CN111422862A - Method for separating graphene quantum dots by using molecular sieve - Google Patents
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 99
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 96
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 30
- 239000002096 quantum dot Substances 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 29
- 239000011148 porous material Substances 0.000 claims abstract description 20
- 238000002604 ultrasonography Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000003480 eluent Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical group O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 12
- 238000000926 separation method Methods 0.000 abstract description 4
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- 238000003795 desorption Methods 0.000 abstract description 2
- 238000000053 physical method Methods 0.000 abstract description 2
- 238000009827 uniform distribution Methods 0.000 abstract description 2
- 238000000502 dialysis Methods 0.000 description 3
- 238000000695 excitation spectrum Methods 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 238000012984 biological imaging Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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Abstract
The invention provides a method for separating graphene quantum dots by using a molecular sieve, which comprises the steps of injecting a graphene quantum dot solution into a compacted molecular sieve, enabling the quantum dots with smaller size and particle size to pass through the pore diameter of the molecular sieve along with a solvent by a physical method, and enabling the graphene quantum dots with the pore diameter similar to that of the molecular sieve to enter the molecular sieve to form a graphene quantum dot-molecular sieve; the graphene quantum dots with the pore diameter larger than that of the molecular sieve can be remained on the molecular sieve, so that the size separation of the graphene quantum dots is realized. Graphene quantum dots in the graphene quantum dot-molecular sieve can be separated from the molecular sieve under the action of ultrasound and a desorption agent, and the obtained quantum dot solution with the residual size can be separated again to obtain the graphene quantum dots with uniform distribution, high purity and target size.
Description
Technical Field
The invention relates to the technical field of graphene quantum dot separation and size control, in particular to a method for separating graphene quantum dots by using a molecular sieve
Background
The graphene quantum dots are quasi-zero-dimensional nano materials, have the particle size of 1-10 nm, have obvious quantum confinement effect and boundary effect, show good chemical inertness, biocompatibility and lower biotoxicity, and are applied to the fields of biological imaging, disease detection, photoelectric devices, energy correlation and the like.
The preparation of the graphene quantum dots generally adopts two main methods of top-down method and bottom-up method. However, the graphene quantum dots prepared by the two methods have the problems of uneven particle size distribution and high impurity content. This problem affects the quality of the graphene quantum dots, and thus the use of the graphene quantum dots. Therefore, the prepared graphene quantum dots must be separated and purified.
In the prior art, few effective methods for separating and purifying graphene quantum dots are available. The impurities in the mother liquor are usually removed by dialysis. However, the dialysis method is not only complicated and time-consuming to operate, but also limited by the pore size of the dialysis membrane itself, and it is difficult to obtain uniform graphene quantum dots. In the prior art, an extraction technology is also adopted to purify and recover the graphene quantum dots, and the method utilizes an organic extractant to extract and separate the graphene quantum dots. However, the organic extractant used in the extraction method is somewhat harmful, and it is difficult to select a suitable organic extractant.
Disclosure of Invention
The invention aims to provide a method for conveniently separating graphene quantum dots and accurately controlling the size of the graphene quantum dots.
In order to achieve the above purpose, the invention provides a method for separating graphene quantum dots by using a molecular sieve, which comprises the following steps:
step 1: placing a molecular sieve with a corresponding model in the injector, and compacting the molecular sieve at the bottom of the injector;
step 2: pouring the initial graphene quantum dot solution into the injector;
and step 3: forcibly squeezing the injector to completely extrude the solution in the injector to obtain a quantum dot solution within a certain size range;
and 4, step 4: adding a quantitative eluent into the injector, and extruding all the solution in the injector; repeatedly eluting for 3-5 times;
and 5: taking out the molecular sieve, and eluting the large-size quantum dots adsorbed on the surface of the molecular sieve;
step 6: replacing the molecular sieve with larger pore diameter and placing the molecular sieve inside the injector; and (3) repeating the steps 1-5, and then replacing the molecular sieve with larger aperture until the graphene quantum dot solution with the target size accurately controlled is obtained.
Preferably, the quantum dot solution is prepared by a top-down method or a bottom-up method.
Preferably, in the step 2, the graphene quantum dot solution and the molecular sieve are prepared in a volume ratio of 2:1-10: 1.
Preferably, in step 4, the eluent is deionized water or absolute ethyl alcohol.
Preferably, in step 5, the molecular sieve is taken out, and graphene quantum dots adsorbed on the surface of the molecular sieve and embedded in the molecular sieve are eluted by centrifugation, ultrasound and heating;
preferably, the heating is direct water bath heating or heating by adopting a condensing reflux mode.
Preferably, the pore size of the molecular sieve is any one of 3nm, 5nm, 8nm and 10 nm.
Preferably, the molecular sieve is any one of an MCM-41 molecular sieve, an SBA-15 molecular sieve and an FDU-12 molecular sieve.
Compared with the prior art, the invention has the advantages that: by utilizing a method of separating by using a molecular sieve and accurately controlling the size of quantum dots, quantum dots with smaller size and particle size can pass through the pore diameter of the molecular sieve along with a solvent by a physical method, and graphene quantum dots with the pore diameter similar to that of the molecular sieve can enter the molecular sieve to form a graphene quantum dot-molecular sieve; the graphene quantum dots with the pore diameter larger than that of the molecular sieve can be remained on the molecular sieve, so that the size separation of the graphene quantum dots is realized. Graphene quantum dots in the graphene quantum dot-molecular sieve can be separated from the molecular sieve under the action of ultrasound and a desorption agent, and the obtained quantum dot solution with the residual size can be separated again to obtain the graphene quantum dots with uniform distribution, high purity and target size.
Drawings
FIG. 1 is a schematic diagram of the principle of precisely controlling the size of quantum dots by using molecular sieves
FIG. 2 TEM image of graphene quantum solution with size of 4-8nm isolated in example 1.
Fig. 4 a graph of fluorescence excitation spectrum of the original graphene quantum solution in example 1.
FIG. 3 is a fluorescence excitation spectrum of a 0-4nm graphene quantum solution isolated in example 1.
FIG. 5 TEM image of graphene quantum solution with size larger than 8nm isolated in example 2.
FIG. 6 is a fluorescence excitation spectrum of a 0-8nm graphene quantum solution isolated in example 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be further described below.
As shown in fig. 1, the present invention provides a method for separating graphene quantum dots by using a molecular sieve, comprising the following steps:
step 1: placing a molecular sieve with a corresponding model in the syringe at room temperature, and compacting the molecular sieve at the bottom of the syringe;
step 2: pouring the initial graphene quantum dot solution into an injector; the graphene quantum dot solution and the molecular sieve are prepared according to the volume ratio of 2:1-10: 1.
And step 3: forcibly squeezing the injector to completely extrude the solution in the injector to obtain a quantum dot solution within a certain size range;
and 4, step 4: adding a quantitative eluent into the injector, and then extruding all the solution in the injector; repeatedly eluting for 3-5 times; the eluent is deionized water or absolute ethyl alcohol; if the quantum dots are not graphene quantum dots, the solvent of the specific quantum dot solution is used as the standard.
And 5: taking out the molecular sieve, and eluting graphene quantum dots adsorbed on the surface of the molecular sieve and embedded in the molecular sieve by centrifugation, ultrasound and heating; the heating is direct water bath heating or heating by adopting a condensing reflux mode.
Step 6: replacing the molecular sieve with larger aperture and placing the molecular sieve in the injector; and (3) repeating the steps 1-5, and then replacing the molecular sieve with larger aperture until the graphene quantum dot solution with the target size accurately controlled is obtained.
In this example, the quantum dot solution was prepared by a "top-down" method or a "bottom-up" method.
In this embodiment, the pore size of the molecular sieve is any one of 3nm, 5nm, 8nm and 10 nm; the molecular sieve is any one of MCM-41 molecular sieve, SBA-15 molecular sieve and FDU-12 molecular sieve. The molecular sieve structure has many pore channels with uniform pore diameter and regularly arranged holes, and the molecular sieves with different pore diameters separate molecules with different sizes and shapes. When the diameter of the molecule or particle is smaller than the aperture of the molecular sieve, the molecule or particle can easily enter the crystal cavity to be adsorbed, and the component with the diameter larger than the aperture is adsorbed on the outer wall of the molecular sieve. It has high adsorption capacity and high selectivity. Therefore, the zeolite molecular sieve acts as a sieve for gas and liquid molecules, and whether the zeolite molecular sieve is adsorbed or not is determined according to the size of the molecules. The common molecular sieve has the pore size of 0-10 nm and is suitable for sieving graphene quantum dot materials with the particle size of 10 nm. And injecting the graphene quantum dot solution into the compacted molecular sieve, wherein the graphene quantum dots with the particle diameter smaller than the pore diameter of the molecular sieve enter the pore diameter, and the particles with the particle diameter larger than the diameter of the molecular sieve are adsorbed on the outer surface of the molecular sieve. Under the action of external force, graphene quantum dots in the molecular sieve flow out of the molecular sieve along with an eluent (water or ethanol) and are collected in a container. The graphene quantum dots with larger particles directly adsorbed on the outer surface of the molecular sieve can be eluted from the outer surface of the molecular sieve by adopting an organic solvent and a heating or heating reflux method. Re-separation is performed. The principle of molecular sieve controlling particle directly in graphite quantum dot solution is shown in figure 1.
The invention will be further described by means of some representative examples:
example one
Step 1, weighing 50mg of MCM-41 molecular sieve with the average pore diameter of 4nm, and putting the molecular sieve into an injector for compaction.
And 2, taking 3ml of centrifuged initial graphene quantum dots, and putting the initial graphene quantum dots into the injector in the step 1.
And 3, extruding the injector, and extruding the solution out of the injector to obtain the graphene quantum dots with the size of 0-4 nm.
And 4, adding 2-3ml of absolute ethyl alcohol into the injector to separate the absolute ethyl alcohol from the rest molecular sieve, and extruding the liquid in the injector out of the injector. Repeating the above operations 3-5 times.
Compared with the fluorescence spectrum of the original graphene quantum dot solution (figure 4), the obtained graphene quantum dot solution with the quantum dot size of 0-4nm has the light-emitting wavelength of 410nm, and the emission peak at the wavelength of 510nm in the original solution disappears (see figure 3). Indicating that the graphene quantum dots with the size of more than 4nm are separated out.
Example two
Step 1, weighing 100mg of SBA-15 molecular sieve with the average pore diameter of 8nm, and putting the SBA-15 molecular sieve into an injector for compaction.
And 2, taking 3ml of centrifuged initial graphene quantum dots, and putting the initial graphene quantum dots into the injector in the step 1.
And 3, extruding the injector, and extruding the solution out of the injector to obtain the graphene quantum dots with the size of 0-8 nm.
And 4, adding 2-3ml of absolute ethyl alcohol into the injector to separate the absolute ethyl alcohol from the rest molecular sieve, and extruding the liquid in the injector out of the injector. Repeating the above operations 3-5 times.
And 5, taking out the mixture of the residual molecular sieve and the graphene quantum dots in the injector, and eluting the large-size quantum dots adsorbed on the molecular sieve by centrifugation, ultrasound and heating means to obtain a graphene quantum dot solution with the size larger than 8 nm.
And 5, taking out the mixture of the residual molecular sieve and the graphene quantum dots in the injector, and eluting the large-size quantum dots adsorbed on the molecular sieve by centrifugation, ultrasound and heating means to obtain a large-size graphene quantum dot solution.
And 6, repeating the operations of the steps 1, 2, 3 and 4 on the graphene quantum dot solution obtained in the step 5 by using an SBA-15 molecular sieve with the aperture of 8nm to obtain the graphene quantum dot solution with the target size of 4-8nm accurately controlled.
FIG. 2 is a Transmission Electron Microscope (TEM) spectrum of the graphene quantum dots with the size of 4-8nm obtained in example II. Through statistical calculation, the maximum size is 8.3nm, and the size of the quantum dots distributed in the graph is 6.7nm on average.
Fig. 5 is a Transmission Electron Microscope (TEM) spectrum of the graphene quantum dots with the size larger than 8nm obtained in the second embodiment of the present invention. As shown in fig. 5, the obtained graphene quantum dots have a statistical average size of 10 nm. Compared with the fluorescence spectrum of the initial graphene quantum dot solution (figure 4), the photoluminescence spectrum of 0-8nm quantum dots in the solution obtained in the steps 3 and 4 can see that the graphene quantum dots with the size of 0-4nm have peaks at the wavelength of 440nm, and the graphene quantum dots with the size of 510nm have peaks but the intensity of the peaks is reduced (figure 6), which shows that the graphene quantum dots with the size of more than 8nm are separated in the step 5
The above description is only a preferred embodiment of the present invention, and does not limit the present invention in any way. It will be understood by those skilled in the art that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. A method for separating graphene quantum dots by using a molecular sieve is characterized by comprising the following steps:
step 1: placing a molecular sieve with a corresponding model in the injector, and compacting the molecular sieve at the bottom of the injector;
step 2: pouring the initial graphene quantum dot solution into the injector;
and step 3: forcibly squeezing the injector to completely extrude the solution in the injector to obtain a quantum dot solution within a certain size range;
and 4, step 4: adding a quantitative eluent into the injector, and extruding all the solution in the injector; repeatedly eluting for 3-5 times;
and 5: taking out the molecular sieve, and eluting graphene quantum dots adsorbed on the surface of the molecular sieve and embedded in the molecular sieve;
step 6: replacing the molecular sieve with larger pore diameter and placing the molecular sieve inside the injector; and (3) repeating the steps 1-5, and then replacing the molecular sieve with larger aperture until the graphene quantum dot solution with the target size accurately controlled is obtained.
2. The method for separating graphene quantum dots by using a molecular sieve according to claim 1, wherein the quantum dot solution is prepared by a top-down method or a bottom-up method.
3. The method for separating graphene quantum dots by using the molecular sieve as claimed in claim 1, wherein in the step 2, the graphene quantum dot solution and the molecular sieve are prepared in a volume ratio of 2:1-10: 1.
4. The method for separating graphene quantum dots by using a molecular sieve according to claim 1, wherein in the step 4, the eluent is deionized water or absolute ethyl alcohol.
5. The method of claim 1, wherein in the step 5, the molecular sieve is taken out, and graphene quantum dots adsorbed on the surface of the molecular sieve and embedded in the molecular sieve are eluted by centrifugation, ultrasound and heating.
6. The method for separating graphene quantum dots by using the molecular sieve as claimed in claim 5, wherein the heating is direct water bath heating or heating by adopting a condensing reflux manner.
7. The method for separating graphene quantum dots by using the molecular sieve according to claim 1, wherein the pore size of the molecular sieve is any one of 3nm, 5nm, 8nm and 10 nm.
8. The method for separating graphene quantum dots by using the molecular sieve as claimed in claim 1, wherein the molecular sieve is any one of an MCM-41 molecular sieve, an SBA-15 molecular sieve and an FDU-12 molecular sieve.
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Application publication date: 20200717 |