CN113387349A - Method for efficiently preparing graphene sol - Google Patents
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- CN113387349A CN113387349A CN202110518231.1A CN202110518231A CN113387349A CN 113387349 A CN113387349 A CN 113387349A CN 202110518231 A CN202110518231 A CN 202110518231A CN 113387349 A CN113387349 A CN 113387349A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 75
- 238000000034 method Methods 0.000 title claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 19
- 230000002687 intercalation Effects 0.000 claims abstract description 14
- 238000009830 intercalation Methods 0.000 claims abstract description 14
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000002994 raw material Substances 0.000 claims abstract description 6
- 238000002604 ultrasonography Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 150000003384 small molecules Chemical class 0.000 claims abstract description 3
- 239000011259 mixed solution Substances 0.000 claims abstract 2
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- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 9
- HJOVHMDZYOCNQW-UHFFFAOYSA-N isophorone Chemical compound CC1=CC(=O)CC(C)(C)C1 HJOVHMDZYOCNQW-UHFFFAOYSA-N 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 6
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 6
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims description 6
- WGQKYBSKWIADBV-UHFFFAOYSA-N benzylamine Chemical compound NCC1=CC=CC=C1 WGQKYBSKWIADBV-UHFFFAOYSA-N 0.000 claims description 6
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 claims description 6
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 claims description 6
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- KDSNLYIMUZNERS-UHFFFAOYSA-N 2-methylpropanamine Chemical compound CC(C)CN KDSNLYIMUZNERS-UHFFFAOYSA-N 0.000 claims description 4
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 4
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 claims description 4
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 claims description 4
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 4
- PFNFFQXMRSDOHW-UHFFFAOYSA-N spermine Chemical compound NCCCNCCCCNCCCN PFNFFQXMRSDOHW-UHFFFAOYSA-N 0.000 claims description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- BWLUMTFWVZZZND-UHFFFAOYSA-N Dibenzylamine Chemical compound C=1C=CC=CC=1CNCC1=CC=CC=C1 BWLUMTFWVZZZND-UHFFFAOYSA-N 0.000 claims description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 claims description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 claims description 3
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 claims description 3
- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 claims description 2
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 2
- SVONRAPFKPVNKG-UHFFFAOYSA-N 2-ethoxyethyl acetate Chemical compound CCOCCOC(C)=O SVONRAPFKPVNKG-UHFFFAOYSA-N 0.000 claims description 2
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- HPNMFZURTQLUMO-UHFFFAOYSA-N diethylamine Chemical compound CCNCC HPNMFZURTQLUMO-UHFFFAOYSA-N 0.000 claims description 2
- JJWLVOIRVHMVIS-UHFFFAOYSA-N isopropylamine Chemical compound CC(C)N JJWLVOIRVHMVIS-UHFFFAOYSA-N 0.000 claims description 2
- XTAZYLNFDRKIHJ-UHFFFAOYSA-N n,n-dioctyloctan-1-amine Chemical compound CCCCCCCCN(CCCCCCCC)CCCCCCCC XTAZYLNFDRKIHJ-UHFFFAOYSA-N 0.000 claims description 2
- 229940063675 spermine Drugs 0.000 claims description 2
- YBRBMKDOPFTVDT-UHFFFAOYSA-N tert-butylamine Chemical compound CC(C)(C)N YBRBMKDOPFTVDT-UHFFFAOYSA-N 0.000 claims description 2
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 claims description 2
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 2
- SYECJBOWSGTPLU-UHFFFAOYSA-N hexane-1,1-diamine Chemical compound CCCCCC(N)N SYECJBOWSGTPLU-UHFFFAOYSA-N 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
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- 238000005229 chemical vapour deposition Methods 0.000 description 4
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- 239000000463 material Substances 0.000 description 3
- 238000005411 Van der Waals force Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001721 carbon Chemical group 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000000527 sonication Methods 0.000 description 2
- 239000012808 vapor phase Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
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Images
Classifications
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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
-
- 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
Abstract
The invention discloses a method for efficiently preparing graphene sol, which comprises the following steps: s1, mixing flake graphite powder serving as a raw material with a small molecular intercalation agent and a dispersion solvent; s2, treating the mixed solution in the S1 for a period of time under ultrasound; s3, separating the small molecule intercalation agent and the graphene dispersion solvent layer; and S4, obtaining the graphene dispersion solvent layer. Under the combined action of the intercalation agent and the dispersing solvent, the high-quality graphene is uniformly dispersed in the dispersing solvent to form sol, the sol is stable, the stable storage time of the sol is at least more than 120 days, and the method has the advantages of simple process, low raw material cost, good quality of prepared graphene sol products and good stability.
Description
Technical Field
The invention relates to the field of inorganic non-metallic materials, in particular to a method for efficiently preparing graphene sol by ultrasonic, micromolecule intercalation and liquid phase stripping of graphene.
Background
Graphene (Graphene), also known as monoatomic layer graphite, is a quasi-two-dimensional material with a thickness of only one atomic layer. Graphene is the thinnest and the highest hardness of the currently known materials. The ideal graphene is almost completely transparent, the structure of the graphene is a two-dimensional hexagonal honeycomb plane structure, each carbon atom is hybridized by sp2, when the adjacent carbon atoms form bonds, the rest electrons do not participate in hybridization, the rest electrons and the electrons of the adjacent carbon atoms on the rest Pz orbit form a large pi band, and the electrons can freely move on the pi band, so that the graphene is endowed with ultrahigh conductivity. In addition, graphene has good optical properties and ultra-strong heat-resistant properties. The surface of the single-layer graphene presents certain folds, which shows that the graphene has certain ductility, and the excellent characteristics enable the graphene to have wide application prospects in the fields of displays, supercapacitors, field-effect tubes, lithium ion batteries, sensors and other devices, photocatalysis, sewage treatment and the like. In a plurality of application fields, the graphene sol loading mode can be realized in a graphene sol loading mode, and the application of graphene is realized. Therefore, the popularization of the application of the graphene prepared from the high-quality graphene sol is very important.
The mass production of graphene is the core for promoting the industrialization of graphene, and one of the key problems is the preparation method of graphene. The mechanical peeling method is a method for preparing a graphene material with fewer layers by breaking van der waals force between carbon atom layers of graphite. The methods of peeling can be classified into a tape method, a light rubbing method, and an ultra-thin slicing method. The graphene obtained by the mechanical stripping method has a large number of excellent characteristics such as complete structure and good conductivity, but the size of the obtained graphene is difficult to determine due to low single-production yield and poor controllability, so that the graphene is suitable for laboratory research and difficult to realize the industrialization of the graphene. The liquid phase or vapor phase direct exfoliation method refers to dispersing graphite in a liquid or vapor phase to prepare graphene by breaking van der waals forces between graphite layers. The graphene obtained by the method has a complete structure, but is not suitable for batch production. The Chemical Vapor Deposition (CVD) method can be classified into a metal substrate CVD method and a non-metal substrate CVD method depending on the substrate. Although the method can prepare large-area high-quality graphene, the process is complex, the preparation cost is high, and the transfer difficulty of the graphene generated on the surface of the substrate is high. At present, a main problem in the field of graphene is to develop a suitable preparation method to produce graphene with high yield, low cost and good controllability, thereby promoting the industrialization of graphene.
Disclosure of Invention
The invention aims to overcome the defects of complex preparation process and high cost of graphene in the prior art and provide a method for efficiently preparing graphene sol.
In order to solve the technical problems, the invention provides the following technical scheme:
the patent provides that the three of ultrasound, micromolecular intercalation and liquid phase stripping graphite are combined to strip graphite, and the graphene is stripped in a dispersion solvent of the graphene, so that the efficient preparation of graphene sol is realized. The preparation method has the outstanding advantages of simple process, low raw material cost, good quality of prepared graphene sol products and the like. The graphene sol prepared by the method has the outstanding characteristics of few graphene layers, high quality, good sol stability and the like.
Specifically, the method comprises the steps of taking crystalline flake graphite powder as a raw material, mixing graphite, a small molecular intercalation agent and a dispersing solvent, and treating the mixture for a period of time under the action of ultrasonic waves. And then separating the small-molecule intercalation agent and the graphene dispersion solvent layer to obtain the high-stability graphene sol.
The micromolecule intercalation agent comprises any one or more of liquid nitrogen, monoethylamine, dimethylamine, formamide, acetamide, aniline, spermine, triethylamine, benzylamine, trioctylamine, rosin amine, dibenzylamine, ethylenediamine, hexamethylenediamine, tert-butylamine, cyclohexylamine, n-propylamine, isobutylamine, n-octylamine, n-butylamine, diethylamine, n-hexylamine, n-pentylamine, isopropylamine, monoethanolamine, diethanolamine, triethanolamine, tetrabutylammonium bromide and ammonia water; the dosage (molar ratio to graphite) of the micromolecule intercalation agent is 50-1000 mol%.
The dispersing solvent has a solubility parameter of 8.3-10.3Cal/em3Preferably any one or more of cyclohexanone, acetone, isophorone, methyl propyl ketone, methyl isobutyl ketone, diethyl ketone, ethylene glycol ethyl ether, ethylene glycol butyl ether and ethylene glycol ethyl ether acetate; the dosage (mass ratio of the dispersion solvent to the graphite) of the dispersion solvent is 1-100: 1.
The ultrasonic treatment time is 0.5h-24 h.
Has the advantages that:
under the combined action of the intercalation agent and the dispersing solvent, the high-quality graphene is uniformly dispersed in the dispersing solvent to form sol, the sol is stable, the stable storage time of the sol is at least more than 120 days, and the method has the advantages of simple process, low raw material cost, good quality of prepared graphene sol products and good stability.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a TEM image of the sol prepared in example 1.
Detailed Description
The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are described herein for the purpose of illustration and explanation and not limitation.
Example 1
0.1g of flake graphite is weighed and placed in a 500mL beaker, then 20mL of liquid nitrogen and 250mL of cyclohexanone are added, and after stirring for 5min, ultrasonic treatment is carried out for 30 min. Separating liquid, obtaining graphene sol, and determining that the graphene sol has a few-layer structure, wherein a TEM picture of the graphene sol is shown in figure 2, and as can be seen from figure 2, the graphene sol prepared by the method has the advantages of few graphene layers and high quality.
Example 2
0.1g of flake graphite is weighed into a 500mL beaker, then 50mL of monoethylamine and 100mL of acetone are added, stirred for 5min and then treated with ultrasound for 24 h. And separating liquid to obtain the graphene sol.
Example 3
0.5g of flake graphite is weighed into a 500mL beaker, 50mL of dimethylamine and 100mL of acetone are added, and after stirring for 5min, sonication is carried out for 24 h. And separating liquid to obtain the graphene sol.
Example 4
0.5g of flake graphite is weighed and placed in a 500mL beaker, then 200mL of n-octylamine and 300mL of isophorone are added, stirred for 5min and ultrasonically treated for 12 h. And separating liquid to obtain the graphene sol.
Example 5
0.3g of flake graphite is weighed and placed in a 500mL beaker, then 200mL of diethanolamine and 300mL of isophorone are added, and after stirring for 5min, ultrasonic treatment is carried out for 5 h. And separating liquid to obtain the graphene sol.
Example 6
0.3g of flake graphite is weighed and placed in a 500mL beaker, then 200mL of triethylamine and 300mL of methyl propyl ketone are added, and after stirring for 5min, ultrasonic treatment is carried out for 5 h. And separating liquid to obtain the graphene sol.
Example 7
0.3g of flake graphite is weighed into a 500mL beaker, then 200mL of benzylamine and 300mL of methyl isobutyl ketone are added, and after stirring for 5min, ultrasonic treatment is carried out for 5 h. And separating liquid to obtain the graphene sol.
Example 8
0.3g of crystalline flake graphite is weighed and placed in a 500mL beaker, then 200mL of dibenzylamine and 300mL of ethylene glycol monobutyl ether are added, and after stirring for 5min, ultrasonic treatment is carried out for 5 h. And separating liquid to obtain the graphene sol.
Example 9
0.3g of flake graphite is weighed and placed in a 500mL beaker, 200mL of triethanolamine and 300mL of ethylene glycol ethyl ether are added, and after stirring for 5min, ultrasonic treatment is carried out for 5 h. And separating liquid to obtain the graphene sol.
Example 10
0.3g of flake graphite was weighed into a 500mL beaker, and then 200mL of n-butylamine and 300mL of diethyl ketone were added thereto, and after stirring for 5min, sonication was carried out for 5 hours. And separating liquid to obtain the graphene sol.
The stable shelf life of the graphene sols of the examples is shown in the following table:
finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A method for efficiently preparing graphene sol is characterized by comprising the following steps:
s1, mixing flake graphite powder serving as a raw material with a small molecular intercalation agent and a dispersion solvent;
s2, treating the mixed solution in the S1 for a period of time under ultrasound;
s3, separating the small molecule intercalation agent and the graphene dispersion solvent layer;
and S4, obtaining the graphene dispersion solvent layer.
2. The method for efficiently preparing graphene sol according to claim 1, comprising the steps of:
the micromolecule intercalation agent comprises any one or more of liquid nitrogen, monoethylamine, dimethylamine, ammonia water, formamide, acetamide, aniline, spermine, triethylamine, benzylamine, trioctylamine, rosin amine, dibenzylamine, ethylenediamine, hexanediamine, tert-butylamine, cyclohexylamine, n-propylamine, isobutylamine, n-octylamine, n-butylamine, diethylamine, n-hexylamine, n-pentylamine, isopropylamine, monoethanolamine, diethanolamine, triethanolamine and tetrabutylammonium bromide.
3. The method for efficiently preparing graphene sol according to claim 2, comprising the steps of: the molar ratio of the small molecular intercalation agent to the graphite powder is 50-1000: 100.
4. the method for efficiently preparing graphene sol according to claim 1, wherein the dispersion solvent has a solubility parameter of 8.3 to 10.3Cal/em3The organic solvent of (1).
5. The method for efficiently preparing graphene sol according to claim 4, wherein the dispersion solvent is any one of cyclohexanone, acetone, isophorone, methyl propyl ketone, methyl isobutyl ketone, diethyl ketone, ethylene glycol ethyl ether, ethylene glycol butyl ether, and ethylene glycol ethyl ether acetate.
6. The method for efficiently preparing graphene sol according to claim 5, wherein the mass ratio of the amount of the dispersion solvent to the graphite is 1-100: 1.
7. The method for efficiently preparing graphene sol according to claim 1, wherein the ultrasonic treatment time is 0.5h to 24 h.
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