CN109786740B - Preparation method of lithium battery positive electrode slurry - Google Patents
Preparation method of lithium battery positive electrode slurry Download PDFInfo
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- CN109786740B CN109786740B CN201811565202.5A CN201811565202A CN109786740B CN 109786740 B CN109786740 B CN 109786740B CN 201811565202 A CN201811565202 A CN 201811565202A CN 109786740 B CN109786740 B CN 109786740B
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- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 42
- 239000011267 electrode slurry Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 213
- 239000006185 dispersion Substances 0.000 claims abstract description 69
- 239000003292 glue Substances 0.000 claims abstract description 67
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims abstract description 65
- 238000009736 wetting Methods 0.000 claims abstract description 48
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 45
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 45
- 239000006229 carbon black Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 38
- 239000002033 PVDF binder Substances 0.000 claims abstract description 37
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims abstract description 37
- 239000006256 anode slurry Substances 0.000 claims abstract description 34
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 claims abstract description 33
- 239000011268 mixed slurry Substances 0.000 claims abstract description 28
- 230000001070 adhesive effect Effects 0.000 claims description 45
- 239000000853 adhesive Substances 0.000 claims description 44
- 238000010438 heat treatment Methods 0.000 claims description 8
- 230000008961 swelling Effects 0.000 claims description 7
- 238000005054 agglomeration Methods 0.000 abstract description 14
- 230000002776 aggregation Effects 0.000 abstract description 14
- 239000002002 slurry Substances 0.000 abstract description 10
- 238000001816 cooling Methods 0.000 abstract description 6
- 230000000903 blocking effect Effects 0.000 abstract description 5
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- 238000000034 method Methods 0.000 description 37
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- 239000002904 solvent Substances 0.000 description 14
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- 239000006258 conductive agent Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 7
- 229910001416 lithium ion Inorganic materials 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
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- 239000004568 cement Substances 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000004537 pulping Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 239000011149 active material Substances 0.000 description 2
- 239000006257 cathode slurry Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000007774 positive electrode material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 230000001360 synchronised effect Effects 0.000 description 2
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
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- 230000005540 biological transmission Effects 0.000 description 1
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- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
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- 229920005596 polymer binder Polymers 0.000 description 1
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- 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
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Abstract
A preparation method of lithium battery positive electrode slurry comprises the steps of preheating polyvinylidene fluoride and N-methyl pyrrolidone, carrying out first stirring operation to obtain wetting glue, adding the N-methyl pyrrolidone into the wetting glue, carrying out second stirring operation, carrying out third stirring operation after cooling to obtain bonding glue solution, preheating carbon nano tubes, superconducting carbon black and the N-methyl pyrrolidone, carrying out fourth stirring operation, then adding lithium iron phosphate powder, carrying out fifth stirring operation to obtain mixed slurry, adding the bonding glue solution into the mixed slurry, carrying out seventh stirring operation, carrying out vacuumizing operation, and carrying out eighth stirring operation to obtain the lithium battery positive electrode slurry. The preparation method of the lithium battery anode slurry can avoid the agglomeration of the anode slurry, improve the dispersion uniformity and viscosity stability of the anode slurry and effectively improve the problem of the blocking of the slurry.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a preparation method of lithium battery anode slurry.
Background
With the wide application of consumer electronics and new energy automobiles, lithium ion batteries become one of the research hotspots, the preparation of the slurry is a key process in the production link of the lithium ion batteries, and the performance of the electrode slurry has an important influence on the performance of the lithium ion batteries. The components in the electrode slurry are dispersed to be uniform, the processing performance of the pole piece is directly influenced, the influence degree of the material mixing process on the quality of a product in the whole production process of the lithium ion battery is more than 30%, and the method is the most important link in the whole production process. In the manufacture of electrodes of lithium ion batteries, the positive and negative electrode pastes are basically composed of active materials, polymer binders, conductive agents and the like. The mixing process of the electrode slurry is roughly divided into two (1) wet mixing processes, and the basic process is that substances such as a binder, a conductive agent and the like are mixed and stirred firstly, then active substances are added to be fully stirred and dispersed, and finally a proper amount of solvent is added to adjust the viscosity so as to be suitable for coating. This is the mainstream technology in China at present. (2) The dry mixing process includes mixing active matter, conducting agent and adhesive powder, adding proper amount of solvent for wetting, adding solvent for high speed dispersion and crushing, diluting and regulating viscosity.
In the conventional dry stirring process, quality problems easily occur due to improper selection of the solvent amount, the stirring speed and the time in the wetting step, which is closely related to the particle size, the size distribution, the specific surface area and the like of the raw materials, the parameters are slightly changed, and the corresponding solvent amount and the stirring process conditions need to be adjusted. If the solvent is added in the first step too much, the particle aggregates are not easy to disperse, and the quality problems of large slurry fineness and uneven distribution of the conductive agent occur. And if the solvent added in the first step is too little, the wetting and stirring action force is large, the binder cannot be fully dispersed and dissolved or the long chain of the binder is damaged, so that the viscosity and the stability of the slurry are caused to be problematic.
The wet pulping process has the advantages of short time consumption, simple process, good slurry fluidity and less air bubbles. However, the wet stirring process has problems that the fluidity of the solvent is poor due to the large surface area of the conductive agent, and the solvent is easily absorbed, and it is not easy to achieve a uniformly dispersed state after the active material is added. Under the condition of the same solid content, the viscosity of the slurry is higher compared with that of the dry-method pulping process.
The main reasons for this are two points: (1) due to the nanoscale effect, the lithium iron phosphate main powder, the carbon nano tube and the carbon black have higher surface energy, so that the agglomeration phenomenon is easy to occur in the stirring pulping process; (2) in the stirring process, serious agglomeration phenomenon also occurs to cause larger fluctuation of viscosity and solid content due to different dispersion time, dispersion speed and feeding sequence.
Therefore, the existing homogenizing method of the lithium battery anode slurry still has the problems of easy agglomeration, poor dispersion uniformity and large fluctuation of the viscosity and solid content of the anode slurry.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a preparation method of lithium battery anode slurry, which can avoid the problem of agglomeration of anode slurry, improve the dispersion uniformity and viscosity stability of the anode slurry, and effectively improve the problem of network blockage of the anode slurry.
The purpose of the invention is realized by the following technical scheme:
a preparation method of lithium battery anode slurry comprises the following steps:
preheating polyvinylidene fluoride and N-methyl pyrrolidone, carrying out first stirring operation, and swelling and wetting polyvinylidene fluoride to obtain a wetting glue;
adding N-methyl pyrrolidone into the wetting glue, carrying out second stirring operation, cooling, and carrying out third stirring operation to obtain an adhesive glue solution;
preheating the carbon nano tube, the superconducting carbon black and the N-methyl pyrrolidone, carrying out fourth stirring operation, wetting the surfaces of the carbon nano tube and the superconducting carbon black, and then adding the lithium iron phosphate powder to carry out fifth stirring operation, so as to obtain mixed slurry;
and adding lithium iron phosphate powder into the mixed slurry to perform sixth stirring operation, then adding the bonding glue solution to perform seventh stirring operation, performing vacuumizing operation, and performing eighth stirring operation to obtain the lithium battery anode slurry.
In one embodiment, the first stirring operation and the second stirring operation are simultaneously performed while performing the vacuum pumping operation.
In one embodiment, the vacuum degree is controlled to be-70 kpa to-80 kpa during the first stirring operation and during the second stirring operation and the synchronous vacuumizing operation.
In one embodiment, the first stirring operation, the second stirring operation, the third stirring operation, the fourth stirring operation, the fifth stirring operation, the sixth stirring operation, the seventh stirring operation, and the eighth stirring operation are performed using a double planetary stirrer, respectively.
In one embodiment, the revolution speed of the second stirring operation is 23 rpm to 30 rpm, and the dispersion speed is 900 rpm to 1100 rpm.
In one embodiment, the revolution speed of the third stirring operation is 15 rpm to 20 rpm, and the dispersion speed is 400 rpm to 600 rpm.
In one embodiment, in the operation process of preheating the polyvinylidene fluoride and the N-methyl pyrrolidone, the mass ratio of the polyvinylidene fluoride to the N-methyl pyrrolidone is (90-100): (500-600);
adding N-methyl pyrrolidone into the wetting glue, and in the process of carrying out second stirring operation, the mass ratio of the wetting glue to the N-methyl pyrrolidone is (590-700): (500-600);
preheating a carbon nano tube, superconducting carbon black and N-methylpyrrolidone, carrying out fourth stirring operation, adding lithium iron phosphate powder after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, and carrying out fifth stirring operation, wherein the mass ratio of the carbon nano tube to the superconducting carbon black to the N-methylpyrrolidone to the lithium iron phosphate powder is (50-100): (2-5): (150-200): (250 to 320);
after adding lithium iron phosphate powder into the mixed slurry to perform a sixth stirring operation, adding the bonding glue solution to perform a seventh stirring operation, wherein the mass ratio of the mixed slurry to the lithium iron phosphate powder is (452-625): (250-320), and the mass ratio of the bonding glue solution to the mixed slurry after the lithium iron phosphate powder is added is (120-180): (702-945).
In one embodiment, polyvinylidene fluoride and N-methyl pyrrolidone are preheated at a temperature of 55 ℃ to 65 ℃ and subjected to a first stirring operation.
In one embodiment, the temperature is reduced to 25 ℃ to carry out a third stirring operation, so as to obtain the adhesive glue solution.
In one embodiment, the stirring time is 75-85 min during the preheating of the carbon nanotubes, the superconducting carbon black and the N-methylpyrrolidone and the fourth stirring operation.
The preparation method of the lithium battery positive electrode slurry comprises the steps of preheating polyvinylidene fluoride and N-methyl pyrrolidone, carrying out first stirring operation to obtain a wetting glue, adding the N-methyl pyrrolidone into the wetting glue, carrying out second stirring operation, cooling, carrying out third stirring operation to obtain an adhesive glue solution, preheating carbon nano tubes, superconducting carbon black and the N-methyl pyrrolidone, carrying out fourth stirring operation, then adding lithium iron phosphate powder, carrying out fifth stirring operation to obtain a mixed slurry, adding the adhesive glue solution into the mixed slurry, carrying out seventh stirring operation, carrying out vacuumizing operation, and carrying out eighth stirring operation to obtain the lithium battery positive electrode slurry. The preparation method of the lithium battery anode slurry can avoid the agglomeration of the anode slurry, improve the dispersion uniformity and viscosity stability of the anode slurry and effectively improve the problem of the blocking of the slurry.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a flowchart illustrating steps of a method for preparing a positive electrode slurry for a lithium battery according to an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. The terms "vertical," "horizontal," "left," "right," and the like as used herein are for illustrative purposes only and do not represent the only embodiments.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
In order to better explain the preparation method of the lithium battery positive electrode slurry, the concept of the preparation method of the lithium battery positive electrode slurry is better understood. Referring to fig. 1, in one embodiment, a method for preparing a positive electrode slurry of a lithium battery includes the following steps:
s110, preheating polyvinylidene fluoride and N-methyl pyrrolidone, carrying out first stirring operation, and swelling and wetting the polyvinylidene fluoride to obtain a wetting glue.
It can be understood that polyvinylidene fluoride has good chemical stability, electrical insulation performance, impact resistance and heat resistance, is widely applied to lithium ion batteries, and can be used as a binder in the process of preparing lithium battery anode slurry, so that the anode slurry has good adhesive property and better adhesive force between a current collector. The N-methyl pyrrolidone is colorless transparent oily liquid, is a polar solvent with strong selectivity and good stability, and has the advantages of low toxicity, high boiling point, strong dissolving power, nonflammability, biodegradability, recyclability, safe use, suitability for various formula purposes and the like. Is commonly used as an electrode auxiliary material for lithium ion batteries. The polyvinylidene fluoride and the N-methyl pyrrolidone are preheated, so that the polyvinylidene fluoride and the N-methyl pyrrolidone can be well dispersed and then wetted, and then a first stirring operation is carried out, so that the wetting glue is obtained after the polyvinylidene fluoride is swelled and wetted by the N-methyl pyrrolidone. In order to achieve better mixing and dispersion of the polyvinylidene fluoride and the N-methyl pyrrolidone, in one embodiment, the polyvinylidene fluoride and the N-methyl pyrrolidone are preheated at a temperature of 55 ℃ to 65 ℃ and subjected to a first stirring operation. So, through with temperature control under 55 ℃ -65 ℃ temperature condition, can make polyvinylidene fluoride dry powder more fluffy for N-methyl pyrrolidone can mix with polyvinylidene fluoride dry powder better, and more even infiltration to polyvinylidene fluoride dry powder, makes polyvinylidene fluoride dry powder carry out abundant swelling and moist, and then obtains the moist glue that dispersion uniformity and stability are better.
In order to obtain a wetting adhesive with better dispersion uniformity and viscosity stability, for example, in one embodiment, during the operation of preheating the polyvinylidene fluoride and the N-methylpyrrolidone, the mass ratio of the polyvinylidene fluoride to the N-methylpyrrolidone is (90-100): (500-600). Therefore, by controlling the specific mass ratio of the adhesive polyvinylidene fluoride to the solvent N-methyl pyrrolidone, the wettability of the polyvinylidene fluoride can be effectively controlled, and the adhesive glue solution with better performance is obtained. For another example, in the operation process of preheating the polyvinylidene fluoride and the N-methyl pyrrolidone, the mass ratio of the polyvinylidene fluoride to the N-methyl pyrrolidone is 93.6:540, so that the polyvinylidene fluoride and the N-methyl pyrrolidone are preheated in the optimized specific ratio, and the first stirring operation is performed, so that the polyvinylidene fluoride can be fully swelled and wetted, and the wetting adhesive with better uniformity and stability is obtained; for another example, the revolution speed of the first stirring operation is 23 rpm to 30 rpm, the dispersion speed is 380 rpm to 420 rpm, and the stirring time is 30 minutes, so that the polyvinylidene fluoride can be fully wetted and dispersed by the N-methylpyrrolidone, a wetting adhesive with better quality is obtained, and the subsequent preparation of the lithium battery positive electrode slurry with more stable viscosity is facilitated.
And S120, adding N-methyl pyrrolidone into the wetting glue, carrying out second stirring operation, cooling, and carrying out third stirring operation to obtain the adhesive glue solution.
The polyvinylidene fluoride is pre-wetted in the step S110 to obtain the wetting glue with high viscosity, N-methyl pyrrolidone is further added into the wetting glue for dilution, and after the second stirring operation is carried out, the solid content of the wetting glue can be reduced, the wetting glue is further uniformly dispersed, and the agglomeration problem is avoided. It can be understood that in the process of wetting and dispersing the binder, if too much solvent is added, the particle aggregates of the subsequent anode slurry are not easy to disperse, the quality problems of large slurry fineness and uneven material distribution occur, and if the amount of the added solvent is large, when the binder is wetted and stirred, a large acting force can be generated, even the binder cannot be sufficiently dispersed and dissolved or the long chain of the binder is damaged, and then the viscosity and poor stability of the subsequently obtained adhesive glue solution are caused. In order to obtain better dilution effect, for example, in the second stirring operation process of adding N-methyl pyrrolidone into the wetting glue, the mass ratio of the wetting glue to the N-methyl pyrrolidone is (590-700): (500-600), so, the wetting glue can be further diluted by controlling the amount of the solvent N-methyl pyrrolidone added again, and the subsequent obtaining of the bonding glue solution with more proper viscosity is facilitated. And then, carrying out third stirring operation after cooling, and further diluting and uniformly mixing the wetting glue to obtain the bonding glue solution with more stable viscosity.
In order to improve the performance of the adhesive glue solution, in one embodiment, a vacuum pumping operation is also performed simultaneously during the first stirring operation and during the second stirring operation. It will be appreciated that during the preparation of the adhesive cement, the N-methylpyrrolidone will evaporate to some extent, meanwhile, other waste gas can be generated, the waste gas in the stirrer can be pumped away through the vacuum pumping operation, the adhesive glue solution with better quality can be obtained, in addition, in the stirring process, N-methyl pyrrolidone still can not avoid some bubbles, and if the prepared adhesive glue liquid contains bubbles, the bubbles are easy to be generated in the lithium battery anode slurry prepared subsequently, after the coating is coated on a current collector, uneven coating or local hollowing or over-thickness is easily caused, so that the quality and the performance of the lithium battery anode slurry are greatly reduced, through the vacuum pumping operation, the problem that bubbles appear in the prepared adhesive liquid can be avoided, and the stability and the viscosity stability of the adhesive liquid are further improved.
In one embodiment, the vacuum degree is controlled to be-70 kpa to-80 kpa during the first stirring operation and during the second stirring operation and the synchronous vacuumizing operation.
In order to more effectively control and eliminate the bubbles in the first stirring operation process and the second stirring operation process, for example, in the vacuumizing operation process, the vacuum degree is controlled to be-70 kpa to-80 kpa, so that the bubbles generated in stirring can be quickly burst in a vacuum state, the bubble amount in the prepared bonding glue solution is greatly reduced, the quality and the performance of the lithium battery anode slurry obtained by subsequent preparation are greatly improved, and the problems that the current collector cannot be tightly bonded due to the bubbles in the anode slurry and the coating of the anode slurry is uneven are solved. For another example, in the process of synchronously performing the vacuum pumping operation, the vacuum degree is controlled to be-80 kpa, so that the bubble elimination amount in the adhesive glue solution is the largest in the processes of performing the first stirring operation and the second stirring operation under the condition of the most appropriate vacuum degree, so that the adhesive glue solution with better quality can be obtained, and the subsequent preparation of the positive electrode slurry with better quality can be facilitated.
In one embodiment, the revolution speed of the second stirring operation is 23 rpm to 30 rpm, and the dispersion speed is 900 rpm to 1100 rpm.
In order to better mix and dissolve the wetting gum and the N-methyl pyrrolidone, for example, the revolution speed of the second stirring operation is 23 to 30 revolutions per minute, and the dispersion speed is 900 to 1100 revolutions per minute, so that the wetting gum can be better diluted by further increasing the dispersion speed of the second stirring operation on the basis of the dispersion speed of the first stirring operation, the solid content of the wetting gum can be reduced, and the wetting gum can be further uniformly dispersed, so that the agglomeration problem can be avoided; for another example, the revolution speed of the second stirring operation is 25 rpm, and the dispersion speed is 1000 rpm, so that the production efficiency can be improved, the production time can be effectively shortened, and the productivity can be improved by further increasing the dispersion speed of the stirring under the condition of adding more solvents.
In one embodiment, the revolution speed of the third stirring operation is 15 rpm to 20 rpm, and the dispersion speed is 400 rpm to 600 rpm.
It can be understood that the high-speed stirring for too long time is easy to heat the stirred raw materials, which is easy to cause the properties of the raw materials to be damaged due to high temperature, and in addition, is easy to cause the long chains of the binder to be damaged, so that after the second stirring operation is performed, a third stirring operation is performed after the temperature is reduced, for example, the revolution speed of the third stirring operation is 15 rpm to 20 rpm, the dispersion speed is 400 rpm to 600 rpm, and the stability of the raw materials at the later stage of the preparation of the adhesive cement is ensured by reducing the revolution speed and the dispersion speed, thereby avoiding the raw materials from being damaged due to too high temperature caused by too high stirring speed and stirring, and causing the viscosity of the adhesive cement to be reduced. For another example, the revolution speed of the third stirring operation is 20 rpm, and the dispersion speed is 500 rpm, so that on the basis of the second stirring operation, the stirring speed is reduced, the quality of the adhesive glue solution is further ensured, the agglomeration of the anode slurry is also avoided, and the subsequent preparation of the anode slurry with better dispersion uniformity and viscosity stability is facilitated.
In one embodiment, the temperature is reduced to 25 ℃ to carry out a third stirring operation, so as to obtain the adhesive glue solution.
By cooling the adhesive glue solution after the second stirring operation, the long-chain damage of the adhesive glue solution due to long-time high-speed stirring can be avoided, for example, the temperature is reduced to 25 ℃ and then the third stirring operation is performed, so that the third stirring operation is performed on the wetting glue and the N-methyl pyrrolidone at a lower temperature, and the quality of the prepared adhesive glue solution is not damaged due to high temperature and too high stirring speed in the stirring process, so that the adhesive glue solution with better quality is obtained, and the subsequent preparation of the positive electrode slurry with better quality is facilitated.
S130, preheating the carbon nano tube, the superconducting carbon black and the N-methyl pyrrolidone, carrying out fourth stirring operation, adding the lithium iron phosphate powder after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, and carrying out fifth stirring operation to obtain mixed slurry.
In order to improve the migration rate of electrons in the lithium battery and reduce the polarization of the battery, the carbon nano tube and the superconducting carbon black are also used as conductive agents and used as raw materials for preparing the positive electrode slurry of the lithium battery. It can be understood that the one-dimensional structure of the carbon nanotube is long column-shaped like a fiber, and the inside of the carbon nanotube is hollow. The carbon nano tube is used as a conductive agent, a perfect conductive network can be well distributed, the carbon nano tube and a living substance are in a point-line contact mode, and the carbon nano tube has great effects on improving the capacity and the rate capability of the battery, prolonging the cycle life of the battery and reducing the interface impedance of the battery. The superconducting carbon black is a functional high-conductivity filler, is in a chain or grape shape under a scanning electron microscope, single superconducting carbon black particles have a very large specific surface area, the high specific surface area and close stacking of the superconducting carbon black particles are beneficial to close contact of the particles, a conductive network in an electrode is formed, and the electronic conductivity of a lithium battery is greatly improved. In order to avoid the agglomeration problem, the carbon nano tube, the superconducting carbon black and the N-methyl pyrrolidone are preheated to improve the dispersion degree of the carbon nano tube and the superconducting carbon black, and then the fourth stirring operation is carried out to enable the N-methyl pyrrolidone to wet the surfaces of the carbon nano tube and the superconducting carbon black, in order to better wet and disperse the carbon nano tube and the superconducting carbon black, for example, in the process of preheating the carbon nano tube, the superconducting carbon black and the N-methyl pyrrolidone, the temperature is controlled to be 57 ℃ to 63 ℃, so that the carbon nano tube and the superconducting carbon black can keep better activity and bulkiness and can be better wetted by the N-methyl pyrrolidone under certain temperature conditions, and further, in the process of preheating the carbon nano tube, the superconducting carbon black and the N-methyl pyrrolidone, the temperature is controlled to be 60 ℃, so that the N-methyl pyrrolidone can better wet the surfaces of the carbon nano tube and the superconducting carbon black, and the subsequent uniform and rapid dispersion is facilitated.
In order to better disperse the carbon nanotubes and the superconducting carbon black, in one embodiment, the stirring time is 75-85 min during the preheating of the carbon nanotubes, the superconducting carbon black and the N-methylpyrrolidone and the fourth stirring operation, so that the stirring time is controlled, the carbon nanotubes and the superconducting carbon black are fully dispersed and wetted, and the long chains of the carbon nanotubes, the superconducting carbon black and the N-methylpyrrolidone are not damaged. Further, in the process of carrying out the fourth stirring operation, the stirring time is 80min, so that the carbon nano tubes and the superconducting carbon black can be better dispersed and wetted, and the problems of agglomeration and slurry blocking in the subsequent preparation process are avoided. For another example, the revolution speed of the fourth stirring operation is 12 to 18 revolutions per minute, and the dispersion speed is 900 to 1100 revolutions per minute. Thus, the carbon nano tube and the superconducting carbon black can be better mixed and dispersed, and are wetted by the N-methyl pyrrolidone; for another example, the revolution speed of the fourth stirring operation is 15 rpm, and the dispersion speed is 1000 rpm, so that the dispersion uniformity of the anode slurry can be greatly improved, and the problems of agglomeration and net blocking are avoided.
And wetting the surfaces of the carbon nano tube and the superconducting carbon black, and then adding the lithium iron phosphate powder to carry out fifth stirring operation, thereby obtaining the mixed slurry. It can be understood that the lithium iron phosphate powder, as a positive electrode active material, also has a high surface energy, and is prone to agglomeration and network blockage problems during the stirring preparation process of the positive electrode slurry, resulting in large fluctuations in the viscosity and solid content of the positive electrode slurry. Therefore, after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, the lithium iron phosphate powder is added to carry out fifth stirring operation, and the mixed slurry with more uniform dispersion and better stability can be obtained. For example, the revolution speed of the fifth stirring operation is 12 rpm to 18 rpm, and the dispersion speed is 400 rpm to 600 rpm, so that the carbon nanotubes, the superconducting carbon black, and the lithium iron phosphate powder can be mixed and uniformly dispersed, and a mixed slurry with more uniform dispersion and better stability can be obtained.
And S140, adding lithium iron phosphate powder into the mixed slurry to perform sixth stirring operation, then adding the bonding glue solution to perform seventh stirring operation, performing vacuumizing operation, and performing eighth stirring operation to obtain the lithium battery anode slurry.
By adding the lithium iron phosphate powder into the mixed slurry again to carry out sixth stirring operation, overfilling and even overflowing of a stirring system caused by adding too many raw materials at one time can be avoided, and the positive active material lithium iron phosphate powder is added twice, so that higher productivity can be realized under the scale of the original stirring system, other stirring equipment is not required to be additionally added, and the production cost is reduced; after the sixth stirring operation is carried out, the conductive agent and the active substance are uniformly mixed, then the bonding glue solution is added for the seventh stirring operation, so that the conductive agent and the active substance of the lithium battery can be uniformly mixed with the bonding glue solution, and the subsequent preparation is facilitated to obtain the cathode slurry with better quality. In order to mix the mixed slurry, the lithium iron phosphate powder and the binder resin solution more uniformly, for example, the revolution speed of the seventh stirring operation is 18 rpm to 23 rpm, the dispersion speed is 1100 rpm to 1500 rpm, further, the revolution speed of the seventh stirring operation is 20 rpm, the dispersion speed is 1200 rpm, and the stirring time is 150 minutes, so that the mixed slurry, the lithium iron phosphate powder and the binder resin solution can be mixed and dispersed more uniformly by increasing the stirring speed, thereby avoiding the problem of agglomeration and improving the viscosity stability of the cathode slurry. After the seventh stirring operation, a vacuumizing operation is further performed, for example, the vacuum degree is controlled to be-80 kpa, so that the waste gas generated in the seventh stirring operation can be pumped away, bubbles generated in the positive electrode slurry are eliminated, and finally, after the eighth stirring operation is performed, the positive electrode slurry of the lithium battery can be obtained, for example, the revolution speed of the eighth stirring operation is 20 revolutions per minute, the dispersion speed is 500 revolutions per minute, and the stirring time is 60 minutes.
In order to shorten the time of the preparation process and improve the productivity, for example, in one of the embodiments, the first stirring operation, the second stirring operation, the third stirring operation, the fourth stirring operation, the fifth stirring operation, the sixth stirring operation, the seventh stirring operation, and the eighth stirring operation are performed using a double planetary stirrer, respectively. It can be understood that the double-planetary stirrer is provided with a low-speed stirring part and a high-speed dispersing part, the low-speed stirring part adopts planetary gear transmission, and the stirring paddle also rotates during revolution to enable the materials to move up and down and around, thereby achieving ideal mixing effect in a short time. So, through adopting two planet agitators to carry out respectively first stirring operation second stirring operation third stirring operation fourth stirring operation fifth stirring operation sixth stirring operation seventh stirring operation with eighth stirring operation further improves the dispersion homogeneity and the viscosity stability of lithium cell positive pole thick liquids to and effectively improve the reunion and the stifled net problem of positive pole thick liquids.
In order to obtain a lithium battery positive electrode slurry with better quality, for example, in the fifth stirring operation process of preheating a carbon nanotube, superconducting carbon black and N-methylpyrrolidone, adding lithium iron phosphate powder after wetting the surfaces of the carbon nanotube and the superconducting carbon black, and stirring, the mass ratio of the carbon nanotube, the superconducting carbon black, the N-methylpyrrolidone and the lithium iron phosphate powder is (50-100): (2-5): (150-200): (250 to 320); after adding lithium iron phosphate powder into the mixed slurry to perform a sixth stirring operation, adding the bonding glue solution to perform a seventh stirring operation, wherein the mass ratio of the mixed slurry to the lithium iron phosphate powder is (452-625): (250-320), and the mass ratio of the bonding glue solution to the mixed slurry after the lithium iron phosphate powder is added is (120-180): (702-945). Therefore, by controlling the specific ratio of the raw materials of the lithium battery anode slurry, the viscosity stability of the lithium battery anode slurry and the consistency of the slurry can be greatly improved, and the homogenization method of the anode slurry is more convenient for realizing large-scale production.
The following is a detailed description of the embodiments.
Example 1
Preparing an adhesive glue solution:
heating a 1200L stirring cylinder to 60 ℃, adding 93.6kg of polyvinylidene fluoride and 540kg of N-methylpyrrolidone, adjusting the revolution speed of the stirring cylinder to 25 revolutions per minute, adjusting the dispersion speed to 400 revolutions per minute, carrying out first stirring operation for 30 minutes, and swelling and wetting the polyvinylidene fluoride to obtain a wetting adhesive;
adding 540kg of N-methyl pyrrolidone into the wetting glue, adjusting the vacuum degree of a stirring cylinder to be-80 kpa, the revolution speed to be 25 rpm and the dispersion speed to be 1000 rpm, and carrying out second stirring operation for 300 minutes; then, the temperature of the stirring cylinder is reduced to 25 ℃, the revolution speed is adjusted to 20 revolutions per minute, the dispersion speed is adjusted to 500 revolutions per minute, and a third stirring operation is carried out for 30 minutes to obtain an adhesive glue solution;
preparing lithium battery anode slurry:
heating 650L of a double-planetary stirrer to 60 ℃, adding 80kg of carbon nano tubes, 3kg of superconducting carbon black and 180kg of N-methylpyrrolidone, then adjusting the revolution speed of a stirring cylinder to 15 revolutions per minute and the dispersion speed to 1000 revolutions per minute, carrying out a fourth stirring operation, and stirring for 80 minutes;
adding 290kg of lithium iron phosphate powder into a 650L double-planet stirrer after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, adjusting the revolution speed to 15 revolutions per minute and the dispersion speed to 500 revolutions per minute, and performing fifth stirring operation for 10 minutes to obtain mixed slurry;
then under the conditions that the revolution speed is 15 revolutions per minute and the dispersion speed is 500 revolutions per minute, 290kg of lithium iron phosphate powder is added into the mixed slurry to carry out sixth stirring operation, 150kg of adhesive glue solution is added, vacuumizing operation is carried out, the vacuum degree of a stirring cylinder is controlled to be-80 kpa, the revolution speed is adjusted to be 20 revolutions per minute, the dispersion speed is adjusted to be 1200 revolutions per minute, and seventh stirring operation is carried out for stirring for 150 minutes;
finally, the eighth stirring operation was performed under a vacuum degree of-80 kpa, a revolution speed of 20 rpm, and a dispersion speed of 500 rpm, to obtain the lithium battery positive electrode slurry of example 1.
Example 2
Preparing an adhesive glue solution:
heating a 1200L stirring cylinder to 55 ℃, adding 100.0kg of polyvinylidene fluoride and 600kg of N-methylpyrrolidone, then adjusting the revolution speed of the stirring cylinder to 25 revolutions per minute and the dispersion speed to 380 revolutions per minute, carrying out a first stirring operation for 30 minutes, and swelling and wetting the polyvinylidene fluoride to obtain a wetting adhesive;
adding 600kg of N-methyl pyrrolidone into the wetting glue, adjusting the vacuum degree of a stirring cylinder to be-75 kpa, the revolution speed to be 23 rpm and the dispersion speed to be 900 rpm, and carrying out second stirring operation for 300 minutes; then, the temperature of the stirring cylinder is reduced to 25 ℃, the revolution speed is adjusted to 15 revolutions per minute, the dispersion speed is adjusted to 400 revolutions per minute, and a third stirring operation is carried out for 30 minutes to obtain an adhesive glue solution;
preparing lithium battery anode slurry:
heating 650L of a double-planetary stirrer to 60 ℃, adding 50kg of carbon nano tubes, 2kg of superconducting carbon black and 150kg of N-methylpyrrolidone, adjusting the revolution speed of a stirring cylinder to 12 revolutions per minute and the dispersion speed to 900 revolutions per minute, carrying out a fourth stirring operation, and stirring for 75 minutes;
adding 250kg of lithium iron phosphate powder into a 650L double-planet stirrer after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, adjusting the revolution speed to 12 revolutions per minute and the dispersion speed to 400 revolutions per minute, and performing fifth stirring operation for 10 minutes to obtain mixed slurry;
then under the conditions that the revolution speed is 15 revolutions per minute and the dispersion speed is 500 revolutions per minute, 250kg of lithium iron phosphate powder is added into the mixed slurry for sixth stirring operation, then 120kg of adhesive glue solution is added, and the vacuum pumping operation is carried out, the vacuum degree of a stirring cylinder is controlled to be-75 kpa, the revolution speed is adjusted to be 18 revolutions per minute, the dispersion speed is adjusted to be 1100 revolutions per minute, the seventh stirring operation is carried out, and the stirring is carried out for 150 minutes;
finally, the eighth stirring operation was performed under a vacuum degree of-80 kpa, a revolution speed of 20 rpm, and a dispersion speed of 500 rpm, to obtain the lithium battery positive electrode slurry of example 2.
Example 3
Preparing an adhesive glue solution:
heating a 1200L stirring cylinder to 65 ℃, adding 90.0kg of polyvinylidene fluoride and 500kg of N-methyl pyrrolidone, adjusting the revolution speed of the stirring cylinder to 25 revolutions per minute and the dispersion speed to 420 revolutions per minute, carrying out first stirring operation for 30 minutes, and swelling and wetting the polyvinylidene fluoride to obtain a wetting adhesive;
adding 500kg of N-methyl pyrrolidone into the wetting glue, adjusting the vacuum degree of a stirring cylinder to be-70 kpa, the revolution speed to be 30 rpm and the dispersion speed to be 1100 rpm, and carrying out second stirring operation for 300 minutes; then, the temperature of the stirring cylinder is reduced to 25 ℃, the revolution speed is adjusted to 18 revolutions per minute, the dispersion speed is adjusted to 600 revolutions per minute, and a third stirring operation is carried out for 30 minutes to obtain an adhesive glue solution;
preparing lithium battery anode slurry:
heating 650L of a double-planetary stirrer to 60 ℃, adding 100kg of carbon nano tubes, 5kg of superconducting carbon black and 200kg of N-methylpyrrolidone, then adjusting the revolution speed of a stirring cylinder to 18 revolutions per minute and the dispersion speed to 1100 revolutions per minute, carrying out a fourth stirring operation, and stirring for 85 minutes;
adding 320kg of lithium iron phosphate powder into a 650L double-planet stirrer after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, adjusting the revolution speed to 18 revolutions per minute and the dispersion speed to 600 revolutions per minute, and carrying out fifth stirring operation for 10 minutes to obtain mixed slurry;
then under the conditions that the revolution speed is 15 revolutions per minute and the dispersion speed is 500 revolutions per minute, 320kg of lithium iron phosphate powder is added into the mixed slurry for sixth stirring operation, 180kg of adhesive glue solution is added, vacuumizing operation is carried out, the vacuum degree of a stirring cylinder is controlled to be-85 kpa, the revolution speed is adjusted to be 23 revolutions per minute, the dispersion speed is adjusted to be 1500 revolutions per minute, seventh stirring operation is carried out, and stirring is carried out for 150 minutes;
finally, the eighth stirring operation was performed under a vacuum degree of-80 kpa, a revolution speed of 20 rpm, and a dispersion speed of 500 rpm, to obtain the lithium battery positive electrode slurry of example 3.
Through experimental analysis and verification, the lithium battery positive electrode slurry in the embodiment 1 to the embodiment 3 has excellent dispersion uniformity and viscosity stability, the viscosity is 10000 mpa.s-20000 mpa.s, the problem of net blocking does not occur, the time of the preparation process is greatly shortened, and the productivity is improved.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (1)
1. The preparation method of the lithium battery positive electrode slurry is characterized by comprising the following steps of:
heating a 1200L stirring cylinder to 60 ℃, adding 93.6kg of polyvinylidene fluoride and 540kg of N-methylpyrrolidone, adjusting the revolution speed of the stirring cylinder to 25 revolutions per minute, adjusting the dispersion speed to 400 revolutions per minute, carrying out first stirring operation for 30 minutes, and swelling and wetting the polyvinylidene fluoride to obtain a wetting adhesive;
adding 540kg of N-methyl pyrrolidone into the wetting glue, adjusting the vacuum degree of a stirring cylinder to be-80 kpa, the revolution speed to be 25 rpm and the dispersion speed to be 1000 rpm, and carrying out second stirring operation for 300 minutes; then, the temperature of the stirring cylinder is reduced to 25 ℃, the revolution speed is adjusted to 20 revolutions per minute, the dispersion speed is adjusted to 500 revolutions per minute, and a third stirring operation is carried out for 30 minutes to obtain an adhesive glue solution;
heating 650L of a double-planetary stirrer to 60 ℃, adding 80kg of carbon nano tubes, 3kg of superconducting carbon black and 180kg of N-methylpyrrolidone, then adjusting the revolution speed of a stirring cylinder to 15 revolutions per minute and the dispersion speed to 1000 revolutions per minute, carrying out a fourth stirring operation, and stirring for 80 minutes;
adding 290kg of lithium iron phosphate powder into a 650L double-planet stirrer after the surfaces of the carbon nano tube and the superconducting carbon black are wetted, adjusting the revolution speed to 15 revolutions per minute and the dispersion speed to 500 revolutions per minute, and performing fifth stirring operation for 10 minutes to obtain mixed slurry;
then under the conditions that the revolution speed is 15 revolutions per minute and the dispersion speed is 500 revolutions per minute, 290kg of lithium iron phosphate powder is added into the mixed slurry to carry out sixth stirring operation, 150kg of adhesive glue solution is added, vacuumizing operation is carried out, the vacuum degree of a stirring cylinder is controlled to be-80 kpa, the revolution speed is adjusted to be 20 revolutions per minute, the dispersion speed is adjusted to be 1200 revolutions per minute, and seventh stirring operation is carried out for stirring for 150 minutes;
and finally, carrying out eighth stirring operation under the conditions that the vacuum degree is-80 kpa, the revolution speed is 20 revolutions per minute and the dispersion speed is adjusted to 500 revolutions per minute to obtain the lithium battery anode slurry.
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