CN104045076A - Graphene oxide quantum dot preparation method - Google Patents
Graphene oxide quantum dot preparation method Download PDFInfo
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- CN104045076A CN104045076A CN201410023150.4A CN201410023150A CN104045076A CN 104045076 A CN104045076 A CN 104045076A CN 201410023150 A CN201410023150 A CN 201410023150A CN 104045076 A CN104045076 A CN 104045076A
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Abstract
The invention provides a graphene oxide quantum dot preparation method. The graphene oxide quantum dot preparation method comprises the following steps that citric acid and concentrated sulfuric acid are mixed and undergo a reaction under normal pressure to produce a graphene oxide quantum dot solution. The graphene oxide quantum dot preparation method has the advantages of simple processes, easy acquisition of raw materials, easy realization of technical conditions and short time consumption.
Description
Technical field
The present invention relates to a kind of New Inorganic Materials technical field, particularly relate to a kind of preparation method of graphene oxide quantum dot.
Background technology
Graphene quantum dot is the zero dimension Graphene that lateral dimension is less than 100nm, is a kind of emerging carbon nanomaterial.Compare with conventional large size two dimension graphene sheet layer, graphene quantum dot has significant fringing effect and quantum confined effect, thereby shows excellent optics and electric property.Compare with rare-earth oxide quantum dot with conventional carbon quantum dot, graphene quantum dot has good water-soluble, stable and regulatable photoluminescence performance, lower cytotoxicity and excellent biocompatibility.These feature performance benefits make graphene quantum dot have application prospect very widely at numerous areas such as photoelectric material and device, electrocatalysis, electrochemica biological sensing and bio-imagings, have become gradually the study hotspot in current Graphene field.
In existing technique, generally adopt graphene oxide quantum dot as presoma, through reduction, process and obtain graphene quantum dot to remove to a certain extent oxygen groups contained in structure and to recover conjugated structure.
The preparation method of graphene oxide quantum dot can be divided into from top to bottom method and from bottom to top method, specific as follows:
From top to bottom method mainly refers to the method for employing " chemical cutting ", and large size graphene oxide or celion are cut into undersized graphene oxide quantum dot.At present, " chemical cutting " mainly contain the modes such as secondary oxidation cutting, hydro-thermal cutting and electrochemistry cutting.As 2012, Zhu etc. are at RSC Adv., 2012,2, in 2717 one literary compositions, reported and take graphene oxide as raw material, in DMF solution, through 200 ℃ of hydro-thermal cutting 8h, prepare graphene oxide quantum dot solution, and can regulate within the specific limits by controlling the degree of oxidation of graphene oxide the fluorescence spectrum of graphene oxide quantum dot.And for example 2013 at Chem.Commun., 2013,49, in 5079 one literary compositions, the people such as Nurunnabi be take carbon fiber as raw material, through the vitriol oil and concentrated nitric acid mixed solution, the cutting through 12～18 hours at 65 ℃～110 ℃ can prepare graphene oxide quantum dot, and research finds that cutting temperature can be used to control the photoluminescence performance of graphene oxide quantum dot.
From bottom to top rule is to take organic molecule as raw material, through chemosynthesis, prepares graphene oxide quantum dot.If the people such as Liu in 2011 are at J.Am.Chem.Soc.2011, in 133,15,221 one literary compositions, reported and a kind ofly from poly aromatic toroidal molecule, through pyrolysis, prepared synthetic graphite, then through oxidation, obtained the method for graphene oxide quantum dot, the about 60nm of quantum dot lateral dimension of gained, distribution of sizes is very narrow.
Yet, no matter be method or from bottom to top method from top to bottom, the preparation technology of current graphene oxide quantum dot exists processing step complicated, and raw material is difficult to the problems such as acquisition.Therefore, research and development is simple, graphene oxide quantum dot preparation method has important practical significance efficiently.
Summary of the invention
The shortcoming of prior art in view of the above, the object of the present invention is to provide a kind of preparation method of graphene oxide quantum dot, and for solving the complicated process of preparation of prior art graphene oxide quantum dot, raw material is difficult to the problems such as acquisition.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of graphene oxide quantum dot, the preparation method of described graphene oxide quantum dot at least comprises:
Citric acid is mixed with the vitriol oil, described citric acid and the vitriol oil are reacted, form the first graphene oxide quantum dot solution.
Preferably, the condition that described citric acid and the vitriol oil react is: temperature of reaction is 25 ℃～100 ℃, and the reaction times is 1 hour～10 hours.
Preferably, after described citric acid mixes with the vitriol oil, the concentration of described citric acid is 0.1mg/mL～100mg/mL.
Preferably, the described mode that citric acid is mixed with the vitriol oil is standing, vibration, stirring or ultrasonic dispersion.
Preferably, the mass percent concentration of the described vitriol oil is 98%.
Preferably, after forming described the first graphene oxide quantum dot solution, also comprise described the first graphene oxide quantum dot solution is gone to deimpurity step.
Preferably, describedly to described the first graphene oxide quantum dot solution, go deimpurity step to comprise:
Regulating the pH value of described the first graphene oxide quantum dot solution is 4～9, obtains the second graphene oxide quantum dot solution;
To described the second graphene oxide quantum dot solution dialyse or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
Preferably, described the first graphene oxide quantum dot solution is removed after impurity, also comprised and being dried, to obtain the step of graphene oxide quantum dot powder.
Preferably, described in, carrying out dry method is lyophilize, rotary evaporation or supercritical drying.
As mentioned above, the preparation method of graphene oxide quantum dot of the present invention, has following beneficial effect:
Utilize citric acid and strong sulfuric acid response to prepare graphene oxide quantum dot, raw materials is easy to obtain, and preparation technology is simple, and the graphene oxide quantum dot making to have purity high, the advantage of the fluorescence property excellence showing.
Accompanying drawing explanation
Fig. 1 is shown as the preparation method's of graphene oxide quantum dot provided by the invention schematic diagram.
Fig. 2 is shown as the chemical structure schematic diagram of the citric acid using in the present invention.
Fig. 3 is the high resolving power TEM figure of the graphene oxide quantum dot that in embodiment mono-, technical scheme obtains.
Fig. 4 is the aqueous solution of the graphene oxide quantum dot that in embodiment mono-, technical scheme the obtains illuminated diagram under 325nm illumination.
Fig. 5 is the graphene oxide quantum dot fluorescence spectrum figure that in embodiment mono-, technical scheme obtains.
Element numbers explanation
S10～S40 step
Embodiment
Technical scheme of the present invention provides a kind of preparation method of graphene oxide quantum dot, adopts citric acid and the vitriol oil under low-temperature atmosphere-pressure, to prepare graphene oxide quantum dot solution, then by techniques such as removal of impurities are dried, obtains the powder of graphene oxide quantum dot.
Below, by specific specific examples explanation embodiments of the present invention, those skilled in the art can understand other advantages of the present invention and effect easily by the disclosed content of this specification sheets.The present invention can also be implemented or be applied by other different embodiment, and the every details in this specification sheets also can be based on different viewpoints and application, carries out various modifications or change not deviating under spirit of the present invention.
Refer to Fig. 1 to Fig. 5.It should be noted that, the diagram providing in the present embodiment only illustrates basic conception of the present invention in a schematic way, satisfy and only show with assembly relevant in the present invention in graphic but not component count, shape and size drafting while implementing according to reality, during its actual enforcement, kenel, quantity and the ratio of each assembly can be a kind of random change, and its assembly layout kenel also may be more complicated.
With reference to figure 1, the preparation method of graphene oxide quantum dot provided by the invention comprises:
Step S10: citric acid is mixed into the vitriol oil, forms the mixing solutions of citric acid and the vitriol oil.
Step S20: make the mixing solutions reaction of described citric acid and the vitriol oil under normal pressure, form the first graphene oxide quantum dot solution.
In embodiment, the preparation method of described graphene oxide quantum dot also comprises:
Step S30: described the first graphene oxide quantum dot solution is removed to impurity.
Step S40: be dried, to obtain graphene oxide quantum dot powder.
Concrete, the preparation method of described graphene oxide quantum dot provided by the invention can be:
First, execution step S10: citric acid is mixed with the vitriol oil, form the mixing solutions of citric acid and the vitriol oil.
Citric acid is a kind of organic monoacid, is colourless crystallization or white crystalline powder.Chemical structure, citric acid is a kind of tricarboxylic acid compounds, is called again 2-hydroxy propane-1,2,3-tricarboxylic acid, and molecular formula is C
6h
8o
7, molecular structure as shown in Figure 2.In general, citric acid is as foodstuff additive, for food mfg.
The vitriol oil is a kind of common inorganic acid, and concentration is generally 98%(concentration and refers to H
2sO
4the aqueous solution in H
2sO
4mass percent), there is dehydration property, strong oxidizing property, difficult volatility, acidity, stability, water-absorbent etc.
In this step, citric acid is mixed with the vitriol oil.The mode of described mixing can be standing, vibration, stirring or ultrasonic dispersion, so that mix full and uniform with the vitriol oil of citric acid.
Described standing mode, for citric acid is put into container, is put into the vitriol oil subsequently, and standing 8h～20h is fully dissolved in the vitriol oil citric acid.
The mode of described vibration, for citric acid is put into container, is put into the vitriol oil subsequently, and the container that then vibrates is fully dissolved in the vitriol oil citric acid.
The mode of described stirring can be put into the vitriol oil subsequently for citric acid is put into container, then with magnetic stirring apparatus, stirs, and the stirring velocity of described magnetic agitation is 200r/min～1500r/min, and churning time is 0.1h～6h.
The power of described ultrasonic dispersion is 100W～500W, and frequency is 10kHz～100kHz, and the time is 0.1h～6h.
After described citric acid mixes with the vitriol oil, the concentration of described citric acid is 0.1mg/mL～100mg/mL, if be less than the waste that this scope can cause the vitriol oil, concentration is greater than this scope and can causes the reaction in subsequent technique to carry out not exclusively, can not get graphene oxide quantum dot.
Next, execution step S20: make the mixing solutions reaction of described citric acid and the vitriol oil under normal pressure, form the first graphene oxide quantum dot solution.
In actually operating, this step is almost carried out with the step that citric acid and the vitriol oil are mixed in previous step simultaneously.Concrete, in by citric acid and vitriol oil mixing, set temperature is 25 ℃～100 ℃, the reaction times is 1 hour～10 hours.Wherein, in actually operating, the time that citric acid and the vitriol oil are mixed and the time of both interreactions link up, and because mixing is the process of dissolving, the time is shorter, and the reaction times is longer.
Compare with traditional technique of preparing graphene oxide quantum dot, in technical scheme of the present invention, described temperature of reaction is relatively low, is convenient to realize.In this step, can, by citric acid and the vitriol oil are placed on to thermostat, by controlling the temperature of thermostat, realize the temperature of controlling citric acid and strong sulfuric acid response.Described thermostat can be water-bath, oil bath etc.
Described temperature is higher, reacts faster, and the reaction times of the reactant of same dose is longer, and described temperature is lower, and the reaction times is longer, and the reaction times of the reactant of same dose is shorter.In technical scheme of the present invention, with respect to other reaction conditions, described temperature is also comparatively gentle on the impact of reaction process, therefore in other embodiment, described temperature of reaction also can surpass this scope, the reaction times also can change accordingly.
In the reaction process of citric acid and the vitriol oil, the vitriol oil can promote dehydrating condensation and the carburizing reagent between citric acid molecule.Concrete, under the effect of the vitriol oil, first citric acid sloughs oxy radicals a large amount of in molecule as carboxyl and hydroxyl, and further carbonization forms aromatic nucleus conjugated structure, and along with the carrying out of reaction, aromatic ring structure is grown up gradually, forms graphene oxide quantum dot.
Through this single step reaction, the mixing liquid of citric acid and the vitriol oil becomes the first graphene oxide quantum dot solution.
Next, execution step S30: described the first graphene oxide quantum dot solution is removed to impurity, described in go deimpurity mode to comprise:
First, regulate pH value to 4～9 of described the first graphene oxide quantum dot solution, obtain the second graphene oxide quantum dot solution;
Then, to described the second graphene oxide quantum dot solution dialyse or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
In the present embodiment, regulate the mode of pH value of described the first graphene oxide quantum dot solution for to add a certain amount of alkaline matter in the first graphene oxide quantum dot solution, described alkaline matter can be ammoniacal liquor, hydroxide aqueous solution, carbonate or sulfide.Concrete, can be strong aqua, sodium hydroxide, sodium carbonate or sodium sulphite etc.
Removal impurity through this step, obtains highly purified the second graphene oxide quantum dot solution.
Next, execution step S40: described the second graphene oxide quantum dot solution is dried, to obtain graphene oxide quantum dot powder.Described drying means can be lyophilize, rotary evaporation or supercritical drying.
By specific specific examples, technical scheme of the present invention is described below.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.
Embodiment 1
To successively adding 30mg citric acid and the 30mL vitriol oil in round-bottomed flask, in 50 ℃ of water-baths, stir 5h, obtain graphene oxide quantum dot solution after cooling.In above-mentioned solution, slowly add 24g NaOH, rapid stirring, regulates pH to 6.5, then solution is placed in to 3000D ultra-filtration centrifuge tube, the centrifugal 20min of 8000r/min, is scattered in filter residue in deionized water again, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 ℃, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.Fig. 3 is the high resolving power TEM figure of the graphene oxide quantum dot that obtains of the present embodiment.The illuminated diagram of the aqueous solution of the graphene oxide quantum dot that Fig. 4 the present embodiment obtains under 325nm illumination.Fig. 5 is the graphene oxide quantum dot fluorescence spectrum figure that the present embodiment obtains, and wherein, in Fig. 5, X-coordinate is wavelength, and unit is nm, and ordinate zou is emissive porwer, and unit is CPS.
Embodiment 2
To successively adding 50mg citric acid and the 40mL vitriol oil in round-bottomed flask, in 70 ℃ of water-baths, stir 7h, obtain graphene oxide quantum dot solution after cooling.In above-mentioned solution, slowly add 34g NaOH, rapid stirring, regulates pH to 7, then solution is placed in to 3000D ultra-filtration centrifuge tube, the centrifugal 20min of 8000r/min, is scattered in filter residue in deionized water again, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 ℃, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.
Embodiment 3
To successively adding 100mg citric acid and the 50mL vitriol oil in round-bottomed flask, in 50 ℃ of water-baths, stir 5h, obtain graphene oxide quantum dot solution after cooling.In above-mentioned solution, slowly add 98gNa
2cO
3, rapid stirring, regulates pH to 7.5, then solution is placed in to 3000D ultra-filtration centrifuge tube, and the centrifugal 20min of 8000r/min, is scattered in filter residue in deionized water again, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 ℃, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.
Embodiment 4
To successively adding 30mg citric acid and the 20mL vitriol oil in round-bottomed flask, in 90 ℃ of water-baths, stir 8h, obtain graphene oxide quantum dot solution after cooling.In above-mentioned solution, slowly add 16g NaOH, rapid stirring, regulates pH to 7, then pours above-mentioned solution into 3000D dialysis tubing, is placed in deionized water and dialyses 2 days, obtains the highly purified graphene oxide quantum dot aqueous solution in dialysis tubing.Finally by above-mentioned solution at-40 ℃, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.
It is simple that the preparation method of graphene oxide quantum dot of the present invention has technique, and raw material easily obtains, and processing condition are easy to realize, the advantage such as short consuming time.And it is high that the graphene oxide quantum dot powder preparing has purity, the advantage of the fluorescence property excellence showing.So the present invention has effectively overcome various shortcoming of the prior art and tool high industrial utilization.
Above-described embodiment is illustrative principle of the present invention and effect thereof only, but not for limiting the present invention.Any person skilled in the art scholar all can, under spirit of the present invention and category, modify or change above-described embodiment.Therefore, such as in affiliated technical field, have and conventionally know that the knowledgeable, not departing from all equivalence modifications that complete under disclosed spirit and technological thought or changing, must be contained by claim of the present invention.
Claims (9)
1. a preparation method for graphene oxide quantum dot, is characterized in that, the preparation method of described graphene oxide quantum dot at least comprises:
Citric acid is mixed with the vitriol oil, described citric acid and the vitriol oil are reacted, form the first graphene oxide quantum dot solution.
2. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: the condition that described citric acid and the vitriol oil react is: temperature of reaction is 25 ℃～100 ℃, and the reaction times is 1 hour～10 hours.
3. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: after described citric acid mixes with the vitriol oil, the concentration of described citric acid is 0.1mg/mL～100mg/mL.
4. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: the described mode that citric acid is mixed with the vitriol oil is standing, vibration, stirring or ultrasonic dispersion.
5. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: the mass percent concentration of the described vitriol oil is 98%.
6. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: after forming described the first graphene oxide quantum dot solution, also comprise described the first graphene oxide quantum dot solution is gone to deimpurity step.
7. the preparation method of graphene oxide quantum dot according to claim 6, is characterized in that: describedly to described the first graphene oxide quantum dot solution, go deimpurity step to comprise:
Regulating the pH value of described the first graphene oxide quantum dot solution is 4～9, obtains the second graphene oxide quantum dot solution;
To described the second graphene oxide quantum dot solution dialyse or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
8. the preparation method of graphene oxide quantum dot according to claim 6, is characterized in that: described the first graphene oxide quantum dot solution is removed after impurity, also comprised and being dried, to obtain the step of graphene oxide quantum dot powder.
9. the preparation method of graphene oxide quantum dot according to claim 8, is characterized in that: described in to carry out dry method be lyophilize, rotary evaporation or supercritical drying.
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| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
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| CN107207963A (en) * | 2015-02-10 | 2017-09-26 | 日产化学工业株式会社 | The manufacture method of carbon system luminescent material |
| CN106315541A (en) * | 2015-06-18 | 2017-01-11 | 北京化工大学 | Method for separating graphene quantum dots |
| CN106938842A (en) * | 2016-01-04 | 2017-07-11 | 天津工业大学 | It is a kind of to be pyrolyzed the method that citric acid prepares graphene quantum dot |
| WO2017190582A1 (en) * | 2016-05-06 | 2017-11-09 | Boe Technology Group Co., Ltd. | Method and apparatus for preparing quantum dots |
| US10907097B2 (en) | 2016-05-06 | 2021-02-02 | Boe Technology Group Co., Ltd. | Method and apparatus for preparing quantum dots |
| CN105967178B (en) * | 2016-06-24 | 2018-04-13 | 中国海洋大学 | A kind of graphene quantum dot prepared with algae and its application in quantum dot sensitization solar battery is prepared |
| CN105967178A (en) * | 2016-06-24 | 2016-09-28 | 中国海洋大学 | Graphene quantum dot prepared from algae and application thereof to preparation of quantum dot-sensitized solar cell |
| CN107572507A (en) * | 2017-10-12 | 2018-01-12 | 山西大学 | A kind of preparation method of amphipathic graphene quantum dot |
| CN109839465A (en) * | 2019-01-24 | 2019-06-04 | 唐玉乐 | The Solid Phase Extraction detection method of antibiotic in a kind of toffee |
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Effective date of registration: 20190329 Address after: Room J3330, 912 Yecheng Road, Jiading Industrial Zone, Shanghai, 201822 Patentee after: Shanghai Mstar Technology Ltd Address before: 200050 No. 865, Changning Road, Shanghai, Changning District Patentee before: Shanghai Institute of Microsystem and Information Technology, Chinese Academy of Sciences |
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Address after: Room j653, building 6, 1288 Yecheng Road, Jiading District, Shanghai, 201822 Patentee after: Zhongke Yueda (Shanghai) material technology Co.,Ltd. Address before: Room J3330, 912 Yecheng Road, Jiading Industrial Zone, Shanghai, 201822 Patentee before: Shanghai Ewang Material Technology Co.,Ltd. |