CN104045076B - The preparation method of graphene oxide quantum dot - Google Patents
The preparation method of graphene oxide quantum dot Download PDFInfo
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- CN104045076B CN104045076B CN201410023150.4A CN201410023150A CN104045076B CN 104045076 B CN104045076 B CN 104045076B CN 201410023150 A CN201410023150 A CN 201410023150A CN 104045076 B CN104045076 B CN 104045076B
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Abstract
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: mixed with the vitriol oil by citric acid, and make described citric acid and the vitriol oil react at ambient pressure, form graphene oxide quantum dot solution.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.
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.Compared with conventional large size two-dimensional graphene lamella, graphene quantum dot has significant fringing effect and quantum confined effect, thus 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, the stable and biocompatibility of regulatable photoluminescence performance, lower cytotoxicity and excellence.These feature performance benefits make graphene quantum dot have application prospect widely at numerous areas such as photoelectric material and device, electrocatalysis, electrochemical biosensor and bio-imagings, have become the study hotspot in current field of graphene gradually.
In existing technique, the general graphene oxide quantum dot that adopts, as presoma, obtains graphene quantum dot through reduction treatment to remove oxygen groups contained in structure to a certain extent 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 RSCAdv., 2012,2, report in 2717 one literary compositions with graphene oxide is raw material, in DMF solution, prepare graphene oxide quantum dot solution through 200 DEG C of hydro-thermal cutting 8h, and the fluorescence spectrum of graphene oxide quantum dot can be regulated by the degree of oxidation of controlled oxidization Graphene within the specific limits.And for example 2013 at Chem.Commun., 2013,49, in 5079 one literary compositions, the people such as Nurunnabi take carbon fiber as raw material, through the vitriol oil and concentrated nitric acid mixed solution, the cutting through 12 ~ 18 hours at 65 DEG C ~ 110 DEG C can prepare graphene oxide quantum dot, and research finds that cutting temperature can be used to the photoluminescence performance of controlled oxidization graphene quantum dot.
From bottom to top rule is raw material with organic molecule, prepares graphene oxide quantum dot through chemosynthesis.If the people such as Liu in 2011 are at J.Am.Chem.Soc.2011, report one in 133,15,221 one literary compositions and prepare synthetic graphite from poly aromatic toroidal molecule through pyrolysis, then obtain the method for graphene oxide quantum dot through oxidation, the quantum dot lateral dimension of gained is about 60nm, and distribution of sizes is very narrow.
But no matter be method or from bottom to top method from top to bottom, there is processing step complexity in the preparation technology of current graphene oxide quantum dot, raw material is difficult to the problems such as acquisition.Therefore, simple, the efficient graphene oxide quantum dot preparation method of research and development has important practical significance.
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 graphene oxide quantum dot in prior art, 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 carry out reacting is: temperature of reaction is 25 DEG C ~ 100 DEG C, 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 mixed with the vitriol oil by citric acid is for leaving standstill, vibrating, stir or ultrasonic disperse.
Preferably, the mass percent concentration of the described vitriol oil is 98%.
Preferably, after the described first graphene oxide quantum dot solution of formation, also comprise and deimpurity step is gone to described first graphene oxide quantum dot solution.
Preferably, describedly deimpurity step is gone to comprise to described first graphene oxide quantum dot solution:
The pH value regulating described first graphene oxide quantum dot solution is 4 ~ 9, obtains the second graphene oxide quantum dot solution;
Described second graphene oxide quantum dot solution is dialysed or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
Preferably, after removal impurity is carried out to described first graphene oxide quantum dot solution, also comprise and carry out drying, to obtain the step of graphene oxide quantum dot powder.
Preferably, carrying out dry method described in 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 obtained graphene oxide quantum dot to have purity high, the advantage of the fluorescence property excellence showed.
Accompanying drawing explanation
Fig. 1 is shown as the schematic diagram of the preparation method of graphene oxide quantum dot provided by the invention.
Fig. 2 is shown as the chemical structure schematic diagram of the citric acid used in the present invention.
The high resolving power TEM figure of the graphene oxide quantum dot that Fig. 3 obtains for technical scheme in embodiment one.
The illuminated diagram of the aqueous solution under 325nm illumination of the graphene oxide quantum dot that Fig. 4 obtains for technical scheme in embodiment one.
Fig. 5 is the graphene oxide quantum dot fluorescence spectrum figure that in embodiment one, 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 to prepare graphene oxide quantum dot solution under low-temperature atmosphere-pressure, then obtains the powder of graphene oxide quantum dot by techniques such as removal of impurities dryings.
Below by way of specific specific examples, embodiments of the present invention are described, those skilled in the art the content disclosed by this specification sheets can understand other advantages of the present invention and effect easily.The present invention can also be implemented or be applied by embodiments different in addition, and the every details in this specification sheets also can based on different viewpoints and application, carries out various modification or change not deviating under spirit of the present invention.
Refer to Fig. 1 to Fig. 5.It should be noted that, the diagram provided in the present embodiment only illustrates basic conception of the present invention in a schematic way, then only the assembly relevant with the present invention is shown in graphic but not component count, shape and size when implementing according to reality is drawn, it is actual when implementing, and the kenel of each assembly, quantity and ratio can be a kind of change arbitrarily, 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 of described citric acid and the vitriol oil react at ambient pressure, form the first graphene oxide quantum dot solution.
In a specific embodiment, the preparation method of described graphene oxide quantum dot also comprises:
Step S30: removal impurity is carried out to described first graphene oxide quantum dot solution.
Step S40: carry out drying, to obtain graphene oxide quantum dot powder.
Concrete, the preparation method of described graphene oxide quantum dot provided by the invention can be:
First, perform step S10: mixed with the vitriol oil by citric acid, form the mixing solutions of citric acid and the vitriol oil.
Citric acid is a kind of organic monoacid, is colourless crystallization or White crystal powder.Chemically in structure, citric acid is a kind of tricarboxylic acid compounds, is also called 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 used as foodstuff additive, in 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, acid, stability, water-absorbent etc.
In this step, citric acid is mixed with the vitriol oil.The mode of described mixing can be leave standstill, vibrate, stir or ultrasonic disperse, to make full and uniform the mixing of citric acid and the vitriol oil.
Described standing mode, for citric acid is put into container, puts into the vitriol oil subsequently, leaves standstill 8h ~ 20h, citric acid is fully dissolved in the vitriol oil.
The mode of described vibration, for citric acid is put into container, puts into the vitriol oil subsequently, and then vibrate container, and citric acid is fully dissolved in the vitriol oil.
The mode of described stirring for citric acid is put into container, can put into the vitriol oil subsequently, then stirs with magnetic stirring apparatus, 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 disperse 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 the reaction in subsequent technique can be caused to carry out not exclusively, can not get graphene oxide quantum dot.
Next, step S20 is performed: make the mixing solutions of described citric acid and the vitriol oil react at ambient pressure, form the first graphene oxide quantum dot solution.
In actually operating, this step is almost carried out with step citric acid and the vitriol oil mixed in previous step simultaneously.Concrete, in by citric acid and vitriol oil mixing, set temperature is 25 DEG C ~ 100 DEG C, and the reaction times is 1 hour ~ 10 hours.Wherein, in actually operating, the time mix citric acid and the vitriol oil and the time of both interreactions are coherent, and because mixing is the process of dissolving, the time is shorter, and the reaction times is longer.
Compared with traditional technique preparing graphene oxide quantum dot, in technical scheme of the present invention, described temperature of reaction is relatively low, be convenient to realize.In this step, by citric acid and the vitriol oil are placed on thermostat, can realize by the temperature controlling thermostat the temperature controlling citric acid and strong sulfuric acid response.Described thermostat can be water-bath, oil bath etc.
Described temperature is higher, and react faster, 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 the inventive solutions, relative 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 exceed this scope, then 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 between citric acid molecule and carburizing reagent.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 carbonization forms aromatic nucleus conjugated structure further, 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, perform step S30: removal impurity is carried out to described first graphene oxide quantum dot solution, described in go deimpurity mode to comprise:
First, regulate pH value to 4 ~ 9 of described first graphene oxide quantum dot solution, obtain the second graphene oxide quantum dot solution;
Then, described second graphene oxide quantum dot solution is dialysed or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
In the present embodiment, regulate the mode of the pH value of described first graphene oxide quantum dot solution for 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.
Through the removal impurity of this step, obtain highly purified second graphene oxide quantum dot solution.
Next, step S40 is performed: drying is carried out, to obtain graphene oxide quantum dot powder to described second graphene oxide quantum dot solution.Described drying means can be lyophilize, rotary evaporation or supercritical drying.
Below by way of specific specific examples, technical scheme of the present invention is described.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.
Embodiment 1
In round-bottomed flask, successively add 30mg citric acid and the 30mL vitriol oil, in 50 DEG C of water-baths, stir 5h, after cooling, obtain graphene oxide quantum dot solution.In above-mentioned solution, slowly add 24gNaOH, rapid stirring, regulate pH to 6.5, then solution is placed in 3000D ultra-filtration centrifuge tube, the centrifugal 20min of 8000r/min, is scattered in deionized water again by filter residue, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 DEG C, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.The high resolving power TEM figure of the graphene oxide quantum dot that Fig. 3 obtains for the present embodiment.The illuminated diagram of the aqueous solution under 325nm illumination of the graphene oxide quantum dot that Fig. 4 the present embodiment obtains.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
In round-bottomed flask, successively add 50mg citric acid and the 40mL vitriol oil, in 70 DEG C of water-baths, stir 7h, after cooling, obtain graphene oxide quantum dot solution.In above-mentioned solution, slowly add 34gNaOH, rapid stirring, regulate pH to 7, then solution is placed in 3000D ultra-filtration centrifuge tube, the centrifugal 20min of 8000r/min, is scattered in deionized water again by filter residue, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 DEG C, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.
Embodiment 3
In round-bottomed flask, successively add 100mg citric acid and the 50mL vitriol oil, in 50 DEG C of water-baths, stir 5h, after cooling, obtain graphene oxide quantum dot solution.Slowly 98gNa is added in above-mentioned solution
2cO
3, rapid stirring, regulate pH to 7.5, then solution is placed in 3000D ultra-filtration centrifuge tube, the centrifugal 20min of 8000r/min, is scattered in deionized water again by filter residue, obtains the highly purified graphene oxide quantum dot aqueous solution.Finally by above-mentioned solution at-40 DEG C, under 1Pa condition, lyophilize obtains fluffy graphene oxide quantum dot powder.
Embodiment 4
In round-bottomed flask, successively add 30mg citric acid and the 20mL vitriol oil, in 90 DEG C of water-baths, stir 8h, after cooling, obtain graphene oxide quantum dot solution.In above-mentioned solution, slowly add 16gNaOH, rapid stirring, regulate pH to 7, then pour above-mentioned solution into 3000D dialysis tubing, be placed in deionized water dialysis 2 days, obtain the highly purified graphene oxide quantum dot aqueous solution in dialysis tubing.Finally by above-mentioned solution at-40 DEG C, 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 prepared has purity, the advantage of the fluorescence property excellence showed.So the present invention effectively overcomes 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 without prejudice under spirit of the present invention and category, can modify above-described embodiment or changes.Therefore, such as have in art usually know the knowledgeable do not depart from complete under disclosed spirit and technological thought all equivalence modify or change, must be contained by claim of the present invention.
Claims (8)
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; The condition that described citric acid and the vitriol oil carry out reacting is: temperature of reaction is 25 DEG C ~ 100 DEG C, and the reaction times is 1 hour ~ 10 hours.
2. 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, and the concentration of described citric acid is 0.1mg/mL ~ 100mg/mL.
3. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: the described mode mixed with the vitriol oil by citric acid is for leaving standstill, vibrating, stir or ultrasonic disperse.
4. 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%.
5. the preparation method of graphene oxide quantum dot according to claim 1, is characterized in that: after the described first graphene oxide quantum dot solution of formation, also comprise and go deimpurity step to described first graphene oxide quantum dot solution.
6. the preparation method of graphene oxide quantum dot according to claim 5, is characterized in that: describedly go deimpurity step to comprise to the first graphene oxide quantum dot solution:
The pH value regulating described first graphene oxide quantum dot solution is 4 ~ 9, obtains the second graphene oxide quantum dot solution;
Described second graphene oxide quantum dot solution is dialysed or ultrafiltration centrifugal, obtain the 3rd graphene oxide quantum dot solution.
7. the preparation method of graphene oxide quantum dot according to claim 5, is characterized in that: after carrying out removal impurity to described first graphene oxide quantum dot solution, also comprise and carry out drying, to obtain the step of graphene oxide quantum dot powder.
8. the preparation method of graphene oxide quantum dot according to claim 7, is characterized in that: described in carry out dry method be lyophilize, rotary evaporation or supercritical drying.
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| CN104401981B (en) * | 2014-11-10 | 2016-03-30 | 朱熹 | A kind of preparation method of nitrogenous graphene oxide quantum dot of three primary colors fluorescence |
| CN104353127B (en) * | 2014-11-18 | 2017-01-25 | 中国科学院上海微***与信息技术研究所 | Composite antibacterial material of graphene quantum dot and fibroin, preparation and application |
| CN104556004A (en) * | 2014-12-26 | 2015-04-29 | 西北大学 | Preparation method of controlled fluorescent graphene quantum dot |
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| 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 |
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