CN103447058A - Preparation method for chlorine element modified carbon quantum dot - Google Patents
Preparation method for chlorine element modified carbon quantum dot Download PDFInfo
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- CN103447058A CN103447058A CN2013104253245A CN201310425324A CN103447058A CN 103447058 A CN103447058 A CN 103447058A CN 2013104253245 A CN2013104253245 A CN 2013104253245A CN 201310425324 A CN201310425324 A CN 201310425324A CN 103447058 A CN103447058 A CN 103447058A
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Abstract
The invention belongs to the field of a carbon nanometer material science, and particularly relates to a preparation method for a chlorine element modified carbon quantum dot, which mainly solves the technical problems that a carbon quantum dot almost has no photocatalysis or has very low catalysis efficiency, raw materials of a preparation method for a carbon quantum dot based compound material are expensive and the preparation method is complicated. According to the technical scheme provided by the invention, the preparation method of the chlorine element modified carbon quantum dot comprises the following steps: firstly, reacting liquid alcohol organic matters at 150-250 DEG C for 4-12 hours; removing large particles in a reaction solution to obtain a carbon quantum dot solution; then, slowly dripping thionyl chloride into the carbon quantum dot solution at the temperature of 0 DEG C in the volume ratio of the carbon quantum dot solution to the thionyl chloride being 20:(1-10) and mixing uniformly; reacting at 150-200 DEG C for 5-10 hours; removing large particles in a reaction solution to obtain the chlorine element modified carbon quantum dot. The chlorine element modified carbon quantum dot provided by the invention has very strong photocatalytic performance; the operation process is simple, the repeatability is good and the raw materials are readily available.
Description
Technical field
The invention belongs to the carbon nanomaterial scientific domain, be specifically related to a kind of preparation method of chlorine element modified carbon quantum dot.
Background technology
The carbon quantum dot is the spherical carbon nano-particle of class that a kind of dispersion, size are less than 10nm, because it has the excellent properties that is different from traditional quantum dot, as special performances such as luminescence generated by light, low toxicity, chemical inertnesses, be widely used in opto-electronic device, biological detection and medicine and other fields, but carbon quantum dot prepared by most methods does not have photocatalysis performance or catalytic efficiency very low substantially, exploitation and the application of its photocatalysis performance have therefore been restricted.Research discovery in recent years, the quantum dot-based composite of carbon has light-catalysed performance.
(Cao L, Sahu S, Anilkumar P, the Sun Y P.Carbon Nanoparticles as Visible-Light Photocatalysts for Efficient CO such as Sun
2conversion and Beyond.J.Am.Chem.Soc.2011,133 (13): 4754 – 4757) coat gold or platinum on the carbon quantum dot, can be by CO under light conditions
2change Hydrocarbon Organic into, but the method prices of raw and semifnished materials costliness, application is extremely restricted.
(Zhang H C, Ming H, the Lee S T.Fe such as Zhang
2o
3/ carbon quantum dots complex photocatalysts and their enhanced photocatalytic activity under visible light.Dalton Trans., 2011,40 (41): 10822 – 10825) with the synthetic carbon quantum dot combined oxidation iron material of hydrothermal method, this compound is the degradable toxic gas under radiation of visible light, but the method preparation procedure complexity, can not be for large-scale production.
Summary of the invention
The objective of the invention is to solve that the carbon quantum dot exists substantially there is no photocatalysis or catalytic efficiency very low and the prices of raw and semifnished materials costliness of the quantum dot-based composite material and preparation method thereof of carbon and the technical problem of preparation method's complexity, a kind of preparation method of chlorine element modified carbon quantum dot is provided.The carbon quantum dot that chlorine element prepared by the present invention is modified has strong photocatalysis, and operating procedure is simple, reproducible, raw material sources abundant.
For solving the problems of the technologies described above, the technical scheme that the present invention takes is:
A kind of preparation method of chlorine element modified carbon quantum dot, its preparation process is:
1) at first the liquid alcohol type organic is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 150～250 ℃, insulation 4～12h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30～60 minutes of the speed that the rotating speed of take is 8000～11000r/min, remove the bulky grain in reactant liquor, or the molecular cut off ultrafiltration membrance filter 24h that is 3～10kD with molecular cut off, the supernatant obtained is the carbon quantum dot solution;
2) proportioning that is 20:1～10 according to carbon quantum dot solution and thionyl chloride volume ratio, at first the carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 150～200 ℃, insulation 5～10h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30～60 minutes of the speed that the rotating speed of take is 8000～11000r/min, remove the bulky grain in reactant liquor, or the molecular cut off ultrafiltration membrance filter 24h that is 3～10kD with molecular cut off, the supernatant obtained is the carbon quantum dot that the chlorine element is modified.
Above-mentioned pure type organic is any one in ethylene glycol, ethanol, butanols, octanol or diethylene glycol alcohol type organic.
The carbon quantum dot that chlorine element prepared by the present invention is modified is applied to photocatalysis to degrade organic matter.
For showing that carbon quantum dot that chlorine element prepared by the present invention is modified can improve the photocatalysis efficiency of carbon quantum dot, carbon quantum dot (Cl-CQDs) after the chlorine prepared with the present invention is element modified and methylene blue and the 2.5mg/L rhodamine B solution (catalytic efficiency is shown in Fig. 5 and Fig. 6) of carbon quantum dot (CQDs) catalytic degradation 2.5mg/L, from test result, the photocatalysis efficiency of the carbon quantum dot that chlorine element prepared by the present invention is modified is all higher than the photocatalysis efficiency of carbon quantum dot.Carbon quantum dot catalytic degradation methylene blue 10min, degradation efficiency is only 25%, and the catalytic efficiency of chlorine element modified carbon quantum dot is up to 94%.The efficiency of the catalytic degradation rhodamine B of the chlorine element modified carbon quantum dot that in addition, prepared by the present invention is 20 times of carbon quantum dot.Thereby the carbon quantum dot that the chlorine element for preparing of the present invention is modified has significant beneficial effect comparing with pure carbon quantum dot aspect the catalytic degradation organic dyestuff.
Compare with background technology, the invention has the advantages that:
(1) the carbon quantum dot that the prepared chlorine element of the present invention is modified utilizes its surperficial oxy radical hydroxyl and the chemical reaction of thionyl chloride, the chlorine element is linked into to carbon quantum dot surface, make the carbon quantum dot of the chlorine element modification of preparation increase substantially the organic efficiency of carbon quantum dot light catalytic degradation, for the carbon quantum dot, in the application of photocatalysis field, provide possibility.
(2) the present invention has the advantages such as operating procedure is simple, reproducible, raw material sources are abundant.
The accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the carbon quantum dot (Cl-CQDs) (embodiment 1 preparation) modified of the chlorine element for preparing of the present invention.
Fig. 2 is the size distribution plot of the carbon quantum dot (Cl-CQDs) (embodiment 1 preparation) modified of the chlorine element for preparing of the present invention.
Fig. 3 is the chlorine element modified carbon quantum dot (Cl-CQDs) for preparing of the present invention and the infrared spectrogram of carbon quantum dot (CQDs).
Fig. 4 is the energy loss spectroscopy of the chlorine element modified carbon quantum dot (Cl-CQDs) for preparing of the present invention.
Fig. 5 is the chlorine element modified carbon quantum dot (Cl-CQDs) for preparing of the present invention and the photocatalysis efficiency figure of carbon quantum dot (CQDs) photocatalytic degradation methylene blue.
Fig. 6 is the chlorine element modified carbon quantum dot (Cl-CQDs) for preparing of the present invention and the photocatalysis efficiency figure of carbon quantum dot (CQDs) photocatalytic degradation rhodamine B.
The specific embodiment
Embodiment 1
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first 25mL ethylene glycol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 150 ℃, insulation 12h, then reaction vessel is naturally cooled to normal temperature, then reactant liquor in reaction vessel is added in centrifuge, centrifugal 60 minutes of the speed that the rotating speed of take is 8000r/min, remove the bulky grain in reactant liquor, obtain carbon quantum dot solution 23mL;
2) measure carbon quantum dot solution 10mL and thionyl chloride 0.5mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 0.5mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 200 ℃, insulation 5h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30 minutes of the speed that the rotating speed of take is 8000r/min, remove the bulky grain in reactant liquor, obtain the carbon quantum dot 8mL that the chlorine element is modified.
The carbon quantum dot that chlorine element prepared by the present embodiment is modified is even by the transmission electron microscope observing particle diameter, and particle diameter is mainly between 3～3.2nm; By infrared spectrum, detect at 750cm
-1the C-Cl stretching vibration peak appears in vicinity; Detect and occur Cl L-edge peak in the 210eV vicinity by energy loss spectroscopy.
The particle diameter of the carbon quantum dot that the chlorine element that as can be seen from Figure 1, prepared by the present embodiment is modified is even;
The particle diameter of the carbon quantum dot that the chlorine element that as can be seen from Figure 2, prepared by the present embodiment is modified is mainly between 3～3.2nm;
As can be seen from Figure 3, the carbon quantum dot that the chlorine element that prepared by the present embodiment is modified detects at 750cm by infrared spectrum
-1the C-Cl stretching vibration peak appears in vicinity;
Cl L-edge peak appears in the carbon quantum dot that the chlorine element that as can be seen from Figure 4, prepared by the present embodiment is modified in the 210eV vicinity;
Complex chart 1～6 is known, and the present embodiment has been prepared the carbon quantum dot that the chlorine element is modified.
Embodiment 2
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first 25mL ethylene glycol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 250 ℃, insulation 4h, then reaction vessel is naturally cooled to normal temperature, then reactant liquor in reaction vessel is added in centrifuge, centrifugal 30 minutes of the speed that the rotating speed of take is 11000r/min, remove the bulky grain in reactant liquor, obtain carbon quantum dot solution 22mL;
2) measure carbon quantum dot solution 10mL and thionyl chloride 5mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 5mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 150 ℃, insulation 10h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 60 minutes of the speed that the rotating speed of take is 11000r/min, remove the bulky grain in reactant liquor, obtain the carbon quantum dot 13.5mL that the chlorine element is modified.
The carbon quantum dot testing result that chlorine element prepared by the present embodiment is modified is identical with the carbon quantum dot testing result that the chlorine element of embodiment 1 preparation is modified.
Embodiment 3
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first 25mL ethylene glycol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 200 ℃, insulation 8h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 10kD with molecular cut off, obtain carbon quantum dot solution 22mL.
2) measure carbon quantum dot solution 10mL and thionyl chloride 2.25mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 2.25mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 175 ℃, insulation 7.5h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 5kD with molecular cut off, obtain the carbon quantum dot 11mL that the chlorine element is modified.
The carbon quantum dot testing result that chlorine element prepared by the present embodiment is modified is identical with the carbon quantum dot testing result that the chlorine element of embodiment 1 preparation is modified.
Embodiment 4
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first 25mL ethylene glycol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 180 ℃, insulation 10h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 3kD with molecular cut off, obtain carbon quantum dot solution 23mL.
2) measure carbon quantum dot solution 10mL and thionyl chloride 1.5mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 1.5mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 180 ℃, insulation 6h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 8kD with molecular cut off, obtain the carbon quantum dot 10mL that the chlorine element is modified.
The carbon quantum dot testing result that chlorine element prepared by the present embodiment is modified is identical with the carbon quantum dot testing result that the chlorine element of embodiment 1 preparation is modified.
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first 25mL ethanol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 200 ℃, insulation 12h, then reaction vessel is naturally cooled to normal temperature, then reactant liquor in reaction vessel is added in centrifuge, centrifugal 40 minutes of the speed that the rotating speed of take is 11000r/min, remove the bulky grain in reactant liquor, obtain carbon quantum dot solution 20mL.
2) measure carbon quantum dot solution 10mL and thionyl chloride 1mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 1mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 150 ℃, insulation 6h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30 minutes of the speed that the rotating speed of take is 11000r/min, remove the bulky grain in reactant liquor, obtain the carbon quantum dot 7mL that the chlorine element is modified.
The carbon quantum dot testing result that chlorine element prepared by the present embodiment is modified is identical with the carbon quantum dot testing result that the chlorine element of embodiment 1 preparation is modified.
Embodiment 6
The carbon quantum dot that chlorine element in the present embodiment is modified, its preparation method is:
1) at first the 25mL diethylene glycol is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 180 ℃, insulation 8h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 4kD with molecular cut off, obtain carbon quantum dot solution 23mL.
2) measure carbon quantum dot solution 10mL and thionyl chloride 2mL, at first 10mL carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, the 2mL thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 185 ℃, insulation 4h, then reaction vessel is naturally cooled to normal temperature, the molecular cut off ultrafiltration membrance filter 24h that is reactant liquor 8kD with molecular cut off, obtain the carbon quantum dot 11mL that the chlorine element is modified.
The carbon quantum dot testing result that chlorine element prepared by the present embodiment is modified is identical with the carbon quantum dot testing result that the chlorine element of embodiment 1 preparation is modified.
Ethylene glycol in above-described embodiment, ethanol or diethylene glycol can also replace with butanols or octanol.
Protection domain of the present invention is not subject to the restriction of above embodiment.
Claims (3)
1. the preparation method of a chlorine element modified carbon quantum dot, it is characterized in that: its preparation process is:
1) at first the liquid alcohol type organic is added in reaction vessel, closed reaction vessel, then reaction vessel is warming up to 150～250 ℃, insulation 4～12h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30～60 minutes of the speed that the rotating speed of take is 8000～11000r/min, remove the bulky grain in reactant liquor, or the molecular cut off ultrafiltration membrance filter 24h that is 3～10kD with molecular cut off, the supernatant obtained is the carbon quantum dot solution;
2) proportioning that is 20:1～10 according to carbon quantum dot solution and thionyl chloride volume ratio, at first the carbon quantum dot solution is added in reaction vessel, at 0 ℃ of temperature, thionyl chloride slowly is added drop-wise in the carbon quantum dot solution, follow ultrasonic processing mixed solution, until the two mixes, closed reaction vessel, reaction vessel is warming up to 150～200 ℃, insulation 5～10h, then reaction vessel is naturally cooled to normal temperature, again reactant liquor in reaction vessel is added in centrifuge, centrifugal 30～60 minutes of the speed that the rotating speed of take is 8000～11000r/min, remove the bulky grain in reactant liquor, or the molecular cut off ultrafiltration membrance filter 24h that is 3～10kD with molecular cut off, the supernatant obtained is the carbon quantum dot that the chlorine element is modified.
2. the preparation method of a kind of chlorine element modified carbon quantum dot according to claim 1 is characterized in that: described pure type organic is any one in ethylene glycol, ethanol, butanols, octanol or diethylene glycol alcohol type organic.
3. the preparation method of a kind of chlorine element modified carbon quantum dot according to claim 1 is characterized in that: the carbon quantum dot that the chlorine element of described preparation is modified is applied to photocatalysis to degrade organic matter.
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Cited By (10)
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| CN103642494A (en) * | 2013-12-27 | 2014-03-19 | 中国科学院上海微系统与信息技术研究所 | Preparation method for fluorescence carbon-based quantum dot |
| CN103787298A (en) * | 2014-01-02 | 2014-05-14 | 南京航空航天大学 | Method for preparing high-brightness fluorescent carbon dots with single organic solvent by one-step ultrasonic method |
| CN103992794A (en) * | 2014-05-26 | 2014-08-20 | 中北大学 | Method for recovering solid carbon quantum dots |
| CN104004516A (en) * | 2014-05-23 | 2014-08-27 | 华南理工大学 | Fluorescence amino carbon quantum dots, and preparation method and application thereof |
| CN105148966A (en) * | 2015-07-10 | 2015-12-16 | 中北大学 | Carbon quantum dot grafted hydroxyapatite photocatalysis material preparation method |
| CN107282084A (en) * | 2017-07-28 | 2017-10-24 | 合肥工业大学 | A kind of efficient degradation antibiotic mixes chlorine carbon quantum dot/g C3N4The preparation method of nanosheet composite material |
| CN107397958A (en) * | 2017-07-21 | 2017-11-28 | 浙江理工大学 | A kind of preparation method for the nanoparticle for being embedded with load cancer therapy drug carbon quantum dot |
| CN112400869A (en) * | 2020-12-04 | 2021-02-26 | 陕西科技大学 | Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and preparation method thereof |
| CN112795379A (en) * | 2021-01-07 | 2021-05-14 | 宁德师范学院 | Preparation method and application of surface-modified nitrogen-doped carbon quantum dot |
| CN114768808A (en) * | 2022-05-27 | 2022-07-22 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
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| CN103642494A (en) * | 2013-12-27 | 2014-03-19 | 中国科学院上海微系统与信息技术研究所 | Preparation method for fluorescence carbon-based quantum dot |
| CN103787298B (en) * | 2014-01-02 | 2016-04-27 | 南京航空航天大学 | A kind of single organic solvent one step ultrasonic method prepares the method for high brightness fluorescent carbon point |
| CN103787298A (en) * | 2014-01-02 | 2014-05-14 | 南京航空航天大学 | Method for preparing high-brightness fluorescent carbon dots with single organic solvent by one-step ultrasonic method |
| CN104004516A (en) * | 2014-05-23 | 2014-08-27 | 华南理工大学 | Fluorescence amino carbon quantum dots, and preparation method and application thereof |
| CN104004516B (en) * | 2014-05-23 | 2016-04-13 | 华南理工大学 | A kind of fluorescence amino-carbon quantum dot and its preparation method and application |
| CN103992794A (en) * | 2014-05-26 | 2014-08-20 | 中北大学 | Method for recovering solid carbon quantum dots |
| CN103992794B (en) * | 2014-05-26 | 2015-10-28 | 中北大学 | A kind of method reclaiming solid carbon quantum dot |
| CN105148966B (en) * | 2015-07-10 | 2017-05-10 | 中北大学 | Carbon quantum dot grafted hydroxyapatite photocatalysis material preparation method |
| CN105148966A (en) * | 2015-07-10 | 2015-12-16 | 中北大学 | Carbon quantum dot grafted hydroxyapatite photocatalysis material preparation method |
| CN107397958A (en) * | 2017-07-21 | 2017-11-28 | 浙江理工大学 | A kind of preparation method for the nanoparticle for being embedded with load cancer therapy drug carbon quantum dot |
| CN107397958B (en) * | 2017-07-21 | 2020-12-18 | 浙江理工大学 | Preparation method of nanoparticles embedded with carbon quantum dots loaded with anticancer drugs |
| CN107282084A (en) * | 2017-07-28 | 2017-10-24 | 合肥工业大学 | A kind of efficient degradation antibiotic mixes chlorine carbon quantum dot/g C3N4The preparation method of nanosheet composite material |
| CN107282084B (en) * | 2017-07-28 | 2020-02-18 | 合肥工业大学 | Chlorine-doped carbon quantum dot/g-C for efficiently degrading antibiotics3N4Preparation method of nanosheet composite material |
| CN112400869A (en) * | 2020-12-04 | 2021-02-26 | 陕西科技大学 | Cl-modified GQD/ZnO/acidified attapulgite nano composite antibacterial agent and preparation method thereof |
| CN112795379A (en) * | 2021-01-07 | 2021-05-14 | 宁德师范学院 | Preparation method and application of surface-modified nitrogen-doped carbon quantum dot |
| CN112795379B (en) * | 2021-01-07 | 2022-11-18 | 宁德师范学院 | Preparation method and application of surface-modified nitrogen-doped carbon quantum dot |
| CN114768808A (en) * | 2022-05-27 | 2022-07-22 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
| CN114768808B (en) * | 2022-05-27 | 2023-12-08 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
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Application publication date: 20131218 |