CN104946252B - Method for preparing fluorescent carbon dots by using coal - Google Patents
Method for preparing fluorescent carbon dots by using coal Download PDFInfo
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- CN104946252B CN104946252B CN201510417503.3A CN201510417503A CN104946252B CN 104946252 B CN104946252 B CN 104946252B CN 201510417503 A CN201510417503 A CN 201510417503A CN 104946252 B CN104946252 B CN 104946252B
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- carbon point
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Abstract
The invention discloses a green, pollution-free method for extracting fluorescent carbon dots from coal. The method comprises the steps of ball-milling, hydrogen peroxide oxidizing reacting, hydrogen peroxide removing, supernatant liquor cooling and drying and the like, and fluorescent carbon dot powder is obtained. The method has the advantages that the reaction is gentle and easy to control, and the yield is high.
Description
Technical field
The invention belongs to low-dimensional field of functional materials is and in particular to a kind of coal method of preparing fluorescent carbon point.
Background technology
Fluorescent carbon point be particle diameter in a kind of nano level emerging carbon nano-functional material, generally by the element group such as c, h, o
Become.Fluorescent carbon point is nontoxic, and has the many excellent optical characteristics of conventional semiconductors quantum dot.The characteristics of luminescence master of fluorescent carbon point
Luminescence generated by light to be shown and electrochemiluminescence, wherein fluorescence property are carbon point performances the most prominent.Carbon has as all living things
The backbone element of body, the fluorescent nano material constituting with respect to other elements, the toxicity of fluorescent carbon point is low and has good
Biocompatibility.Therefore it is the preferable substitution material of toxic semiconductor quantum dot, in photovoltaic device, biological detection, photocatalysis
It is widely used prospect in field.
At present, carbon quantum dot synthetic method is a lot, but existing method has high cost, not environmentally or raw material is difficult to obtain
Defect.So, development cost is lower, simple, eco-friendly synthetic method is imperative.Coal is as the abundant carbon of deposit
Source, has the characteristics that low cost, distribution are wide, easily obtains if it is possible to extract high-quality carbon amounts from coal with suitable method
Sub-, experimental cost will be substantially reduced and advance fluorescent carbon point in the application of every field.Prepare fluorescent carbon point with coal, report
Method be only limitted to process coal dust in the case of boiling with the mixed liquor of the strong oxidizers such as concentrated nitric acid, concentrated sulphuric acid, potassium permanganate
And separate carbon point, but this method not only results in a large amount of toxic gas releases, also can reduce utilization rate and the carbon point of coal
Yield not high.Further, since fluorescent carbon point is dispersed in strong acid solution, the means deacidifying are gone to be exactly to be neutralized with alkali.This is not only
Cost can be led to improve, and can therefore produce substantial amounts of salt, thus causing many adverse effects, such as the performance of impact carbon point with
Apply, go when desalination, to lead to carbon point loss etc..
Content of the invention
Present invention aim to address the above-mentioned technical problem that existing fluorescent carbon point preparation method exists, provide a kind of green
The method that fluorescent carbon point prepared by color, free of contamination coal.
The method preparing fluorescent carbon point with coal, it adopts following steps:
(1) coal dust is put in ball grinder, make the solid amount of coal dust and ceramic grinding ball account for the 1/3-2/ of ball milling tank volume
3, add deionized water to make it cover coal dust surface, be then placed on planetary ball mill with the rotating speed room temperature of 300-600r/min
Lower ball milling 3-8 hour, obtains the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 10-20%, then
Stirring reaction 2-5 hour at 30-90 DEG C, mixing speed is 400-1000r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
10-30min remove unreacted hydrogen peroxide, then again liquid is poured in centrifuge tube, with the rotating speed of 4000-11000r/min from
Heart 10-30min, obtains the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 10-20%, stirring reaction 2-5 hour at 30-90 DEG C, mixing speed be 400-1000r/min, will react
Mixed solution afterwards filters again, obtains not coal particle and the filtrate containing fluorescent carbon point of reaction completely, will not react completely
Coal particle abandon, the filtrate containing fluorescent carbon point is boiled at 100 DEG C 10-30min remove unreacted hydrogen peroxide, then
Again liquid is poured in centrifuge tube, 10-30min is centrifuged with the rotating speed of 4000-11000r/min, obtains upper containing fluorescent carbon point
Clear liquid；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Described coal dust is one of anthracite, brown coal, bituminous coal or semianthractie coal dust.
The recovery rate of fluorescent carbon point of the present invention is 40-60%.
Due to present invention employs technique scheme, solve the high cost that existing fluorescent carbon point preparation method exists,
Technical problem not environmentally, therefore, compared with background technology, it is excellent to have that reaction is gentle, easily controllable, yield is high etc. for the present invention
Point.
Brief description
Fig. 1 is the transmission electron microscope picture that the present invention prepares fluorescent carbon point；
Fig. 2 is the high-resolution-ration transmission electric-lens figure that the present invention prepares fluorescent carbon point；
Fig. 3 is the fluorescence emission spectrum that fluorescent carbon point prepared by the present invention excites lower acquisition in different wave length；
Fig. 4 is the photocatalytic activity sign that the present invention prepares fluorescent carbon point.
Specific embodiment
Introduce detailed technology scheme of the present invention below in conjunction with accompanying drawing:
Adopt following steps with the method that fluorescent carbon point prepared by coal:
(1) coal dust is put in ball grinder, make coal dust and the solid amount of ceramic grinding ball account for the 1/3～2/ of ball milling tank volume
3, add deionized water to make it cover coal dust surface, be then placed on planetary ball mill with the rotating speed room temperature of 300-600r/min
Lower ball milling 3-8 hour, obtains the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 10-20%, then
Stirring reaction 2-5 hour at 30-90 DEG C, mixing speed is 400-1000r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
10-30min remove unreacted hydrogen peroxide, then again liquid is poured in centrifuge tube, with the rotating speed of 4000-11000r/min from
Heart 10-30min, obtains the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 10-20%, stirring reaction 2-5 hour at 30-90 DEG C, mixing speed be 400-1000r/min, will react
Mixed solution afterwards filters again, obtains not coal particle and the filtrate containing fluorescent carbon point of reaction completely, will not react completely
Coal particle abandon, the filtrate containing fluorescent carbon point is boiled at 100 DEG C 10-30min remove unreacted hydrogen peroxide, then
Again liquid is poured in centrifuge tube, 10-30min is centrifuged with the rotating speed of 4000-11000r/min, obtains upper containing fluorescent carbon point
Clear liquid；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Described coal dust is one of anthracite, brown coal, bituminous coal or semianthractie coal dust.
The recovery rate of above-mentioned fluorescent carbon point is 40-60%.
Embodiment 1
The method preparing fluorescent carbon point with coal in the present embodiment, it adopts following steps:
(1) 2g anthracite coal dust is put in ball grinder, add deionized water to make it cover coal dust surface, be then placed on row
With ball milling under the rotating speed room temperature of 400r/min 6 hours on planetary ball mill, obtain the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 15%, at 60 DEG C
Stirring 3 hours, mixing speed is 1000r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
25min removes unreacted hydrogen peroxide, then pours liquid in centrifuge tube into again, is centrifuged 25min with the rotating speed of 5000r/min,
Obtain the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 15%, stirring reaction 3 hours at 60 DEG C, mixing speed be 1000r/min, by reacted mixed solution
Filter again, obtain not coal particle and the filtrate containing fluorescent carbon point of reaction completely, the coal particle of not reaction completely is abandoned,
By the filtrate containing fluorescent carbon point boil at 100 DEG C 25min remove unreacted hydrogen peroxide, then again by liquid pour into from
In heart pipe, 25min is centrifuged with the rotating speed of 5000r/min, obtains the supernatant containing fluorescent carbon point；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Embodiment 2
The method preparing fluorescent carbon point with coal in the present embodiment, it adopts following steps:
(1) 2g anthracite coal dust is put in ball grinder, add deionized water to make it cover coal dust surface, be then placed on row
With ball milling under the rotating speed room temperature of 300r/min 8 hours on planetary ball mill, obtain the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 12%, at 90 DEG C
Stirring 2 hours, mixing speed is 600r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
30min removes unreacted hydrogen peroxide, then pours liquid in centrifuge tube into again, is centrifuged 10min with the rotating speed of 11000r/min,
Obtain the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 12%, stirring reaction 2 hours at 90 DEG C, mixing speed be 600r/min, by reacted mixed solution
Filter again, obtain not coal particle and the filtrate containing fluorescent carbon point of reaction completely, the coal particle of not reaction completely is abandoned,
By the filtrate containing fluorescent carbon point boil at 100 DEG C 30min remove unreacted hydrogen peroxide, then again by liquid pour into from
In heart pipe, 10min is centrifuged with the rotating speed of 11000r/min, obtains the supernatant containing fluorescent carbon point；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Embodiment 3
The method preparing fluorescent carbon point with coal in the present embodiment, it adopts following steps:
(1) 2g anthracite coal dust is put in ball grinder, add deionized water to make it cover coal dust surface, be then placed on row
With ball milling under the rotating speed room temperature of 600r/min 3 hours on planetary ball mill, obtain the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 20%, at 30 DEG C
Stirring 5 hours, mixing speed is 400r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
15min removes unreacted hydrogen peroxide, then pours liquid in centrifuge tube into again, is centrifuged 15min with the rotating speed of 9000r/min,
Obtain the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 20%, stirring reaction 5 hours at 30 DEG C, mixing speed be 400r/min, by reacted mixed solution
Filter again, obtain not coal particle and the filtrate containing fluorescent carbon point of reaction completely, the coal particle of not reaction completely is abandoned,
By the filtrate containing fluorescent carbon point boil at 100 DEG C 15min remove unreacted hydrogen peroxide, then again by liquid pour into from
In heart pipe, 15min is centrifuged with the rotating speed of 9000r/min, obtains the supernatant containing fluorescent carbon point；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Embodiment 4
The method preparing fluorescent carbon point with coal in the present embodiment, it adopts following steps:
(1) 2g anthracite coal dust is put in ball grinder, add deionized water to make it cover coal dust surface, be then placed on row
With ball milling under the rotating speed room temperature of 500r/min 4 hours on planetary ball mill, obtain the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 10%, at 50 DEG C
Stirring 4 hours, mixing speed is 800r/min；
(3) filter to isolate unreacted coal particle from the mixed solution that step (2) reaction obtains and contain fluorescent carbon
The filtrate of point；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point is boiled at 100 DEG C
10min removes unreacted hydrogen peroxide, then pours liquid in centrifuge tube into again, is centrifuged 30min with the rotating speed of 4000r/min,
Obtain the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, hydrogen peroxide in mixed solution
Volumetric concentration be 10%, stirring reaction 4 hours at 50 DEG C, mixing speed be 800r/min, by reacted mixed solution
Filter again, obtain not coal particle and the filtrate containing fluorescent carbon point of reaction completely, the coal particle of not reaction completely is abandoned,
By the filtrate containing fluorescent carbon point boil at 100 DEG C 10min remove unreacted hydrogen peroxide, then again by liquid pour into from
In heart pipe, 30min is centrifuged with the rotating speed of 4000r/min, obtains the supernatant containing fluorescent carbon point；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
Anthracite coal dust in above-described embodiment can also be replaced with one of brown coal, bituminous coal or semianthractie coal dust.
As shown in 1-2 figure, for showing the shape characteristic of the fluorescent carbon point of present invention preparation, to fluorescent carbon point (carbon of the present invention
Nano-particle) make transmission electron microscope detection, result shows that carbon point is in dispersity, and distribution of sizes is 1-3nm.High-resolution transmission
Electronic Speculum result shows that carbon point is in crystal characteristic, and containing defective.
As shown in 3 figures, for showing that carbon nano-particle of the present invention has the property of luminescence generated by light, the present invention have detected different ripples
Length excites the fluorescence emission spectrum giving carbon point, and result shows that the fluorescence emission spectrum of carbon point mainly covers in 400-600nm scope
Interior, and glow peak has certain dependency to excitation wavelength.
As shown in 4 figures, the fluorescent carbon point for showing present invention acquisition has photocatalysis performance, and the present invention is the fluorescence of preparation
Carbon point is directly placed in 1-10mol/l methylene blue and methyl orange solution, degradation of methylene blue and methyl orange, and result shows
In 30min, photocatalysis efficiency is up to 80%, far above the degradation rate of business nano titanium oxide (p25) photocatalyst.
The present invention only has co in preparation process2With a small amount of o2Release, nonhazardous gas produce.
Claims (3)
1. with coal prepare fluorescent carbon point method it is characterised in that: adopt following steps:
(1) coal dust is put in ball grinder, make the solid amount of coal dust and ceramic grinding ball account for the 1/3-2/3 of ball milling tank volume, plus
Entering deionized water makes it cover coal dust surface, is then placed on planetary ball mill with ball under the rotating speed room temperature of 300-600r/min
Mill 3-8 hour, obtains the coal dust suspension of black；
(2) coal dust suspension is mixed with hydrogen peroxide, in mixed solution, the volumetric concentration of hydrogen peroxide is 10-20%, then in 30-
Stirring reaction 2-5 hour at 90 DEG C, mixing speed is 400-1000r/min；
(3) filter to isolate unreacted coal particle and containing fluorescent carbon point from the mixed solution that step (2) reaction obtains
Filtrate；Unreacted coal particle is processed further according to step (4), and the filtrate containing fluorescent carbon point boils 10- at 100 DEG C
30min removes unreacted hydrogen peroxide, then pours liquid in centrifuge tube into again, with the rotating speed centrifugation of 4000-11000r/min
10-30min, obtains the supernatant containing fluorescent carbon point；
(4) the unreacted coal particle filtering to isolate in step (3) is mixed with hydrogen peroxide again, the body of hydrogen peroxide in mixed solution
Long-pending concentration is 10-20%, stirring reaction 2-5 hour at 30-90 DEG C, and mixing speed is 400-1000r/min, will be reacted
Mixed solution filters again, obtains not coal particle and the filtrate containing fluorescent carbon point of reaction completely, by the coal of not reaction completely
Granule abandons, and the filtrate containing fluorescent carbon point is boiled at 100 DEG C 10-30min and removes unreacted hydrogen peroxide, then will again
Liquid is poured in centrifuge tube, is centrifuged 10-30min with the rotating speed of 4000-11000r/min, obtains the supernatant containing fluorescent carbon point
Liquid；
(5) the supernatant lyophilization that will obtain in step (3) and (4), prepared fluorescent carbon point powder body.
2. coal according to claim 1 prepare fluorescent carbon point method it is characterised in that: described coal dust is smokeless
One of coal, brown coal, bituminous coal or semianthractie.
3. coal according to claim 1 prepare fluorescent carbon point method it is characterised in that: the receiving of described fluorescent carbon point
Rate is 40-60%.
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| CN106167256B (en) * | 2016-07-07 | 2018-06-01 | 中北大学 | The method that multicolor luminous adjustable carbon dots is prepared using coal quality pitch |
| CN106479493A (en) * | 2016-09-21 | 2017-03-08 | 大连理工大学 | A kind of method for carbon source, carbon quantum dot being prepared by hydrogen peroxide low-temperature oxidation with brown coal |
| CN106566542B (en) * | 2016-10-25 | 2019-04-05 | 大连理工大学 | A kind of preparation of the carbon quantum dot based on coal tar asphalt base and the detection method of HCHO |
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| CN107033893B (en) * | 2017-06-05 | 2019-09-10 | 中北大学 | Preparation method with double centre of luminescence fluorescent carbon points |
| CN109437154B (en) * | 2018-10-25 | 2020-12-11 | 河南理工大学 | Method for preparing energy band controllable carbon quantum dots by taking coal as raw material |
| CN111151278B (en) * | 2020-01-18 | 2022-07-26 | 中北大学 | Preparation method of carbon dot composite bismuthyl carbonate visible-light-driven photocatalyst |
| CN112608743B (en) * | 2020-12-24 | 2022-06-14 | 中国矿业大学(北京) | Preparation method of coal-based fluorescent carbon quantum dots |
| CN113528133B (en) * | 2021-07-07 | 2022-09-16 | 安徽工业大学 | Preparation method of brown coal-based white fluorescent carbon dots |
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