CN106916590A - A kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell - Google Patents
A kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell Download PDFInfo
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- CN106916590A CN106916590A CN201511005050.XA CN201511005050A CN106916590A CN 106916590 A CN106916590 A CN 106916590A CN 201511005050 A CN201511005050 A CN 201511005050A CN 106916590 A CN106916590 A CN 106916590A
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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 for preparing fluorescent carbon point by waste material pumpkin seeds shell, belong to nanometer material science field, the present invention prepares the carbon point of fluorescent brightness high by hydro-thermal method using the pumpkin seeds 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, it may be said that be to kill two birds with one stone.And synthetic method environmental protection, the carbon point of preparation can excite with different wave length, and launch wavelength is located at 400~600nm or so, and fluorescence signal intensity is high, and fluorescent stabilization 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 hydro-thermal method, fluorescence is prepared by waste material pumpkin seeds shell
The method of carbon point, the fluorescent carbon point fluorescence intensity of preparation is high, can apply to fluorescence imaging and fluorescent staining field.
Background technology
Carbon quantum dot is that after after the carbon family member such as CNT, carbon nano rod, diamond, fullerene, discovery has
The carbon nanomaterial of premium properties.Fluorescent carbon point has that photoluminescent property is stable, nontoxic, preparation method simple, low cost, biofacies
The advantages of capacitive is good, more and more extensive concern has been obtained in fields such as bioanalysis, photocatalysis and optics, is expected to turn into
The fluorescent material of a new generation's substitution organic fluorescence reagent and inorganic heavy metal nano material.
At present, the synthesis of fluorescent carbon point is mainly synthesized using hydro-thermal method or microwave method.Using chemical reagent Hydrothermal Synthesiss, such as
Although citric acid and various ethylenediamine hydro-thermal reactions are synthesized carbon point yield (Highly Photoluminescent high by zhu etc.
Carbon Dots for Multicolor Patterning, Sensors, and Bioimaging.Shoujun Zhu,
Qingnan Meng, Lei Wang, Junhu Zhang, Yubin Song, Han Jin, Kai Zhang, Hongchen Sun,
Haiyu Wang, and Bai Yang.Angew.Chem.Int.Ed.2013,52,3953-3957.), but raw material used
Poisonous and high cost.Natural materials are nontoxic in itself, safety, and the focus of research is turned into using natural materials synthesis carbon point.At present, profit
Synthesizing carbon point with natural materials mainly has：Silk, soymilk, egg, orange peel, pomelo peel, Folium Pterocaryae, bananas juice etc., people
On the one hand fluorescence quantum yield high is being pursued, is on the one hand pursuing low cost.Wherein carbon is prepared using the waste material in life
Point is a new bright spot, for current environmental protection, can both solve waste disposal problem, it is also possible to make full use of waste,
Play the maximum value of waste.Litchi rind Hydrothermal Synthesiss are prepared carbon point by Vidhi etc., and method is simply green non-poisonous, realizes useless
Thing utilizes (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 the method that carbon point is prepared with orange peel and pomelo peel is had been reported that in document, but with pumpkin seeds shell
Have not been reported.Melon seed cases prepare carbon point for raw material by hydro-thermal method on the south patent of the present invention.Pumpkin seeds shell is Pumpkin Seed
Crust, many kernel peeling factories largely discard as waste material, not only waste of materials but also environment have been polluted.If will return
The pumpkin seeds shell of receipts as carbon source, can both ensure with natural products as materials safety it is nontoxic the characteristics of, it is also possible to solve waste
The problem for utilizing, it may be said that be to kill two birds with one stone.And synthetic method environmental protection, the carbon point of preparation can excite with different wave length,
Launch wavelength is located at 400~600nm or so, and fluorescence signal intensity is high, fluorescent stabilization do not allow it is degradable, in fluorescence imaging, fluorescence
Sensor aspect has potential application value.
The content of the invention
The purpose of the present invention is directed to the problem of current chemical reagent synthesis toxicity and high cost, is produced in being lived using people
Raw waste pumpkin seeds shell, by hydro-thermal reaction, obtains fluorescence intensity high, good stability, fluorescence emission wavelengths model as carbon source
Enclose fluorescent carbon point wide.
1. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell, it is characterized in that：Using pumpkin seeds shell as carbon source, warp
Hydro-thermal reaction is crossed, the nano-sized carbon point of high fluorescent is obtained.The carbon point of preparation is nontoxic, and pollution-free, preparation cost is low, can be used for point
The fields such as sub- fluoroscopic examination, cell imaging.The described method comprises the following steps：
(1) pumpkin seeds shell high speed broken wall mixer is ground into superfines；
(2) superfines that will be crushed is added in reactor, adds ultra-pure water, heating response 1 to 24 hour；
(3) filtered after being cooled to room temperature, obtain brown color liquid；
(4) the brown color liquid for obtaining by supercentrifuge be centrifuged, obtain supernatant liquor, by bag filter dialysis 15 to
48 hours, you can obtain carbon dots solution.
2. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Step
(1) pumpkin seeds shell described in are the crust of common Pumpkin Seed, can be obtained by waste recovery.Homogenizer is power rotating speed
More than 40000 rpms of wall-breaking machine, powder is thinner, is more conducive to improving fluorescent brightness.
3. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Step
(2) pumpkin seeds shell described in are 1: 20~1: 500 (quality of pumpkin seeds shell: the volume of ultra-pure water) with ultra-pure water mixed proportion,
Between 150~240 DEG C, the heat time is between 1~24 hour for mixture heating-up temperature.
4. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Step
(3) filtering with microporous membrane of 0.22um is filtered into described in.
5. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell, it is characterized in that：High speed centrifugation described in step (4)
It is at least more than 8000 rpms centrifuges, supernatant is obtained after centrifugation, is 1000D~3500D with molecular cut off
Bag filter dialyse 15~48 hours, you can obtain carbon dots solution.
6. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Prepare
Carbon point there is high brightness fluorescent luminosity, can apply to the fields such as fluorescence imaging.
The advantage of the invention is that pumpkin seeds shell be life waste material, if can fully recycle, its bioluminescence into
The potential using value in image space face is huge.And preparation method is simple, low cost, the carbon point good water solubility of synthesis, fluorescent quantum are produced
Rate is high, launch wavelength scope is long, and fluorescence most strength is predominantly located at the green Region of 500nm or so, is that one kind simply prepares safe nothing
The method of malicious fluorometric reagent.
Brief description of the drawings
Accompanying drawing is fluorescence contrast picture of the carbon point under 365nm and under natural light.
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) by pumpkin seeds shell 100 grams be ground into superfines with homogenizer；
(2) superfines that will be crushed weighs 4 grams and is added in 100mL hydrothermal reaction kettles, adds ultra-pure water 75mL to mix
Sealed after conjunction, be heated to 180 DEG C and react 16 hours；
(3) sample after (2) have been reacted is filtered after being cooled to room temperature, obtains brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by the supercentrifuge of 8000 revs/min of rotating speed, obtains supernatant liquor.
By supernatant liquor by molecular cut off for the bag filter of 500D~1000D is dialysed 48 hours, you can obtain carbon dots solution.
Embodiment 2
(1) by pumpkin seeds shell 100 grams be ground into superfines with homogenizer；
(2) superfines that will be crushed weighs 4 grams and is added in 100mL hydrothermal reaction kettles, adds ultra-pure water 75mL to mix
Sealed after conjunction, be heated to 180 DEG C and react 24 hours；
(3) sample after (2) have been reacted is filtered after being cooled to room temperature, obtains brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by the supercentrifuge of 8000 revs/min of rotating speed, obtains supernatant liquor.
By supernatant liquor by molecular cut off for the bag filter of 500D~1000D is dialysed 48 hours, you can obtain carbon dots solution.
During 180 DEG C of preferred heating-up temperature, the reaction time is 24 hours.
Embodiment 3
(1) by pumpkin seeds shell 100 grams be ground into superfines with mixer；
(2) superfines that will be crushed weighs 4 grams and is added in 100mL hydrothermal reaction kettles, adds ultra-pure water 75mL to mix
Sealed after conjunction, be heated to 220 DEG C and react 12 hours；
(3) sample after (2) have been reacted is filtered after being cooled to room temperature, obtains brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by the supercentrifuge of 8000 revs/min of rotating speed, obtains supernatant liquor.
By supernatant liquor by molecular cut off for the bag filter of 500D~1000D is dialysed 48 hours, you can obtain carbon dots solution.
Embodiment 4
(1) by pumpkin seeds shell 100 grams be ground into superfines with homogenizer；
(2) superfines that will be crushed weighs 8 grams and is added in 100mL hydrothermal reaction kettles, adds ultra-pure water 75mL to mix
Sealed after conjunction, be heated to 220 DEG C and react 24 hours；
(3) sample after (2) have been reacted is filtered after being cooled to room temperature, obtains brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by the supercentrifuge of 8000 revs/min of rotating speed, obtains supernatant liquor.
By supernatant liquor by molecular cut off for the bag filter of 500D~1000D is dialysed 48 hours, you can obtain 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, carbonization
Degree is weaker.Select suitable carburizing temperature most important to the yield impact that reacts, in 220 DEG C of heating-up temperature, preferably
Reaction time is 12 hours.
Embodiment 5
(1) by pumpkin seeds shell 100 grams be ground into superfines with homogenizer；
(2) superfines that will be crushed weighs 8 grams and is added in 100mL hydrothermal reaction kettles, adds ultra-pure water 75mL to mix
Sealed after conjunction, be heated to 220 DEG C and react 12 hours；
(3) sample after (2) have been reacted is filtered after being cooled to room temperature, obtains brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by the supercentrifuge of 8000 revs/min of rotating speed, obtains supernatant liquor.
By supernatant liquor by molecular cut off for the bag filter of 500D~1000D is dialysed 48 hours, you can obtain carbon dots solution.
Selecting suitable concentration has certain influence on yield, and in 180~200 DEG C of heating-up temperature, it is 4 grams preferably to feed intake
75~80mL of powder water distribution.
The yield of carbon point is influenceed by three factors of reaction time and temperature and concentration, obtains anti-after preferably three conditions
With temperature and the optimum value of concentration, 220 DEG C of reaction temperature between seasonable, 12 hours reaction time, concentration is the superfine powder for crushing
Last quality is 1: 20 with water volume ratio.
Fluorescence imaging experiments：
Embodiment 6
Absorbed with pen as ink after the carbon dots solution dilution that will be prepared in embodiment 5, ultraviolet after being mapped on paper
Taken pictures under lamp, obtain fluorescence picture.
Claims (6)
1. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell, it is characterized in that：Using pumpkin seeds shell as carbon source, by water
Thermal response, obtains the nano-sized carbon point of high fluorescent.The carbon point of preparation is nontoxic, and pollution-free, preparation cost is low, can be used for molecule glimmering
The fields such as light detection, cell imaging.The described method comprises the following steps：
(1) pumpkin seeds shell high speed broken wall mixer is ground into superfines；
(2) the superfine powder art that will be crushed is added in reactor, adds ultra-pure water, heating response 1 to 24 hour；
(3) filtered after being cooled to room temperature, obtain brown color liquid；
(4) the brown color liquid for obtaining is centrifuged by supercentrifuge, obtains supernatant liquor, small by bag filter dialysis 15 to 48
When, you can obtain carbon dots solution.
2. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Step (1)
Described in pumpkin seeds shell be common Pumpkin Seed crust, can be obtained by waste recovery.Homogenizer is power rotating speed
More than 40000 rpms of wall-breaking machine, powder is thinner, is more conducive to improving fluorescent brightness.
3. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：Step (2)
Described in pumpkin seeds shell and ultra-pure water mixed proportion be 1: 20~1: the 500 (quality of pumpkin seeds shell：The volume of ultra-pure water), mixing
Between 150~240 DEG C, the heat time is between 1~24 hour for thing heating-up temperature.
4. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds 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.
5. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell, it is characterized in that：High speed centrifugation described in step (4) be to
Few more than 8000 rpms centrifuges, obtain supernatant after centrifugation, be the saturating of 1000D~3500D with molecular cut off
Analysis bag is dialysed 15~48 hours, you can obtain carbon dots solution.
6. a kind of method that fluorescent carbon point is prepared by waste material pumpkin seeds shell as claimed in claim 1, it is characterized in that：The carbon of preparation
Point has high brightness fluorescent luminosity, can apply to the fields such as fluorescence imaging.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113287604A (en) * | 2021-04-21 | 2021-08-24 | 泉州市旭丰粉体原料有限公司 | Biomass antibacterial mildew preventive, incense stick containing biomass antibacterial mildew preventive and preparation method of biomass antibacterial mildew preventive |
| CN114854402A (en) * | 2022-03-22 | 2022-08-05 | 桂林师范高等专科学校 | Preparation method of fluorescent nano material capable of promoting growth of cherokee rose group culture seedling |
| CN115247063A (en) * | 2021-04-27 | 2022-10-28 | 郑州大学 | Red carbon quantum dot based on eggshell and preparation method and application thereof |
| CN116103042A (en) * | 2023-01-16 | 2023-05-12 | 河北大学 | Preparation method of fluorescent carbon quantum dot with castor seeds as carbon source |
-
2015
- 2015-12-28 CN CN201511005050.XA patent/CN106916590A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113287604A (en) * | 2021-04-21 | 2021-08-24 | 泉州市旭丰粉体原料有限公司 | Biomass antibacterial mildew preventive, incense stick containing biomass antibacterial mildew preventive and preparation method of biomass antibacterial mildew preventive |
| CN115247063A (en) * | 2021-04-27 | 2022-10-28 | 郑州大学 | Red carbon quantum dot based on eggshell and preparation method and application thereof |
| CN114854402A (en) * | 2022-03-22 | 2022-08-05 | 桂林师范高等专科学校 | Preparation method of fluorescent nano material capable of promoting growth of cherokee rose group culture seedling |
| CN116103042A (en) * | 2023-01-16 | 2023-05-12 | 河北大学 | Preparation method of fluorescent carbon quantum dot with castor seeds as carbon source |
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Application publication date: 20170704 |