CN103708446A - Preparation method of graphene oxide quantum dot powder - Google Patents
Preparation method of graphene oxide quantum dot powder Download PDFInfo
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- CN103708446A CN103708446A CN201310740350.7A CN201310740350A CN103708446A CN 103708446 A CN103708446 A CN 103708446A CN 201310740350 A CN201310740350 A CN 201310740350A CN 103708446 A CN103708446 A CN 103708446A
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Abstract
The invention provides a preparation method of graphene oxide quantum dot powder. The preparation method at least comprises the following steps: providing a graphene oxide quantum dot aqueous solution; adding an ammonium salt to the graphene oxide quantum dot aqueous solution to form a mixed solution of the graphene oxide quantum dot and the ammonium salt; adding an aprotic polar solvent to the mixed solution of the graphene oxide quantum dot and the ammonium salt to obtain a mixed precipitate of the graphene oxide quantum dot and the ammonium salt; carrying out heat treatment on the mixed precipitate of the graphene oxide quantum dot and the ammonium salt to remove the ammonium salt and obtain the graphene oxide quantum dot powder. The preparation method of graphene oxide quantum dot powder is wide in applicability, capable of quickly obtaining fluffy graphene oxide quantum dot powder from the graphene oxide quantum dot aqueous solution prepared by various methods, simple in operation process and short in time consumption, so that the preparation method is suitable for large-scale production of the graphene oxide quantum dot powder.
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 powder.
Background technology
Graphene oxide quantum dot is the zero dimension Graphene that lateral dimension is less than 100nm, is a kind of emerging nano-carbon material.Because graphene oxide quantum dot has fringing effect and the quantum confined effect of highly significant, broken through the zero band gap limitation of big size graphene material, thereby shown excellent photoluminescence and electric property.And, compare with rare-earth oxide quantum dot with conventional carbon quantum dot, graphene oxide quantum dot also has good water-soluble, abundant chemical group can be for chemically modified and functionalization, regulatable fluorescence spectrum, lower cytotoxicity and excellent biocompatibility, and can be converted into easily graphene quantum dot, these feature performance benefits make graphene oxide quantum dot in the numerous areas such as photoelectric material and device, electrocatalysis, electrochemica biological sensing and the bio-imaging prospect that is widely used.
At present; take Graphene, graphene oxide or graphite oxide as raw material; adopt secondary oxidation legal system to there is relatively high productive rate for graphene oxide quantum dot; be expected to promote graphene oxide quantum dot large-scale production, as wet chemical methods such as improved Brodie method, improved Staudenmaier method or improved Hummers methods.
But in the general technology in secondary oxidation legal system for graphene oxide quantum dot, raw material is after oxidation, filtration and dialysis treatment, and what conventionally obtain is the aqueous solution of graphene oxide quantum dot., from the business-like angle of graphene oxide quantum dot, graphene oxide quantum dot powder has significant advantage with respect to the quantum dot aqueous solution in storage, packing and transportation.Therefore, remove water solvent keeps the faling apart property of graphene quantum dot extremely important simultaneously.
But the moisture of directly removing in graphene oxide quantum dot solution by the method for heating evaporation cannot obtain graphene oxide quantum dot powder fluffy, that dispersibility is good, generally more adopts lyophilize to realize.Yet lyophilize generally need to be carried out under very low temperature, vacuum condition, higher to equipment requirements, and time of drying is long, efficiency is lower, is not suitable for the extensive preparation of graphene quantum dot.Therefore, research and development is simple, graphene oxide quantum dot extracting method will further promote industrialization and the application of graphene oxide quantum dot 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 powder, for solving prior art, from the graphene oxide quantum aqueous solution, obtain graphene oxide quantum dot powder technology difficulty and the higher problem of operation easier of good dispersity.
For achieving the above object and other relevant objects, the invention provides a kind of preparation method of graphene oxide quantum dot powder, comprising:
The graphene oxide quantum dot aqueous solution is provided;
In the described graphene oxide quantum dot aqueous solution, add ammonium salt, to form the mixing solutions of described graphene oxide quantum dot and ammonium salt;
In the mixing solutions of described graphene oxide quantum dot and ammonium salt, add aprotic polar solvent, to obtain the mixed precipitation of described graphene oxide quantum dot and ammonium salt;
The mixed precipitation of graphene oxide quantum dot and ammonium salt described in thermal treatment, to remove described ammonium salt, and obtains graphene oxide quantum dot powder.
Preferably, add aprotic polar solvent in described mixing solutions after, before the mixed precipitation of graphene oxide quantum dot and ammonium salt described in described thermal treatment, also comprise and stir described mixing solutions and non-polarity proton solvent, then carry out standing step.
Preferably, described ammonium salt is ammonium chloride or brometo de amonio.
Preferably, described aprotic polar solvent is ethanol, methyl alcohol, Virahol, dimethyl sulfoxide (DMSO), DMF, N,N-dimethylacetamide or N-Methyl pyrrolidone.
Preferably, the mass ratio of described ammonium salt and the described graphene oxide quantum dot aqueous solution is 10:1～100:1.
Preferably, the volume ratio of described aprotic polar solvent and the described graphene oxide quantum dot aqueous solution is 1:1～1:20.
Preferably, described heat treated temperature is 100 ℃～300 ℃, and the time of carrying out is 1 hour～12 hours.
Preferably, add in the step of ammonium salt or also comprise the step of mixing in the described graphene oxide quantum dot aqueous solution in the step that adds aprotic polar solvent in described mixing solutions, the mode of described mixing is concussion, stirring or ultrasonic.
Preferably, the described graphene quantum dot aqueous solution is that strong acid oxidation style, Brodie method, Staudenmaier method or Hummers method make.
Preferably, in the described graphene quantum dot aqueous solution, the lateral dimension of graphene quantum dot is less than 100nm, and in described graphene quantum dot, carbon is 2:1～20:1 with Sauerstoffatom ratio.
As mentioned above, the preparation method of graphene oxide quantum dot powder of the present invention, has following beneficial effect:
This extracting method suitability is wide, and the graphite oxide aqueous solution that can prepare from the whole bag of tricks obtains fluffy graphene oxide quantum dot powder fast, and operating procedure is simple, consuming time short, is applicable to the scale operation of graphene oxide quantum dot powder.
Accompanying drawing explanation
Fig. 1 is shown as the preparation method's of graphene oxide quantum dot powder provided by the invention schematic diagram.
The black oxidation graphene quantum dot powder schematic diagram that the preparation method of the graphene oxide quantum dot powder providing of the present invention obtains is provided Fig. 2.
Element numbers explanation
S10～S40 step
Embodiment
The object of the present invention is to provide a kind of method of extracting graphene oxide quantum dot from the aqueous solution, mainly utilize the co-precipitation in water-aprotic, polar mixing solutions of graphene oxide quantum dot and ammonium salt, first prepare graphene oxide quantum dot-ammonium salt mixed sediment, then through low-temperature heat treatment, remove the ammonium salt in mixed sediment, obtain fluffy graphene oxide quantum dot powder, and again stable dispersion in deionized water.
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. 2.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.
Concrete, as shown in Figure 1, the preparation method of described graphene oxide quantum dot powder at least comprises:
First, execution step S10: the graphene oxide quantum dot aqueous solution is provided;
The graphene quantum dot aqueous solution that the described graphene oxide quantum dot aqueous solution can obtain for any preparation method, such as existing strong acid oxidation style, Brodie method, Staudenmaier method or Hummers method.
And in the present embodiment, in the described graphene quantum dot aqueous solution, the lateral dimension of graphene oxide quantum dot is less than 100nm, and in described graphene oxide quantum dot, carbon is 2:1～20:1 with Sauerstoffatom ratio.
Next, execution step S20: add ammonium salt in the described graphene oxide quantum dot aqueous solution, to form the mixing solutions of described graphene oxide quantum dot and ammonium salt;
In the present embodiment, preferred, described ammonium salt is ammonium chloride or brometo de amonio, does not have water and generate in the mixture that these two kinds of ammonium salts form with graphene oxide quantum dot in subsequent technique.
As in this step, adopt other ammonium salts as bicarbonate of ammonia or volatile salt, in subsequent technique, in the mixture forming with bicarbonate of ammonia or volatile salt and graphene quantum dot, have water and generate, make the graphene oxide quantum dot powder reuniting that forms serious, not fluffy.
In addition, in this step, add after ammonium salt, also comprise the step that the described graphene oxide quantum dot aqueous solution and the ammonium salt adding are mixed, so that described ammonium salt can be by fully, be mixed in the described graphene oxide quantum dot aqueous solution uniformly, wherein, the mode of described mixing is concussion, stirring or ultrasonic dispersion.
Concrete, in this step, for graphite oxide quantum dot can be precipitated out completely from the aqueous solution, need enough ammonium salts, but ammonium salt is too many, can cause waste, and heat treatment time also can extend below.Preferably, the described ammonium salt adding and the mass ratio of the described graphene oxide quantum dot aqueous solution are 10:1～100:1.
Next, execution step S30: add aprotic polar solvent in the mixing solutions of described graphene oxide quantum dot and ammonium salt, to obtain the mixed precipitation of described graphene oxide quantum dot and ammonium salt;
In this step, after adding aprotic polar solvent, also comprise and stir described mixing solutions and non-polarity proton solvent, then carry out standing step.
Wherein, described aprotic polar solvent is ethanol, methyl alcohol, Virahol, dimethyl sulfoxide (DMSO), DMF, N,N-dimethylacetamide or N-Methyl pyrrolidone.
Aprotic polar solvent is abundant, so that ammonium salt and quantum dot precipitation are completely, causes again too much solvent waste.Preferably, the volume ratio of described aprotic polar solvent and the described graphene oxide quantum dot aqueous solution is 1:1～1:20.
Next, execution step S40: the mixed precipitation of graphene oxide quantum dot and ammonium salt described in thermal treatment, to remove described ammonium salt, and obtains graphene oxide quantum dot powder.
Described heat treated temperature is 100 ℃～300 ℃, and the time of carrying out is 1 hour～12 hours.
Embodiment 1
Get 50mL, concentration is the 10mg/mL graphene oxide quantum dot aqueous solution, and the described graphene oxide quantum dot aqueous solution is for utilizing improved Brodie method secondary oxidation to prepare.
Add wherein 5g ammonium chloride, stir and make chloride leach;
Then add aprotic polar solvent, described aprotic polar solvent is ethanol, 100mL;
Standing 10min after stirring 5min, obtains the grey black precipitation that ammonium chloride and graphene oxide quantum dot mix;
Then remove supernatant liquid, obtain described grey black precipitation, be the solids mixing throw out of ammonium chloride and graphene oxide quantum dot;
Described solids mixing throw out is put into heat treatment furnace, and set temperature is 200 ℃, and insulation 12h, obtains fluffy black oxidation graphene quantum dot powder as shown in Figure 2.
By the fluffy black oxidation graphene quantum dot powder that above-mentioned technique is obtained, carry out XPS analysis, obtain the content of principal element C, O and N etc. in described fluffy black oxidation graphene quantum dot powder, as shown in following table table one:
Table one: the content of principal element C, O and N etc. in the fluffy black oxidation graphene quantum dot powder that above-mentioned technique obtains.
Can see, the atomic percentage conc of C and O is 11.84% than 2.7, N content.Gained graphene oxide quantum dot powder can stable dispersion in deionized water.
Embodiment 2
Get 50mL, concentration is the 10mg/mL graphene oxide quantum dot aqueous solution, and the described graphene oxide quantum dot aqueous solution is for utilizing improved Staudenmaier method secondary oxidation to prepare;
Add wherein 10g brometo de amonio, stir and bromizate ammonium dissolving;
Then add 200mL ethanol;
Standing 10min after stirring 5min, obtains the grey black precipitation that brometo de amonio and graphene oxide quantum dot mix;
Remove supernatant liquid, obtain described grey black precipitation, be the solids mixing throw out of ammonium chloride and graphene oxide quantum dot;
Described solids mixing throw out is put into heat treatment furnace, and set temperature is 150 ℃, insulation 12h, obtain the fluffy graphene oxide quantum dot powder of black, and again stable dispersion in deionized water.
Embodiment 3
Get 50mL, the graphene oxide quantum dot aqueous solution that concentration is 20mg/mL, the described graphene oxide quantum dot aqueous solution is for utilizing improved Hummers method secondary oxidation to prepare;
Add wherein 20g ammonium chloride, stir and make chloride leach;
Then add 100mL Virahol;
Standing 10min after stirring 5min, obtains the grey black precipitation that ammonium chloride and graphene oxide quantum dot mix;
Remove supernatant liquid, obtain solids mixing throw out;
Get above-mentioned solids mixing throw out and be incubated 12h in 200 ℃ of heat treatment furnace, obtain the fluffy graphene oxide quantum dot powder of black, and again stable dispersion in deionized water.
Embodiment 4
Get 50mL, the graphene oxide quantum dot aqueous solution that concentration is 20mg/mL, the described graphene oxide quantum dot aqueous solution is for utilizing improved Hummers method secondary oxidation to prepare;
Add wherein 50mg ammonium chloride, stir and make chloride leach;
Then add 400mL methyl-sulphoxide;
Standing 10min after stirring 5min, obtains the grey black precipitation that ammonium chloride and graphene oxide quantum dot mix;
Remove supernatant liquid, obtain solids mixing throw out;
Get above-mentioned solids mixing throw out and be incubated 12h in 250 ℃ of heat treatment furnace, obtain the fluffy graphene oxide quantum dot powder of black, and again stable dispersion in deionized water.
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 (10)
1. a preparation method for graphene oxide quantum dot powder, is characterized in that, the preparation method of described graphene oxide quantum dot powder at least comprises:
The graphene oxide quantum dot aqueous solution is provided;
In the described graphene oxide quantum dot aqueous solution, add ammonium salt, to form the mixing solutions of described graphene oxide quantum dot and ammonium salt;
In the mixing solutions of described graphene oxide quantum dot and ammonium salt, add aprotic polar solvent, to obtain the mixed precipitation of described graphene oxide quantum dot and ammonium salt;
The mixed precipitation of graphene oxide quantum dot and ammonium salt described in thermal treatment, to remove described ammonium salt, and obtains graphene oxide quantum dot powder.
2. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, it is characterized in that: add aprotic polar solvent in described mixing solutions after, before the mixed precipitation of graphene oxide quantum dot and ammonium salt described in described thermal treatment, also comprise and stir described mixing solutions and non-polarity proton solvent, then carry out standing step.
3. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, is characterized in that: described ammonium salt is ammonium chloride or brometo de amonio.
4. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, it is characterized in that: described aprotic polar solvent is ethanol, methyl alcohol, Virahol, dimethyl sulfoxide (DMSO), N, dinethylformamide, N,N-dimethylacetamide or N-Methyl pyrrolidone.
5. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, is characterized in that: the mass ratio of described ammonium salt and the described graphene oxide quantum dot aqueous solution is 10:1～100:1.
6. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, is characterized in that: the volume ratio of described aprotic polar solvent and the described graphene oxide quantum dot aqueous solution is 1:1～1:20.
7. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, is characterized in that: described heat treated temperature is 100 ℃～300 ℃, and the time of carrying out is 1 hour～12 hours.
8. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, it is characterized in that: in the described graphene oxide quantum dot aqueous solution, add in the step of ammonium salt or also comprise the step of mixing in the step that adds aprotic polar solvent in described mixing solutions, the mode of described mixing is concussion, stirring or ultrasonic.
9. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, is characterized in that: the described graphene quantum dot aqueous solution is that strong acid oxidation style, Brodie method, Staudenmaier method or Hummers method make.
10. the preparation method of graphene oxide quantum dot powder as claimed in claim 1, it is characterized in that: in the described graphene quantum dot aqueous solution, the lateral dimension of graphene quantum dot is less than 100nm, and in described graphene quantum dot, carbon is 2:1～20:1 with Sauerstoffatom ratio.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108328612A (en) * | 2018-03-15 | 2018-07-27 | 成都科中云方科技有限公司 | A kind of method of quaternary ammonium salt collaboration separation graphene oxide |
| WO2020155286A1 (en) * | 2019-01-31 | 2020-08-06 | 安徽大学 | Graphene quantum dot-gadolinium ion chelate magnetic resonance contrast agent and preparation method therefor |
| CN114014312A (en) * | 2021-12-02 | 2022-02-08 | 河南大学 | Preparation method and application of water-soluble efficient luminescent graphene oxide quantum dots |
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| CN102616774A (en) * | 2012-04-12 | 2012-08-01 | 复旦大学 | Method for preparing graphene quantum dot |
| CN103320125A (en) * | 2013-06-06 | 2013-09-25 | 上海大学 | Multicolor fluorescence fluorescent graphene quantum dot material preparation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102616774A (en) * | 2012-04-12 | 2012-08-01 | 复旦大学 | Method for preparing graphene quantum dot |
| CN103320125A (en) * | 2013-06-06 | 2013-09-25 | 上海大学 | Multicolor fluorescence fluorescent graphene quantum dot material preparation method |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328612A (en) * | 2018-03-15 | 2018-07-27 | 成都科中云方科技有限公司 | A kind of method of quaternary ammonium salt collaboration separation graphene oxide |
| WO2020155286A1 (en) * | 2019-01-31 | 2020-08-06 | 安徽大学 | Graphene quantum dot-gadolinium ion chelate magnetic resonance contrast agent and preparation method therefor |
| CN114014312A (en) * | 2021-12-02 | 2022-02-08 | 河南大学 | Preparation method and application of water-soluble efficient luminescent graphene oxide quantum dots |
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Effective date of registration: 20190325 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. |
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