CN105419793A - Method for microwave synthesis of carbon quantum dots on basis of citric acid and hexamethylene tetramine - Google Patents
Method for microwave synthesis of carbon quantum dots on basis of citric acid and hexamethylene tetramine Download PDFInfo
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- CN105419793A CN105419793A CN201511004821.3A CN201511004821A CN105419793A CN 105419793 A CN105419793 A CN 105419793A CN 201511004821 A CN201511004821 A CN 201511004821A CN 105419793 A CN105419793 A CN 105419793A
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Abstract
The invention discloses a method for microwave synthesis of carbon quantum dots on basis of citric acid and hexamethylene tetramine. The method comprises the following steps: respectively adding citric acid and hexamethylene tetramine to a 50-100mL conical flask, adding 5-15mL of deionized water, oscillating the conical flask to completely dissolve citric acid and hexamethylene tetramine, placing the conical flask in a microwave oven, carrying out microwave heating for 3-6min, taking out the conical flask, naturally cooling the conical flask, adding 20-100mL of deionized water, stirring the obtained solution to dissolve in order to obtain a suspension, centrifuging the suspension to remove insoluble substances, taking the obtained supernatant, dialyzing to remove impurities in order to obtain an aqueous solution of fluorescence carbon quantum dots, and freeze-drying the aqueous solution of fluorescence carbon quantum dots to obtain carbon quantum dot powder. The method has the advantages of simple process, wide sources, non-toxicity and harmlessness of raw materials, and high solution stability, is hopeful to be applied in fields of cell imaging and analysis and detection.
Description
Technical field
The invention belongs to carbon nanomaterial preparation technology field, be specifically related to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot.
Background technology
Carbon quantum dot is a kind of novel fluorescence carbon nano-particles occurred in recent years.2004, (the JAm.Chem.Soc such as Xu, 2004,126, Late Cambrian sends the material of fluorescence under ultra violet lamp when Single Walled Carbon Nanotube prepared by cigarette ash 12736-12737) produced at purification arc-over, obtain three groups of different fluorescent carbon nano-particles of molecular weight through further electrophoretic separation, send blue-greenish colour, yellow and orange fluorescence respectively.Carbon quantum dot is once discovery, and just cause people and study interest greatly, compare with traditional quantum dot, carbon quantum dot has hypotoxicity, and chemical stability is good, and light emitting region is adjustable, without optical flare, can synthesize on a large scale, substantially the not characteristic such as damaging cells.Therefore, the quantum dot that hypotoxic carbon quantum dot has now started to replace bio-toxicity larger is applied to the life sciences such as bio-imaging, biochemical analysis detection, pharmaceutical carrier, is the fluorescent nano material being expected to most realize applying in disease detection.
At present, define the preparation method of multiple carbon quantum dot both at home and abroad, comprising: laser ablation method, electrochemical process, acid oxidation, hydrothermal method, but these methods mostly need exacting terms, tediously long process.Preparation process is complicated, high energy consumption, expensive starting materials, uses the shortcoming such as strong acid and organic solvent to become and restricts the important factor that carbon quantum dot is generalized to practical application.Therefore, seek a kind of simple, cheap, green, the method being applicable to scale operation prepares the significant challenge that carbon quantum dot becomes this field.
Summary of the invention
The object of the present invention is to provide a kind of preparation process simple, raw material is easy to get, and mass-producing can prepare the method for carbon quantum dot.
To achieve these goals, a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot is provided.Be achieved through the following technical solutions: respectively citric acid and hexamethylenetetramine are added in 50-100mL Erlenmeyer flask, add 5-15mL deionized water, vibration makes it dissolve completely, is placed in microwave heating 3-6min in microwave oven, takes out after its naturally cooling, add 20-100mL deionized water, stirring and dissolving obtains suspension, centrifugal removing insolubles, gets supernatant liquor dialysis removing impurity, namely obtain the fluorescent carbon quantum dot aqueous solution, at-50 DEG C, after lyophilize, namely obtain carbon quantum dot powder.
Described citric acid and the mol ratio of hexamethylenetetramine are between 1: 1 ~ 2, and optimum proportion is 1: 0.6.
Described microwave heating power is 400w-800w.
Described centrifugal speed is 8000r/min-10000r/min.
Described dialysis adopts the dialysis tubing of 1000-3000Da.
The excitation wavelength range 310-600nm of described carbon quantum dot, maximum excitation wavelength 420-430nm; Emission wavelength ranges 330-700nm, maximum emission wavelength 470-510nm.
Adopt fluorescent carbon quantum dot prepared by method of the present invention, preparation method is simple, and cost is low, and the operating time is short, raw material citric acid and hexamethylenetetramine safety non-toxic, and the fluorescent carbon quantum dot stability obtained is high.
Below in conjunction with drawings and Examples, the present invention is further illustrated, but following examples should not regard limitation of the invention as.
Accompanying drawing explanation
Fig. 1 is the reaction schematic diagram of fluorescent carbon quantum dot prepared by the embodiment of the present invention 1.
Fig. 2 is the transmission electron microscope picture of fluorescent carbon quantum dot prepared by the embodiment of the present invention 1.
Fig. 3 is uv-absorbing and the fluorescence spectrum figure of fluorescent carbon quantum dot prepared by the embodiment of the present invention 1, and illustration is the photo of the carbon quantum dot aqueous solution under natural light and under ultra violet lamp.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Take citric acid 5.25g respectively, hexamethylenetetramine 2.16g, jointly join in 100mL Erlenmeyer flask, 10mL deionized water is added in Erlenmeyer flask, abundant vibration makes it dissolve completely, being placed in microwave oven take microwave power as 800w microwave heating reaction 5min, taking-up is after its naturally cooling, add 30mL deionized water, stirring and dissolving obtains suspension, with the centrifugation of 10000r/min removing insolubles, dialysis removing impurity in the dialysis tubing of 3000Da specification, namely the fluorescent carbon quantum dot aqueous solution is obtained, namely carbon quantum dot powder is obtained after lyophilize at-50 DEG C.
Embodiment 2
Take citric acid 5.25g respectively, hexamethylenetetramine 3.60g, jointly join in 100mL Erlenmeyer flask, 15mL deionized water is added in Erlenmeyer flask, abundant vibration makes it dissolve completely, being placed in microwave oven take microwave power as 600w microwave heating reaction 3min, taking-up is after its naturally cooling, add 100mL deionized water, stirring and dissolving obtains suspension, with the centrifugation of 8000r/min removing insolubles, dialysis removing impurity in the dialysis tubing of 1000Da specification, namely the fluorescent carbon quantum dot aqueous solution is obtained, namely carbon quantum dot powder is obtained after lyophilize at-50 DEG C.
Embodiment 3
Take citric acid 5.25g respectively, hexamethylenetetramine 1.80g, jointly join in 50mL Erlenmeyer flask, 5mL deionized water is added in Erlenmeyer flask, abundant vibration makes it dissolve completely, being placed in microwave oven take microwave power as 400w microwave heating reaction 3min, taking-up is after its naturally cooling, add 20mL deionized water, stirring and dissolving obtains suspension, with the centrifugation of 9000r/min removing insolubles, and dialysis removing impurity in the dialysis tubing of 2000Da specification, namely obtain the fluorescent carbon quantum dot aqueous solution, at-50 DEG C, after lyophilize, namely obtain carbon quantum dot powder.
Embodiment 4
Take citric acid 5.25g respectively, hexamethylenetetramine 2.88g, jointly join in 100mL Erlenmeyer flask, 10mL deionized water is added in Erlenmeyer flask, abundant vibration makes it dissolve completely, being placed in microwave oven take microwave power as 500w microwave heating reaction 6min, taking-up is after its naturally cooling, add 50mL deionized water, stirring and dissolving obtains suspension, with the centrifugation of 10000r/min removing insolubles, dialysis removing impurity in the dialysis tubing of 3000Da specification, namely the fluorescent carbon quantum dot aqueous solution is obtained, namely carbon quantum dot powder is obtained after lyophilize at-50 DEG C.
Claims (6)
1. the method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot, it is characterized in that, comprise the following steps: respectively citric acid and hexamethylenetetramine are added in 50-100mL Erlenmeyer flask, add 5-15mL deionized water, vibration makes it dissolve completely, be placed in microwave heating 3-6min in microwave oven, taking-up is after its naturally cooling, add 20-100mL deionized water, stirring and dissolving obtains suspension, centrifugal removing insolubles, get supernatant liquor dialysis removing impurity, namely the fluorescent carbon quantum dot aqueous solution is obtained, namely carbon quantum dot powder is obtained after lyophilize at-50 DEG C.
2., according to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot described in claim 1, it is characterized in that, citric acid used and the mol ratio of hexamethylenetetramine are between 1: 1 ~ 2, and optimum proportion is 1: 0.6.
3., according to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot described in claim 1, it is characterized in that, described microwave heating power is 400w-800w.
4., according to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot described in claim 1, it is characterized in that, described centrifugal speed is 8000r/min-10000r/min.
5., according to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot described in claim 1, it is characterized in that, described dialysis adopts the dialysis tubing of 1000-3000Da.
6., according to a kind of method based on citric acid and hexamethylenetetramine Microwave synthesize carbon quantum dot described in claim 1, it is characterized in that, the excitation wavelength range 310-600nm of described carbon quantum dot, maximum excitation wavelength 420-430nm; Emission wavelength ranges 330-700nm, maximum emission wavelength 470-510nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106892420A (en) * | 2017-02-22 | 2017-06-27 | 太原理工大学 | A kind of fast preparation method of the solid luminescent carbon point of high-fluorescence quantum yield |
| CN107057686A (en) * | 2017-05-12 | 2017-08-18 | 临沂大学 | A kind of New Solid yellow fluorescent powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103045242A (en) * | 2013-01-21 | 2013-04-17 | 吉林大学 | Preparation method of carbon dot having high fluorescent quantum yield |
| CN104017576A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction |
| CN104709891A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Hydrothermal preparation method of fluorescent nano carbon dots |
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- 2015-12-28 CN CN201511004821.3A patent/CN105419793A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103045242A (en) * | 2013-01-21 | 2013-04-17 | 吉林大学 | Preparation method of carbon dot having high fluorescent quantum yield |
| CN104709891A (en) * | 2013-12-11 | 2015-06-17 | 江南大学 | Hydrothermal preparation method of fluorescent nano carbon dots |
| CN104017576A (en) * | 2014-06-20 | 2014-09-03 | 上海交通大学 | Method for synthesizing nitrogen-doped carbon quantum dots based on calcium citrate and urea microwave reaction |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106892420A (en) * | 2017-02-22 | 2017-06-27 | 太原理工大学 | A kind of fast preparation method of the solid luminescent carbon point of high-fluorescence quantum yield |
| CN107057686A (en) * | 2017-05-12 | 2017-08-18 | 临沂大学 | A kind of New Solid yellow fluorescent powder |
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Application publication date: 20160323 |