CN117038346A - Supercapacitor electrode homogenate slurry and preparation process thereof - Google Patents
Supercapacitor electrode homogenate slurry and preparation process thereof Download PDFInfo
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- CN117038346A CN117038346A CN202310883632.6A CN202310883632A CN117038346A CN 117038346 A CN117038346 A CN 117038346A CN 202310883632 A CN202310883632 A CN 202310883632A CN 117038346 A CN117038346 A CN 117038346A
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- 239000002002 slurry Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 39
- 239000002904 solvent Substances 0.000 claims abstract description 27
- 239000000839 emulsion Substances 0.000 claims abstract description 26
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000011230 binding agent Substances 0.000 claims abstract description 18
- 239000006258 conductive agent Substances 0.000 claims abstract description 18
- 239000002270 dispersing agent Substances 0.000 claims abstract description 18
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 14
- 229920003048 styrene butadiene rubber Polymers 0.000 claims abstract description 10
- 239000001768 carboxy methyl cellulose Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 7
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 6
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 6
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 6
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002174 Styrene-butadiene Substances 0.000 claims abstract description 5
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000006229 carbon black Substances 0.000 claims abstract description 5
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 claims abstract description 5
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 claims abstract description 5
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 3
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 3
- 239000010439 graphite Substances 0.000 claims abstract description 3
- 229920001495 poly(sodium acrylate) polymer Polymers 0.000 claims abstract description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 3
- NNMHYFLPFNGQFZ-UHFFFAOYSA-M sodium polyacrylate Chemical compound [Na+].[O-]C(=O)C=C NNMHYFLPFNGQFZ-UHFFFAOYSA-M 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 22
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 9
- 239000011265 semifinished product Substances 0.000 claims description 8
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000000047 product Substances 0.000 claims description 2
- 239000011267 electrode slurry Substances 0.000 claims 8
- 239000003292 glue Substances 0.000 abstract description 4
- 239000003990 capacitor Substances 0.000 description 12
- 238000000265 homogenisation Methods 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 235000010948 carboxy methyl cellulose Nutrition 0.000 description 3
- 239000008112 carboxymethyl-cellulose Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 238000010008 shearing Methods 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention provides supercapacitor electrode homogenate slurry and a preparation process thereof, wherein the mass ratio of active carbon, conductive agent, dispersing agent and binder emulsion in the slurry is 100:1-10:1-10:1-10, wherein the binder emulsion comprises 40% of binder and 60% of solvent, wherein the binder emulsion is at least one of styrene-butadiene rubber emulsion SBR, sodium polyacrylate emulsion and polytetrafluoroethylene PTFE emulsion, and the solvent is N-methyl pyrrolidone or deionized water; the conductive agent is graphite, carbon nano tube or carbon black; the dispersing agent is polyvinylpyrrolidone or sodium carboxymethyl cellulose; the slurry is free from preparation of dispersant glue solution, the procedure is omitted, the overall homogenizing time is reduced, the viscosity is 500-800 mPa.s, is far lower than that of the original process, and the fluidity is excellent.
Description
Technical Field
The invention relates to the field of manufacturing of supercapacitor electrodes, in particular to supercapacitor electrode homogenate slurry and a preparation process thereof.
Background
Compared with a lithium ion battery, the super capacitor is a high-power environment-friendly energy storage component, and has a power density which is 1-2 orders of magnitude higher, so that the super capacitor has a wide application prospect in various fields such as wind power generation, smart grids, electric power energy storage, rail transit, application equipment and the like. The super capacitor battery has the characteristics of high power density, light weight, quick charging, no memory benefit, long service life and the like, and becomes the important research and development direction in most countries.
Supercapacitors are generally composed of a housing, a pole piece, a diaphragm and an electrolyte, while the pole piece contains the main core technology of capacitor manufacture, and the manufacturing quality and productivity thereof are the subject of research and improvement by most manufacturers. In the process of manufacturing the electrode, the mixing operation of the active carbon, the conductive agent, the adhesive and the solvent is called as homogenate, the principle is that powder and the solvent are uniformly stirred by a closed stirrer to form slurry, the slurry is uniformly coated on a foil, and then the foil is dried to form a pole piece, and finally the pole piece is rolled and sheared to form the electrode. As the first process of electrode manufacture, the active carbon, the solvent and the conductive agent are fully mixed, stirred for a long time at a low speed, and uniformly dispersed slurry is formed by virtue of friction force among the pellets, so that the performance requirement can be met, the homogenization time is generally 3-6 hours and even more is 8 hours on the premise of ensuring the homogenization quality, the low-efficiency process is seriously unmatched with the productivity of subsequent rolling, shearing and monomer assembly, and the productivity is matched only by adding homogenization equipment or subsequent intermittent production stopping, so that the development of the supercapacitor industry is seriously restricted. Therefore, there is a strong need to develop a fast homogenization process to increase the homogenization efficiency, and the performance of the electrode sheet is comparable to or even higher than that of the original process, and finally the productivity of electrode manufacturing is improved.
Disclosure of Invention
The invention aims to provide supercapacitor electrode homogenate.
The invention aims to provide a preparation process of the supercapacitor electrode homogenate.
The technical scheme adopted by the invention is as follows:
the supercapacitor electrode homogenate slurry consists of active carbon, a conductive agent, a dispersing agent and a binder emulsion, wherein the mass ratio of the active carbon to the conductive agent to the dispersing agent to the binder emulsion is 100:1-10:1-10:1-10, wherein the binder emulsion comprises 40% of binder and 60% of solvent, wherein the binder emulsion is at least one of styrene-butadiene rubber emulsion SBR, sodium polyacrylate emulsion (PAA) and polytetrafluoroethylene PTFE emulsion, and the solvent is N-methylpyrrolidone or deionized water; the conductive agent is graphite, carbon nano tube or carbon black; the dispersing agent is polyvinylpyrrolidone (PVP) or sodium carboxymethylcellulose (CMC).
Preferably, the mass ratio of the active carbon, the conductive agent, the dispersing agent and the binder emulsion of the supercapacitor electrode homogenate is 100:3:5:7.
the preparation process of the supercapacitor electrode homogenate comprises the following steps:
(1) Adding active carbon, conductive agent powder and dispersing agent into a stirring tank, and hermetically stirring to obtain a dry powder mixture;
(2) Adding a solvent into the dry powder mixture, and stirring to obtain a primary slurry semi-finished product;
(3) Adding a solvent into the dry powder mixture, stirring, and then adding high-speed dispersion to obtain a slurry secondary initial semi-finished product;
(4) Adding a solvent into the secondary initial semi-finished product of the slurry for 2-5 times, and uniformly stirring to obtain a final semi-finished product of the slurry;
(5) And adding the binder emulsion into the final semi-finished slurry, and uniformly stirring for 1-15 min to obtain a final slurry finished product.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the solvent is N-methyl pyrrolidone or deionized water.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the stirring paddle speed and the dispersing paddle speed in the step (1) are respectively 20rpm-50rpm and 1000rpm-1500rpm, and the rotating speed can be adjusted according to the sizes of the paddles and the tank body.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the stirring speed in the step (2) is 20rpm-40rpm.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the stirring paddle speed and the dispersing paddle speed in the step (3) are respectively 30rpm-60rpm and 1500rpm-3000rpm, and the rotating speed can be adjusted according to the sizes of the paddles and the tank body.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the stirring paddle speed and the dispersing paddle speed in the step (4) are respectively 20rpm-50rpm and 300rpm-1500rpm, and the rotating speed can be adjusted according to the sizes of the paddles and the tank body.
Preferably, in the preparation process of the supercapacitor electrode homogenate, in the step (5), the stirring paddle speed and the dispersing paddle speed are respectively 20rpm-50rpm and 200rpm-500rpm, and the rotating speed can be adjusted according to the sizes of the paddles and the tank body.
Preferably, in the preparation process of the supercapacitor electrode homogenate, the mixing and stirring time in the step (1) is 1-10min; in the step (2), mixing and stirring are carried out for 5-15min; in the step (3), mixing and stirring are carried out for 5-30min; in the step (4), mixing and stirring are carried out for 10-30min; in the step (5), the mixing and stirring time is 1-10min.
The beneficial effects of the invention are as follows:
the viscosity of the supercapacitor electrode homogenate slurry is 500-800 mPa.s, which is far lower than that of the original process, and the slurry has excellent fluidity, and meanwhile, the solid content of the supercapacitor electrode homogenate slurry is about 30 percent, which is far lower than that of the original process, so that the coating error is reduced, the porosity of the electrode is improved, and the low-coating-amount coating operation is facilitated; the preparation process of the slurry has the following advantages:
(1) The active carbon, the conductive agent powder and the dispersing agent are mixed at a high speed to ensure uniform mixing and form a dry powder mixture;
(2) The preparation of the dispersant glue solution is not carried out, so that the process is omitted, and the overall homogenization time is shortened;
(3) The dry powder mixture is directly mixed with the solvent at a high speed, and the shearing force generated by the high-speed rotation of the dispersing paddles is more beneficial to the full mixing of the dry powder and the solvent, so that no particles are generated, the efficiency is high, and the time is saved;
(4) The whole homogenizing time is 10% -30% of the existing homogenizing technology, so that the time is greatly saved.
Drawings
FIG. 1 is a graph of viscosity contrast of a process according to the present invention versus a raw process slurry;
FIG. 2 is a graph of the solids content of the process according to the invention compared with the solids content of the raw process slurry;
FIG. 3 is a graph of the electrode bonding force of a process slurry according to the present invention;
FIG. 4 is a graph of raw process slurry electrode bonding force;
FIG. 5 is a graph showing the comparison of electrode surface topography produced by the process of the present invention and the raw process slurry;
FIG. 6 is a graph showing the electrical performance of a capacitor made from the process of the present invention and the original process slurry;
fig. 7 is a graph comparing the lifetime of a capacitor made from the process of the present invention and the raw process slurry.
Detailed Description
To further illustrate the invention, the following examples are provided in connection with:
example 1
The electrode homogenate slurry for the super capacitor is prepared by the following specific preparation process:
1) In a double planetary stirring device of 100L, carrying out dry mixing on 100 parts of active carbon, 3 parts of conductive agent carbon black and 5 parts of dispersing agent sodium carboxymethyl cellulose (CMC) for 5min, stirring at 35rpm and dispersing at 1000rpm;
2) Adding deionized water as a solvent, mixing for 5min, and stirring at 35rpm;
3) Adding the solvent in the step 2, continuously mixing for 15min, stirring at 35rpm, and dispersing at 2000rpm;
4) Adding the solvent in the step 2, mixing for 5min, stirring at 35rpm, and dispersing at 1000rpm;
5) Adding the solvent in the step 2, mixing for 5min, stirring at 35rpm, and dispersing at 500rpm;
6) Adding the solvent in the step 2, mixing for 20min, stirring at 35rpm, and dispersing at 300rpm;
7) 7 parts of a binder 50% styrene-butadiene rubber emulsion (SBR) was added, mixed for 5 minutes, stirred at 35rpm and dispersed at 300rpm.
The original process for process comparison of the invention comprises the following steps,
1) In a 100L double planetary stirring device, 100 parts of active carbon, 3 parts of conductive agent carbon black and 5 parts of dispersing agent sodium carboxymethyl cellulose (CMC) are dry-mixed for 30min, and stirring is carried out at 20rpm;
2) Mixing 1000 parts of solvent deionized water and 3.2 parts of dispersant dry powder polyvinylpyrrolidone (PVP) for 50min to form a glue solution, stirring at 30rpm and dispersing at 500rpm;
3) Adding the glue solution formed in the step 2 into the dry powder mixture formed in the step 1, mixing for 80min, and stirring at 30rpm;
4) Adding solvent, mixing for 80min, stirring at 30rpm;
5) Adding the solvent in the step 4, mixing for 40min, stirring at 40rpm, and dispersing at 800rpm;
6) 7 parts of a binder 50% styrene-butadiene rubber emulsion (SBR) was added, mixed for 40 minutes, stirred at 15rpm and dispersed at 200rpm.
Comparing the total homogenization time, slurry viscosity, slurry solid content, slurry supported pole piece adhesion force, pole piece surface morphology, electrical performance of assembled capacitor and life time of assembled capacitor of the process with the original process, the results are as follows:
as shown in Table 1, compared with the total time for homogenizing obtained by the original process, the total time for homogenizing is reduced by 80%, and the productivity is greatly improved;
as shown in figure 1, compared with the original process, the viscosity of the slurry is reduced by more than 2000mpa.s, the fluidity of the slurry is improved, and the high-speed coating is facilitated;
as shown in FIG. 2, the solid content of the process and the original process slurry is reduced by 7%, which is beneficial to low-coating-amount coating;
as shown in figures 3 and 4, the adhesive force of the process disclosed by the invention is equivalent to that of the pole piece prepared by coating the original process slurry, and is 40-45gf;
as shown in FIG. 5, the process of the invention has the same surface morphology as that of the pole piece prepared by coating the original process slurry, and the phenomenon of uneven distribution of the conductive agent does not occur;
as shown in fig. 6, the electrical performance of the capacitor prepared by the process of the invention is equivalent to that of the capacitor prepared by the original process slurry, and ESR is not obviously different from deltau;
as shown in fig. 7, the process of the present invention performed comparably to the life of the capacitor made from the raw process slurry, with a 1000hESR increase of 40% and a capacity fade of 17%.
The above examples are only illustrative of the preferred embodiments of the present invention and are not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the scope of protection defined by the claims of the present invention without departing from the spirit of the design of the present invention.
Claims (10)
1. A supercapacitor electrode homogenate characterized by: the conductive adhesive consists of active carbon, a conductive agent, a dispersing agent and adhesive emulsion, wherein the mass ratio of the active carbon to the conductive agent to the dispersing agent to the adhesive emulsion is 100:1-10:1-10:1-10, wherein the binder emulsion comprises 40% of binder and 60% of solvent, wherein the binder emulsion is at least one of styrene-butadiene rubber emulsion SBR, sodium polyacrylate emulsion and polytetrafluoroethylene PTFE emulsion, and the solvent is N-methyl pyrrolidone or deionized water; the conductive agent is graphite, carbon nano tube or carbon black; the dispersing agent is polyvinylpyrrolidone or sodium carboxymethyl cellulose.
2. The supercapacitor electrode slurry according to claim 1, wherein: the mass ratio of the active carbon to the conductive agent to the dispersing agent to the binder emulsion is 100:3:5:7.
3. the process for preparing the supercapacitor electrode homogenate according to claim 1, wherein the process comprises the following steps: comprising the following steps:
(1) Adding active carbon, conductive agent powder and dispersing agent into a stirring tank, and hermetically stirring to obtain a dry powder mixture;
(2) Adding a solvent into the dry powder mixture, and stirring to obtain a primary slurry semi-finished product;
(3) Adding a solvent into the dry powder mixture, stirring, and then adding high-speed dispersion to obtain a slurry secondary initial semi-finished product;
(4) Adding a solvent into the secondary initial semi-finished product of the slurry for 2-5 times, and uniformly stirring to obtain a final semi-finished product of the slurry;
(5) And adding the binder emulsion into the final semi-finished slurry, and uniformly stirring for 1-15 min to obtain a final slurry finished product.
4. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the solvent is N-methyl pyrrolidone or deionized water.
5. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the stirring paddle speed and the dispersing paddle speed in the step (1) are 20rpm-50rpm and 1000rpm-1500rpm respectively.
6. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the stirring paddle speed in the step (2) is 20rpm-40rpm.
7. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the stirring paddle speed and the dispersing paddle speed in the step (3) are 30rpm-60rpm and 1500rpm-3000rpm respectively.
8. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the stirring paddle speed and the dispersing paddle speed in the step (4) are 20rpm-50rpm and 300rpm-1500rpm, respectively.
9. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the stirring paddle speed and the dispersing paddle speed in the step (5) are 20rpm-50rpm and 200rpm-500rpm, respectively.
10. A process for preparing a supercapacitor electrode slurry according to claim 3, wherein: the mixing and stirring time in the step (1) is 1-10min; in the step (2), mixing and stirring are carried out for 5-15min; in the step (3), mixing and stirring are carried out for 5-30min; in the step (4), mixing and stirring are carried out for 10-30min; in the step (5), the mixing and stirring time is 1-10min.
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