CN105523543A - Method for preparing graphene quantum dots with grading increase - Google Patents
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Abstract
The invention relates to a method for preparing graphene quantum dots with grading increase, belongs to the carbon material science field, and in particular, relates to the method for preparing the graphene quantum dots. The method comprises the steps: firstly, adding an aromatic compound into nitric acid, heating the mixture, cooling the mixture to room temperature, adding water into the mixture, filtering, washing, and drying to obtain a yellow powder; and secondly, adding the yellow powder into an alkaline substance, carrying out ultrasonic treatment, then pouring the mixture into a stainless steel reaction kettle, sealing, heating, naturally cooling to room temperature, filtering, taking the filtrate, pouring the filtrate into a dialysis bag, dialyzing, drying, and thus obtaining the graphene quantum dots. Firstly, naphthalene is subjected to nitration, and then hydro-thermal treatment is carried out in the alkaline solution to form the graphene quantum dots. The quantum dots are small in size and easy to disperse; no agglomeration phenomenon appears; with increase of the addition amount of the raw materials, the product yield is also increased correspondingly; and the method is simple, mild in conditions, and conducive to future large-scale production and application.
Description
Technical field
The invention belongs to carbon material scientific domain, particularly a kind of method preparing graphene quantum dot.
Background technology
Graphene quantum dot, as the novel quantum dot of one, attracts a large amount of investigators.Due to its significant quantum confinement and fringing effect, present optics unusual in a large number, the character such as electricity, have potential applicability in a lot of field, the method for current synthesizing graphite alkene quantum dot can be divided into two classes: method from top to bottom and from bottom to top.Because of from upper hot laxative remedy abundant raw material, operate the advantage such as relatively simple and be widely used.But a common disadvantage is that output is little in these class methods, as utilized Graphite Powder 99 to be all difficult to reach higher productive rate by oxidation style, solvent-thermal method or vapour deposition process, thus limit the large-scale application of graphene quantum dot.
Summary of the invention
The object of the invention is to solve the little technical problem of the existing method output preparing quantum dot, provide a kind of become rank increase the method preparing graphene quantum dot.
Rank is become to increase the method preparing graphene quantum dot as follows:
One, the aromatics of 0.02 ~ 2g being joined 3 ~ 320mL mass concentration is in the nitric acid of 56%, under rotating speed is 300 ~ 600rpm agitation condition, be heated to 70 ~ 100 degree, heat 1 ~ 20 hour, be cooled to room temperature, add 20 ~ 1000mL water, with microporous fibre element membrane filtration, and with water, product washing is extremely neutral, dry under 60 degree, obtain yellow powder (0.03 ~ 4g);
Two, it is in the alkaline matter of 0.2 ~ 1.5mol/L that the yellow powder (0.03 ~ 4g) step one obtained joins 6 ~ 600mL concentration, in the ultrasonic middle process 4 ~ 12 hours of 100 ~ 500W, then pouring 10 ~ 1000mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heat 10 hours under 200 degree, naturally cool to after room temperature until it, with microporous fibre element membrane filtration, getting filtrate pours in dialysis tubing, dialyse 2 days in 1L water, until solution is neutral, collect the solution in dialysis tubing, lyophilization under-50 degree, obtain graphene quantum dot (0.012 ~ 1.2g black powder),
Alkaline matter described in step 2 is sodium hydroxide solution, potassium hydroxide solution, ammoniacal liquor or hydrazine.
Graphene quantum dot prepared by the present invention disperses very well in water.The material adopting the inventive method to prepare is graphene quantum dot.Distribution of sizes is 1 ~ 2nm, and is dispersed in water, soilless sticking phenomenon.The most high-fluorescence quantum yield of the obtained graphene quantum dot of method of the present invention is 16%, and its fluorescence emission wavelengths is relevant with the type adding alkaline matter.
The present invention is first by naphthalene nitration, and in basic solution, hydrothermal treatment consists forms graphene quantum dot subsequently.This quantum dot size is little and be easy to dispersion, soilless sticking phenomenon, and the add-on with raw material increases, and the output of product also correspondingly increases, and simply, mild condition, is conducive to following scale operation and application to the inventive method.
Accompanying drawing explanation
Fig. 1 is the photo of graphene quantum dot prepared by experiment one;
Fig. 2 is the transmission electron microscope picture of graphene quantum dot prepared by experiment four;
Fig. 3 is the ultraviolet visible absorption spectra figure of graphene quantum dot prepared by experiment one and the fluorescent emission spectrogram that excites with 360nm;
Fig. 4 is the infrared spectrum of graphene quantum dot prepared by experiment one;
Fig. 5 is the ultraviolet visible absorption spectra figure of graphene quantum dot prepared by experiment four and the fluorescent emission spectrogram that excites with 360nm;
Fig. 6 is the infrared spectrum of graphene quantum dot prepared by experiment four.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: it is as follows that present embodiment becomes rank to increase the method preparing graphene quantum dot:
One, the aromatics of 0.02 ~ 2g being joined 3 ~ 320mL mass concentration is in the nitric acid of 56%, under rotating speed is 300 ~ 600rpm agitation condition, be heated to 70 ~ 100 degree, heat 1 ~ 20 hour, be cooled to room temperature, add 20 ~ 1000mL water, with microporous fibre element membrane filtration, and with water, product washing is extremely neutral, dry under 60 degree, obtain yellow powder;
Two, the yellow powder that step one obtains being joined 6 ~ 600mL concentration is in the alkaline matter of 0.2 ~ 1.5mol/L, in the ultrasonic middle process 4 ~ 12 hours of 100 ~ 500W, then pouring 10 ~ 1000mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heat 10 hours under 200 degree, naturally cool to after room temperature until it, with microporous fibre element membrane filtration, getting filtrate pours in dialysis tubing, dialyse 2 days in 1L water, until solution is neutral, collect the solution in dialysis tubing, lyophilization under-50 degree, obtains graphene quantum dot;
Alkaline matter described in step 2 is sodium hydroxide solution, potassium hydroxide solution, ammoniacal liquor or hydrazine.
Embodiment two: present embodiment and embodiment one are naphthalene, anthracene or pyrene unlike aromatics described in step one.Other is identical with embodiment one.
Embodiment three: one of present embodiment and embodiment one or two are 0.22 μm unlike the element of microporous fibre described in step one filter membrane hole dimension.Other is identical with one of embodiment one or two.
Embodiment four: one of present embodiment and embodiment one to three are deionized water or ultrapure water unlike water described in step one neutralization procedure two.Other is identical with one of embodiment one to three.
Embodiment five: one of present embodiment and embodiment one to four, unlike being heated to 80 ~ 90 degree in step one, heat 5 ~ 15 hours.Other is identical with one of embodiment one to four.
Embodiment six: one of present embodiment and embodiment one to five are 0.22 μm unlike the element of microporous fibre described in step 2 filter membrane hole dimension.Other is identical with one of embodiment one to five.
Embodiment seven: one of present embodiment and embodiment one to six are 3500Da unlike the molecular weight of dialysis tubing described in step 2.Other is identical with one of embodiment one to six.
Embodiment eight: one of present embodiment and embodiment one to seven are 0.5 ~ 1mol/L unlike the concentration of alkaline matter described in step 2.Other is identical with one of embodiment one to seven.
Embodiment nine: one of present embodiment and embodiment one to eight are 0.8mol/L unlike the concentration of alkaline matter described in step 2.Other is identical with one of embodiment one to eight.
Embodiment ten: one of present embodiment and embodiment one to nine are unlike the ultrasonic middle process 5 ~ 10 hours at 200 ~ 400W in step 2.Other is identical with one of embodiment one to nine.
Adopt following experimental verification effect of the present invention:
Experiment one:
Rank is become to increase the method preparing graphene quantum dot:
One, the naphthalene of 0.254g being joined 32mL mass concentration is in the nitric acid of 56%, under rotating speed is 450rpm agitation condition, is heated to 80 degree, heats 12 hours.After being cooled to room temperature, add 200mL water, with the microporous fibre element membrane filtration of 0.22um, and with water, product washing is extremely neutral, dry under 60 degree, obtain the yellow powder of 0.357g.
Two, the yellow powder 0.17g of step one being joined 60mL concentration is in the sodium hydroxide solution of 0.2mol/L, in the ultrasonic middle process 8 hours of 300W, all pouring 100mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heats 10 hours under 200 degree.Naturally cool to after room temperature until it, with the microporous fibre element membrane filtration of 0.22um, get its filtrate, pouring molecular weight into is in the dialysis tubing of 3500Da, dialyses 2 days in 1L water, until solution is neutral.Collect the solution in dialysis tubing, lyophilization under-50 degree, obtains 0.12g black powder.
As can be seen from Fig. 1 photo, in higher concentrations, solution is still transparent, shows that graphene quantum dot disperses very well in water.
The graphene quantum dot high-fluorescence quantum yield that this experimental technique obtains is 12%.
Experiment two:
Rank is become to increase the method preparing graphene quantum dot:
One, the naphthalene of 1.27g is joined 160mL, mass concentration is in the nitric acid of 56%, under rotating speed is 450rpm agitation condition, is heated to 80 degree, heats 12 hours.After being cooled to room temperature, add 1000mL water, with the microporous fibre element membrane filtration of 0.22um, and with water, product washing is extremely neutral, dry under 60 degree, obtain the yellow powder of 1.8g.
Two, the yellow powder 1.8g of step one being joined 600mL concentration is in the sodium hydroxide solution of 0.2mol/L, in the ultrasonic middle process 8 hours of 300W, all pouring 1000mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heats 10 hours under 200 degree.Naturally cool to after room temperature until it, with the microporous fibre element membrane filtration of 0.22um, get its filtrate, pouring molecular weight into is in the dialysis tubing of 3500Da, dialyses 2 days in 1L water, until solution is neutral.Collect the solution in dialysis tubing, lyophilization under-50 degree, obtains 0.8g black powder.
The graphene quantum dot high-fluorescence quantum yield that this experimental technique obtains is 13%.
Experiment three:
Rank is become to increase the method preparing graphene quantum dot:
One, the pyrene of 2g is joined 160mL, mass concentration is in the nitric acid of 56%, under rotating speed is 450rpm agitation condition, is heated to 80 degree, heats 12 hours.After being cooled to room temperature, add 1000mL water, with the microporous fibre element membrane filtration of 0.22um, and with water, product washing is extremely neutral, dry under 60 degree, obtain the yellow powder of 3g.
Two, the yellow powder 3g of step one being joined 600mL concentration is in the sodium hydroxide solution of 0.2mol/L, in the ultrasonic middle process 8 hours of 300W, all pouring 1000mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heats 10 hours under 200 degree.Naturally cool to after room temperature until it, with the microporous fibre element membrane filtration of 0.22um, get its filtrate, pouring molecular weight into is in the dialysis tubing of 3500Da, dialyses 2 days in 1L water, until solution is neutral.Collect the solution in dialysis tubing, lyophilization under-50 degree, obtains 1.2g black powder.
The graphene quantum dot high-fluorescence quantum yield that this experimental technique obtains is 14%.
Experiment four:
Rank is become to increase the method preparing graphene quantum dot:
One, the naphthalene of 0.254g is joined 32mL, mass concentration is in the nitric acid of 56%, under rotating speed is 450rpm agitation condition, is heated to 80 degree, heats 12 hours.After being cooled to room temperature, add 200mL water, with the microporous fibre element membrane filtration of 0.22um, and with water, product washing is extremely neutral, dry under 60 degree, obtain the yellow powder of 0.357g.
Two, the yellow powder 0.17g of step one being joined 60mL concentration is in the ammonia soln of 0.4mol/L, in the ultrasonic middle process 8 hours of 300W, all pouring 100mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heats 10 hours under 200 degree.Naturally cool to after room temperature until it, with the microporous fibre element membrane filtration of 0.22um, get its filtrate, pouring molecular weight into is in the dialysis tubing of 3500Da, dialyses 2 days in 1L water, until solution is neutral.Collect the solution in dialysis tubing, lyophilization under-50 degree, obtains 0.12g black powder.
Can find out that the material adopting this experimental technique to prepare is graphene quantum dot from Fig. 2 transmission electron microscope (TEM) picture.Distribution of sizes is 1 ~ 2nm, and is dispersed in water, soilless sticking phenomenon.
The graphene quantum dot high-fluorescence quantum yield that this experimental technique obtains is 16%.
Experiment five:
Rank is become to increase the method preparing graphene quantum dot:
One, the naphthalene of 0.254g is joined 32mL, mass concentration is in the nitric acid of 56%, under rotating speed is 450rpm agitation condition, is heated to 80 degree, heats 12 hours.After being cooled to room temperature, add 200mL water, with the microporous fibre element membrane filtration of 0.22um, and with water, product washing is extremely neutral, dry under 60 degree, obtain the yellow powder of 0.357g.
Two, the yellow powder 0.17g of step one being joined 60mL concentration is in the hydrazine solution of 1.5mol/L, and in the ultrasonic middle process 8 hours of 300W, all pouring 100mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heating 10 hours under 200 degree.Naturally cool to after room temperature until it, with the microporous fibre element membrane filtration of 0.22um, get its filtrate, pouring molecular weight into is in the dialysis tubing of 3500Da, dialyses 2 days in 1L water, until solution is neutral.Collect the solution in dialysis tubing, lyophilization under-50 degree, obtains 0.12g black powder.
The graphene quantum dot high-fluorescence quantum yield that this experimental technique obtains is 15%.
Claims (10)
1. become rank to increase and prepare the method for graphene quantum dot, it is characterized in that into rank, to increase the method preparing graphene quantum dot as follows:
One, the aromatics of 0.02 ~ 2g being joined 3 ~ 320mL mass concentration is in the nitric acid of 56%, under rotating speed is 300 ~ 600rpm agitation condition, be heated to 70 ~ 100 degree, heat 1 ~ 20 hour, be cooled to room temperature, add 20 ~ 1000mL water, with microporous fibre element membrane filtration, and with water, product washing is extremely neutral, dry under 60 degree, obtain yellow powder;
Two, the yellow powder that step one obtains being joined 6 ~ 600mL concentration is in the alkaline matter of 0.2 ~ 1.5mol/L, in the ultrasonic middle process 4 ~ 12 hours of 100 ~ 500W, then pouring 10 ~ 1000mL tetrafluoroethylene into is in the stainless steel cauldron of liner, sealing, heat 10 hours under 200 degree, naturally cool to after room temperature until it, with microporous fibre element membrane filtration, getting filtrate pours in dialysis tubing, dialyse 2 days in 1L water, until solution is neutral, collect the solution in dialysis tubing, lyophilization under-50 degree, obtains graphene quantum dot;
Alkaline matter described in step 2 is sodium hydroxide solution, potassium hydroxide solution, ammoniacal liquor or hydrazine.
2. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that aromatics described in step one is naphthalene, anthracene or pyrene.
3. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that the element of microporous fibre described in step one filter membrane hole dimension is 0.22 μm.
4. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that water described in step one neutralization procedure two is deionized water or ultrapure water.
5. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that in step one, being heated to 80 ~ 90 degree, heat 5 ~ 15 hours.
6. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that the element of microporous fibre described in step 2 filter membrane hole dimension is 0.22 μm.
7. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that the molecular weight of dialysis tubing described in step 2 is 3500Da.
8. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that the concentration of alkaline matter described in step 2 is 0.5 ~ 1mol/L.
9. become rank to increase the method preparing graphene quantum dot according to claim 1, it is characterized in that the concentration of alkaline matter described in step 2 is 0.8mol/L.
10. become rank to increase according to claim 1 and prepare the method for graphene quantum dot, it is characterized in that the ultrasonic middle process 5 ~ 10 hours at 200 ~ 400W in step 2.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107737944A (en) * | 2017-09-05 | 2018-02-27 | 杨蕾 | A kind of preparation method of golden nanometer particle graphene quantum dot chiral dimer |
| WO2018020247A3 (en) * | 2016-07-27 | 2018-03-22 | Kainos Innovation Limited | Improvements relating to graphene nanomaterials |
| CN109592671A (en) * | 2018-04-20 | 2019-04-09 | 上海大学 | Graphene quantum dot and its application and the microwave-assisted lower method for preparing graphene quantum dot |
| CN109762560A (en) * | 2019-03-06 | 2019-05-17 | 泉州师范学院 | A kind of preparation method of two kinds of fluorescence property graphene quantum dots of disposable synthesis |
| CN110921657A (en) * | 2019-12-03 | 2020-03-27 | 西北工业大学 | Preparation method and application of graphene quantum dots |
| CN111039280A (en) * | 2019-12-16 | 2020-04-21 | 华南理工大学 | Lignin-based graphene quantum dot and preparation method and application thereof |
| WO2020119678A1 (en) * | 2018-12-12 | 2020-06-18 | 深圳先进技术研究院 | Carbon dot simple preparation method |
| CN113277502A (en) * | 2021-05-24 | 2021-08-20 | 武汉理工大学 | Method for preparing graphene quantum dots by taking aromatic hydrocarbon as raw material and utilizing multi-field coupling |
| US11104579B2 (en) | 2018-01-31 | 2021-08-31 | Kainos Innovation Limited | Process for preparing graphene |
| CN113385143A (en) * | 2021-04-22 | 2021-09-14 | 华南农业大学 | Magnetic nano carbon dot/ferroferric oxide composite material and preparation method and application thereof |
| CN113651319A (en) * | 2021-08-25 | 2021-11-16 | 深圳华算科技有限公司 | Preparation method of graphene quantum dot nanocluster |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2018020247A3 (en) * | 2016-07-27 | 2018-03-22 | Kainos Innovation Limited | Improvements relating to graphene nanomaterials |
| US11124416B2 (en) | 2016-07-27 | 2021-09-21 | Kainos Innovation Limited | Relating to graphene nanomaterials |
| CN107737944A (en) * | 2017-09-05 | 2018-02-27 | 杨蕾 | A kind of preparation method of golden nanometer particle graphene quantum dot chiral dimer |
| US11104579B2 (en) | 2018-01-31 | 2021-08-31 | Kainos Innovation Limited | Process for preparing graphene |
| CN109592671A (en) * | 2018-04-20 | 2019-04-09 | 上海大学 | Graphene quantum dot and its application and the microwave-assisted lower method for preparing graphene quantum dot |
| WO2020119678A1 (en) * | 2018-12-12 | 2020-06-18 | 深圳先进技术研究院 | Carbon dot simple preparation method |
| CN109762560A (en) * | 2019-03-06 | 2019-05-17 | 泉州师范学院 | A kind of preparation method of two kinds of fluorescence property graphene quantum dots of disposable synthesis |
| CN109762560B (en) * | 2019-03-06 | 2021-11-02 | 泉州师范学院 | Preparation method for synthesizing two kinds of fluorescent graphene quantum dots at one time |
| CN110921657A (en) * | 2019-12-03 | 2020-03-27 | 西北工业大学 | Preparation method and application of graphene quantum dots |
| CN111039280A (en) * | 2019-12-16 | 2020-04-21 | 华南理工大学 | Lignin-based graphene quantum dot and preparation method and application thereof |
| CN113385143A (en) * | 2021-04-22 | 2021-09-14 | 华南农业大学 | Magnetic nano carbon dot/ferroferric oxide composite material and preparation method and application thereof |
| CN113385143B (en) * | 2021-04-22 | 2023-02-10 | 华南农业大学 | Magnetic nano carbon dot/ferroferric oxide composite material and preparation method and application thereof |
| CN113277502A (en) * | 2021-05-24 | 2021-08-20 | 武汉理工大学 | Method for preparing graphene quantum dots by taking aromatic hydrocarbon as raw material and utilizing multi-field coupling |
| CN113277502B (en) * | 2021-05-24 | 2023-05-12 | 武汉理工大学 | Method for preparing graphene quantum dots by using aromatic hydrocarbon as raw material and utilizing multi-field coupling |
| CN113651319A (en) * | 2021-08-25 | 2021-11-16 | 深圳华算科技有限公司 | Preparation method of graphene quantum dot nanocluster |
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Application publication date: 20160427 |