CN115196627A - Graphene slurry pre-dispersion process - Google Patents
Graphene slurry pre-dispersion process Download PDFInfo
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- CN115196627A CN115196627A CN202211018854.3A CN202211018854A CN115196627A CN 115196627 A CN115196627 A CN 115196627A CN 202211018854 A CN202211018854 A CN 202211018854A CN 115196627 A CN115196627 A CN 115196627A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 128
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 128
- 239000002002 slurry Substances 0.000 title claims abstract description 65
- 239000006185 dispersion Substances 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000008569 process Effects 0.000 title claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 50
- 239000004094 surface-active agent Substances 0.000 claims abstract description 47
- 239000002994 raw material Substances 0.000 claims abstract description 32
- 239000002904 solvent Substances 0.000 claims abstract description 31
- 239000003607 modifier Substances 0.000 claims abstract description 19
- 238000005303 weighing Methods 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 20
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 18
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 12
- 239000010949 copper Substances 0.000 claims description 12
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims description 12
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 claims description 12
- 229940112669 cuprous oxide Drugs 0.000 claims description 12
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 8
- 229920002845 Poly(methacrylic acid) Polymers 0.000 claims description 8
- 229920002125 Sokalan® Polymers 0.000 claims description 8
- 229910000431 copper oxide Inorganic materials 0.000 claims description 8
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 8
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 8
- 229920002401 polyacrylamide Polymers 0.000 claims description 8
- 239000004584 polyacrylic acid Substances 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 8
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 3
- 230000000694 effects Effects 0.000 abstract description 12
- 230000003993 interaction Effects 0.000 abstract description 6
- 230000002776 aggregation Effects 0.000 abstract description 5
- 238000005411 Van der Waals force Methods 0.000 abstract description 4
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000002135 nanosheet Substances 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000004220 aggregation Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000007405 data analysis Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 239000012065 filter cake Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a graphene slurry pre-dispersion process, which comprises the following steps: s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent in a certain proportion; s2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred; s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A; and S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B. The invention can overcome the interaction of Van der Waals force and pi-pi, avoid the agglomeration of graphene, improve the dispersion effect, and can be modified according to the needs, and the graphene slurry is not restricted.
Description
Technical Field
The invention relates to the technical field of graphene slurry, in particular to a graphene slurry pre-dispersion process.
Background
Graphene is a new material with a monolayer two-dimensional honeycomb lattice structure formed by tightly packing sp2 hybridized and connected carbon atoms. The graphene has excellent optical, electrical and mechanical properties, and has important application prospects in the aspects of materials science, micro-nano processing, energy, biomedicine, drug delivery and the like. Graphene can be formed by a micro-mechanical lift-off method, a redox method, a SiC epitaxial growth method, a chemical vapor deposition method.
The preparation of the graphene slurry is an industrial application approach aiming at graphene, and can improve the dispersibility of the graphene in various systems so as to enhance the comprehensive properties of the composite material, such as electric conductivity, heat conductivity, mechanics and the like. Graphene is a plane conjugated structure formed by sp2 hybridized carbon atoms, and a very strong pi-pi effect and a van der waals acting force exist between sheet layers of the graphene, so that the oleophobic and hydrophobic graphene is easy to agglomerate, the graphene slurry with good dispersion stability is difficult to obtain, and the practical application of the graphene is severely restricted.
Therefore, we propose a graphene slurry pre-dispersion process to solve the above problems.
Disclosure of Invention
The invention aims to provide a graphene slurry pre-dispersion process to solve the problems in the background art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a graphene slurry pre-dispersion process comprises the following steps: s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent in a certain proportion; s2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersion tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the graphene raw material, the surfactant, the dispersing agent and the solvent are uniformly stirred; s3, weighing a modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm, and stirring uniformly to obtain graphene slurry A; and S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
Preferably, the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
Preferably, the dispersant is polyvinyl alcohol.
Preferably, the modifier is one of copper, nickel and cuprous oxide.
Preferably, the ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
Preferably, the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 5-20:3-6:5-8:60-80.
Compared with the prior art, the invention has the beneficial effects that:
1. the surfactant in the invention can reduce surface energy and surface tension, has the functions of wetting solid surface, splitting and deagglomerating particle groups, and reagglomerating dispersed particles of tissues;
2. the dispersing agent dispersion method is mainly based on Van der Waals force, pi-pi interaction and the like, can avoid damaging the conjugated structure on the surface of the graphene sheet layer, well keeps the characteristics of graphene, and is high in efficiency and convenient to use;
3. according to the invention, a modifier, generally copper, nickel, cuprous oxide and the like, can be slowly added into the slurry, the slurry is coated on the powder without agglomeration, the conductive effect can be improved by coating copper, and the antibacterial effect can be greatly improved by coating cuprous oxide;
4. the dispersion effect of the graphene nanosheets can be remarkably improved by prolonging the ultrasonic time or increasing the ultrasonic power, the ultrasonic power is 960w, the dispersion effect of the graphene nanosheets is the best when the ultrasonic time is 4h, and the crushing degree is relatively low;
5. in conclusion, the graphene composite material can overcome the interaction between van der Waals force and pi-pi, avoid the aggregation of graphene, improve the dispersion effect, and can be modified according to the needs, so that the graphene slurry is not restricted.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example 1
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 9:3-6:5-8: 60;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred;
s3, weighing a modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm, and stirring uniformly to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
The graphene raw material and solvent mass ratio in the embodiment reaches 15%, the graphene composite electrothermal film has ultrahigh graphene concentration, can be added into electrothermal slurry to be made into an electrothermal film product, and has the advantages of quick and uniform heating, stable power, high electrothermal conversion efficiency, high safety, long service life and the like, and the graphene slurry has a filter cake shape at a concentration exceeding 15%, so that high filling and high performance can be realized.
Operators need to wear appropriate protective gloves and protective clothes to avoid direct contact with human bodies, and if the operators carelessly contact with the human bodies, the operators can wash the human bodies clean by a large amount of clear water; the storage in a cool, ventilated and dry storehouse reduces the exposure time to air.
Example 2
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 5:3-6:5-8: 80;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred;
s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
The ratio of the graphene raw material to the solvent in the embodiment is minimum, the graphene slurry has a low graphene concentration, and can be used as an aqueous graphene slurry to provide permanent antistatic and excellent heat-conducting properties for aqueous paint and coating. The conductivity of the graphene slurry is inversely related to the surface resistance of the coating along with the addition amount of the graphene raw material.
Example 3
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is (5-20): 3-6: 5:60-80 parts;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred;
s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
Example 4
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 5-20:3-6: 8:60-80 parts of;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred;
s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
Example 3 differs from example 4 in that: the proportion of the dispersant was different, and the proportion of the dispersant in example 3 was larger than that in example 4.
After the graphene slurry in the embodiments 3 and 4 is pre-dispersed, ultraviolet absorption spectrum tests are performed when the graphene slurry is respectively kept still for 0d, 1d, 4d and 7d, so as to perform data analysis of different types and different amounts, and the concentration of the dispersing agent can be obtained to effectively improve the dispersion stability of the graphene and inhibit the aggregation of graphene sheets. And the discharge specific capacity and the coulombic efficiency of the battery prepared by preparing different graphene slurries can be cycled for 50 times under the multiplying power of 1C.
Example 5
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 5-20:3:5-8: 60-80 parts;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersion tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the graphene raw material, the surfactant, the dispersing agent and the solvent are uniformly stirred;
s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
Example 6
A graphene slurry pre-dispersion process comprises the following steps:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent according to a certain proportion, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is (5-20): 6:5-8:60-80 parts;
the surfactant is one of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid and polyacrylamide.
The dispersing agent is polyvinyl alcohol.
S2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersion tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the graphene raw material, the surfactant, the dispersing agent and the solvent are uniformly stirred;
s3, weighing the modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm until the mixture is uniformly stirred to obtain graphene slurry A;
the modifier is one of copper, nickel and cuprous oxide.
And S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
The ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
Example 5 differs from example 6 in that: the ratio of the surfactants in example 5 and example 6, and the ratio of the surfactant in example 5 is greater than that in example 6, the types of the surfactants can be classified, and the influence on the graphene slurry when different types of surfactants with the same amount and different types of surfactants with different amounts are prepared is that 3 types of surfactants, namely, anionic surfactant, cationic surfactant and nonionic surfactant, are respectively selected, and the influence on the structure and concentration of the graphene slurry is researched through ultraviolet-visible spectroscopy.
The surfactant in the invention can reduce surface energy and surface tension, has the functions of wetting solid surface, splitting and deagglomerating particle groups, and reagglomerating dispersed particles of tissues, but it should be noted that when the surfactant is added, the added surfactant can not cause influence;
1. generally, graphene is neither hydrophilic nor oleophilic, so that a common dispersant molecule is difficult to form a strong physical adsorption effect with graphene, the dispersion effect on graphene is poor, and graphene can be dispersed and stabilized only by adopting a dispersant with a special structure. The dispersant requires that one end of the dispersant can have a strong effect with the graphene sheet and the other end of the dispersant has good compatibility with a resin system. Only when the dispersant and the graphene lamellar structure form stronger interaction and the pi-pi interaction between graphene sheets is overcome, the dispersant can be relatively stably dispersed in the coating resin. Compared with a chemical modification dispersion method, the dispersing agent dispersion method is mainly based on Van der Waals force, pi-pi interaction and the like, can avoid damage to a conjugated structure on the surface of a graphene sheet layer, well keeps the characteristics of graphene, and is high in efficiency and convenient to use. The polyvinyl alcohol is used as a dispersing agent to enable the graphene to be dispersed in the solution more effectively. In the prepared composite film, the graphene sheet layer is wrapped by the PVA long chain, and the two phases are combined very tightly, so that the graphene is uniformly dispersed in the solution.
2. Modifiers, generally copper, nickel, cuprous oxide and the like, can be slowly added into the slurry, the slurry is coated on the powder without agglomeration, the conductive effect can be improved by coating the powder with copper, and the antibacterial effect can be greatly improved by coating the powder with cuprous oxide;
3. the dispersion effect of the graphene nanosheets can be remarkably improved by prolonging the ultrasonic time or increasing the ultrasonic power, but the sizes of the graphene nanosheets are correspondingly reduced to a certain extent, a large number of edge defects are generated, particularly vacancy defects occur even when the power is too large or the time is too long, from the microscopic viewpoint, the electrostatic force dominates, the surface is researched, the ultrasonic power is 960w, the dispersion effect of the graphene nanosheets is the best when the ultrasonic time is 4h, and the crushing degree is relatively low.
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 (6)
1. The graphene slurry pre-dispersion process is characterized by comprising the following steps of:
s1, weighing a graphene raw material, a surfactant, a dispersant and a solvent in a certain proportion;
s2, adding the graphene raw material, the surfactant, the dispersing agent and the solvent weighed in the S1 into a pre-dispersing tank in proportion, adjusting the rotating speed of a stirrer to be 1000-1200rpm, and increasing the rotating speed with the increase of the adding amount until the mixture is uniformly stirred;
s3, weighing a modifier with the mass ratio of 10-15, setting the rotating speed of a stirrer to be 1000rpm, and stirring uniformly to obtain graphene slurry A;
and S4, placing the graphene slurry A in the step S3 into an ultrasonic instrument for ultrasonic vibration to obtain a final graphene slurry B.
2. The graphene slurry predispersion process according to claim 1, wherein the surfactant is one of polyvinylpyrrolidone, sodium dodecylbenzene sulfonate, sodium lignosulfonate, polyvinyl alcohol, polyethylene oxide, polyacrylic acid, polymethacrylic acid, and polyacrylamide.
3. The graphene slurry predispersion process according to claim 1, wherein the dispersant is polyvinyl alcohol.
4. The graphene slurry predispersion process according to claim 1, wherein the modifier is one of copper, nickel and cuprous oxide.
5. The graphene slurry predispersion process according to claim 1, wherein the ultrasonic power of the ultrasonic instrument is 960w, and the ultrasonic time is 4h.
6. The graphene slurry pre-dispersion process according to claim 1, wherein the mass ratio of the graphene raw material to the surfactant to the dispersant to the solvent is 5-20:3-6:5-8:60-80.
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CN109147988A (en) * | 2018-08-02 | 2019-01-04 | 中国科学院苏州纳米技术与纳米仿生研究所南昌研究院 | A kind of preparation method of thin graphene slurry |
CN109939611A (en) * | 2019-03-21 | 2019-06-28 | 山东华冠智能卡有限公司 | Graphene-based electrocondution slurry dispersing agent and preparation method thereof |
CN112275159A (en) * | 2020-10-15 | 2021-01-29 | 焦作熔创石墨科技有限公司 | Graphene slurry pre-dispersing device |
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CN115924897A (en) * | 2023-02-20 | 2023-04-07 | 江苏希诚新材料科技有限公司 | Device and method for centrifugally stripping single-layer/few-layer graphene dispersion liquid |
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