, 400 DEG C is heated to and is reacted 2 hours；
(3) sample after (2) have been reacted grinds to form fine powder after being cooled to room temperature, is stirred 24 hours after adding absolute ethyl alcohol,
0.22um filtering with microporous membrane is used, brown color liquid is obtained；
(4) the brown color liquid for obtaining obtains powder by decompression rotary evaporation after removing solvent.The powder for obtaining spend again from
Sub- water is stirred 24 hours, then uses 0.22um filtering with microporous membrane, obtains carbon dots solution.
Embodiment 4
(1) superfines will be ground into high speed broken wall mixer after longan shell cleaning, drying；
(2) 5 grams of superfines are weighed to be added in Muffle furnace, 430 DEG C is heated to and is reacted 2 hours；
(3) sample after (2) have been reacted grinds to form fine powder after being cooled to room temperature, is stirred 24 hours after adding absolute ethyl alcohol,
0.22um filtering with microporous membrane is used, brown color liquid is obtained；
(4) the brown color liquid for obtaining obtains powder by decompression rotary evaporation after removing solvent.The powder for obtaining spend again from
Sub- water is stirred 24 hours, then uses 0.22um filtering with microporous membrane, obtains carbon dots solution.
Reaction temperature is different, and carbonizing degree is different, and reaction temperature is higher, and carbonizing degree is stronger, and reaction temperature is lower, and be carbonized journey
Degree is weaker.Select suitable carburizing temperature most important to the yield impact of reaction, heating response 2 hours, preferable reaction temperature
430℃。
The yield of carbon point is influenceed by three factors of reaction time and temperature and concentration, and the reaction time is obtained after preferably three conditions
With temperature and the optimum value of concentration, 430 DEG C of reaction temperature, 2 hours reaction time.
Fluorescence imaging experiments：
Embodiment 5
Absorbed with pen as ink after the carbon dots solution dilution that will be prepared in embodiment 4, clapped under uviol lamp after being mapped on paper
According to obtaining fluorescence picture.
Picture illustrates that the carbon point for preparing has good application value in terms of fluorescence labeling as shown in accompanying drawing.
Claims (6)
1. a kind of method that fluorescent carbon point is prepared by waste material longan shell, it is characterized in that：Using longan shell as carbon source, by after crushing
High temperature pyrolysis reaction is carried out, the nano-sized carbon point of high fluorescent is obtained.The carbon point of preparation is nontoxic, and pollution-free, preparation cost is low,
Twice laid is realized, can be used for the fields such as fluorescence imaging.The described method comprises the following steps：
(1) longan shell homogenizer is ground into superfines；
(2) superfines that will be crushed is added in Muffle furnace, and 350~460 DEG C of high-temperature heating reacts 1~5 hour；
(3) powder is ground into after being cooled to room temperature, is extracted with absolute ethyl alcohol, be filtrated to get brown color liquid；
(4) the brown color liquid that will be obtained boils off solvent, the powder for obtaining after with deionized water dissolving, by 0.22um's
Filtering with microporous membrane, you can obtain carbon dots solution.
2. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (1)
Described in longan shell be common longan pulp crust, can be obtained by waste recovery.Homogenizer is power rotating speed 40000
Wall-breaking machine more than rpm, powder is thinner, is more conducive to improving fluorescent brightness.
3. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (2)
Described in Muffle furnace heating-up temperature between 350~460 DEG C, the heat time is between 1~5 hour.
4. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：Step (3)
Described in be filtered into the filtering with microporous membrane of 0.22um, remove the impurity of bulky grain.
5. a kind of method that fluorescent carbon point is prepared by waste material longan shell, it is characterized in that：Step heats vapo(u)rizing temperature described in (4)
Below 60 DEG C, using decompression rotary evaporation method.Extracting and washing step (3) and step (4) can be repeated, with
Obtain pure carbon point product.
6. a kind of method that fluorescent carbon point is prepared by waste material longan shell as claimed in claim 1, it is characterized in that：The carbon point of preparation
With high brightness fluorescent luminosity, the fields such as fluorescence imaging are can apply to.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109181689A (en) * | 2018-09-26 | 2019-01-11 | 东华大学 | A kind of preparation method of photochromic adjustable hydrophobicity N doping fluorescent carbon point |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Cork oak acorn-cup base carbon quantum dot and its application on fluorescent ink are prepared using cork oak acorn-cup |
| CN109504377A (en) * | 2018-12-26 | 2019-03-22 | 南京林业大学 | Cork oak shell base carbon quantum dot and its application on fluorescent ink are prepared using cork oak shell |
| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN116285968A (en) * | 2022-12-06 | 2023-06-23 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
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2015
- 2015-12-28 CN CN201511005048.2A patent/CN106916589A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109181689A (en) * | 2018-09-26 | 2019-01-11 | 东华大学 | A kind of preparation method of photochromic adjustable hydrophobicity N doping fluorescent carbon point |
| CN109181689B (en) * | 2018-09-26 | 2021-09-21 | 东华大学 | Preparation method of photochromic adjustable hydrophobic nitrogen-doped fluorescent carbon dots |
| CN109336087A (en) * | 2018-12-26 | 2019-02-15 | 南京林业大学 | Cork oak acorn-cup base carbon quantum dot and its application on fluorescent ink are prepared using cork oak acorn-cup |
| CN109504377A (en) * | 2018-12-26 | 2019-03-22 | 南京林业大学 | Cork oak shell base carbon quantum dot and its application on fluorescent ink are prepared using cork oak shell |
| CN109593524A (en) * | 2018-12-26 | 2019-04-09 | 南京林业大学 | Use radiation loose wire preparation Water-soluble carbon quantum dot and the method and its application of fluorescent ink |
| CN116285968A (en) * | 2022-12-06 | 2023-06-23 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
| CN116285968B (en) * | 2022-12-06 | 2024-03-15 | 延安大学 | Cerium-nitrogen co-doped biomass carbon quantum dot and preparation method and application thereof |
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