CN111137880A - Separation and purification method of graphene - Google Patents
Separation and purification method of graphene Download PDFInfo
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- CN111137880A CN111137880A CN201911311672.3A CN201911311672A CN111137880A CN 111137880 A CN111137880 A CN 111137880A CN 201911311672 A CN201911311672 A CN 201911311672A CN 111137880 A CN111137880 A CN 111137880A
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
- C01B32/196—Purification
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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
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
Abstract
The invention discloses a separation and purification method of graphene, and belongs to the technical field of graphene. The method comprises the following steps of taking biomass charcoal or resin modified asphalt to isolate oxygen and heat at 1300-1350 ℃ to obtain a mixture containing graphene, taking the mixture to obtain 1-15 layers of graphene through liquid phase separation in a solvent, and specifically comprising the following steps: 1) grinding the mixture into particles with the mesh number not less than 3000 meshes, adding the particles into a solvent, adding edetate disodium, and uniformly stirring and mixing to obtain a mixed solution; 2) taking the mixed solution, carrying out ultrasonic oscillation for 20-180 min, then carrying out centrifugal separation, controlling the centrifugal rotation speed to be 1000-8000 r/min, carrying out centrifugal time to be 10-60 min, and collecting the graphene suspension; 3) repeating the step 2) for at least 1 time, filtering, and drying filtered substances to obtain the graphene. The separation method designed by the invention has high recovery rate and can ensure higher purity of the graphene.
Description
Technical Field
The invention relates to purification of graphene, belongs to the technical field of graphene, and particularly relates to a separation and purification method of graphene.
Background
The graphene is oneTwo-dimensional carbon atom crystals with a thickness of about 0.335nm formed by close packing of a monolayer of carbon atoms, wherein carbon-carbon bonds are formed by SP2Hybridization results, the bond length is about 0.142nm, and each carbon atom is connected with three adjacent carbon atoms in a graphene plane through sigma bonds, so that the whole sheet layer has high structural strength. Meanwhile, each carbon atom has an unbound pi electron, and thus a pi orbital can be formed in the vertical direction. Due to the existence of the pi orbit, electrons can move freely in the graphene crystal, so that the graphene has excellent electron transfer performance, and the electron mobility on the plane at room temperature is 15000cm2V-1s-1The resistivity corresponding to this value was 10-6Omega cm, resistivity slightly less than silver 1.59X 10-6Ω · cm, graphene has excellent conductivity. Meanwhile, the specific surface area of graphene (2630 m)2/g) is very large, tensile modulus (1.01TPa) and ultimate strength (116GPa) are comparable to single-walled nanotubes. Compared with expensive fullerene and carbon nano-tube, the graphene has low price and easily obtained raw materials, and is expected to be finally applied in the fields of electronic materials, composite materials, medicines, aerospace and the like.
Since the discovery in 2004, the main preparation methods of graphene are: tape lift-off (or micro-mechanical lift-off), silicon carbide (SiC) epitaxial growth, Chemical Vapor Deposition (CVD), and chemical lift-off. The chemical stripping method is the most widely applied synthesis method at present, and graphene obtained based on the micro-mechanical stripping method is not easy to control in size and is only suitable for basic research; however, the epitaxial growth method and the chemical vapor deposition method cannot obtain uniform large-area graphene, and the low preparation efficiency and the high preparation cost limit the application of the two methods.
In recent years, it has been reported that graphite can be directly exfoliated or dissolved in a specific solution to form graphene, and then the graphene is separated from the liquid by filtration and centrifugation, but experiments show that the purpose of purifying and classifying the graphene cannot be completely achieved.
The chinese invention patent application (application publication No. CN 103613095 a, application publication date: 2014-03-05) discloses a patent of a method for purifying and grading graphene, and the technical scheme of the invention is as follows: the method is characterized in that graphene with different sizes is subjected to chromatography through centrifugation, metaborate crystallization is utilized for solidification, and impurities in the graphene preparation process are removed to obtain high-purity graded graphene. The method has high technical requirements, and finally, the graphene with high purity is difficult to obtain.
The chinese invention patent application (application publication No. CN 103613095 a, application publication date: 2014-03-05) discloses a method based on the separation and purification of graphene from pyrolytic carbon. Comprises pulverizing high-temperature carbonized product containing resin and at least one of asphalt or biomass into powder with a pulverizer, adding solvent, and dispersing the mixed solution with a high-speed disperser; centrifugally separating the dispersed solution, removing the precipitate, and collecting the graphene suspension; placing the graphite thin suspension into a high-speed dispersion machine again for dispersion, and then performing centrifugal separation; and filtering the suspension, recycling the filtrate, and drying the filtered substance to obtain a graphene product, wherein the recovery rate of the method for purifying graphene designed by the invention can reach 30.0-80.0%. Compared with other separation and purification methods, the method has the advantages of simple process, wide application range, low cost, environmental protection, easily controlled operation conditions, high product purity and the like. However, the recovery rate is not sufficient and the purity is not sufficient.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for separating and purifying graphene,
in order to achieve the purpose, the invention discloses a method for separating and purifying graphene, which comprises the following steps of taking biomass charcoal or resin modified asphalt to isolate oxygen and heat at 1300-1350 ℃ to obtain a mixture containing graphene, and taking the mixture to obtain 1-15 layers of graphene through liquid phase separation in a solvent, wherein the method comprises the following specific steps:
1) grinding the mixture into particles with the mesh number not less than 3000 meshes, adding the particles into a solvent, adding edetate disodium, and uniformly stirring and mixing to obtain a mixed solution;
2) taking the mixed solution, carrying out ultrasonic oscillation for 20-180 min, then carrying out centrifugal separation, controlling the centrifugal rotation speed to be 1000-8000 r/min, carrying out centrifugal time to be 10-60 min, and collecting a graphene suspension;
3) repeating the step 2) for at least 1 time, filtering, and drying filtered substances to obtain the graphene.
Further, the biomass charcoal is a porous solid substance generated by cracking at least one of straw, wood or rice hull at 300-500 ℃ under an anaerobic condition. The porous solid substance forms a graphene sheet layer with more folds and bends in the subsequent rapid temperature rise process.
Further, the resin-modified asphalt includes polyolefin-modified asphalt. The polyolefin modified asphalt can be continuously dehydrogenated in the subsequent rapid heating process, and a stable graphene sheet layer is formed.
Further, the method comprises the step of taking the biomass charcoal or the resin modified asphalt, rapidly heating to 1300-1350 ℃, and heating for 6-8 hours in an oxygen-isolated mode.
Further, in the step 1), the particles are 3000-5000 meshes. The particle size is controlled within a certain range, which facilitates subsequent dispersion.
Further, in the step 1), the dosage of the particles and the solvent is 8-14 mg/mL.
Further, in the step 1), the mass ratio of the particles to the edetate disodium is (1-10): 1.
Preferably, in the step 1), the mass ratio of the particles to the edetate disodium is (1-5) to 1; in this case, the disodium edetate can be used as an auxiliary agent.
Further, the solvent contains any one of N, N-dimethylformamide, N-methylpyrrolidone, dimethylsulfoxide, propanol, chlorosulfonic acid, o-dichlorobenzene, acetone, isopropanol, chloroform, ethanol, styrene, methanesulfonic acid, benzylamine, cyclohexanone, octafluorotoluene, pentafluoropyridine, hexafluorobenzene, pentafluorophenylnitrile, 1-butyl-3-methylimidazole (trifluoromethylsulfonyl) imide salt, 1-hexyl-3-methylimidazole hexafluorophosphate; or one of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, sodium taurodeoxycholate, sodium cholate, Pluronic P-123 and cetyl trimethyl ammonium bromide.
The beneficial effects of the invention are mainly embodied in the following aspects:
the separation method designed by the invention is simple to operate, the recovery rate of the separation method is as high as about 90%, and the separated graphene can be applied to the field of capacitors.
Drawings
Fig. 1 is a raman spectrum of graphene separated according to the present invention.
Detailed Description
In order to better explain the invention, the following further illustrate the main content of the invention in connection with specific examples, but the content of the invention is not limited to the following examples.
Example 1
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) taking a porous solid substance generated by cracking straws at 300 ℃ under an anaerobic condition, heating the porous solid substance for 6-8 hours at 1300 ℃ under the anaerobic condition to obtain a mixture containing graphene and graphite, grinding the mixture into particles with the mesh number of 3000-4000, adding 1g of the particles into 100mL of N, N-dimethylformamide, adding 1g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 20min, performing centrifugal separation, controlling the centrifugal rotation speed to be 1000r/min, performing centrifugal time to be 10min, and collecting a graphene suspension;
3) and (3) repeating the step 2) twice, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 93.2%.
Example 2
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) taking a porous solid substance generated by cracking pine tree branches at 500 ℃ under the anaerobic condition, heating the porous solid substance for 6-8 hours at 1300 ℃ under the anaerobic condition to obtain a mixture containing graphene and graphite, grinding the mixture into particles with the mesh number of about 4000, adding 1g of the particles into 80mL of N, N-dimethylformamide, adding 0.5g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 180min, performing centrifugal separation, controlling the centrifugal rotation speed to be 8000r/min, performing centrifugal time to be 60min, and collecting a graphite thin suspension;
3) and (3) repeating the step 2) twice, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 95.4%.
Example 3
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) taking a porous solid substance generated by cracking dry rice hulls at 400 ℃ under the anaerobic condition, taking the porous solid substance, heating the porous solid substance for 6-8 hours at 1300 ℃ under the anaerobic condition to obtain a mixture containing graphene and graphite, grinding the mixture into particles with the mesh number of about 5000, adding 1g of the particles into 140mL of N-methyl pyrrolidone, adding 1g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 50min, performing centrifugal separation, controlling the centrifugal rotation speed to be 2000r/min, performing centrifugal time to be 20min, and collecting the graphene suspension;
3) repeating the step 2) for three times, filtering, and drying filtered substances to obtain the graphene with 1-15 layers of sheets. The calculated recovery was 90.5%.
Example 4
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) taking a porous solid substance generated by cracking pine tree branches at 500 ℃ under the anaerobic condition, heating the porous solid substance for 6-8 hours at 1300 ℃ under the anaerobic condition to obtain a mixture containing graphene and graphite, grinding the mixture into particles with the mesh number of about 4000, adding 1g of the particles into 80mL of sodium dodecyl benzene sulfonate aqueous solution, adding 0.5g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 180min, performing centrifugal separation, controlling the centrifugal rotation speed to be 8000r/min, performing centrifugal time to be 60min, and collecting a graphite thin suspension;
3) and (3) repeating the step 2) twice, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 93.4%.
Example 5
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) cracking polyethylene modified asphalt at 1320-1325 ℃ under an oxygen-free condition to generate a mixture containing graphite, graphene and carbon residue, grinding the mixture into particles with the mesh number of about 5000 meshes, adding 1g of the particles into 120mL of N-methyl pyrrolidone, adding 0.2g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 100min, performing centrifugal separation, controlling the centrifugal rotation speed to be 5000r/min, performing centrifugal time to be 40min, and collecting a graphene suspension;
3) and (3) repeating the step 2) for four times, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 88.7%.
Example 6
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) cracking polyethylene modified asphalt at 1345-1350 ℃ under an oxygen-free condition to generate a mixture containing graphite, graphene and carbon residue, grinding the mixture into particles with the mesh number of about 5000 meshes, adding 1g of the particles into 120mL of N-methylpyrrolidone, adding 1g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 100min, performing centrifugal separation, controlling the centrifugal rotation speed to be 8000r/min, performing centrifugal time to be 40min, and collecting a graphite thin suspension;
3) and (3) repeating the step 2) for four times, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 89.2%.
Example 7
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) cracking polypropylene modified asphalt at 1345-1350 ℃ under an oxygen-free condition to generate a mixture containing graphite, graphene and carbon residue, grinding the mixture into particles with the mesh number of about 5000 meshes, adding 1g of the particles into 120mL of N-methylpyrrolidone, adding 1g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 100min, performing centrifugal separation, controlling the centrifugal rotation speed to be 8000r/min, performing centrifugal time to be 40min, and collecting a graphite thin suspension;
3) and (3) repeating the step 2) for four times, filtering, and drying filtered substances to obtain the graphene with 1-15 layers. The calculated recovery was 86.3%.
Example 8
The embodiment discloses a method for separating and purifying graphene, which comprises the following steps:
(1) cracking polyethylene modified asphalt at 1345-1350 ℃ under an oxygen-free condition to generate a mixture containing graphite, graphene and carbon residue, grinding the mixture into particles with the mesh number of about 5000 meshes, adding 1g of the particles into 120mL of sodium dodecyl benzene sulfonate aqueous solution, adding 1g of edetate disodium, and stirring and mixing uniformly to obtain a mixed solution;
2) taking the mixed solution, performing ultrasonic oscillation for 100min, performing centrifugal separation, controlling the centrifugal rotation speed to be 8000r/min, performing centrifugal time to be 40min, and collecting a graphite thin suspension;
3) repeating the step 2) for three times, filtering, and drying filtered substances to obtain the graphene with 1-15 layers of sheets. The calculated recovery was 87.5%.
Fig. 1 is a laser raman spectrum of the graphene separated in example 2, and it can be seen from the obvious characteristic peak in fig. 1 that the graphene with higher purity is indeed separated in the present invention.
The recovery rates of the separated graphene according to the embodiments of the present invention are tabulated to obtain the following table 1;
TABLE 1 recovery tabulation
Wherein, the comparative example 1 is that 1g of carbonized product of phenolic resin containing graphene and petroleum asphalt (in any mass ratio between the phenolic resin and the petroleum asphalt) is taken and crushed into powder smaller than 0.1mm by a crusher, then 100mL of DMSO solvent and 0.1g of sodium citrate are taken to dissolve the powder, a high-speed dispersion machine is used for dispersing the powder for half an hour after dissolution to obtain mixed solution, the mixed solution is centrifugally separated for 20min, the rotating speed of a centrifugal machine is controlled to be 5000r/min, and the graphite dilute suspension is collected after removing precipitates; and dispersing the graphene suspension at a high speed for half an hour, then performing centrifugal separation for 15min, controlling the rotating speed of a centrifugal machine to be 5000r/min, filtering, and drying filtered substances to obtain the graphene with 1-10 layers, wherein the recovery rate can reach 60.3%.
Comparative example 2 is taking 1g of carbonized product of phenolic resin containing graphene and straw (the mass ratio of the phenolic resin to the straw is 1:1), crushing the carbonized product into powder smaller than 0.1mm by using a crusher, dissolving the powder by taking 100mL of NMP solvent and 0.1g of NaOH, dispersing the dissolved powder for half an hour by using a high-speed dispersion machine to obtain a mixed solution, centrifugally separating the mixed solution for 15min, controlling the rotating speed of a centrifugal machine to be 6000r/min, removing precipitates, and collecting a graphite dilute suspension; and dispersing the graphene suspension at a high speed for half an hour, then performing centrifugal separation for 8min, controlling the rotating speed of a centrifugal machine to be 6000r/min, filtering, and drying filtered substances to obtain the graphene with 1-10 layers, wherein the recovery rate can reach 80.0%.
As can be seen from table 1, the recovery rate of the raw material of the present application after stripping with the organic solvent and the auxiliary agent is higher than that of the comparative example, and graphene with high purity is obtained and can be applied to capacitors.
The above examples are merely preferred examples and are not intended to limit the embodiments of the present invention. In addition to the above embodiments, the present invention has other embodiments. All technical solutions formed by adopting equivalent substitutions or equivalent transformations fall within the protection scope of the claims of the present invention.
Claims (8)
1. A graphene separation and purification method comprises the steps of taking biomass charcoal or resin modified asphalt, insulating oxygen and heating at 1300-1350 ℃ to obtain a mixture containing graphene, taking the mixture, and carrying out liquid phase separation in a solvent to obtain 1-15 layers of graphene, wherein the specific steps are as follows:
1) grinding the mixture into particles with the mesh number not less than 3000 meshes, adding the particles into a solvent, adding edetate disodium, and uniformly stirring and mixing to obtain a mixed solution;
2) taking the mixed solution, carrying out ultrasonic oscillation for 20-180 min, then carrying out centrifugal separation, controlling the centrifugal rotation speed to be 1000-8000 r/min, carrying out centrifugal time to be 10-60 min, and collecting a graphene suspension;
3) repeating the step 2) for at least 1 time, filtering, and drying filtered substances to obtain the graphene.
2. The graphene separation and purification method according to claim 1, wherein the biomass charcoal is a porous solid substance obtained by cracking at least one of straw, wood or rice hull at 300-500 ℃ under an oxygen-free condition.
3. The method for separating and purifying graphene according to claim 1, wherein the resin-modified asphalt comprises polyolefin-modified asphalt.
4. The method for separating and purifying the graphene according to claim 1, 2 or 3, wherein the method comprises the steps of taking biomass charcoal or resin modified asphalt, rapidly heating the biomass charcoal or the resin modified asphalt to 1300-1350 ℃, and heating the biomass charcoal or the resin modified asphalt for 6-8 hours under the condition of oxygen isolation.
5. The method for separating and purifying graphene according to claim 4, wherein in the step 1), the particles are 3000-5000 meshes.
6. The method for separating and purifying graphene according to claim 5, wherein in the step 1), the amount of the particulate matter and the solvent is 8-14 mg/mL.
7. The method for separating and purifying graphene according to claim 6, wherein in the step 1), the mass ratio of the particulate matter to edetate disodium is (1-10): 1.
8. The method for separating and purifying graphene according to claim 1, 2, 3, 5, 6 or 7, wherein the solvent comprises any one of N, N-dimethylformamide, N-methylpyrrolidone, dimethylsulfoxide, propanol, chlorosulfonic acid, o-dichlorobenzene, acetone, isopropanol, chloroform, ethanol, styrene, methanesulfonic acid, benzylamine, cyclohexanone, octafluorotoluene, pentafluoropyridine, hexafluorobenzene, pentafluorophenylnitrile, 1-butyl-3-methylimidazol (trifluoromethylsulfonyl) imide salt, and 1-hexyl-3-methylimidazol hexafluorophosphate; or one of sodium dodecyl benzene sulfonate, polyvinylpyrrolidone, sodium taurodeoxycholate, sodium cholate, Pluronic P-123 and cetyl trimethyl ammonium bromide.
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| US20160340791A1 (en) * | 2015-05-20 | 2016-11-24 | The Board Of Trustees Of The University Of Illinois | Electrocatalyst for acidic media and method of making an electrocatalyst for acidic media |
| CN108439390A (en) * | 2018-05-29 | 2018-08-24 | 武汉科技大学 | Based on the method for isolating and purifying graphene from Pintsch process charcoal |
| CN108893755A (en) * | 2018-07-09 | 2018-11-27 | 南京师范大学 | Mixing removing one-step method prepares the method and its application of nano-scale molybdenum disulfide and graphene complex |
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| CN102910624A (en) * | 2012-11-08 | 2013-02-06 | 南京师范大学 | Preparation method of high-yield graphene without defects |
| CN103553030A (en) * | 2013-11-05 | 2014-02-05 | 中国石油大学(北京) | Preparation method of few-layer graphene |
| CN104045077A (en) * | 2014-05-27 | 2014-09-17 | 陈永 | Graphene three-dimensional hierarchical porous carbon material and preparation method thereof |
| US20160340791A1 (en) * | 2015-05-20 | 2016-11-24 | The Board Of Trustees Of The University Of Illinois | Electrocatalyst for acidic media and method of making an electrocatalyst for acidic media |
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