CN105565302A - Method for preparation of graphene quantum dots on the basis of hypochlorite radical oxidation - Google Patents
Method for preparation of graphene quantum dots on the basis of hypochlorite radical oxidation Download PDFInfo
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Abstract
The present invention discloses a method for preparation of graphene quantum dots on the basis of hypochlorite radical oxidation, the specific steps are as follows: solid graphite oxide is dispersed in deionized water and dispersed under ultrasonic action, so that the graphite oxide is dispersed and peeled into monolayers, and a graphene oxide aqueous solution is obtained; then the graphene oxide aqueous solution is mixed with an aqueous solution containing hypochlorite radicals at room temperature to obtain a mixed solution; and finally, the mixed solution is irradiated by ultraviolet light for 5min-3h to obtain the graphene quantum dots. By use of ultraviolet radiation and other means, the graphene quantum dots can be obtained by direct reaction of the strong oxidizing aqueous solution containing the hypochlorite radicals of graphene oxide, preparation process is greatly abbreviated, compared with the prior art, the reaction time of the method is shortened from as long as 20 days to tens of minutes, and compared with inefficient physical methods, the yield of the method is nearly 80%.
Description
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind ofly carry out method prepared by graphene quantum dot based on hypochlorite oxidation.
Background technology
Since the discovery of Graphene in 2004, Graphene causes the research boom of basic science and Application Areas because of the electricity of its excellence, calorifics, the character such as optics and mechanics.Such as, Graphene has high carrier mobility (200,000cm2V-1s-1) with thermal conductivity (~ 5,000Wm-1K-1), and room-temperature quantum Hall effect (QuantumHallEffect), be expected to replace the desirable material that silicon becomes high performance electronics.But Graphene is a kind of semi-metallic of zero band gap, this property limits its application in the field such as semiconducter device and opto-electronic device, as field-effect transistor (FETs).Opening Graphene band gap, it is transformed into semiconductor material from semi-metallic, is a frontier nature research topic of Graphene research field.At present, open Graphene band gap and mainly comprise both direction, one is based on quantum effect, and Graphene is cut into nano belt, and nanometer sieve or quantum dot, one dimension or two-dimensional directional realize nano-scale dimension.Two is carry out doping and surface-functionalized to destroy its π-electron conjugated system to Graphene.Graphene quantum dot (GQDs) is the graphene nanometer sheet that two-dimensional is less than 100nm, and due to quantum effect, it has special photoelectronics character, is with a wide range of applications in fields such as biological medicine, solar cell, opto-electronic devices.
The preparation method of the relevant graphene quantum dot that document has been reported is mainly divided into from bottom to top and two kinds of methods from top to bottom.Self-absorption Correction Factor mainly refers to organic molecule to be presoma, forms carbon-carbon bond, organic molecule is aggregated into the graphene quantum dot with large conjugated structure by chemical polycondensation.The method preparation process complexity is loaded down with trivial details, reaction time consumption long and productivity ratio is lower.In addition, in building-up process, GQDs very easily reunites, and is difficult to the GQDs obtaining large-size.Be from top to bottom with Graphene or carbon fiber for raw material, by chemical oxidation, its oxygen cutting is become quantum dot.But the graphene quantum dot productive rate utilizing the method to prepare is low, and carbon conjugated backbone wrecks, degree is comparatively serious.The people such as Ajayan are at " NanoLetters " (2012,12,844-849) magazine is delivered the article being entitled as " Graphenequantumdotsderivedfromcarbonfibers (being that graphene quantum dot prepared by raw material with carbon fiber) ", the author of this article utilizes carbon fiber to have Rotating fields, and the advantage of its diameter in nano-scale range, (the vitriol oil: concentrated nitric acid=3:1 under nitration mixture condition, V/V), high-temperature stirring, destroyed the laminate structure of carbon fiber by the method being oxidized intercalation, prepare graphene quantum dot.But the graphene quantum dot obtained by the method has the thickness of one deck to multilayer, it is not the graphene quantum dot with monoatomic layer thickness truly.The people such as XuejiaoZhou are at " ACSNano " (2012, 6, 6592) magazine has been delivered the article being entitled as " Photo-FentonReactionofGrapheneOxide:ANewStrategytoPrepar eGrapheneQuantumDotsforDNAcleavage (light of graphene oxide assists-fenton reaction: a kind of novel processing step of graphene quantum dot and the cutting action research to DNA thereof) ", under UV-irradiation, author utilizes the light of graphene oxide to assist-fenton reaction, by controlling the reaction times, successfully prepare graphene quantum dot, the method is utilized to prepare the system of graphene quantum dot without the need to using strong acid and hot conditions, by product is less, be a kind of reaction be one graphene quantum dot preparation method fast and effectively.But, the pH value of system needs more strictly to control in 3 ~ 4 scopes, under comparatively strong acidic condition (pH<3), graphene oxide is easily reunited, as system pH>4, speed of reaction reduces, and mainly because when solution alkaline, is unfavorable for the generation of hydroxyl radical free radical (OH).In addition, it is low all to there is productive rate in the method preparing graphene quantum dot existed at present, consuming timely waits not enough, therefore, urgently seeks a kind of simple and quick and within the scope of wider pH, prepare the novel method of graphene quantum dot.
Summary of the invention
The object of this invention is to provide and a kind ofly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, solve existing graphene quantum dot preparation process consuming time, the problem that the productive rate of graphene quantum dot is low.
The technical solution adopted in the present invention is, be oxidized the method for carrying out graphene quantum dot and preparing based on hypochlorite, concrete steps are:
Step 1: by solid oxidation graphite dispersion in deionized water, disperses under ultrasonication, makes graphite oxide disperse to peel off into individual layer, obtains graphene oxide water solution;
Step 2: step 1 gained graphene oxide water solution and the aqueous solution containing hypochlorite are at room temperature mixed, obtains mixing solutions; Utilize UV-light to carry out irradiation 5min ~ 5h to mixing solutions subsequently, obtain graphene quantum dot.
Feature of the present invention is also,
In step 1, ultrasonication process is: be 40kHz in frequency, and power is disperse 1h under the ultrasonic wave of 160W.
The concentration of step 1 gained graphene oxide water solution is 0.01 ~ 4mg/mL.
In step 2, the aqueous solution containing hypochlorite is the one in hypochlorous acid, clorox or calcium hypochlorite solution.
Be 1 ~ 30% containing available chlorine content in the aqueous solution of hypochlorite.
Graphene oxide water solution is 10 ~ 100:1 with the aqueous solution volume ratio containing hypochlorite.
In step 2, the pH of gained mixing solutions is 3 ~ 14.
In step 2, the wavelength of UV-light is 190 ~ 400nm, and power is 100 ~ 1000W.
The invention has the beneficial effects as follows, the present invention is by means such as uv irradiatings, in aqueous phase system, utilize the hypochlorite aqueous solution with Strong oxdiative performance and graphene oxide directly to react, prepare graphene quantum dot, this process is breviaty preparation technology's flow process greatly, and compared to prior art, the inventive method reaction times reaches 20 days foreshorten to dozens of minutes from lasting, compared with the physical method of inefficiency, productive rate closely reaches 80%.
Accompanying drawing explanation
Fig. 1 is the atomic force microscope figure of graphene oxide;
Fig. 2 the present invention is based on the atomic force microscope figure that embodiment of the method 3 gained graphene quantum dot prepared by graphene quantum dot is carried out in hypochlorite oxidation;
Fig. 3 be the present invention is based on hypochlorite oxidation carry out embodiment of the method 3 gained graphene quantum dot low range prepared by graphene quantum dot under transmission electron microscopy figure.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
The present invention is a kind of is oxidized the method for carrying out graphene quantum dot and preparing based on hypochlorite, concrete steps are:
Step 1: to utilize Hummers legal system for the graphene oxide of gained for initiator, disperseed in deionized water, disperse under ultrasonication, makes graphite oxide disperse to peel off into individual layer, obtains graphene oxide water solution; Wherein, ultrasonication process is: be 40kHz in frequency, and power is disperse 1h under the ultrasonic wave of 160W; The concentration of gained graphene oxide water solution is 0.01 ~ 4mg/mL.
Step 2: step 1 gained graphene oxide water solution and the aqueous solution containing hypochlorite are at room temperature mixed, obtaining pH is 3 ~ 14 mixing solutionss; Utilize wavelength to be 190 ~ 400nm subsequently, power is that the UV-light of 100 ~ 1000W carries out irradiation 5min ~ 5h to mixing solutions, obtains graphene quantum dot.Wherein, the aqueous solution containing hypochlorite is the one in hypochlorous acid, clorox or calcium hypochlorite solution.Be 1 ~ 30% containing available chlorine content in the aqueous solution of hypochlorite.Graphene oxide water solution is 10 ~ 100:1 with the aqueous solution volume ratio containing hypochlorite.
Embodiment 1
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 0.01mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 1.0% aqueous sodium hypochlorite solution by volume 10 ︰ 1 mix, regulator solution system pH is 3, use power 100W, predominant wavelength be the ultraviolet lamp of 190nm to mixing solutions irradiation 5h, obtain graphene quantum dot.
Embodiment 2
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 0.05mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 5.0% aqueous sodium hypochlorite solution by volume 20 ︰ 1 mix, regulator solution system pH is 5, use power 200W, predominant wavelength be the ultraviolet lamp of 254nm to mixing solutions irradiation 3h, prepare graphene quantum dot.
Embodiment 3
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 0.5mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 5.0% aqueous sodium hypochlorite solution by volume 30 ︰ 1 mix, regulator solution system pH is 10, the ultraviolet lamp by power 1000W, predominant wavelength being 254nm, to mixing solutions irradiation 10min, obtains graphene quantum dot.
As can be seen from atomic force microscope figure (Fig. 2) and transmission electron microscope figure (Fig. 3), gained graphene quantum dot its two-dimensional compared with graphene oxide (Fig. 1) is reduced to 20-30 nano level from micron order, distribution of sizes is homogeneous, and only has an atomic layer level thickness.
Embodiment 4
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 0.5mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 15.0% the Losantin aqueous solution by volume 50 ︰ 1 mix, regulator solution system pH is 10, use power 500W, predominant wavelength be the ultraviolet lamp of 365nm to mixing solutions irradiation 30min, prepare graphene quantum dot.
Embodiment 5
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 1.0mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 20.0% aqueous sodium hypochlorite solution by volume 50 ︰ 1 mix, regulator solution system pH is 14, use power 1000W, predominant wavelength be the ultraviolet lamp of 365nm to mixing solutions irradiation 15min, prepare graphene quantum dot.
Embodiment 6
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 4.0mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 30% hypochloric acid water solution by volume 100 ︰ 1 mix, regulator solution system pH is 14, use power 1000W, predominant wavelength be the ultraviolet lamp of 400nm to mixing solutions irradiation 15min, obtain graphene quantum dot.
Embodiment 7
Take graphene oxide water solution as initiator, under ultraviolet radiation, utilize hypochlorite to carry out oxidation to it and prepare graphene quantum dot, specifically comprise the following steps:
(1) by graphene oxide solid dispersal in deionized water, at frequency 40kHz, under the ultrasonication of power 160W, disperse 1h, individual layer is peeled off in graphite oxide dispersion, obtains the graphene oxide water solution that concentration is 0.5mg/mL;
(2) by step 1 gained graphene oxide water solution and available chlorine content be 10.0% aqueous sodium hypochlorite solution by volume 30 ︰ 1 mix, regulator solution system pH is 7, use power 1000W, predominant wavelength be the ultraviolet lamp of 365nm to mixing solutions irradiation 5min, obtain graphene quantum dot.
The power of the inventive method medium ultraviolet light and the consumption of hypochlorite directly have influence on the preparation efficiency of product, hypochlorous acid, clorox and Losantin are common oxygenant, be widely used in the fields such as bleaching, Industrial Wastewater Treatment, himself easily decomposes and forms oxyradical, when reacting with organic molecule, micromolecular compound can be oxidized to.Graphene oxide can regard the containing oxygen derivative of Graphene as, and its conjugated structure surface is containing a large amount of oxygen-containing functional group and defect, and angle is chemically a kind of organic conjugated molecule with larger molecular weight.And hypochlorite more easily and the carbon atom of fault location react, and the comparatively complete region of conjugated backbone structure is retained, the final oxidized cutting of graphene oxide and form the nanometer sheet that two-dimensional is less than 100nm, i.e. graphene quantum dot.Meanwhile, because the active substance participating in reaction is oxyradical, so reaction can complete fast within the extremely short time, and the consumption of hypochlorite directly affects the output capacity of graphene quantum dot, and therefore, the add-on of hypochlorite needs strict control.In addition, under certain density graphene oxide water solution and hypochlorite content condition, when the power of UV-light increases to 1000W by 500W, graphene quantum dot is prepared required time and is shortened to 15min by 1h.
Claims (8)
1. be oxidized the method for carrying out graphene quantum dot and preparing based on hypochlorite, it is characterized in that, concrete steps are:
Step 1: by solid oxidation graphite dispersion in deionized water, disperses under ultrasonication, makes graphite oxide disperse to peel off into individual layer, obtains graphene oxide water solution;
Step 2: step 1 gained graphene oxide water solution and the aqueous solution containing hypochlorite are at room temperature mixed, obtains mixing solutions; Utilize UV-light to carry out irradiation 5min ~ 5h to mixing solutions subsequently, obtain graphene quantum dot.
2. according to claim 1ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, in step 1, ultrasonication process is: be 40kHz in frequency, and power is disperse 1h under the ultrasonic wave of 160W.
3. according to claim 2ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, the concentration of step 1 gained graphene oxide water solution is 0.01 ~ 4mg/mL.
4. according to claim 1ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, in step 2, the aqueous solution containing hypochlorite is the one in hypochlorous acid, clorox or calcium hypochlorite solution.
5. according to claim 4ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, be 1 ~ 30% containing available chlorine content in the aqueous solution of hypochlorite.
6. according to claim 1ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, graphene oxide water solution is 10 ~ 100:1 with the aqueous solution volume ratio containing hypochlorite.
7. according to claim 1ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, in step 2, the pH of gained mixing solutions is 3 ~ 14.
8. according to claim 1ly carry out method prepared by graphene quantum dot based on hypochlorite oxidation, it is characterized in that, in step 2, the wavelength of UV-light is 190 ~ 400nm, and power is 100 ~ 1000W.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098336A (en) * | 2017-04-28 | 2017-08-29 | 成都川烯科技有限公司 | A kind of method that graphene quantum dot is prepared based on photochemical method |
| CN108946716A (en) * | 2018-09-30 | 2018-12-07 | 西安理工大学 | A kind of method that anacidity method prepares graphene quantum dot |
| CN112875686A (en) * | 2021-02-04 | 2021-06-01 | 上海交通大学 | Preparation method of porous graphene based on sodium hypochlorite |
| CN113620273A (en) * | 2021-08-13 | 2021-11-09 | 苏州大学 | Carbon-based metal-free functional quantum dot and preparation and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102336404A (en) * | 2011-07-19 | 2012-02-01 | 上海交通大学 | Preparation method of graphene oxide quantum dot based on photocatalytic oxidation |
| WO2014179708A1 (en) * | 2013-05-02 | 2014-11-06 | William Marsh Rice University | Methods of producing graphene quantum dots from coal and coke |
| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102336404A (en) * | 2011-07-19 | 2012-02-01 | 上海交通大学 | Preparation method of graphene oxide quantum dot based on photocatalytic oxidation |
| WO2014179708A1 (en) * | 2013-05-02 | 2014-11-06 | William Marsh Rice University | Methods of producing graphene quantum dots from coal and coke |
| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107098336A (en) * | 2017-04-28 | 2017-08-29 | 成都川烯科技有限公司 | A kind of method that graphene quantum dot is prepared based on photochemical method |
| CN108946716A (en) * | 2018-09-30 | 2018-12-07 | 西安理工大学 | A kind of method that anacidity method prepares graphene quantum dot |
| CN112875686A (en) * | 2021-02-04 | 2021-06-01 | 上海交通大学 | Preparation method of porous graphene based on sodium hypochlorite |
| CN113620273A (en) * | 2021-08-13 | 2021-11-09 | 苏州大学 | Carbon-based metal-free functional quantum dot and preparation and application thereof |
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