CN110436447B - Colloidal graphene aqueous slurry and preparation method thereof - Google Patents
Colloidal graphene aqueous slurry and preparation method thereof Download PDFInfo
- Publication number
- CN110436447B CN110436447B CN201910685027.1A CN201910685027A CN110436447B CN 110436447 B CN110436447 B CN 110436447B CN 201910685027 A CN201910685027 A CN 201910685027A CN 110436447 B CN110436447 B CN 110436447B
- Authority
- CN
- China
- Prior art keywords
- graphene
- aqueous slurry
- graphene aqueous
- surfactant
- stabilizer
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 142
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 137
- 239000002002 slurry Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title abstract description 16
- 238000007613 slurry method Methods 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000008367 deionised water Substances 0.000 claims abstract description 31
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 31
- 239000004094 surface-active agent Substances 0.000 claims abstract description 27
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 16
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 16
- 239000000080 wetting agent Substances 0.000 claims abstract description 13
- 239000003292 glue Substances 0.000 claims abstract description 11
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 51
- 239000004576 sand Substances 0.000 claims description 37
- 239000003381 stabilizer Substances 0.000 claims description 37
- 239000000843 powder Substances 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 17
- 238000003801 milling Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 17
- -1 polyoxyethylene nonylphenol Polymers 0.000 claims description 16
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 14
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 14
- 239000011324 bead Substances 0.000 claims description 14
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 12
- 239000000194 fatty acid Substances 0.000 claims description 12
- 229930195729 fatty acid Natural products 0.000 claims description 12
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 12
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 6
- 239000007791 liquid phase Substances 0.000 claims description 6
- 238000009736 wetting Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 4
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 4
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 4
- 239000001866 hydroxypropyl methyl cellulose Substances 0.000 claims description 4
- 229920003088 hydroxypropyl methyl cellulose Polymers 0.000 claims description 4
- 235000010979 hydroxypropyl methyl cellulose Nutrition 0.000 claims description 4
- UFVKGYZPFZQRLF-UHFFFAOYSA-N hydroxypropyl methyl cellulose Chemical compound OC1C(O)C(OC)OC(CO)C1OC1C(O)C(O)C(OC2C(C(O)C(OC3C(C(O)C(O)C(CO)O3)O)C(CO)O2)O)C(CO)O1 UFVKGYZPFZQRLF-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920001577 copolymer Polymers 0.000 claims description 3
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims 2
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims 1
- 241000709400 Ruba Species 0.000 claims 1
- 239000002585 base Substances 0.000 claims 1
- 238000004299 exfoliation Methods 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
- 229910002804 graphite Inorganic materials 0.000 abstract description 4
- 239000010439 graphite Substances 0.000 abstract description 4
- 229920000642 polymer Polymers 0.000 abstract description 3
- 239000002562 thickening agent Substances 0.000 abstract 1
- 150000002148 esters Chemical class 0.000 description 11
- 150000004665 fatty acids Chemical class 0.000 description 11
- 238000002156 mixing Methods 0.000 description 10
- 230000001105 regulatory effect Effects 0.000 description 10
- 241000221095 Simmondsia Species 0.000 description 9
- 235000004433 Simmondsia californica Nutrition 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000000576 coating method Methods 0.000 description 3
- 235000019387 fatty acid methyl ester Nutrition 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002736 nonionic surfactant Substances 0.000 description 2
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000722826 Ardisia Species 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 235000014676 Phragmites communis Nutrition 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000013332 literature search Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000002834 transmittance Methods 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a colloidal graphene aqueous slurry and a preparation method thereof, wherein the graphene aqueous slurry comprises the following components in percentage by weight: 0.1-8 wt% of graphene; 0.1-5 wt% of wetting agent; 0.05-2 wt% of surfactant; 3 to 6 weight percent of thickener and 79 to 96.75 weight percent of deionized water. The excellent water locking performance of the Douglas glue is utilized, and the graphene is cooperated with the high polymer polyvinyl alcohol to limit the graphene sheets to small clusters, so that the graphene is prevented from overlapping again to form graphite. The surfactant is adsorbed on the graphene sheet layer, so that the graphene can be stably suspended in water. The graphene slurry has high concentration, low viscosity and excellent stability, and can be directly stirred to obtain a uniformly dispersed graphene solution.
Description
Technical Field
The invention relates to the technical field of graphene materials, in particular to low-viscosity colloidal graphene aqueous slurry and a preparation method thereof.
Background
Graphene is a two-dimensional planar structure formed by single-layer carbon atoms, has excellent physical properties such as high thermal conductivity, high strength, high visible light transmittance, high specific surface area, extremely low resistivity and the like, and has the characteristics of chemical inertness and the like, so that the graphene has potential application in the fields of energy storage, heat conduction, electronic devices, coatings and the like. And aiming at the application of graphene in the fields of lithium batteries, supercapacitors, heat-conducting coatings, anti-corrosion coatings and the like, the graphene needs to be dispersed in a solvent to prepare slurry, and then the slurry is applied to the fields. Through patent and literature search, the method for preparing the graphene powder at low cost is concentrated in a liquid phase stripping method and a redox method. The liquid phase stripping method is to obtain graphene in a liquid phase through physical methods such as machinery, microwaves and the like, and then obtain graphene powder through a method of centrifugation, filtration or spray drying. In order to inhibit graphene from being stacked again into graphite, some high-molecular dispersing agents are added, and graphene powder still has a stacking phenomenon, so that the graphene powder cannot be easily dispersed in a solvent.
CN201610213618.5 discloses a high-concentration and high-purity graphene slurry, a preparation method and application thereof, the viscosity of the graphene slurry is up to 10000 mpa.s, and the graphene slurry is difficult to disperse uniformly in a solvent again. CN201210018109.9 discloses a preparation method of graphene uniform dispersion liquid, and only graphene dispersion liquid with concentration less than 1% is obtained through the action of a surfactant. CN201810446500.6 discloses a preparation method of graphene slurry, which uses polyvinylpyrrolidone (PVP) as a dispersing agent to obtain graphene slurry with the maximum concentration of only 2wt%, and low-content PVP is easy to sink, so that graphene is sunk. The graphene powder has the defects of uneven dispersion, low concentration and the like in application, so that the application of the graphene powder is limited, and the preparation of the high-concentration, low-viscosity, stable and easily-dispersible graphene slurry can accelerate the application of graphene in downstream products.
Disclosure of Invention
In view of the above, the technical problem to be solved by the invention is to provide a colloidal low-viscosity graphene aqueous slurry and a preparation method thereof, wherein the colloidal graphene aqueous slurry prepared by the method has very good stability while keeping higher depth and lower viscosity, and is easy to disperse in water again, so that the application convenience and the application field are greatly increased.
The invention provides a colloidal graphene aqueous slurry and a preparation method thereof, wherein the preparation method comprises the following steps:
the graphene aqueous slurry comprises the following components in percentage by weight:
0.1-8 wt% of graphene;
0.1-5 wt% of wetting agent;
0.05-2 wt% of surfactant;
3-6wt% of stabilizer
79wt% to 96.75wt% of deionized water.
The graphene is graphene powder prepared by a liquid phase stripping method, the surface of the graphene powder does not contain functional groups, the thickness of the graphene powder is 1-2.4 nm, and the size of the graphene powder is 1-15 um.
Wherein the wetting agent is one or the combination of carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, polyethylene glycol, ethanol and propylene glycol.
Wherein the surfactant is one or a combination of nonionic surfactant, nonylphenol polyoxyethylene ether, high-carbon fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, fatty acid methyl ester ethoxylate, polyoxyethylene ether and polyoxypropylene phase-embedded copolymer.
Wherein the stabilizer is a mixture of the Philippine reed rhizome gum, the polyvinyl alcohol (PVA), the propylene glycol and the alkali, and the alkali in the stabilizer is an aqueous solution of potassium hydroxide, sodium hydroxide, triethanolamine and ammonia water with the weight percent of 0.1-5 percent; the mass ratio of the components of the stabilizer is (1-8): (0.1-1) 5:0.5.
The invention also provides a preparation method of the colloidal graphene aqueous slurry, which comprises the following steps:
a) Dispersing a wetting agent in deionized water to form a wetting solution;
b) Adding graphene powder into a wetting solution, uniformly stirring, transferring to a sand mill for sand milling to obtain a primarily dispersed graphene aqueous solution;
c) Adding a surfactant into the graphene aqueous solution and uniformly stirring;
d) And adding a stabilizer into the graphene aqueous solution, and uniformly stirring to obtain the graphene aqueous slurry.
The rotating speed of the sand mill in the step B) is 500-4000 r/min, the sand milling time is 0.5-24 h, and the diameter of sand milling beads is 0.4mm.
Compared with the prior art, the invention provides the colloidal graphene aqueous slurry and the preparation method thereof, which utilize the excellent water locking performance of the Ardisia rufimbriae, and the cooperation of the colloidal graphene aqueous slurry and high polymer polyvinyl alcohol (PVA) acts on graphene to limit the graphene into small clusters, and avoid the graphene from overlapping again to form graphite. The surfactant is adsorbed on the graphene sheet layer, so that the graphene can be stably suspended in water. The graphene slurry has high concentration, low viscosity and excellent stability, and can be used for dispersing the graphene in water again by simply stirring to destroy small clusters of the graphene, so that the thermal movement of the graphene is prevented from being limited by increasing the viscosity of a system through a large number of polymers.
Drawings
Fig. 1 is a SEM image of graphene used in example 1 of the present invention.
Fig. 2 is a comparative physical diagram of the graphene aqueous slurries obtained in example 1 and comparative example 1 of the present invention after standing for 2 months.
Fig. 3 is an optical diagram of the aqueous graphene slurry obtained in example 1 of the present invention.
Fig. 4 is an optical diagram of the aqueous graphene slurry obtained in example 1 of the present invention.
Fig. 5 is an optical diagram of dispersion of the aqueous slurry of graphene obtained in example 1 of the present invention in water.
Detailed Description
The invention provides a colloidal graphene aqueous slurry and a preparation method thereof, wherein the colloidal graphene aqueous slurry comprises the following parts:
the gel-type graphene aqueous slurry comprises the following components in percentage by weight:
0.1-8 wt% of graphene;
0.1-5 wt% of wetting agent;
0.05-2 wt% of surfactant;
3-6wt% of stabilizer
79wt% to 96.75wt% of deionized water.
Preferably, the components are as follows:
0.1-6wt% of graphene;
0.1-5 wt% of wetting agent;
0.05-2 wt% of surfactant;
3-6wt% of stabilizer
81 to 96.75 weight percent of deionized water.
More preferably, the components are as follows:
0.1-5 wt% of graphene;
0.1-5 wt% of wetting agent;
0.05-2 wt% of surfactant;
3-4wt% of stabilizer
84 to 96.75 weight percent of deionized water.
The preparation method of the colloidal graphene aqueous slurry comprises the following steps:
a) Dispersing a wetting agent in deionized water to form a wetting solution;
b) Adding graphene powder into a wetting solution, uniformly stirring, transferring to a sand mill for sand milling to obtain a primarily dispersed graphene aqueous solution;
c) Adding a surfactant into the graphene aqueous solution and uniformly stirring;
d) And adding a stabilizer into the graphene aqueous solution, and uniformly stirring to obtain the graphene aqueous slurry.
According to the invention, the wetting agent of step A) is not limited, but is well known to the person skilled in the art; the wetting agent is preferably one or more selected from carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, polyethylene glycol, ethanol, propylene glycol and the like; more preferably one or more of carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, polyethylene glycol.
According to the invention, the graphene powder prepared by the liquid phase stripping method for the graphene in the step B) does not contain functional groups on the surface, and has the thickness of 1-2.4 nm and the size of 1-15 um.
According to the invention, the materials of the sand mill model and the sand mill beads in the step B) are not limited, and the rotating speed of the sand mill is preferably 500-4000 r/min, more preferably 1200-3000 r/min, and most preferably 1800-3000 r/min. The sanding period is preferably 0.5-24 hours, more preferably 1-12 hours, and most preferably 2-8 hours. The sand beads used in the sand mill are preferably 0.4mm in diameter.
According to the invention, the surfactant in the step C) is selected from nonionic surfactants, preferably one or a combination of nonylphenol polyoxyethylene ether, higher fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, fatty acid methyl ester ethoxylate, polyoxyethylene ether and polyoxypropylene embedded copolymer; more preferably one or the combination of higher fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, fatty acid methyl ester ethoxylate and polyoxyethylene ether; most preferred is one or a combination of fatty acid polyoxyethylene esters, polyoxyethylene ethers.
According to the invention, for step D) the stabilizer is selected from the group consisting of a mixture of Ardisia, PVA, propylene glycol and alkali, wherein the alkali in the stabilizer is preferably one or a combination of aqueous solutions of potassium hydroxide, sodium hydroxide, triethanolamine and ammonia water in an amount of 0.1-5 wt%; more preferably 0.1wt% to 5wt% of one or a combination of aqueous solutions of triethanolamine and ammonia water; most preferably 0.1wt% to 5wt% triethanolamine. The mass ratio of the components of the stabilizer is preferably (1-8): (0.1-1): 5:0.5, more preferably (2-8): (0.1-1): 5:0.5, most preferably (4-8): (0.5-1) 5:0.5.
According to the invention, the graphene aqueous solution is prepared, the sequence of adding substances to the graphene aqueous solution is preferably surfactant and stabilizer, specifically, the surfactant is added to the graphene aqueous solution and stirred uniformly, and then the stabilizer is added to the graphene aqueous solution and stirred uniformly.
In order to further illustrate the present invention, the following describes in detail the preparation method of the colloidal graphene aqueous slurry provided by the present invention with reference to examples.
Example 1
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 1: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
Fig. 1 is a SEM image of graphene used in example 1 of the present invention; as can be seen from fig. 1, the untreated graphene powder has a serious stacking phenomenon. Fig. 2 is an optical diagram of the aqueous graphene slurry obtained in example 1 of the present invention; from fig. 2 it can be seen that graphene forms small clusters locally, but is not stacked into graphite. Fig. 3 is an optical diagram of dispersion of the aqueous slurry of graphene obtained in example 1 of the present invention in water, and it can be seen from fig. 3 that graphene is uniformly dispersed in water, and bound graphene small clusters are not found. The obtained graphene aqueous slurry was subjected to viscosity measurement by using an NDJ-1 rotational viscometer, the viscosity was 763mpa.s, 2 parts of the graphene aqueous slurry was dispersed in 98 parts of an aqueous solution, and the pH was measured and was 8.00.
Comparative example 1
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer comprises deionized water, PVA, propylene glycol and triethanolamine, and the mass ratio is 1: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was measured as 169mpa.s and the ph was 9.0 according to the method of example 1.
Comparative example 2
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. Then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant sodium dodecyl sulfate is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 1: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was 5921mpa.s and ph was 8.20 as tested in the method of example 1.
Comparative example 3
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer comprises jojoba gum, deionized water, propylene glycol and triethanolamine, and the mass ratio is 1: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was 52mpa.s and the ph was 8.14, tested as in example 1.
Example 2
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 4: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was measured as 823mpa and ph was 8.20 according to the method of example 1.
Example 3
Uniformly mixing 0.1 part of polyethylene glycol 400 and 95 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer comprises jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 8: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was measured as 1082mpa and the ph was 8.12 according to the method of example 1.
Example 4
Uniformly mixing 4 parts of polyvinylpyrrolidone and 87.9 parts of deionized water to prepare a solution A. Then adding 1 part of graphene powder into the solution A, and uniformly stirring. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 0.1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 4: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was 896mpa and ph 8.30, tested as in example 1.
Example 5
Uniformly mixing 4 parts of polyvinylpyrrolidone and 87 parts of deionized water to prepare a solution A. Then 5 parts of graphene powder is added into the solution A and stirred uniformly. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 1 part of surfactant fatty acid polyoxyethylene ester is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 4: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was 1262mpa and the ph was 8.24, tested according to the method of example 1.
Example 6
Uniformly mixing 4 parts of polyvinylpyrrolidone and 87 parts of deionized water to prepare a solution A. Then 5 parts of graphene powder is added into the solution A and stirred uniformly. Then transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 1 part of the surfactant polyoxyethylene ether is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer is composed of jojoba glue, PVA, propylene glycol and triethanolamine, and the mass ratio is 4: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The viscosity of the resulting graphene aqueous slurry was measured as in example 1 at 1250mpa and ph at 8.32.
Example 7
Uniformly mixing 4 parts of polyvinylpyrrolidone and 87 parts of deionized water to prepare a solution A. Then 5 parts of graphene powder is added into the solution A and stirred uniformly. And transferred to a sander for sanding, the sanded beads were 0.4mm in diameter and 1.5 times the mass of deionized water. The rotation speed of the sand mill is 2000r/min, and the sand milling time is 4h. And then the rotating speed is regulated to 200r/min, and 1 part of the surfactant polyoxyethylene ether is slowly added. After half an hour, 3 parts of stabilizer are slowly added, wherein each group of stabilizer comprises jojoba glue, PVA, propylene glycol and ammonia water, and the mass ratio is 4: 0.1:5:0.5. And (5) continuously sanding for 1h at the rotating speed of 200r/min, and finally obtaining the graphene aqueous slurry.
The resulting graphene aqueous slurry was tested according to the method of example 1 to have a viscosity of 1742mpa and a ph of 8.50.
The foregoing is merely a preferred embodiment of the invention, and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the principles of the present invention, which are intended to be comprehended within the scope of the present invention.
Claims (5)
1. The colloidal graphene aqueous slurry is characterized by comprising the following components in percentage by weight:
0.1-8 wt% of graphene;
0.1-5 wt% of wetting agent;
0.05-2 wt% of surfactant;
3-6 wt% of stabilizer;
79 to 96.75 weight percent of deionized water;
the stabilizer is a mixture of the ruba glue, the polyvinyl alcohol, the propylene glycol and the alkali;
the surfactant is one or a combination of polyoxyethylene nonylphenol ether, polyoxyethylene higher fatty alcohol ether, polyoxyethylene fatty acid ester, polyoxyethylene methyl ester ethoxylate, polyoxyethylene ether and polyoxypropylene embedded copolymer;
the mass ratio of the reed-solomon glue to the polyvinyl alcohol to the propylene glycol to the alkali is (1-8): (0.1-1) 5:0.5;
the wetting agent is one or the combination of carboxymethyl cellulose, hydroxypropyl methyl cellulose, polyvinylpyrrolidone, polyethylene glycol, ethanol and propylene glycol.
2. The colloidal graphene aqueous slurry according to claim 1, wherein the base is one or a combination of triethanolamine and ammonia water in an amount of 0.1wt% to 5wt%.
3. The colloidal graphene aqueous slurry according to claim 1, wherein the graphene is graphene powder prepared by a liquid phase exfoliation method; the surface does not contain functional groups, the thickness is 1-2.4 nm, and the size is 1-15 um.
4. A method for preparing the colloidal graphene aqueous slurry according to any one of claims 1 to 3, wherein the method for preparing the colloidal graphene aqueous slurry comprises the following steps:
a) Dispersing a wetting agent in deionized water to form a wetting solution;
b) Adding graphene powder into a wetting solution, uniformly stirring, transferring to a sand mill for sand milling to obtain a primarily dispersed graphene aqueous solution;
c) Adding a surfactant into the graphene aqueous solution and uniformly stirring;
d) And adding a stabilizer into the graphene aqueous solution, and uniformly stirring to obtain the graphene aqueous slurry.
5. The method according to claim 4, wherein the rotational speed of the sand mill in the step B) is 500-4000 r/min, the sand milling time is 0.5-24 h, and the diameter of the sand milling beads is 0.4mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910685027.1A CN110436447B (en) | 2019-07-26 | 2019-07-26 | Colloidal graphene aqueous slurry and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910685027.1A CN110436447B (en) | 2019-07-26 | 2019-07-26 | Colloidal graphene aqueous slurry and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110436447A CN110436447A (en) | 2019-11-12 |
| CN110436447B true CN110436447B (en) | 2023-12-19 |
Family
ID=68431793
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910685027.1A Active CN110436447B (en) | 2019-07-26 | 2019-07-26 | Colloidal graphene aqueous slurry and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110436447B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112309609B (en) * | 2020-10-10 | 2021-06-04 | 山东华冠智能卡有限公司 | Water-based graphene conductive paste, preparation method thereof and RFID label |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106860031A (en) * | 2017-03-06 | 2017-06-20 | 江西联锴新材料有限公司 | A kind of Graphene aqueous dispersion pulp used for cosmetic and preparation method thereof |
-
2019
- 2019-07-26 CN CN201910685027.1A patent/CN110436447B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106860031A (en) * | 2017-03-06 | 2017-06-20 | 江西联锴新材料有限公司 | A kind of Graphene aqueous dispersion pulp used for cosmetic and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110436447A (en) | 2019-11-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102618107B (en) | Conductive graphite cream and preparation method thereof | |
| JP5367826B2 (en) | Dispersant for carbon filler | |
| CN108028386A (en) | Carbon nano tube dispersion liquid and preparation method thereof | |
| CN106047015B (en) | Conductive coating material of lithium ion battery, preparation method of conductive coating material and lithium ion battery | |
| CN106752878A (en) | A kind of Graphene low-voltage heating coating and preparation method thereof | |
| CN109004220B (en) | Boric acid compound modified lithium ion battery silicon cathode and preparation method thereof | |
| CN108530996A (en) | A kind of one-step method prepares graphene-based water-soluble conducting ink and preparation method thereof | |
| JPWO2010123137A1 (en) | Carbon black polar dispersion composition | |
| JP2014019619A (en) | Fine carbon dispersion liquid and method of producing the same, and electrode paste and electrode for lithium ion battery using the same | |
| Cerbelaud et al. | Numerical and experimental study of suspensions containing carbon blacks used as conductive additives in composite electrodes for lithium batteries | |
| CN102702796A (en) | Method for improving dispersion property of nanosilicon grinding fluid | |
| CN106299524A (en) | A kind of it is prone to carbon coated collector that powder separates and application and recovery method with foil | |
| CN108165069A (en) | A kind of watersoluble plumbago alkene dispersion liquid of high-content and preparation method thereof | |
| CN110436447B (en) | Colloidal graphene aqueous slurry and preparation method thereof | |
| TWI428285B (en) | Micro-scaled flake silver particles and method for producing the same | |
| CN108735345A (en) | A kind of painting carbon electrode electrocondution slurry and preparation method thereof | |
| CN109148886A (en) | Binder and preparation method thereof, anode plate for lithium ionic cell | |
| CN101260234A (en) | High conductivity polyaniline water dispersion liquid and preparation method thereof | |
| CN104194580A (en) | Antistatic scratch-resistant coating and coating method thereof | |
| CN110790236A (en) | Method for coating nano ammonium perchlorate by graphene wet process | |
| CN104241606A (en) | Preparation method of lithium iron phosphate positive plate with high rate and superior low-temperature performance | |
| CN103865092B (en) | Modified carbon nano-tube and PVDF hydridization prepare the method for anion-exchange membrane | |
| CN115196627A (en) | Graphene slurry pre-dispersion process | |
| CN110010361A (en) | The preparation method of composite conducting slurry and the preparation method of electrode | |
| TW201533960A (en) | Silicon carbon composite electrode material and method of preparing the same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |