CN104386666A - Method for preparing carbon quantum dots through alcohol decomposition - Google Patents
Method for preparing carbon quantum dots through alcohol decomposition Download PDFInfo
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- CN104386666A CN104386666A CN201410566040.2A CN201410566040A CN104386666A CN 104386666 A CN104386666 A CN 104386666A CN 201410566040 A CN201410566040 A CN 201410566040A CN 104386666 A CN104386666 A CN 104386666A
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Abstract
The invention relates to a method for preparing carbon quantum dots through alcohol decomposition. The method comprises the following steps: preparing an alkaline matter alcoholic solution of which the concentration is 0.1 to 10 mol/L to obtain a dispersing liquid containing carbon quantum dots, wherein the temperature is 15 to 200 DEG C, and the carbonization time is 2 to 360 h; conducting dialyzing and vacuum drying on the dispersing liquid to obtain solid carbon quantum dots. The method takes alcohol as a carbon source, and adopts a room temperature standing or heating manner to obtain the carbon quantum dots, thereby being simple, wide in raw material source, low in cost and high in mass production possibility.
Description
Technical field
The invention belongs to the preparing technical field of carbon quantum dot, be specifically related to a kind of preparation method of carbon quantum dot.
Background technology
Carbon quantum dot (CQDs), due to the performance of its uniqueness, is attracted wide attention by as a kind of general fluorescent nano material.Compare with traditional semiconductor-quantum-point, carbon quantum dot has low optical flare, low photofading, hypotoxicity, high quantum production rate, the excellent advantage such as Photophysical Behaviors, good biocompatibility.
The method preparing carbon quantum dot reported has: laser ablation, plasma treatment, electrochemical synthesis, Hydrothermal Synthesis, chemical oxidation, Microwave synthesize, ultrasonic synthesis etc.But these methods prepare carbon quantum dot that mostly process is complicated, energy consumption is high, yield poorly.
Patent application CN201310378455.2 discloses the method that fluorescent carbon quantum dot is prepared in the carbonization of a kind of alcohol electrochemistry, comprise the steps: to take alcohol as carbon source, using alkaline matter and mixed alkoxide solution as electrolytic solution, platinized platinum is as working electrode with to electrode, calomel is as reference electrode, carry out electrolysis, collect reaction soln, add in acid in reaction soln and alkaline matter extremely neutrality, leave standstill and salt is precipitated, get supernatant liquor, alcohol is added in supernatant liquor, to salt out further, again get supernatant liquor, obtain carbon quantum dot alcoholic solution the method and obtain carbon quantum dot, carbon quantum dot alcoholic solution is evaporated to obtain solid, by the solid ultrasonic disperse in water obtained, and by the aqueous solution obtaining carbon quantum dot after dialysis tubing dialysis of the liquid after dispersion.Although the method productive rate is higher, complicated operation, its electrode will use platinized platinum, and also want additional electric energy, need voltage-regulation instrument, cost is higher, has limitation.
Summary of the invention
The object of this invention is to provide a kind of method preparing carbon quantum dot that method is simple, cost is low, energy consumption is low, productive rate is high.
The method that carbon quantum dot is prepared in a kind of alcohol decomposition of the present invention is as follows: the alcoholic solution of preparation alkaline matter, standing and reacting, obtains the dispersion liquid of carbon containing quantum dot, and purified for this dispersion liquid, drying are obtained carbon quantum dot solid.
Described alcohol is that carbonatoms is more than or equal to 2, is less than or equal to the monohydroxy-alcohol of 30, dibasic alcohol or polyvalent alcohol.
Described alcohol is preferably one or more in ethanol, propyl alcohol, butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, lauryl alcohol, tridecanol, tetradecyl alcohol, pentadecanol, hexadecanol, heptadecyl alcohol, stearyl alcohol, nonadecanol, eicosanol, behenyl alcohol, tetracosanol, hexacosyl alcohol, octacosanol, triacontanol, ethylene glycol, glycerol, vinyl carbinol, phenylcarbinol, phenylethyl alcohol.
Described alkaline matter is one or more in lithium hydroxide, potassium hydroxide, sodium hydroxide, phosphoric acid salt, carbonate.
The concentration of described alkaline matter in alcoholic solution is 0.1-10mol/L.
The above-mentioned reaction times is 2-360h; Temperature of reaction is 15-200 DEG C.The preferred reaction time is 48-120h; Preferable reaction temperature is 25-120 DEG C.
Described way of purification is dialysis.Described dialysis adopts molecular weight cut-off to be the dialysis tubing of 500-5000; Dialysis time is 10-120h.Described carbon quantum dot size is less than 5nm.
Described drying is vacuum-drying, and temperature is 80-150 DEG C; Time of drying is 4-24h.
Described vacuum-drying temperature is 80-150 DEG C.
The described vacuum-drying time is 4-24h.
The present invention utilizes alcohol chemical decomposition method to prepare carbon quantum dot innovatively.Owing to have employed above scheme, beneficial effect of the present invention is: preparation method is simple, and mild condition is controlled, and without the need to using expensive instrument, the method is with low cost, less energy consumption, and raw material sources are extensive, are expected to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 1;
Fig. 2 is the fluorescence spectrum of the carbon quantum dot obtained in embodiment 1;
Fig. 3 is the XRD figure of the carbon quantum dot obtained in embodiment 1;
Fig. 4 is the XPS figure of the carbon quantum dot obtained in embodiment 1;
Fig. 5 is the reaction soln colour-change photo of differential responses time in embodiment 1;
Fig. 6 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 2;
Fig. 7 is the transmission electron microscope photo of the carbon quantum dot obtained in embodiment 3;
Fig. 8 is the carbon quantum dot solid photo obtained in embodiment 3.
Embodiment
Following examples are to explain the present invention in more detail, and these embodiments do not form any restriction to the present invention, and the present invention can implement by the either type described in summary of the invention.
Embodiment 1
The ethanolic soln of preparation 0.5mol/L sodium hydroxide, room temperature (25 DEG C) standing and reacting 360h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 60h of 2000 through the molecule that dams by carbon quantum dot dispersion liquid, vacuum-drying 24h at 80 DEG C, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 1, and particle diameter is comparatively even, is less than 5nm.Fig. 2 is its fluorescence spectrum figure, and have the feature changed along with the change of exciting light spectrum, its optimal fluorescence emission peak is 440nm, and corresponding excitation wavelength is 340nm.Fig. 3 is its X-ray diffraction (XRD) spectrogram, and the carbon quantum dot obtained is decolorizing carbon.Fig. 4 is its photoelectron spectrum (XPS), and 284.7eV peak corresponds to greying sp2 carbon atom, and the peak of 286.3eV and 287.8eV corresponds to C-O and C=O carbon atom, carbon quantum dot oxygen-containing functional group.Fig. 5 is the photo of its differential responses time, and along with time lengthening, quantum dot concentration increases gradually, color burn.
Embodiment 2
The butanol solution of preparation 1.5mol/L sodium hydroxide, room temperature standing and reacting 120h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 60h of 2000 through the molecular weight that dams by carbon quantum dot dispersion liquid, vacuum-drying 12h at 120 DEG C, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 6, and particle diameter is comparatively even, is less than 5nm.
Embodiment 3
The ethylene glycol solution of preparation 5mol/L sodium hydroxide, oil bath is heated, and reacts 2h at 200 DEG C, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 120h of 2000 through the molecular weight that dams by carbon quantum dot dispersion liquid, vacuum-drying 4h at 150 DEG C, obtains carbon quantum dot solid.Its transmission electron microscope picture is Fig. 7, and particle diameter is comparatively even, and be less than 5nm, Fig. 8 is for obtaining carbon quantum dot solid photo.
Embodiment 4
The ethanolic soln of preparation 0.5mol/L lithium hydroxide, room temperature (25 DEG C) standing and reacting 360h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 10h of 500 through the molecular weight that dams by carbon quantum dot dispersion liquid, vacuum-drying 24h at 80 DEG C, obtains carbon quantum dot solid.
Embodiment 5
The butanol solution of preparation 1.5mol/L potassium hydroxide, room temperature standing and reacting 240h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 120h of 5000 through the molecular weight that dams by carbon quantum dot dispersion liquid, vacuum-drying 10h at 120 DEG C, obtains carbon quantum dot solid.
Embodiment 6
The ethylene glycol solution of preparation 2mol/L potassium hydroxide, oil bath is heated, and reacts 4h at 120 DEG C, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; Be the dialysis tubing dialysis 120h of 5000 through the molecular weight that dams by carbon quantum dot dispersion liquid, vacuum-drying 10h at 120 DEG C, obtains carbon quantum dot solid.
Embodiment 7
The ethanolic soln of preparation 10mol/L potassium hydroxide, room temperature standing and reacting 48h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; By the dialysis tubing dialysis 120h of carbon quantum dot dispersion liquid through molecular weight cut-off 2000, vacuum-drying 10h at 120 DEG C, obtains carbon quantum dot solid.
Embodiment 8
The decyl alcohol solution of preparation 2mol/L sodium hydroxide, room temperature standing and reacting 120h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; By the dialysis tubing dialysis 120h of carbon quantum dot dispersion liquid through molecular weight cut-off 2000, vacuum-drying 12h at 100 DEG C, obtains carbon quantum dot solid.
Embodiment 9
The stearyl alcohol solution of preparation 1mol/L sodium hydroxide, oil bath is heated, and reacts 8h at 100 DEG C, take out the dispersion liquid that supernatant liquor obtains carbon quantum dot; By the dialysis tubing dialysis 120h of carbon quantum dot dispersion liquid through molecular weight cut-off 2000, vacuum-drying 10h at 120 DEG C, obtains carbon quantum dot solid.
Embodiment 10
The benzyl alcohol solution of preparation 3mol/L potassium hydroxide, room temperature standing and reacting 100h, takes out the dispersion liquid that supernatant liquor obtains carbon quantum dot; By the dialysis tubing dialysis 96h of carbon quantum dot dispersion liquid through molecular weight cut-off 3000, vacuum-drying 8h at 150 DEG C, obtains carbon quantum dot solid.
The alcohol selected in the embodiment of the present invention is that carbonatoms is more than or equal to 2, be less than or equal to the monohydroxy-alcohol of 30, dibasic alcohol, polyvalent alcohol, as ethanol, propyl alcohol, butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, lauryl alcohol (lauryl alcohol), tridecanol, tetradecyl alcohol (tetradecyl alcohol), pentadecanol, hexadecanol (palmityl alcohol), heptadecyl alcohol, stearyl alcohol (stearyl alcohol), nonadecanol, eicosanol (n-Eicosanol), behenyl alcohol (behenyl alcohol), tetracosanol (wooden burnt alcohol), hexacosyl alcohol (ceryl alcohol), octacosanol, triacontanol (myricyl alcohol), ethylene glycol, glycerol, vinyl carbinol, phenylcarbinol, one or more in phenylethyl alcohol, alkali comprises: lithium hydroxide, potassium hydroxide, sodium hydroxide, phosphoric acid salt, carbonate, ammonia etc.
Claims (10)
1. alcohol decomposes the method preparing carbon quantum dot, it is characterized in that, the alcoholic solution of preparation alkaline matter, standing and reacting, obtains the dispersion liquid of carbon containing quantum dot, and purified for this dispersion liquid, drying are obtained carbon quantum dot solid.
2. method according to claim 1, is characterized in that, described alcohol is that carbonatoms is more than or equal to 2, is less than or equal to the monohydroxy-alcohol of 30, dibasic alcohol or polyvalent alcohol.
3. method according to claim 2, it is characterized in that, described alcohol is one or more in ethanol, propyl alcohol, butanols, amylalcohol, hexanol, enanthol, octanol, nonyl alcohol, decyl alcohol, lauryl alcohol, tridecanol, tetradecyl alcohol, pentadecanol, hexadecanol, heptadecyl alcohol, stearyl alcohol, nonadecanol, eicosanol, behenyl alcohol, tetracosanol, hexacosyl alcohol, octacosanol, triacontanol, ethylene glycol, glycerol, vinyl carbinol, phenylcarbinol, phenylethyl alcohol.
4. method according to claim 1, is characterized in that, described alkaline matter is one or more in lithium hydroxide, potassium hydroxide, sodium hydroxide, phosphoric acid salt, carbonate.
5. the method according to claim 1 or 4, is characterized in that, the concentration of described alkaline matter in alcoholic solution is 0.1-10mol/L.
6. the method according to any one of claim 1-4, is characterized in that, the reaction times is 2-360h; Temperature of reaction is 15-200 DEG C.
7. method according to claim 6, is characterized in that, the reaction times is 48-120h; Temperature of reaction is 25-120 DEG C.
8. method according to claim 1, is characterized in that, described way of purification is dialysis.
9. method according to claim 1, is characterized in that, described carbon quantum dot size is less than 5nm.
10. method according to claim 1, is characterized in that, described drying is vacuum-drying, and temperature is 80-150 DEG C; Time of drying is 4-24h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927848A (en) * | 2015-06-16 | 2015-09-23 | 复旦大学 | Bioimaging probe and material of oxygen reduction catalyst and preparation method thereof |
| CN105129764A (en) * | 2015-07-14 | 2015-12-09 | 中南大学 | Method of quickly preparing carbon quantum dots at high yield through aldehyde compound |
| CN109337682A (en) * | 2018-12-26 | 2019-02-15 | 赵方浩 | A kind of method that room temperature prepares fluorescent carbon quantum dot |
| CN110257060A (en) * | 2019-07-09 | 2019-09-20 | 西南大学 | Utilize the method and product of resveratrol preparation carbon dots and application |
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| CN102942924A (en) * | 2012-10-22 | 2013-02-27 | 上海交通大学 | Preparation method of carbon quantum dots based on chemical reaction of fructose and sodium hydroxide |
| CN103449404A (en) * | 2013-08-27 | 2013-12-18 | 湖南师范大学 | Method for preparing fluorescent carbon dots (C-dots) from alcohol through electrochemical carbonization |
| CN103482598A (en) * | 2013-08-30 | 2014-01-01 | 吉林大学 | Preparation method for monophosphate-adjuvant water-soluble fluorescent carbon quantum dot solid powder |
| CN104031642A (en) * | 2014-06-24 | 2014-09-10 | 山西大学 | Fluorescence carbon quantum dots, and preparation method and application thereof |
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- 2014-10-22 CN CN201410566040.2A patent/CN104386666B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102942924A (en) * | 2012-10-22 | 2013-02-27 | 上海交通大学 | Preparation method of carbon quantum dots based on chemical reaction of fructose and sodium hydroxide |
| CN103449404A (en) * | 2013-08-27 | 2013-12-18 | 湖南师范大学 | Method for preparing fluorescent carbon dots (C-dots) from alcohol through electrochemical carbonization |
| CN103482598A (en) * | 2013-08-30 | 2014-01-01 | 吉林大学 | Preparation method for monophosphate-adjuvant water-soluble fluorescent carbon quantum dot solid powder |
| CN104031642A (en) * | 2014-06-24 | 2014-09-10 | 山西大学 | Fluorescence carbon quantum dots, and preparation method and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104927848A (en) * | 2015-06-16 | 2015-09-23 | 复旦大学 | Bioimaging probe and material of oxygen reduction catalyst and preparation method thereof |
| CN104927848B (en) * | 2015-06-16 | 2017-03-29 | 复旦大学 | Material of bio-imaging probe and oxygen reduction catalyst and preparation method thereof |
| CN105129764A (en) * | 2015-07-14 | 2015-12-09 | 中南大学 | Method of quickly preparing carbon quantum dots at high yield through aldehyde compound |
| CN109337682A (en) * | 2018-12-26 | 2019-02-15 | 赵方浩 | A kind of method that room temperature prepares fluorescent carbon quantum dot |
| CN110257060A (en) * | 2019-07-09 | 2019-09-20 | 西南大学 | Utilize the method and product of resveratrol preparation carbon dots and application |
| CN110257060B (en) * | 2019-07-09 | 2020-08-28 | 西南大学 | Method for preparing carbon dots by using resveratrol, product and application |
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