CN108423662B - Method for preparing high-concentration graphene based on extraction technology - Google Patents
Method for preparing high-concentration graphene based on extraction technology Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 80
- 238000000034 method Methods 0.000 title claims abstract description 44
- 238000000605 extraction Methods 0.000 title claims abstract description 40
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 33
- 239000007791 liquid phase Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 11
- 239000004094 surface-active agent Substances 0.000 claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 230000010355 oscillation Effects 0.000 claims abstract description 3
- 238000010008 shearing Methods 0.000 claims abstract description 3
- 239000006228 supernatant Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 41
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 12
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical group CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 claims description 11
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 claims description 11
- 229940116411 terpineol Drugs 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000001856 Ethyl cellulose Substances 0.000 claims description 8
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 claims description 8
- 235000019325 ethyl cellulose Nutrition 0.000 claims description 8
- 229920001249 ethyl cellulose Polymers 0.000 claims description 8
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- 229910021382 natural graphite Inorganic materials 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- OHSHFZJLPYLRIP-BMZHGHOISA-M Riboflavin sodium phosphate Chemical compound [Na+].OP(=O)([O-])OC[C@@H](O)[C@@H](O)[C@@H](O)CN1C=2C=C(C)C(C)=CC=2N=C2C1=NC(=O)NC2=O OHSHFZJLPYLRIP-BMZHGHOISA-M 0.000 claims description 2
- 229920004890 Triton X-100 Polymers 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229960003201 flavin mononucleotide sodium salt Drugs 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- NRHMKIHPTBHXPF-TUJRSCDTSA-M sodium cholate Chemical compound [Na+].C([C@H]1C[C@H]2O)[C@H](O)CC[C@]1(C)[C@@H]1[C@@H]2[C@@H]2CC[C@H]([C@@H](CCC([O-])=O)C)[C@@]2(C)[C@@H](O)C1 NRHMKIHPTBHXPF-TUJRSCDTSA-M 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 9
- 238000002360 preparation method Methods 0.000 abstract description 4
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- 239000010410 layer Substances 0.000 description 29
- 238000012360 testing method Methods 0.000 description 7
- 239000010902 straw Substances 0.000 description 6
- 238000004299 exfoliation Methods 0.000 description 4
- 239000000976 ink Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
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- 238000011161 development Methods 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 238000005229 chemical vapour deposition Methods 0.000 description 1
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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Abstract
The invention discloses a method for preparing high-concentration graphene based on an extraction technology, which relates to the technical field of graphene preparation and comprises the following steps: adding graphite powder into a stripping agent, stirring, carrying out stripping dispersion through ultrasonic and/or mechanical shearing, centrifuging, and taking supernatant to obtain a low-concentration graphene solution; and adding an extracting agent into the low-concentration graphene solution, and performing oscillation separation to obtain the high-concentration graphene dispersion liquid. According to the method, the concentration of the liquid-phase exfoliated graphene is improved in the solvent conversion process through a solution extraction technology, the graphene sheet layer is prevented from agglomerating in the concentration process, the prepared graphene is high in purity and few in defects, and the surfactant is added into the liquid-phase exfoliated graphene solution, so that the graphene is favorably dispersed in the extractant, the extraction time can be effectively shortened, the method is simple in process and low in cost, and the industrial preparation of the liquid-phase exfoliated graphene is expected to be realized.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a method for preparing high-concentration graphene based on an extraction technology.
Background
The development trend of modern electronic devices is to maintain the same high performance as that of traditional rigid electronic devices, have large deformation capacity, meet the requirements of humanized markets, accurately meet commercial application, have low cost input and realize the goal of short-time return period. To achieve this goal, there is a need for a rapid and low-cost manufacturing process for solubilized material inks, targeted market investment, and high-performance electronic devices as research directions. Therefore, it is a primary objective to achieve a solubilized material ink to meet the goals of consistency of film topography and high resolution of patterns for flexible electronic devices that matches the chosen manufacturing process.
Graphene materials are considered as one of the main materials of conductive ink due to their high specific surface area, high electrical conductivity, high thermal conductivity, and low cost. The methods for preparing graphene today are mainly mechanical exfoliation, liquid phase exfoliation, epitaxial growth, redox methods and chemical vapour deposition, which are more or less deficient. In contrast, the liquid phase stripping method isThe specific solvent slowly enters the graphite layer gap under the action of ultrasonic waves, the interlayer distance is gradually enlarged along with the infiltration of solvent molecules on the graphite sheet layer, and the energy of the vibration of the solvent molecules overcomes the acting force of the graphite sheet layer, so that the graphene is stripped and produced, and the method has the advantages of high purity, few defects, simple process and low cost of the obtained graphene. The specific solvent is that the surface energy of the solvent is close to that of the graphite raw material, graphene can be efficiently stripped, and the surface tension value of the solvent with the best effect is 30-50mJ/m2Within the range. However, the concentration of the liquid-phase-stripped graphene is low and easy to agglomerate, which seriously affects the subsequent use process, and at present, three methods are mainly used for improving the concentration of the liquid-phase-stripped graphene. Firstly, solvent exchange is carried out by Li and the like (Jianontg Li.Adv.Mater.2013) in a reduced pressure distillation mode, the concentration of graphene stripped from a liquid phase is finally improved by 60 times, and finally 1.2mg/mL graphene ink is obtained, but the method needs a reduced pressure distillation device and has higher operation difficulty; secondly, like Finn et al (D.J.Finn.J.Mater.chem.C.2014), the concentration is increased by adopting a high-speed centrifugation method, expensive equipment is required, and the single treatment amount is less; for example, Secor et al (E.B.Secor.J.Phys.chem.Lett.2013) adopt a method of drying a solvent to obtain powder, and the powder is reconfigured and dispersed, wherein the method can cause the restacking of graphene sheets in the baking process, and the redispersion can damage the sheet structure and morphology.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a method for preparing high-concentration graphene based on an extraction technology, which can efficiently and nondestructively improve the concentration of liquid-phase exfoliated graphene, is low in cost, and can meet the requirement of a flexible electronic development trend.
The invention provides a method for preparing high-concentration graphene based on an extraction technology, which comprises the following steps:
s1, liquid phase stripping: adding graphite powder into a stripping agent, stirring, carrying out stripping dispersion through ultrasonic and/or mechanical shearing, centrifuging, and taking supernatant to obtain a low-concentration graphene solution;
s2, extraction and separation: and adding an extracting agent into the low-concentration graphene solution, and performing oscillation separation to obtain the high-concentration graphene dispersion liquid.
Preferably, in S1, the surface tension of the release agent is 30-50mJ/m2Preferably, the stripping agent is one of N-methyl pyrrolidone, N-dimethyl formamide, tetrahydrofuran, isopropanol, ethanol solution of ethyl cellulose and aqueous solution of flavin mononucleotide sodium salt.
Preferably, in S1, the graphite powder is one or more of flake graphite, spherical graphite, natural graphite, micro-intercalated graphite, graphite oxide, and oriented pyrolytic graphite.
Preferably, in S1, the mass-to-volume ratio of the graphene to the stripping agent is 0.5-30 g/L.
Preferably, in S1, the ultrasonic time is 0.5-24 h; preferably, the centrifugation time is 5-30min, and the centrifugation rotating speed is 2000-.
Preferably, in S1, the method further includes a surface modification step, in which a surfactant is added to the low-concentration graphene solution, and the mixture is stirred and ultrasonically treated to obtain a stable graphene dispersion.
Preferably, the surfactant is one of ethyl cellulose, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium cholate, tween 80 and triton X100.
Preferably, the addition ratio of the surfactant is 0.05-5 mg/mL.
Preferably, in S2, the extracting agent is a target solvent that is insoluble or slightly soluble in the selected stripping agent, preferably, the extracting agent is miscible with the surfactant, and preferably, the extracting agent is terpineol or a mixed solvent of terpineol and cyclohexanone.
Preferably, in S2, the extraction separation time is 10min-24 h.
Has the advantages that: according to the invention, the concentration of the liquid-phase exfoliated graphene is improved in the solvent conversion process by a solution extraction technology, the agglomeration of graphene sheets in the concentration process is avoided, the prepared graphene has high purity and few defects, and the surfactant is added into the liquid-phase exfoliated graphene solution, so that the dispersion of the graphene in the extractant is facilitated, and the extraction time can be effectively shortened. The method is simple in process and low in cost, can efficiently and nondestructively improve the concentration of the liquid-phase exfoliated graphene, can meet the requirement of the development trend of flexible electrons, and is expected to realize the industrial preparation of the liquid-phase exfoliated graphene.
Drawings
Fig. 1 is a schematic diagram of extraction and separation in example 1 of the present invention, where a is a low-concentration graphene solution, b is the graphene solution obtained by extraction and separation, and c is the prepared high-concentration graphene solution;
fig. 2 is a TEM representation of graphene sheets prepared by liquid phase exfoliation in example 1 of the present invention.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps:
s1, liquid phase stripping: adding 100mg of micro-expanded graphite into 100mL of ethyl cellulose ethanol solution, wherein the concentration of ethyl cellulose is 1mg/mL, simply stirring, carrying out ultrasonic crushing for 3h, transferring into a 50mL test tube, centrifuging at the rotating speed of 8000r/min for 10min, and taking out the upper-layer solution by using a straw;
s2, extraction and separation: and adding 5mL of mixed solution of terpineol serving as an extractant and cyclohexanone into 60mL of upper-layer solution, oscillating, standing for 10h for extraction, and carefully removing the lower-layer stripping agent to obtain the high-concentration graphene solution.
Fig. 1 is a schematic diagram of extraction and separation, where 1-a is a low-concentration graphene solution with a light color, which shows that the content of graphene is low, after an extraction agent is added into the graphene solution, the graphene solution is layered, the lower layer is a release agent layer, the upper layer is an extraction agent layer in which graphene is dispersed, and the release agent layer is removed, so that a high-concentration graphene solution is obtained.
Fig. 2 is a TEM representation of graphene sheets prepared by liquid phase exfoliation, from which it can be seen that graphene is effectively exfoliated.
Example 2
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 1g of natural graphite powder into 100mL of N, N-dimethylformamide, simply stirring, ultrasonically stripping for 12h, transferring into a 50mL test tube, centrifuging at the rotating speed of 6000r/min for 5min, and taking out an upper layer solution by using a straw; adding 5mL of terpineol serving as an extractant into 60mL of upper-layer solution, oscillating, standing for 24h for extraction, and carefully removing the lower-layer stripping agent to obtain a high-concentration graphene solution.
Example 3
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 50mg of flake graphite powder into 100mL of N-methylpyrrolidone, simply stirring, ultrasonically stripping for 60min, transferring into a 50mL test tube, centrifuging at the rotating speed of 2000r/min for 30min, and taking out an upper layer solution by using a straw; adding 3mg of ethyl cellulose into 60mL of upper layer solution, stirring for 30min, adding 5mL of terpineol serving as an extractant, oscillating, standing for 10min for extraction, and carefully removing the lower layer stripping agent to obtain the high-concentration graphene solution.
Example 4
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 100mg of micro-expanded graphite into 100mL of tetrahydrofuran, simply stirring, carrying out ultrasonic crushing for 90min, transferring into a 50mL test tube, centrifuging at the rotating speed of 5000r/min for 20min, and taking out an upper-layer solution by using a straw; adding 10mg of ethyl cellulose into 60mL of upper layer solution, stirring for 30min, adding 5mL of terpineol serving as an extractant, oscillating, standing for 30min for extraction, and carefully removing the lower layer stripping agent to obtain the high-concentration graphene solution.
Example 5
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 200mg of natural graphite powder into 100mL of N, N-dimethylformamide, simply stirring, ultrasonically stripping for 6h, transferring into a 50mL test tube, centrifuging at the rotating speed of 6000r/min for 15min, and taking out an upper layer solution by using a straw; adding 20mg of sodium dodecyl benzene sulfonate into 60mL of upper-layer solution, stirring for 30min, adding 5mL of terpineol/cyclohexanone mixed solution serving as an extracting agent, oscillating, standing for 30min for extraction, and carefully removing a lower-layer stripping agent to obtain the high-concentration graphene solution.
Example 6
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 2g of micro-intercalated graphite powder into 100mL of N, N-dimethylformamide, simply stirring, ultrasonically stripping for 18h, transferring into a 50mL test tube, centrifuging at the rotating speed of 5000r/min for 10min, and taking out an upper layer solution by using a straw; adding 180mg of polyvinylpyrrolidone into 60mL of upper-layer solution, stirring for 30min, adding 5mL of terpineol/cyclohexanone mixed solution serving as an extractant, oscillating, standing for 8h for extraction, and carefully removing a lower-layer stripping agent to obtain a high-concentration graphene solution.
Example 7
A method for preparing high-concentration graphene based on an extraction technology comprises the following steps: adding 3g of graphite oxide powder into 100mL of N, N-dimethylformamide, simply stirring, ultrasonically stripping for 24h, transferring into a 50mL test tube, centrifuging at the rotating speed of 4000r/min for 20min, and taking out an upper layer solution by using a suction tube; adding 300mg of sodium dodecyl benzene sulfonate into 60mL of upper-layer solution, stirring for 30min, adding 5mL of extracting agent terpineol/cyclohexanone mixed solution, oscillating, standing for 10h, taking out, and carefully removing the lower-layer stripping agent to obtain the high-concentration graphene solution.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (7)
1. A method for preparing high-concentration graphene based on an extraction technology is characterized by comprising the following steps:
s1, liquid phase stripping: adding graphite powder into a stripping agent, stirring, carrying out stripping dispersion through ultrasonic and/or mechanical shearing, centrifuging, and taking supernatant to obtain a low-concentration graphene solution;
s2, extraction and separation: adding an extracting agent into the low-concentration graphene solution, and performing oscillation separation to obtain a high-concentration graphene dispersion liquid;
the method comprises the following steps of S1, wherein the method further comprises a surface modification step, namely adding a surfactant into the low-concentration graphene solution, and stirring and ultrasonically treating the mixture to obtain a stable graphene dispersion liquid;
in S2, the extracting agent is a target solvent which is insoluble or slightly soluble with the selected stripping agent, the extracting agent is mutually soluble with the surfactant, and the extracting agent is terpineol or a mixed solvent of terpineol and cyclohexanone;
the surfactant is one of ethyl cellulose, polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium cholate, tween 80 and triton X100.
2. The method for preparing high-concentration graphene based on the extraction technology as claimed in claim 1, wherein in S1, the surface tension of the stripping agent is 30-50mJ/m2The stripping agent is one of N-methyl pyrrolidone, N-dimethylformamide, tetrahydrofuran, isopropanol, ethanol solution of ethyl cellulose and aqueous solution of flavin mononucleotide sodium salt.
3. The method for preparing high-concentration graphene based on extraction technology according to claim 1, wherein in S1, the graphite powder is one or more of flake graphite, spherical graphite, natural graphite, micro-intercalated graphite, graphite oxide and oriented pyrolytic graphite.
4. The method for preparing high-concentration graphene based on the extraction technology as claimed in claim 1, wherein the mass-to-volume ratio of the graphene to the stripping agent in S1 is 0.5-30 g/L.
5. The method for preparing high-concentration graphene based on the extraction technology as claimed in claim 1, wherein in S1, the ultrasonic time is 0.5-24 h; the centrifugal time is 5-30min, and the centrifugal speed is
2000-6000r/min。
6. The method for preparing high-concentration graphene based on the extraction technology as claimed in claim 1, wherein the surfactant is added in a ratio of 0.05-5 mg/mL.
7. The method for preparing high-concentration graphene based on the extraction technology as claimed in claim 1, wherein in S2, the extraction separation time is 10min-24 h.
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| CN111355134A (en) * | 2018-12-21 | 2020-06-30 | 汉能移动能源控股集团有限公司 | Fullerene negative ion release head, preparation method thereof and negative ion generating electrode |
| CN111355135A (en) * | 2018-12-21 | 2020-06-30 | 汉能移动能源控股集团有限公司 | Composite material negative ion release head, preparation method thereof and negative ion generating electrode |
| CN110042284A (en) * | 2019-05-08 | 2019-07-23 | 东南大学 | A kind of preparation method of high-strength aluminum alloy |
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| CN104876212A (en) * | 2015-04-14 | 2015-09-02 | 上海大学 | Method for efficiently purifying and recycling graphene quantum dots based on extraction technique |
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| EP2703347A1 (en) * | 2012-08-29 | 2014-03-05 | Ambrogi S.A.S. Di Ligi Simone & C. | Nanostructured carbon-based material |
| CN103864059A (en) * | 2012-12-18 | 2014-06-18 | 中国科学院兰州化学物理研究所 | Graphene high-efficiency preparation method based on extraction purification technology |
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| CN104876212A (en) * | 2015-04-14 | 2015-09-02 | 上海大学 | Method for efficiently purifying and recycling graphene quantum dots based on extraction technique |
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