CN106315541A - Method for separating graphene quantum dots - Google Patents
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- CN106315541A CN106315541A CN201510338221.4A CN201510338221A CN106315541A CN 106315541 A CN106315541 A CN 106315541A CN 201510338221 A CN201510338221 A CN 201510338221A CN 106315541 A CN106315541 A CN 106315541A
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Abstract
The invention discloses a method for separating different graphene quantum dots in a mixed solution containing graphene quantum dots with different fluorescence properties through adjustment of pH and belongs to the technical field of nano-material separation.
Description
Technical field
The invention belongs to nano material separation technology field, a kind of method particularly relating to graphene quantum dot being separated different fluorescence property by regulation and control pH value.
Background technology
Graphene quantum dot is the most emerging carbonaceous material.When the radial dimension of graphene sheet layer little to a certain extent time, its Exciton Bohr Radius can be more than its radial dimension, now will produce dimensional effect and edge effect and make it have certain fluorescence activity, it is widely considered to be this size within 10 nm, and recent research indicate that graphene quantum dot [Ponomarenko, the et al. Science 2008 that can also obtain having fluorescence property within 100 nm;320:356-358].Graphene quantum dot has a series of excellent properties [Dong Y, et al. Analytical such as the light stability of hypotoxicity, high fluorescence activity, higher chemical stability and excellence
chemistry 2012;84(19):8378-8382].It is ideal material [Zhu S, the et al. Chem. Commun. 2011 of a new generation's detection, microelectronics and biological medicine etc.;47(24):6858-6860].
The graphene quantum dot preparation method reported at present can be divided into two kinds.The first is that single prepares single type (referring to lamella size, oxygen-containing functional group content or fluorescence property etc.) graphene quantum dot.This kind of method obtains different types of product often through controlling reaction condition (such as temperature, concentration, time etc.).[Li H, the et al. Angewandte Chemie International such as Li
Edition 2010;49 (26): 4430-4434] generally adjusted the fluorescence property of product by controlling electric current density by the former technology of Adjust and use.[Yang Z C, the et al. Chemical such as Yang
Communications 2011;47 (42): 11615-11617] then obtain, by the concentration of the KH2PO4 in control water-heat process, the product that fluorescence property is different.But, due to the limitation of method so that this method is inefficient, it is impossible to enough reach the most mass-produced requirement.
Another kind is to prepare polytype (referring to lamella size, oxygen-containing functional group content or fluorescence property) graphene quantum dot mixture simultaneously.Yang Bai et al. [China of Jilin University, CN201210134688.3,
2012-9-12] prepare many fluorescence properties graphene quantum dot mixed solution by hydro-thermal method after, utilize chromatographic column that product carries out later separation, so obtain three kinds have different fluorescence newly can graphene quantum dots.But this method is time-consuming longer, complex steps separates the most thorough.
As can be seen here, different types of graphene quantum dot can not very efficiently be separated by the preparation of current graphene quantum dot and isolation technics the most up hill and dale, thus is difficult to play respective performance.
Its fluorescence property can be affected greatly owing to the number of the Fluorescence Mechanism of graphene quantum dot, its lamella size and oxygen-containing functional group is equal.Therefore, oxygen-containing functional group and lamella size, by regulation and control pH value, are control effectively by we, have obtained a kind of cleaning, the graphene quantum dot of different fluorescence properties is effectively separated by efficient, easy method.
Summary of the invention
A kind of method that the invention provides graphene quantum dot being separated different fluorescence property by pH value, and then the graphene quantum dot that fluorescence property is different can be obtained.
A kind of way separating graphene quantum dot, comprises the steps:
Step one: obtain the aqueous dispersions of graphene quantum dot.It is worthy of note, referring herein to the way obtaining dispersion liquid can be all kinds of to prepare the product aqueous solution that graphene quantum dot method obtains, it is also possible to being that product is soluble in water obtains；
Step 2: use the pH value of the dispersion liquid obtained in concentrated acid regulating step one to extremely low；
Step 3: use the acid solution pH obtained in olefin(e) acid and diluted alkaline regulating step two to obtain the supernatant to certain value, centrifuging and taking；Step 4: supernatant step 3 obtained is put into bag filter and carried out post processing and obtain neutral separating solution；
Step 5: lower sediment step 3 obtained repeats step one and obtains the neutral solution sample of isolated under another kind of pH to step 4.
The further preferred version of the present invention is: the preparation process of described graphene quantum dot dispersion can be to prepare graphene quantum dot aqueous solution by current known method, it is possible to dissolve in water obtain for preparing graphene quantum dot solid material by current known method.Graphene quantum dot aqueous solution is directly prepared preferably by current known method.
The further preferred version of the present invention is: the concentrated acid described in step 2 can be dense H2SO4, dense HNO3, one or more in dense HCl, but be not limited to this several acid.
The further preferred version of the present invention is: the olefin(e) acid described in step 3 can be dilute H2SO4, dilute HNO3, one or more in dilute HCl, but be not limited to this several acid.
The further preferred version of the present invention is: the diluted alkaline described in step 3 can be dilute KOH, dilute NaOH, dilute NH3•H2One or more in O, but it is not limited to this several alkali.
The further preferred version of the present invention is: the described pH value range after solution regulation is 1-14.PH value and pH value control interval after solution regulation change according to the difference of material.
The invention have the advantages that
Utilize regulation and control pH value to separate the graphene quantum dot of different fluorescence property, compare additive method, have that universality is higher, operation is easier, separate more thoroughly, separate the fineness more high advantage of regulation and control degree.
Accompanying drawing explanation
Fig. 1 is the separation method flow chart of graphene quantum dot of the present invention.
The fluorescence excitation spectrum of the dissimilar graphene quantum dot that Fig. 2 is separated by embodiment 1.
The fluorescence emission spectrum of the dissimilar graphene quantum dot that Fig. 3 is separated by embodiment 1.
The fluorescence excitation spectrum of the dissimilar graphene quantum dot that Fig. 4 is separated by embodiment 2.
The fluorescence emission spectrum of the dissimilar graphene quantum dot that Fig. 5 is separated by embodiment 2.
Detailed description of the invention
The present invention is described in detail with embodiment below in conjunction with the accompanying drawings:
Embodiment 1
By dense H2SO4+KMnO4+
NaNO3Oxidizing process prepares the strong acid solution of graphene quantum dot.
Dilute KOH solution (0.1 mol/L) and dilute HCl solution (1 mol/L) is used repeatedly to be added drop-wise in strong acid solution, until by its pH value regulation to pH=8.
4000 rpm are centrifugal obtains the supernatant, and the neutral solution obtained after dialysis treatment is labeled as pH-8.
After lower floor dissolves again, repeat the above steps respectively obtains pH-10, pH-12, pH-14 sample three times.
Tetra-samples of pH-8, pH-10, pH-12, pH-14 are carried out respectively fluorescence excitation and launches test, as shown in Figures 2 and 3.
Embodiment 2
By dense H2SO4+
H2O2(30%) oxidizing process obtains graphene quantum dot strong acid solution.
This solution is carried out that 4000 rpm are centrifugal obtains the supernatant, obtains after dialysis treatment being labeled as stock solution upper strata.
Its lower sediment is dissolved again, uses dilute KOH solution (0.1 mol/L) and dilute HCl solution (1 mol/L) to be repeatedly added drop-wise in this solution, until by its pH value regulation to pH=2.
It is centrifuged and obtains the supernatant, obtain after dialysis treatment being labeled as pH-2.
After lower floor dissolves again, repeat the above steps obtains pH-3, pH-4.
Stock solution upper strata, tetra-samples of pH-2, pH-3, pH-4 are carried out fluorescence excitation respectively and launch test, as shown in Figure 4 and Figure 5.
Below presently preferred embodiments of the present invention is illustrated, but the present invention is not limited to described embodiment, those of ordinary skill in the art also can make modification or the replacement of all equivalents on the premise of spirit of the present invention, and modification or the replacement of these equivalents are all contained in the application claim limited range.
Claims (6)
1. the method separating graphene quantum dot, it is characterised in that follow these steps to carry out:
Step one: preparation graphene quantum dot dispersion；
Step 2: use the pH value of the dispersion liquid obtained in concentrated acid regulating step one；
Step 3: after using the pH value of the acid solution obtained in diluted acid and diluted alkaline regulating step two to arrive certain value, centrifuging and taking obtains the supernatant；
Step 4: supernatant step 3 obtained is put into bag filter and carried out post processing and obtain neutral screening solution；
Step 5: lower sediment step 3 obtained repeats step one and obtains the neutral solution sample of isolated under another kind of pH to step 4.
A kind of method separating graphene quantum dot the most as claimed in claim 1, it is characterized in that: obtain the aqueous dispersions of graphite alkene quantum dot, it is worthy of note, referring herein to the way obtaining dispersion liquid can be all kinds of once to prepare the product aqueous solution that graphite alkene quantum dot method obtains, it is also possible to being that solid-state admixed graphite alkene quantum dot is soluble in water obtains；Graphene quantum dot aqueous solution is directly prepared preferably by current known method.
A kind of method separating graphene quantum dot the most as claimed in claim 1, it is characterised in that: the concentrated acid described in step 2 is dense H2SO4, dense HNO3, one or more in dense HCl, but be not limited to this several acid.
A kind of method separating graphene quantum dot the most as claimed in claim 1, it is characterised in that: the olefin(e) acid described in step 3 is dilute H2SO4, dilute HNO3, one or more in dilute HCl, but be not limited to this several acid.
5. the method separating dissimilar graphene quantum dot by regulation and control pH value as claimed in claim 1, it is characterised in that: the diluted alkaline described in step 3 is dilute KOH, dilute NaOH, dilute NH3·H2One or more in O, but it is not limited to this several alkali.
6. the method separating dissimilar graphene quantum dot by regulation and control pH value as claimed in claim 1, it is characterised in that: the solution ph scope after described regulation is 1-14, and pH value and the pH value control interval after solution regulation changes according to the difference of material.
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| CN201510338221.4A CN106315541A (en) | 2015-06-18 | 2015-06-18 | Method for separating graphene quantum dots |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
| CN104045076A (en) * | 2014-01-17 | 2014-09-17 | 中国科学院上海微***与信息技术研究所 | Graphene oxide quantum dot preparation method |
| CN104109534A (en) * | 2013-04-18 | 2014-10-22 | 国家纳米科学中心 | Preparation and application of nitrogen-doped graphene quantum-dot two-photon fluorescence |
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- 2015-06-18 CN CN201510338221.4A patent/CN106315541A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104109534A (en) * | 2013-04-18 | 2014-10-22 | 国家纳米科学中心 | Preparation and application of nitrogen-doped graphene quantum-dot two-photon fluorescence |
| CN103738941A (en) * | 2013-11-14 | 2014-04-23 | 盐城增材科技有限公司 | Graphene quantum dot preparation method |
| CN104045076A (en) * | 2014-01-17 | 2014-09-17 | 中国科学院上海微***与信息技术研究所 | Graphene oxide quantum dot preparation method |
Non-Patent Citations (1)
| Title |
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| 张兵: "碳量子点的制备与性质研究", 《中国学位论文全文数据库》 * |
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