CN107601457A - A kind of method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method - Google Patents
A kind of method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method Download PDFInfo
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Abstract
The invention belongs to field of material synthesis technology, a kind of method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method, step is as follows：Bagasse 7h of high temperature cabonization 2 at 300 700 DEG C, the black solid after being carbonized, is ground into black powder；Black powder is dispersed in acetic acid and 30wt% hydrogen peroxide, ultrasound, is heated to reflux 6 24h under 100 140 DEG C of temperature conditionss, cools down；Solution filters, and removes large granular impurity and the complete solid matter of unreacted；10 60min are centrifuged under 4000 12000r/min revolutions, supernatant 12 48h of dialysis, obtain the carbon quantum dot aqueous solution.The preparation process of the present invention is simple, is not required to special instrument equipment, product is without cumbersome post processing；Preparation condition is gentle, without using strong acid and strong base and other poisonous and harmful substances；The carbon quantum dot prepared has good surface topography and high fluorescent.
Description
Technical field
The invention belongs to field of material synthesis technology, is related to one kind and prepares carbon by utilization of carbon source chemical oxidization method of bagasse
The method of quantum dot.
Background technology
Bagasse is the Main By product of sugar industry, and sugarcane forms bagasse after squeezing, often produces 1 ton of sugarcane
Sugar will produce about 1 ton of bagasse.Bagasse typically contains dry 90%~92%, wherein thick protein 1.5%, crude fibre
44%~46%, crude fat 0.7%, NFE 42%, coarse ash 2%~3%；Without SO2And crude fibre therein
Cellulose containing about 46%, the lignin of 25% hemicellulose 20%, and about 9% other materials, it is a kind of cleaning, excellent
Matter, the biomass energy of sustainable development.Compared to crop material, bagasse has seldom residues of pesticides, but due to bagasse
Degree of lignification is high, the reason such as nutrient is uncoordinated, along with the backwardness of trans-utilization technological means, cause bagasse substantially
All go out of use do not have to or it is most be only used for doing fuel, so utilization rate of the bagasse in China is still very low.This is not only
A kind of waste of resource, and bagasse can also produce CO during burning2Isothermal chamber gas pollutes to environment, enters
One step endangers to the health care belt of humans and animals.
Carbon quantum dot is a kind of nano material of zero dimension, and it refers to that radius is less than or close to the rail in excitation state electronics
The semiconductor nano of road radius.Carbon quantum dot has good fluorescent stability, after laser prolonged exposure a few hours,
Its fluorescence intensity does not change substantially, and photobleaching will not also occur.The cytotoxicity of other carbon quantum dot is low, biocompatibility
Well.Because there is much free group (such as hydroxyl, carboxyl) on carbon quantum dot surface, it is easy to functional modification.With biography
System organic fluorescent dye is compared, and carbon quantum dot also has the characteristics such as upper converting photoluminescent.These characteristics cause carbon quantum dot to exist
Photocatalysis, photoelectricity, biotechnology field have a wide range of applications.
The main method for being presently used for preparing carbon quantum dot has chemical oxidization method, electrochemical stripping method, hydro-thermal method, template
Synthetic method etc..No matter which kind of method, which prepares carbon quantum dot, is required for carbon source, more commonly used to provide carbon source to prepare carbon quantum dot
Material has graphite, graphene, CNT and various organic reagents (glucose, ascorbic acid etc.).With natural green carbon source
It is to grow up in recent years and one of important directions of following carbon quantum dot development to prepare carbon quantum dot.Sahu et al. is then utilized
Orange juice provides carbon source for the preparation of carbon quantum dot, by a step hydro-thermal reaction, obtains the carbon quantum that quantum yield is 26%
(Sahu S,Behera B,Tapas K,et al.Simple one-step synthesis of highly
luminescent carbon dots from orange juice:application as excellent bio-
imaging agents.Chem.Commun.2012,48(70):8835-8837.).Zhou et al. leads to using watermelon peel as matrix
Carbonization is crossed, two steps is separated, has prepared carbon quantum dot (Zhou J J, Sheng Z, Han H, et al.Facile
synthesis of fluorescent carbon dots using watermelon peel as a carbon
sou.Materials Letters,2012,66(1):222-224.)。
The main component of bagasse is organic matter, can be provided for the preparation of carbon quantum dot needed for carbon source, it is and favourable
It is the correlative study that matrix prepares carbon quantum dot with natural materials.It is a kind of recycling to prepare carbon quantum dot as matrix using bagasse
Utilize, can not only promote the development of recycling economy also to play very big effect to environmental protection.
The content of the invention
The present invention constructs a kind of method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method, solves
Bagasse is the technical problem that carbon source prepares carbon quantum dot, and also the recycling for bagasse provides new direction and technology
Support.
Technical scheme：
A kind of method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method, step are as follows：
1) bagasse carries out high temperature cabonization 2-7h at 300-700 DEG C, the black solid after being carbonized, grinding, obtains
Black powder；
2) black powder made from step 1) is taken to be dispersed in acetic acid and 30wt% hydrogen peroxide, acetic acid and 30wt% peroxides
It is 1 to change hydrogen volume ratio:5-5:1, the quality of black powder and the total mass ratio of acetic acid and hydrogen peroxide are 1 in above-mentioned mixed liquor:
300-1:500；Ultrasonic 20-360min, 6-24h is heated to reflux under 100-140 DEG C of temperature conditionss, cool down；
3) solution for obtaining step 2) filters, and removes large granular impurity and the complete solid matter of unreacted；4000-
10-60min is centrifuged under 12000r/min revolutions, supernatant dialysis 12-48h, obtains the carbon quantum dot aqueous solution.
Beneficial effects of the present invention：
(1) preparation process is simple, is not required to special instrument equipment, product is without cumbersome post processing.
(2) preparation condition is gentle, without using strong acid and strong base and other poisonous and harmful substances.
(3) carbon quantum dot prepared has good surface topography and high fluorescent.
Brief description of the drawings
Fig. 1 is ultrasonic time 50min, acetic acid 40mL, hydrogen peroxide 20mL, and 16h, dialysis 24h institutes are heated to reflux at 100 DEG C
The TEM pictures of the carbon quantum dot obtained.
Fig. 2 is carbon quantum dot fluorescence spectrum prepared by the present invention.
Fig. 3 is carbon quantum dot uv absorption spectra prepared by the present invention.
Fig. 4 is the carbon quantum dot fluorescence that the chemical oxidization method used in the present invention is prepared with ultrasonic, nitric acid oxidation method
Intensity contrast figure.
Embodiment
The present invention relates to a kind of method that carbon quantum dot is prepared using bagasse as carbon source.Specific method is chemical oxidization method,
Chemical oxidation is carried out by acetic acid and hydrogen peroxide, carbon quantum dot is prepared by being heated to reflux.
Technical solution of the present invention is described in detail below, but protection scope of the present invention is not limited to the implementation
Example.
Embodiment 1：It is a kind of to prepare carbon quantum dot by utilization of carbon source chemical oxidization method of bagasse, comprise the following steps：
(1) bagasse is subjected to high temperature cabonization at 400 DEG C, the black solid after being carbonized, grinds and black powder is made
Body.
(2) take black powder 0.2g made from step (1) in 250mL round-bottomed flasks, add 40mL acetic acid (analysis is pure)
With the hydrogen peroxide of 20mL 30%, ultrasonic 50min, 16h is heated to reflux at 100 DEG C, cool down.
(3) solution for obtaining step (2) filters, and removes large granular impurity and the complete solid matter of unreacted.
20min, supernatant dialysis 24h are centrifuged under 4000r/min revolutions.Obtain the carbon quantum dot aqueous solution.
Embodiment 2：It is a kind of to prepare carbon quantum dot by utilization of carbon source chemical oxidization method of bagasse, comprise the following steps：
(1) bagasse is subjected to high temperature cabonization at 500 DEG C, the black solid after being carbonized, grinds and black powder is made
Body.
(2) take black powder 0.1g made from step (1) in 250mL round-bottomed flasks, add 20mL acetic acid (analysis is pure)
With the hydrogen peroxide of 10mL 30%, ultrasonic 30min, 10h is heated to reflux at 100 DEG C, cool down.
(3) solution for obtaining step (2) filters, and removes large granular impurity and the complete solid matter of unreacted.
20min, supernatant dialysis 12h are centrifuged under 8000r/min revolutions.Obtain the carbon quantum dot aqueous solution.
Embodiment 3：It is a kind of to prepare carbon quantum dot by utilization of carbon source chemical oxidization method of bagasse, comprise the following steps：
(1) bagasse is subjected to high temperature cabonization at 700 DEG C, the black solid after being carbonized, grinds and black powder is made
Body.
(2) take black powder 0.3g made from step (1) in 250mL round-bottomed flasks, add 40mL acetic acid (analysis is pure)
With the hydrogen peroxide of 80mL 30%, ultrasonic 30min, 12h is heated to reflux at 100 DEG C, cool down.
(3) solution for obtaining step (2) filters, and removes large granular impurity and the complete solid matter of unreacted.
20min, supernatant dialysis 24h are centrifuged under 4000r/min revolutions.Obtain the carbon quantum dot aqueous solution.
Comparative example 1：It is a kind of to prepare carbon quantum dot by utilization of carbon source ultrasonic of bagasse, comprise the following steps：
(1) bagasse is subjected to high temperature cabonization at 700 DEG C, the black solid after being carbonized, grinds and black powder is made
Body.
(2) take black powder 0.5g made from step (1) to be dispersed in 50mL deionized waters, ultrasonic 2h, stand cold
But to room temperature.
(3) solution for obtaining step (2) centrifuges 20min under 4000r/min revolutions, and the supernatant after centrifugation is put into
Bag filter, dialyse 24h.Obtain the carbon quantum dot aqueous solution.
Comparative example 2：It is a kind of to prepare carbon quantum dot by utilization of carbon source nitric acid oxidation method of bagasse, comprise the following steps：
(1) bagasse is subjected to high temperature cabonization at 700 DEG C, the black solid after being carbonized, grinds and black powder is made
Body.
(2) black powder 0.2g made from step (1) is taken to be dispersed in 20mL nitric acid (analysis is pure), ultrasonic 30min.
3h is heated to reflux at 121 DEG C, is cooled to room temperature.
(3) saturated sodium carbonate solution is added in the solution obtained to step (2) to pH to be neutral, then in 4000r/min
20min is centrifuged under revolution.Supernatant after centrifugation is put into bag filter, dialyse 24h.
Contrast the fluorescence intensity for the carbon quantum dot prepared using bagasse as utilization of carbon source distinct methods, concrete numerical value such as table
Shown in 1.It can be seen that the fluorescence for the carbon quantum dot prepared using bagasse as utilization of carbon source chemical oxidization method provided by the invention
The fluorescence intensity for the carbon quantum dot that intensity is prepared apparently higher than ultrasonic and nitric acid oxidation method.
The bagasse of table 1 is the carbon quantum dot fluorescence intensity contrast that carbon source distinct methods are prepared
Fig. 4 is comparative example 3, fluorescence of the carbon quantum dot prepared by comparative example 1 and 2 under different excitation wavelengths is strong
Spend distribution map.Wherein, the excitation wavelength of the carbon quantum dot prepared by each method be followed successively by from left to right 300nm, 320nm,
340nm, 360nm, 380nm, 400nm and 420nm.As can be seen from the figure in whole excitation wavelength range, closed using ultrasound
The fluorescence intensity of the carbon quantum dot prepared into method and nitric acid oxidation method is significantly lower than and institute in technical scope provided by the invention
The carbon quantum dot prepared.
Further contrast the carbon quantum dot fluorescence intensity prepared using different biomass carbon sources, specific data such as table 2
It is shown.By contrast as can be seen that the fluorescence for the carbon quantum dot fluorescence intensity that the bagasse used in the present invention is prepared is strong
Spend the carbon quantum dot prepared apparently higher than other several biomass carbon sources.This has close pass with dry matter content height in bagasse
System.High fluorescence intensity is to determine the important indicator that can carbon quantum dot be applied, and this also illustrates the carbon quantum that the present invention prepares
Point has more preferable application prospect.
The carbon quantum dot fluorescence intensity contrast that the different biomass carbon sources of table 2 are prepared
Claims (1)
- A kind of 1. method that carbon quantum dot is prepared using bagasse as utilization of carbon source chemical oxidization method, it is characterised in that step is as follows：1) bagasse carries out high temperature cabonization 2-7h at 300-700 DEG C, the black solid after being carbonized, grinding, obtains black Powder；2) black powder made from step 1) is taken to be dispersed in acetic acid and 30wt% hydrogen peroxide, acetic acid and 30wt% hydrogen peroxide Volume ratio is 1:5-5:1, the quality of black powder and the total mass ratio of acetic acid and hydrogen peroxide are 1 in above-mentioned mixed liquor:300- 1:500；Ultrasonic 20-360min, 6-24h is heated to reflux under 100-140 DEG C of temperature conditionss, cool down；3) solution for obtaining step 2) filters, and removes large granular impurity and the complete solid matter of unreacted；4000- 10-60min is centrifuged under 12000r/min revolutions, supernatant dialysis 12-48h, obtains the carbon quantum dot aqueous solution.
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Cited By (8)
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|---|---|---|---|---|
| CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
| CN110040711A (en) * | 2019-02-12 | 2019-07-23 | 辽宁工业大学 | A kind of preparation method of carbon quantum dot |
| CN112293502A (en) * | 2020-10-31 | 2021-02-02 | 江南大学 | Carbon quantum dot antioxidant, preparation method thereof and application thereof in frying oil |
| CN113023708A (en) * | 2021-02-24 | 2021-06-25 | 云南大学 | Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalizing carbon dots |
| CN113089015A (en) * | 2021-03-29 | 2021-07-09 | 西北大学 | Nitrogen-doped carbon quantum dot and preparation method thereof, reduced graphene oxide and preparation method and application thereof |
| CN113371692A (en) * | 2021-07-14 | 2021-09-10 | 合肥学院 | Preparation method of different fluorescent biomass carbon quantum dot nanoparticles |
| CN113528107A (en) * | 2021-07-13 | 2021-10-22 | 东北石油大学 | Coal-based carbon quantum dot oil displacement agent and application thereof in oil and gas exploitation |
| TWI835654B (en) * | 2023-05-18 | 2024-03-11 | 龍華科技大學 | Quantum chemical high-energy molecular water-tight cement manufacturing method |
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Cited By (10)
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|---|---|---|---|---|
| CN109054825A (en) * | 2018-08-24 | 2018-12-21 | 华南理工大学 | A kind of fluorescent carbon quantum dot and its high efficiency preparation method |
| CN109054825B (en) * | 2018-08-24 | 2020-09-22 | 华南理工大学 | Fluorescent carbon quantum dot and efficient preparation method thereof |
| CN110040711A (en) * | 2019-02-12 | 2019-07-23 | 辽宁工业大学 | A kind of preparation method of carbon quantum dot |
| CN112293502A (en) * | 2020-10-31 | 2021-02-02 | 江南大学 | Carbon quantum dot antioxidant, preparation method thereof and application thereof in frying oil |
| CN113023708A (en) * | 2021-02-24 | 2021-06-25 | 云南大学 | Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalizing carbon dots |
| CN113023708B (en) * | 2021-02-24 | 2023-10-27 | 云南大学 | Method for separating and extracting carbon dots from biomass combustion smoke dust and functionalization thereof |
| CN113089015A (en) * | 2021-03-29 | 2021-07-09 | 西北大学 | Nitrogen-doped carbon quantum dot and preparation method thereof, reduced graphene oxide and preparation method and application thereof |
| CN113528107A (en) * | 2021-07-13 | 2021-10-22 | 东北石油大学 | Coal-based carbon quantum dot oil displacement agent and application thereof in oil and gas exploitation |
| CN113371692A (en) * | 2021-07-14 | 2021-09-10 | 合肥学院 | Preparation method of different fluorescent biomass carbon quantum dot nanoparticles |
| TWI835654B (en) * | 2023-05-18 | 2024-03-11 | 龍華科技大學 | Quantum chemical high-energy molecular water-tight cement manufacturing method |
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