CN115849355A - Graphene quantum dot and preparation method thereof - Google Patents
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 47
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002096 quantum dot Substances 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 27
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000006185 dispersion Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 15
- 150000003140 primary amides Chemical class 0.000 claims abstract description 12
- 235000019270 ammonium chloride Nutrition 0.000 claims abstract description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 230000004048 modification Effects 0.000 claims abstract description 5
- 238000012986 modification Methods 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims description 25
- 239000003153 chemical reaction reagent Substances 0.000 claims description 17
- 238000007167 Hofmann rearrangement reaction Methods 0.000 claims description 15
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 15
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 239000000047 product Substances 0.000 claims description 13
- 239000012265 solid product Substances 0.000 claims description 12
- 238000000502 dialysis Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 125000003277 amino group Chemical group 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- 235000010265 sodium sulphite Nutrition 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- 239000011521 glass Substances 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- CRWJEUDFKNYSBX-UHFFFAOYSA-N sodium;hypobromite Chemical compound [Na+].Br[O-] CRWJEUDFKNYSBX-UHFFFAOYSA-N 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 101710134784 Agnoprotein Proteins 0.000 claims description 5
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 5
- 229920002472 Starch Polymers 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 5
- 235000019698 starch Nutrition 0.000 claims description 5
- 239000008107 starch Substances 0.000 claims description 5
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 150000001408 amides Chemical class 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Chemical compound BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims description 2
- 238000007254 oxidation reaction Methods 0.000 claims description 2
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 238000006462 rearrangement reaction Methods 0.000 claims 1
- 238000005520 cutting process Methods 0.000 abstract description 5
- 125000004442 acylamino group Chemical group 0.000 abstract description 3
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 27
- 229910052799 carbon Inorganic materials 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000006105 Hofmann reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000543 intermediate Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002064 nanoplatelet Substances 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 125000001749 primary amide group Chemical group 0.000 description 1
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
Abstract
The invention discloses a graphene quantum dot and a preparation method thereof, wherein the method comprises the steps of firstly, performing acylamino modification on graphene oxide, then cutting the graphene oxide into the graphene quantum dot, neutralizing a graphene oxide solution by ammonia water, and adding ammonium chloride; evaporating the dispersion liquid to dryness and converting the surface carboxyl of the graphene oxide into primary amide; re-dispersing and adding hypohalite under the protection of ice bath; and filtering and dialyzing the reaction solution to obtain the graphene quantum dots. The reaction device is simple, and the reaction conditions are mild.
Description
Technical Field
The invention relates to the field of carbon nanomaterials, in particular to a graphene quantum dot and a preparation method thereof.
Background
The graphene quantum dots are graphene nanoplatelets having a lateral dimension of less than 100 nm, and the preparation method thereof can be simply divided into two methods, i.e., a "top-down" method for preparing the graphene quantum dots by cutting a substance having a graphite-like hexagonal structure, such as graphene, graphene oxide, carbon nanotubes, and the like, and a "bottom-up" method for preparing the graphene quantum dots. Since the hexagonal graphite-like structure is very stable, which makes the cutting of the reactant difficult, long-term heating treatment with concentrated acid and strong oxidant (electrostatic Analysis and Purification of Fluorescent Single-Walled Carbon Nanotube Fragments [ J ]. 2004.) or high-power ultraviolet irradiation (Zhou X, zhang Y, wang C, et al, photo-Fenton reaction of graphene oxide: a new energy to prepare graphene oxides [ J ]. Acs Nano, 2012, 6 (8): 6592-6599.) are often required to advance the reaction, which is not favorable for large-scale preparation.
Hofmann rearrangement (Hofmann rearrangement) is a reaction in which hypohalite is used as an oxidizing agent to convert a primary amide into a corresponding primary amine, and the general reaction formula can be represented as follows:
R-CO-NH 2 + NaOX + 2NaOH → R-NH 2 +Na 2 CO 3 + NaX +H 2 O （1）
studies have shown that when a primary amide group is attached to an aromatic group, the reactivity is significantly improved, probably because the aromatic group effectively stabilizes intermediates of the hofmann rearrangement reaction. This reaction removes the carbonyl group between the aromatic group and the amine group, is a "carbon reduction" reaction, and is also known as hofmann degradation.
Disclosure of Invention
Aiming at the problem of preparing graphene quantum dots by graphene oxide, the invention aims to provide a preparation method of the graphene quantum dots.
Still another object of the present invention is to: the graphene quantum dot prepared by the method is provided.
The invention is realized by the following scheme: a preparation method of graphene quantum dots is a method for first modifying graphene oxide through acylamino and then cutting the graphene oxide into graphene quantum dots, and comprises the following steps:
(1) Dispersing graphene oxide into an aqueous dispersion;
(2) Adding ammonia water into the dispersion liquid obtained in the step (1) to neutralize the acidity of the dispersion liquid, and additionally adding an ammonium chloride solution as an amine group source;
(3) Heating and evaporating the dispersion liquid obtained in the step (2) to dryness so as to convert carboxyl on the surface of the graphene oxide into primary amide;
(4) Cleaning and grinding the substance obtained in the step (3), controlling the temperature, adding a Hofmann reaction reagent, and quickly stirring;
(5) Adding sodium sulfite into the reaction liquid obtained in the step (4) until the reaction liquid does not discolor the starch potassium iodide test paper any more;
(6) And (5) filtering the reaction liquid obtained in the step (5) and recovering residual solids. Repeatedly dialyzing the obtained liquid in a dialysis bag until the obtained liquid is added with AgNO 3 No precipitate is generated; and (5) obtaining the water dispersion of the product graphene quantum dots in a dialysis bag.
Preferably, the concentration of the graphene oxide prepared in the step (1) is 1 g L -1 。
Preferably, the evaporating temperature in step (3) is 85 ℃.
Preferably, a sodium hypochlorite solution or a newly prepared sodium hypobromite solution is used as the Hofmann rearrangement reagent in the step (4).
Preferably, the reaction temperature in step (4) is controlled to 5 ℃.
Preferably, the reagent for quenching the Hofmann rearrangement reaction in step (5) is sodium sulfite.
Preferably, the permeability of the dialysis bag in step (6) is 14000 molecular weight.
The invention provides a graphene quantum dot prepared by the method.
The mechanism of the invention is as follows:
firstly, converting carboxyl in graphene oxide into primary amide, and expressing graphene oxide by GO, wherein in the step (2):
GO-COOH + NH 3 → GO-COONH 4 （2）
the reaction is a reversible reaction. Further conversion to the primary amide in step (3):
GO-COONH 4 → GO-CO-NH 2 + H 2 O (↑) (3)
GO-COOH + NH 4 Cl → GO-CO-NH 2 + H 2 O (↑) + HCl (↑) (4)
in the evaporation conditions, the reactions (3) and (4) are shifted to the right sufficiently and are complete by virtue of the volatility of the water and hydrogen chloride molecules at 85 ℃.
In step (4), the primary amide first undergoes a hofmann rearrangement:
GO-COONH 2 → GO-NH 2 (5)
one carbon is lost and the amine as product is unstable in oxidizing conditions and is oxidized again to the amide:
GO-NH 2 → GO-CO-NH 2 （6）
in reaction (6), the product is reconverted to the primary amide, but the parent GO is reduced by one carbon atom. Under the condition of Hofmann rearrangement reaction, the reactions (5) and (6) can alternately occur, so that the parent GO continuously loses carbon atoms at the position, the reaction result is equivalent to that the parent GO is cut by a Hofmann rearrangement reaction reagent under the catalysis of a nitrogen-containing group, and after the reaction cycle is repeatedly performed, the graphene oxide is cut into small enough sheets, namely graphene quantum dots, and the graphene quantum dots have good dispersibility and can be recovered from a reaction solution.
Under the technical background, the invention provides a preparation method of graphene quantum dots aiming at the problem of preparing the graphene quantum dots by graphene oxide, and the preparation method has the advantages that:
(1) The reaction device is simple;
(2) The reaction conditions are mild.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified. Materials, reagents and the like used in the following examples are commercially available unless otherwise specified. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention.
Example 1.
The method for preparing the graphene quantum dots by taking a sodium hypochlorite aqueous solution as a Hoffman reagent, firstly performing acylamino modification on graphene oxide, and then cutting the graphene oxide into the graphene quantum dots comprises the following steps:
(1) Adding 0.05 g of graphene oxide powder into 50 mL of pure water at room temperature, and stirring and ultrasonically dispersing to obtain an aqueous dispersion;
(2) Stirring is maintained and commercial concentrated ammonia water is added to the dispersion obtained in step (1) to the pH of the solution>7 to neutralize the acidity and add 1 mL of 10 g L -1 Taking the ammonium chloride solution as an amine group source, and stirring for 0.5 h;
(3) Transferring all the liquid in the step (2) into a glass evaporation dish, drying at 85 ℃ until the moisture completely disappears, and keeping the temperature for continuous drying for 2 hours to convert the carboxyl on the surface of the graphene oxide into primary amide;
(4) Washing and grinding the solid product obtained in the step (3) by using a glass plug, transferring the solid product into a 100 mL beaker, adding 10 mL of pure water to wash the product for 2 times, and washing away excessive ammonium chloride; adding 30 mL of pure water into the obtained solid product, cooling the solid product to 5 ℃ by using an ice bath, adding 5 mL of a commercially available sodium hypochlorite solution (4-7% of available chlorine), fully and quickly stirring the mixture, placing the mixture in a refrigerator, and reacting the mixture for 48 hours at the temperature of 5 ℃ to obtain a reaction solution;
(5) Quenching the Hofmann rearrangement reaction reagent, transferring to the reaction solution obtained in the step (4) and stirring at room temperature, and adding 5 g L -1 The sodium sulfite solution does not discolor the potassium iodide starch test paper until the reaction solution shows that the solution has no oxidability and ClO - Converting into Cl; filtering the reaction solution with filter paper, recovering residual solid, recovering unreacted raw materials, and dialyzing the recovered solution in 14000 molecular weight dialysis bag until the external solution is no longer mixed with 17 g L -1 AgNO 3 And precipitating the solution, and obtaining the product graphene quantum dots in a dialysis bag.
Example 2.
The preparation method comprises the following steps of (1) preparing the graphene quantum dots by taking sodium hypobromite as a Hofmann reagent, wherein the sodium hypobromite has stronger reaction activity but needs to be prepared at present:
(1) Adding 0.05 g of graphene oxide powder into 50 mL of water at room temperature, and stirring and ultrasonically dissolving to obtain an aqueous dispersion;
(2) Stirring is maintained and commercial concentrated ammonia water is added to the dispersion obtained in step (1) to the pH of the solution>7 to neutralize the acidity and additionally 1 mL of 10 g L -1 Taking the ammonium chloride solution as an amine group source, and stirring for 0.5 h;
(3) Transferring all the liquid in the step (2) into an evaporation pan, keeping the temperature at 85 ℃ for drying until the moisture completely disappears, and keeping the temperature for continuously drying for 2 hours to convert the carboxyl on the surface of the graphene oxide into primary amide;
(4) Grinding the solid product obtained in the step (3) by using a glass plug, transferring the solid product into a 100 mL beaker, adding 10 mL pure water to wash the product for 2 times, and washing away excessive ammonium chloride; dissolving 0.25 g of sodium hydroxide in 30 mL of pure water, rapidly stirring at room temperature, adding 80 uL of liquid bromine, continuously stirring for 0.5 h, and cooling to 5 ℃ to obtain a prepared Hoffman reagent; adding the newly prepared sodium hypobromite solution into the washed and ground product solid, quickly and fully stirring, placing in a refrigerator, and reacting at 5 ℃ for 18 h to obtain a reaction solution.
(5) Quenching the Hofmann rearrangement reaction reagent, stirring the reaction solution obtained in the step (4) at room temperature, and adding 5 g L of the reaction solution -1 The sodium sulfite solution does not change the color of the starch potassium iodide test paper until the reaction solution shows that the solution has no oxidation, and BrO - Conversion to Br - (ii) a Recovering the raw materials which are not completely reacted, filtering the reaction solution by using filter paper and recovering residual solids; putting the recovered liquid into 14000 molecular weight dialysis bag, and dialyzing until the external liquid is no longer mixed with 17 g L -1 AgNO 3 The solution generates a precipitate; and obtaining the product graphene quantum dots in the dialysis bag.
The above examples are merely examples for clearly illustrating the present invention and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (8)
1. A preparation method of graphene quantum dots is characterized in that graphene oxide is subjected to amide modification and then is cut into the graphene quantum dots, and the method comprises the following steps:
(1) Dispersing graphene oxide into an aqueous dispersion;
(2) Adding ammonia water into the dispersion liquid obtained in the step (1) to neutralize the acidity of the dispersion liquid, and additionally adding an ammonium chloride solution as an amine group source;
(3) Heating and evaporating the dispersion liquid obtained in the step (2) to dryness so as to convert carboxyl on the surface of the graphene oxide into primary amide;
(4) Cleaning and grinding the substance obtained in the step (3), controlling the temperature, adding a Hofmann rearrangement reagent, and quickly stirring;
(5) Quenching the Hoffmann rearrangement reaction reagent, recovering the raw materials which are not completely reacted, and dialyzing the reaction liquid to obtain the graphene quantum dots.
2. The method for preparing the graphene quantum dot according to claim 1, wherein in the step (3), the evaporation temperature is 85 ℃.
3. The method for preparing the graphene quantum dot according to claim 1, wherein in the step (4), a sodium hypochlorite solution or a newly prepared sodium hypobromite solution is used as a Hofmann rearrangement reagent.
4. The method for preparing the graphene quantum dot according to claim 1, wherein in the step (4), the reaction temperature is controlled to be 5 ℃.
5. The method for preparing the graphene quantum dot according to claim 1, wherein in the step (5), the reagent for quenching the Hofmann rearrangement reaction is sodium sulfite.
6. The preparation method of the graphene quantum dot according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) Adding 0.05 g of graphene oxide powder into 50 mL of pure water at room temperature, and stirring and ultrasonically dispersing to obtain an aqueous dispersion;
(2) Stirring is maintained and commercial concentrated ammonia water is added to the dispersion obtained in step (1) to the pH of the solution>7 to neutralize the acidity and 1 mL of 10 g L -1 The ammonium chloride solution is taken as an amine group source and is stirred for 0.5 h;
(3) Transferring all the liquid in the step (2) into a glass evaporation dish, drying at 85 ℃ until the moisture completely disappears, and keeping the temperature for continuously drying for 2 hours to convert the surface carboxyl of the graphene oxide into primary amide;
(4) Washing and grinding the solid product obtained in the step (3) by using a glass plug, transferring the solid product into a 100 mL beaker, adding 10 mL of pure water to wash the product for 2 times, and washing away excessive ammonium chloride; adding 30 mL of pure water into the obtained solid product, cooling the solid product to 5 ℃ by using an ice bath, adding 5 mL of a commercially available sodium hypochlorite solution (4-7% of available chlorine), fully and quickly stirring the mixture, placing the mixture in a refrigerator, and reacting the mixture for 48 hours at the temperature of 5 ℃ to obtain a reaction solution;
(5) Quenching the Hofmann rearrangement reagent, transferring to the reaction solution obtained in the step (4) and stirring at room temperature, adding 5 g L -1 The sodium sulfite solution does not discolor the starch potassium iodide test paper until the reaction solution shows that the solution has no oxidation and ClO - Converting into Cl; filtering the reaction solution with filter paper, recovering residual solid, recovering unreacted raw material, placing the recovered liquid in 14000 molecular weight dialysis bag, dialyzing until the external liquid is no longer mixed with 17 g L -1 AgNO 3 And precipitating the solution, and obtaining the product graphene quantum dots in a dialysis bag.
7. The preparation method of the graphene quantum dot according to any one of claims 1 to 5, characterized by comprising the following steps:
(1) Adding 0.05 g of graphene oxide powder into 50 mL of water at room temperature, and stirring and ultrasonically dissolving to obtain an aqueous dispersion;
(2) Stirring is maintained and commercial concentrated ammonia water is added to the dispersion obtained in step (1) to the pH of the solution>7, to neutralize the acidity thereof,and 1 mL of 10 g L of additional solution was added -1 Taking the ammonium chloride solution as an amine group source, and stirring for 0.5 h;
(3) Transferring all the liquid in the step (2) into an evaporation dish, keeping the temperature at 85 ℃ for drying until the moisture completely disappears, keeping the temperature for continuously drying for 2 hours, and converting the surface carboxyl of the graphene oxide into primary amide;
(4) Grinding the solid product obtained in the step (3) by using a glass plug, transferring the solid product into a 100 mL beaker, adding 10 mL pure water to wash the product for 2 times, and washing away excessive ammonium chloride; dissolving 0.25 g of sodium hydroxide in 30 mL of pure water, rapidly stirring at room temperature, adding 80 uL of liquid bromine, continuously stirring for 0.5 h, and cooling to 5 ℃ to obtain a prepared Hoffman reagent; adding the newly prepared sodium hypobromite solution into the washed and ground product solid, quickly and fully stirring, placing in a refrigerator, and reacting at 5 ℃ for 18 h to obtain a reaction solution.
(5) Quenching the Hofmann rearrangement reaction reagent, stirring the reaction solution obtained in the step (4) at room temperature, and adding 5 g L of the reaction solution -1 The sodium sulfite solution does not discolor the potassium iodide starch test paper until the reaction solution, indicating that the solution has no oxidability, brO - Conversion to Br - (ii) a Recovering the raw materials which are not completely reacted, filtering the reaction solution by using filter paper and recovering residual solids; putting the recovered liquid into 14000 molecular weight dialysis bag, and dialyzing until the external liquid is no longer mixed with 17 g L -1 AgNO 3 The solution generates a precipitate; and obtaining the product graphene quantum dots in the dialysis bag.
8. Graphene quantum, characterized in that it is prepared according to the method of any one of claims 1-7.
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| CN104922675A (en) * | 2015-05-25 | 2015-09-23 | 东华大学 | Preparation method of graphene oxide composite material mediated by carboxymethyl chitosan and modified by hyaluronic acid |
| US20160325999A1 (en) * | 2014-01-17 | 2016-11-10 | Shenzhen Cantonnet Energy Services Co., Ltd | Large-scale preparation method for graphene quantum dots |
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| US20160325999A1 (en) * | 2014-01-17 | 2016-11-10 | Shenzhen Cantonnet Energy Services Co., Ltd | Large-scale preparation method for graphene quantum dots |
| CN104922675A (en) * | 2015-05-25 | 2015-09-23 | 东华大学 | Preparation method of graphene oxide composite material mediated by carboxymethyl chitosan and modified by hyaluronic acid |
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