CN115498190A - Dispersing agent for lithium iron phosphate anode slurry, preparation method of lithium iron phosphate anode slurry and lithium ion battery - Google Patents
Dispersing agent for lithium iron phosphate anode slurry, preparation method of lithium iron phosphate anode slurry and lithium ion battery Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dispersing agent for lithium iron phosphate anode slurry, the lithium iron phosphate anode slurry, a preparation method of the dispersing agent and a lithium ion battery, wherein the dispersing agent for the lithium iron phosphate anode slurry comprises sodium dodecyl sulfate and fatty alcohol-polyoxyethylene ether, and the dispersing agent comprises the following components in percentage by weight based on 100% of the total weight of the dispersing agent: 20-40% of sodium dodecyl sulfate and 60-80% of fatty alcohol-polyoxyethylene ether. The dispersing agent provided by the invention has excellent dispersing capacity for the positive pole slurry, and simultaneously, the positive pole slurry has excellent stability, and a positive pole piece prepared from the positive pole slurry has strong peeling strength and conductivity.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to a dispersing agent for lithium iron phosphate anode slurry, the lithium iron phosphate anode slurry, a preparation method of the lithium iron phosphate anode slurry and a lithium ion battery.
Background
Lithium ion batteries, because of their advantages of high energy density, long cycle life, and environmental friendliness, are now widely used in portable devices such as mobile phones, notebook computers, and digital electronic products. The lithium ion battery anode slurry occupies a core position in a lithium battery, the performance of the lithium ion battery anode slurry directly influences various performance indexes of the lithium ion battery, and the cost of the lithium ion battery anode slurry also directly determines the cost of the battery.
The current commercial lithium iron phosphate (LFP) is basically obtained by jet milling spherical LFP, the particle size of the lithium iron phosphate is about 100-500 nm, and compared with blocky and micron-sized electrode materials, the nano-structured material has the advantages of short transmission distance, large specific surface area, high reversible capacity, stable cycle performance, high electron transmission speed and the like. Although nanoscale particles have a stronger electrolyte adsorption capacity than micron-sized particles, the surface energy due to their large specific surface area also makes them highly susceptible to agglomeration. Meanwhile, the conductive agent also has a large specific surface area, and is difficult to completely disperse in the glue solution, which brings inconvenience to processing. In the pulping process, the slurry is not uniformly dispersed due to agglomeration, the conductive agent cannot be uniformly covered on the active material, the conductivity of the anode is reduced, and the capacity, the cycle performance and the consistency of the lithium ion battery are directly reduced. The aggregation causes a decrease in the adhesive force of the paste during coating, increasing the internal resistance of the battery, and the positive electrode is easily pressed to pierce the separator during assembly of the protruding portion, decreasing the safety of the battery.
At present, a surfactant (a dispersing agent including an anionic surfactant and a nonionic surfactant) is added into lithium iron phosphate slurry to disperse small particles, so that the performance of the slurry is improved, and the small particles are prevented from being agglomerated. However, the addition of the traditional dispersant generally has adverse effects on the performance of the battery, for example, only the addition of the anionic surfactant can generate a salting-out effect, so that the peeling strength of the electrode is obviously reduced, and the stability of the slurry is poor; for example, chinese patent CN109167068B discloses a positive electrode slurry for a lithium battery and a processing process thereof, wherein a dispersant in a raw material of the positive electrode slurry is polyvinylpyrrolidone, and a positive electrode prepared from the positive electrode slurry has poor conductivity. Therefore, a novel dispersant which has excellent dispersing ability for the positive electrode slurry, and simultaneously enables the positive electrode slurry to have excellent stability, and a positive electrode plate prepared from the positive electrode slurry has strong peeling strength and conductivity is urgently needed to be researched.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a dispersing agent for lithium iron phosphate positive electrode slurry, the lithium iron phosphate positive electrode slurry, a preparation method of the lithium iron phosphate positive electrode slurry and a lithium ion battery.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a dispersing agent for lithium iron phosphate anode slurry, which comprises sodium dodecyl sulfate and fatty alcohol-polyoxyethylene ether, and the dispersing agent comprises the following components in percentage by weight, based on 100% of the total weight of the dispersing agent: 20-40% of sodium dodecyl sulfate (for example, 20%, 30% or 40% can be used), and 60-80% of fatty alcohol-polyoxyethylene ether (for example, 60%, 70% or 80% can be used).
The dispersing agent provided by the invention has excellent dispersing capacity for the positive pole slurry, and simultaneously, the positive pole slurry has excellent stability, and a positive pole piece prepared from the positive pole slurry has strong peeling strength and conductivity.
In the above dispersant for lithium iron phosphate positive electrode slurry, as a preferred embodiment, the fatty alcohol-polyoxyethylene ether is at least one of AEO-3, AEO-7 and AEO-9.
In the above dispersing agent for lithium iron phosphate positive electrode slurry, as a preferred embodiment, the dispersing agent for lithium iron phosphate positive electrode slurry is composed of the sodium dodecyl sulfate and the fatty alcohol-polyoxyethylene ether.
In a second aspect, the present invention provides a lithium iron phosphate positive electrode slurry, including the dispersant for a lithium iron phosphate positive electrode slurry according to the first aspect.
The lithium iron phosphate anode slurry provided by the invention has the advantages of small fineness, good dispersibility and excellent stability, and the anode plate prepared from the anode slurry has strong peel strength and conductivity.
In the above lithium iron phosphate positive electrode slurry, as a preferred embodiment, the lithium iron phosphate positive electrode slurry includes lithium iron phosphate, a conductive agent, a binder, and the dispersant for lithium iron phosphate positive electrode slurry, wherein the mass ratio of the lithium iron phosphate, the conductive agent, the binder, and the dispersant for lithium iron phosphate positive electrode slurry is (94 to 96): (1-3): (1-3): (0.5 to 1) (for example, the mass ratio may be 95: 2.5: 94: 2), wherein the total of the respective amounts of the lithium iron phosphate, the conductive agent, the binder and the dispersing agent for lithium iron phosphate positive electrode slurry is 100, that is, the mass fraction of the lithium iron phosphate in the total amount of the slurry main material is 94 to 96%, the mass fraction of the conductive agent in the total amount of the slurry main material is 1 to 3%, the mass fraction of the binder in the total amount of the slurry main material is 1 to 3%, the mass fraction of the dispersing agent for lithium iron phosphate positive electrode slurry in the total amount of the slurry main material is 0.5 to 1%, and the total amount of the slurry main material is the sum of the masses of the lithium iron phosphate, the conductive agent, the binder and the dispersing agent for lithium iron phosphate positive electrode slurry.
In the above lithium iron phosphate positive electrode slurry, as a preferred embodiment, the conductive agent includes at least one of acetylene black, super-P (conductive carbon black), ketjen black, vapor-grown carbon fiber, and carbon nanotube.
In the above lithium iron phosphate positive electrode slurry, as a preferred embodiment, the binder includes at least one of PVDF (polyvinylidene fluoride) and PVA (polyvinyl alcohol).
In a preferred embodiment of the lithium iron phosphate positive electrode slurry, the solid content of the lithium iron phosphate positive electrode slurry is 50% to 65% (for example, 50%, 52%, 54%, 56%, 58%, 60%, or 65% solid content) and the viscosity is 4000mPa · s to 8000mPa · s (for example, 4000mPa · s, 5000mPa · s, 6000mPa · s, 7000mPa · s, 8000mPa · s, or the like).
In a third aspect, the invention provides a preparation method of the lithium iron phosphate positive electrode slurry according to the second aspect, which includes the following steps:
s1, mixing and stirring a binder and an organic solvent to obtain a glue solution, and then adding the fatty alcohol-polyoxyethylene ether into the glue solution to obtain a first mixed material;
s2, adding a conductive agent and lithium iron phosphate into a ball mill for ball milling and premixing to obtain a second mixed material, and then adding the sodium dodecyl sulfate into the second mixed material to obtain a third mixed material;
S3, adding the third mixed material into the first mixed material, and performing first stirring and dispersing to obtain a fourth mixed material;
and S4, adding the organic solvent into the fourth mixed material, carrying out second stirring and dispersing to obtain a fifth mixed material, and then carrying out viscosity regulation to obtain the lithium iron phosphate anode slurry.
Here, the viscosity adjustment may refer to adjusting the viscosity of the fifth mixture to obtain the lithium iron phosphate cathode slurry with the viscosity within a desired viscosity range.
The lithium iron phosphate anode slurry prepared by the invention has small fineness, good dispersibility and excellent stability, and the anode plate prepared by the anode slurry has stronger peel strength and conductivity.
In a preferred embodiment of the method for preparing lithium iron phosphate positive electrode slurry, the organic solvent includes at least one of an NMP (N-methylpyrrolidone) solvent, ethanol, and acetone.
In the above method for preparing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S1, the mixing and stirring sequentially includes medium-speed stirring, high-speed stirring, and low-speed vacuum reverse defoaming, wherein the revolution speed of the medium-speed stirring is 20 to 30rpm (for example, 20rpm, 22rpm, 24rpm, 26rpm, 28rpm, or 30rpm may be used), the dispersion speed is 5 to 8m/S (for example, 5m/S, 6m/S, 7m/S, or 8m/S may be used), and the time is 5 to 15min (for example, 5min, 7min, 9min, 13min, or 15min may be used); the revolution speed of the high-speed stirring is 30-40 rpm (for example, 30rpm, 32rpm, 34rpm, 36rpm, 38rpm or 40rpm can be selected), the dispersion speed is 8-11 m/s (for example, 8m/s, 9m/s, 10m/s or 11m/s can be selected), and the time is 140-160 min (for example, 140min, 142min, 144min, 146min, 148min, 150min, 155min or 160min can be selected); the revolution speed of the low-speed vacuum reverse defoaming is 10-20 rpm (for example, 10rpm, 12rpm, 14rpm, 16rpm, 18rpm, 20rpm and the like can be selected), the dispersion speed is 0rpm, and the time is 20-40 min (for example, 20min, 25min, 30min, 35min, 40min and the like can be selected).
In a preferred embodiment of the method for preparing the lithium iron phosphate positive electrode slurry, the solid content of the glue solution is 5% to 10% (for example, 5%, 7%, 10%, or the like).
In the above method for producing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S2, the rotation speed of the ball mill is 100 to 200rpm (for example, 100rpm, 120rpm, 140rpm, 160rpm, 180rpm, 200rpm, or the like), the premixing time is 1 to 3 hours (for example, 1 hour, 2 hours, or 3 hours, or the like), and the ball-to-material ratio (mass ratio) is (2.
In the above method for preparing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S3, the third mixture is added to the first mixture twice, and first stirring dispersion is performed, where the first stirring dispersion includes stirring dispersion after the first addition of the third mixture and stirring dispersion after the second addition of the third mixture, and the stirring dispersion after the first addition of the third mixture includes stirring dispersion at a revolution speed of 10 to 20rpm (for example, 10rpm, 12rpm, 14rpm, 16rpm, 18rpm, or 20rpm, etc.), stirring dispersion at a dispersion speed of 1 to 5m/S (for example, 1m/S, 2m/S, 3m/S, 4m/S, or 5m/S, etc.), stirring dispersion at a dispersion speed of 5 to 15min (for example, 5min, 10min, or 15min, etc.), and then stirring dispersion at a revolution speed of 20 to 30rpm (for example, 20rpm, 22rpm, 24rpm, 26rpm, 28rpm, 30rpm, etc.), and dispersion speed of 5 to 10min, or 15min (for example, 20 to 30min, 20 to 20min, 20 to 30min (for example, 20 to 40 to 20min, 8 to 20min, or 20 m/S, or 20 to 20 m/S, etc.); the stirring and dispersing after the second mixing step includes firstly stirring and dispersing at a revolution speed of 10 to 20rpm (for example, 10rpm, 12rpm, 14rpm, 16rpm, 18rpm or 20rpm, etc.), a dispersion speed of 1 to 5m/s (for example, 1m/s, 2m/s, 3m/s, 4m/s or 5m/s, etc.), a stirring and dispersing speed of 5 to 15min (for example, 5min, 10min or 15min, etc.), a revolution speed of 20 to 30rpm (for example, 20rpm, 22rpm, 24rpm, 26rpm, 28rpm or 30rpm, etc.), a dispersion speed of 5 to 8m/s (for example, 5m/s, 6m/s, 7m/s or 8m/s, etc.), and a stirring and dispersing speed of 70 to 90min (for example, 70min, 72min, 74min, 76min, 78min, 80min, 85min or 90min, etc.).
In the above method for producing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S4, the second stirring dispersion is performed at a revolution speed of 30 to 40rpm (for example, 30rpm, 32rpm, 34rpm, 36rpm, 38rpm, 40rpm, or the like), a dispersion speed of 8 to 11m/S (for example, 8m/S, 9m/S, 10m/S, or 11m/S, or the like), and a time of 80 to 100min (for example, 80min, 82min, 84min, 86min, 88min, 90min, 95min, or 100min, or the like).
In a preferred embodiment of the method for preparing the lithium iron phosphate positive electrode slurry, the solid content of the fifth mixture is 50% to 70% (for example, 50%, 55%, 60%, 65%, 70%, or the like).
In the above method for preparing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S4, the organic solvent is added to the fifth mixture to adjust viscosity.
In the above method for producing a lithium iron phosphate positive electrode slurry, as a preferred embodiment, in step S4, before discharging, vacuum inversion defoaming is performed.
In a fourth aspect, the present invention provides a lithium ion battery, including a positive electrode plate, a negative electrode plate, a diaphragm and an electrolyte, where the positive electrode plate is prepared from a positive electrode slurry provided in the second aspect or a positive electrode slurry prepared by a preparation method of a lithium iron phosphate positive electrode slurry provided in the third aspect, and the preparation method of the positive electrode plate is as follows:
And coating the lithium iron phosphate anode slurry on the surface of a current collector, and rolling to obtain the lithium iron phosphate anode piece.
The positive pole piece prepared by the invention has stronger peel strength and conductivity.
Compared with the prior art, the invention has the beneficial effects that at least one of the following items is included:
(1) The dispersing agent provided by the invention has excellent dispersing capacity for the positive pole slurry, and simultaneously, the positive pole slurry has excellent stability, and a positive pole piece prepared from the positive pole slurry has strong peeling strength and conductivity.
(2) According to the invention, the problems of agglomeration and particle size of the lithium iron phosphate anode slurry are solved by means of mechanical grinding and chemical dispersion, and the performance of the slurry is optimized.
(3) According to the invention, two surfactants are compounded as the dispersing agent, so that the dispersing performance of the slurry is improved, the agglomeration of the slurry is reduced, the stability of the slurry is improved, the peel strength and the conductivity of the pole piece are improved, and the performance of the battery is optimized.
Drawings
Fig. 1 is a graph showing the change in viscosity of lithium iron phosphate positive electrode slurry according to an embodiment of the present invention and a comparative example.
Detailed Description
For a further understanding of the present invention, preferred embodiments of the present invention are described below in conjunction with the following examples, and the scope of the present application includes, but is not limited to, the following examples. The following examples are only for illustrating the advantages and effects of the technical solutions of the present application and do not limit the scope of protection of the present application. Equivalents may be substituted for those skilled in the art based on the teachings herein without departing from the scope of the present application.
Unless defined otherwise, technical terms used in the following examples have the same meanings as commonly understood by one of ordinary skill in the art to which the present invention belongs. The experimental reagents used in the following examples, unless otherwise specified, are all conventional biochemical reagents; the dosage of the experimental reagent is the dosage of the reagent in the conventional experimental operation if no special description exists; the experimental methods are conventional methods unless otherwise specified.
In a first aspect, the invention provides a dispersing agent for lithium iron phosphate anode slurry, which is composed of sodium dodecyl sulfate and fatty alcohol-polyoxyethylene ether, and the dispersing agent comprises the following components in percentage by weight, based on 100% of the total weight of the dispersing agent: 20-40% of sodium dodecyl sulfate and 60-80% of fatty alcohol-polyoxyethylene ether, wherein the fatty alcohol-polyoxyethylene ether is at least one of AEO-3, AEO-7 and AEO-9.
The dispersing agent provided by the invention consists of lauryl sodium sulfate and fatty alcohol-polyoxyethylene ether, wherein the lauryl sodium sulfate is an anionic surfactant, is ionized to generate anions, is adsorbed on the surface of LFP, and is prevented from agglomerating by repulsive force, and the fatty alcohol-polyoxyethylene ether is a nonionic surfactant, so that the dispersibility of the slurry is improved to a certain extent, the distance between particles is increased, and the stability and the flowability of the slurry are improved by lubricating the particles.
The two components in the dispersant have a synergistic effect, and the dispersant is a novel composite dispersant which not only has excellent dispersing capacity for anode slurry, but also simultaneously enables the anode slurry to have excellent stability, and a positive pole piece prepared from the anode slurry has strong peel strength and electrical conductivity.
In a second aspect, the invention provides a lithium iron phosphate positive electrode slurry, which includes lithium iron phosphate, a conductive agent, a binder and the dispersant for lithium iron phosphate positive electrode slurry provided in the first aspect, wherein the mass ratio of the lithium iron phosphate, the conductive agent, the binder and the dispersant for lithium iron phosphate positive electrode slurry is (94-96): (1-3): (1-3): (0.5-1), the conductive agent comprises at least one of acetylene black, super-P (conductive carbon black), ketjen black, vapor-grown carbon fiber and carbon nano tube, the binder comprises at least one of PVDF (polyvinylidene fluoride) and PVA (polyvinyl alcohol), the solid content of the lithium iron phosphate anode slurry is 50-65%, and the viscosity is 4000-8000 mPa.
In a third aspect, the invention provides a preparation method of the lithium iron phosphate positive electrode slurry, which comprises the following steps:
S1, mixing and stirring a binder and an organic solvent to obtain a glue solution, and then adding fatty alcohol-polyoxyethylene ether into the glue solution to obtain a first mixed material, wherein the solid content of the glue solution is 5-10%, the organic solvent comprises at least one of an NMP (N-methyl pyrrolidone) solvent, ethanol and acetone, and the mixing and stirring sequentially comprises medium-speed stirring, high-speed stirring and low-speed vacuum reverse defoaming, wherein the revolution speed of the medium-speed stirring is 20-30 rpm, the dispersion speed is 5-8 m/S, and the time is 5-15 min; the revolution speed of the high-speed stirring is 30-40 rpm, the dispersion speed is 8-11 m/s, and the time is 140-160 min; the revolution speed of the low-speed vacuum reverse defoaming is 10-20 rpm, the dispersion speed is 0rpm, and the time is 20-40 min.
S2, adding a conductive agent and lithium iron phosphate into a ball mill for ball milling and premixing to obtain a second mixed material, and then adding the lauryl sodium sulfate into the second mixed material to obtain a third mixed material, wherein the rotating speed of the ball mill is 100-200 rpm, the premixing time is 1-3 h, and the ball-to-material ratio is (2.
S3, adding the third mixed material into the first mixed material, and performing first stirring dispersion to obtain a fourth mixed material, wherein the third mixed material is added into the first mixed material twice to perform first stirring dispersion, and the first stirring dispersion comprises stirring dispersion after the third mixed material is added for the first time and stirring dispersion after the third mixed material is added for the second time, wherein the stirring dispersion after the third mixed material is added for the first time comprises stirring dispersion for 5-15 min at a revolution speed of 10-20 rpm and a dispersion speed of 1-5 m/S, and then stirring dispersion for 20-40 min at a revolution speed of 20-30 rpm and a dispersion speed of 5-8 m/S; the stirring and dispersing after the third mixed material is added for the second time comprises stirring and dispersing for 5-15 min at a revolution speed of 10-20 rpm and a dispersion speed of 1-5 m/s, and then stirring and dispersing for 70-90 min at a revolution speed of 20-30 rpm and a dispersion speed of 5-8 m/s.
And S4, adding the organic solvent into the fourth mixed material, carrying out second stirring dispersion to obtain a fifth mixed material, and then adding the organic solvent for viscosity regulation to obtain the lithium iron phosphate anode slurry, wherein the solid content of the fifth mixed material is 50% -70%, the revolution speed of the second stirring dispersion is 30-40 rpm, the dispersion speed is 8-11 m/S, and the time is 80-100 min.
In a fourth aspect, the present invention provides a lithium ion battery, including a positive electrode plate, a negative electrode plate, a diaphragm and an electrolyte, where the positive electrode plate is prepared by using the positive electrode slurry provided in the second aspect or the positive electrode slurry prepared by using the preparation method of the lithium iron phosphate positive electrode slurry provided in the third aspect, and the preparation method of the positive electrode plate is as follows:
and coating the lithium iron phosphate anode slurry on the surface of a current collector, and rolling to obtain the lithium iron phosphate anode piece.
In order to further understand the present invention, the dispersant for lithium iron phosphate positive electrode slurry, the preparation method thereof, and the lithium ion battery provided by the present invention are described in detail below with reference to the following examples, and the protection scope of the present invention is not limited by the following examples.
Example 1
The lithium iron phosphate anode slurry provided by the embodiment of the invention comprises lithium iron phosphate (LiFePO) 4 (LFP)), a conductive agent (Super-P), a binder (polyvinylidene fluoride (PVDF)) and a dispersing agent (sodium dodecyl sulfate and fatty alcohol-polyoxyethylene ether (AEO-7)) for the lithium iron phosphate positive electrode slurry, wherein the mass ratio of the lithium iron phosphate to the Super-P to the PVDF to the sodium dodecyl sulfate to the AEO-7 is 95:2:2.5:0.2:0.3.
the preparation method of the lithium iron phosphate anode slurry provided by the embodiment of the invention comprises the following steps:
s1, at room temperature, adding PVDF binder into NMP to be completely dissolved, firstly stirring at a medium speed, wherein the revolution speed of the medium-speed stirring is 25rpm, the dispersion speed is 5m/S, and the time is 10min, then stirring at a high speed, wherein the revolution speed of the high-speed stirring is 35rpm, the dispersion speed is 9m/S, and the time is 150min, finally carrying out low-speed vacuum reverse rotation defoaming, wherein the revolution speed of the low-speed vacuum reverse rotation defoaming is 15rpm, the dispersion speed is 0rpm, and the time is 30min, so as to obtain glue solution with the solid content of 6.5%, and then adding AEO-7 into the glue solution, so as to obtain a first mixed material.
And S2, carrying out dry mixing and grinding on the SP and the LFP through a planetary ball mill to obtain a second mixed material, wherein the rotating speed of the ball mill is 150rpm, the dry mixing time is 2h, and the ball-to-material ratio is 3.
And S3, adding the third mixed material into the first mixed material twice, fully dispersing to obtain a fourth mixed material, stirring and dispersing at a low speed after the first feeding, wherein the revolution speed of the low-speed stirring and dispersing is 15rpm, the dispersion speed is 3m/S, and the time is 10min, then stirring and dispersing at a medium speed, the revolution speed of the medium-speed stirring and dispersing is 25rpm, the dispersion speed is 6m/S, and the time is 30min, stirring and dispersing at a low speed after the second feeding, the revolution speed of the low-speed stirring and dispersing is 15rpm, the dispersion speed is 3m/S, and the time is 10min, then stirring and dispersing at a medium speed, the revolution speed of the medium-speed stirring and dispersing is 25rpm, the dispersion speed is 6m/S, and the time is 80min.
S4, adding a proper amount of NMP into the fourth mixed material to carry out high-speed stirring dispersion (second stirring dispersion) to obtain a fifth mixed material with the solid content of 68%, wherein the revolution speed of the high-speed stirring dispersion is 35rpm, the dispersion speed is 11m/S, and the time is 90min;
and finally adding NMP for adjusting viscosity to obtain lithium iron phosphate anode slurry, and performing vacuum reversal defoaming before discharging, wherein the revolution reversal speed is 10rpm, the vacuum degree is-90 kpa, and the time is 30 minutes.
The lithium iron phosphate anode slurry prepared by the embodiment of the invention has the solid content of 58% and the viscosity of 6532mPa & s.
Example 2
The lithium iron phosphate anode slurry provided by the embodiment of the invention comprises lithium iron phosphate (LiFePO) 4 (LFP)), conductive agent (Super-P)The lithium iron phosphate positive electrode slurry comprises a binder (polyvinylidene fluoride (PVDF)) and a dispersing agent (sodium dodecyl sulfate and fatty alcohol-polyoxyethylene ether (AEO-3)) for the lithium iron phosphate positive electrode slurry, wherein the mass ratio of the lithium iron phosphate to the Super-P to the PVDF to the sodium dodecyl sulfate to the AEO-3 is 95:2:2.5:0.1:0.4.
with reference to the preparation method of the lithium iron phosphate positive electrode slurry provided in example 1, the lithium iron phosphate positive electrode slurry is prepared, and the prepared lithium iron phosphate positive electrode slurry has a solid content of 57.6% and a viscosity of 6323mPa · s.
Comparative example 1
The lithium iron phosphate positive electrode slurry provided by the present comparative example is substantially the same as that in example 1, except that the lithium iron phosphate positive electrode slurry does not include the dispersant for lithium iron phosphate positive electrode slurry (sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether (AEO-7)), that is, the raw material does not include the dispersant, and the mass ratio of lithium iron phosphate, super-P, and PVDF is 95:2.5:2.5.
the preparation method of the lithium iron phosphate positive electrode slurry provided by the comparative example is basically the same as that of example 1, except that AEO-7 is not added in step S1, and sodium dodecyl sulfate is not added in step S2, and the solid content of the lithium iron phosphate positive electrode slurry is 57.2%, and the viscosity is 6630mPa · S.
Comparative example 2
The lithium iron phosphate anode slurry provided by the comparative example is basically the same as that in example 1, except that the lithium iron phosphate anode slurry does not include AEO-7, and the mass ratio of the formula is LiFePO 4 : super-P: PVDF: sodium lauryl sulfate =95:2:2.5:0.5.
the preparation method of the lithium iron phosphate positive electrode slurry provided by the comparative example is substantially the same as that of example 1, except that AEO-7 is not added in step S1, the solid content of the lithium iron phosphate positive electrode slurry is 58.4%, and the viscosity is 6848mPa · S.
Comparative example 3
The lithium iron phosphate anode slurry provided by the comparative example is basically the same as that in example 1, except that the lithium iron phosphate anode slurry does not include sodium dodecyl sulfate, and the mass ratio of the formula is LiFePO 4 ：Super-P：PVDF：AEO-7＝95：2：2.5：0.5。
The preparation method of the lithium iron phosphate positive electrode slurry provided by the comparative example is substantially the same as that in example 1, except that sodium dodecyl sulfate is not added in step S2, the solid content of the lithium iron phosphate positive electrode slurry is 58%, and the viscosity is 5782mPa · S.
Comparative example 4
The lithium iron phosphate anode slurry provided by the comparative example is basically the same as that in example 1, except that sodium dodecyl sulfate is replaced by PAAS (sodium polyacrylate), and the mass ratio of lithium iron phosphate to Super-P to PVDF to PAAS to AEO-7 is 95:2:2.5:0.2:0.3.
The preparation method of the lithium iron phosphate positive electrode slurry provided by the comparative example is basically the same as that in example 1, except that in step S2, the sodium dodecyl sulfate is replaced by PAAS, and the PAAS is added, so that the solid content of the lithium iron phosphate positive electrode slurry is 57.5%, and the viscosity is 6400mPa · S.
Comparative example 5
The lithium iron phosphate positive electrode slurry provided by the comparative example is basically the same as that in example 1, except that the dispersing agent (sodium dodecyl sulfate and fatty alcohol polyoxyethylene ether (AEO-7)) for the lithium iron phosphate positive electrode slurry is replaced by PAAS, and the mass ratio of lithium iron phosphate to Super-P to PVDF to PAAS is 95:2:2.5:0.5.
the preparation method of the lithium iron phosphate positive electrode slurry provided by the comparative example is substantially the same as that in example 1, except that AEO-7 is not added in step S1, and in step S2, PAAS is added instead of sodium dodecyl sulfate, and the solid content of the lithium iron phosphate positive electrode slurry is 58.6%, and the viscosity is 6323mPa · S.
Performance testing
Particle size tests were performed on the lithium iron phosphate positive electrode pastes prepared in examples 1 to 2 and comparative examples 1 to 5, fineness tests and sedimentation tests were performed on the lithium iron phosphate positive electrode pastes prepared in examples 1 to 2 and comparative examples 1 to 5, the prepared positive electrode paste was coated on both sides of a carbon-coated aluminum foil of 12+2 (the aluminum foil was 12 micrometers thick, carbon-coated layers were respectively provided on both sides of the aluminum foil, and the total thickness of the carbon-coated layers was 2 micrometers) to obtain a positive electrode sheet, and sheet resistance and peel strength of the positive electrode sheet were tested, and the test results are shown in table 1 and fig. 1.
The settlement test method comprises the following steps: and standing the positive slurry for 24 hours at the temperature of 25 +/-2 ℃ and the humidity of 8%, and measuring the change rate of the viscosity of the slurry.
The testing method of the membrane resistance comprises the following steps: the diaphragm resistance was tested using an ACCFILM diaphragm resistance tester, the pole piece was cut into 25mm diameter discs and placed under a test probe at a test pressure of 0.3t for a 2s dwell time, and the data of the measured diaphragm resistance was obtained as shown in table 1.
The test method of the peel strength comprises the following steps: cutting the pole piece into strip-shaped samples with the size of 25 x 100mm, fixing one side of each sample on a stainless steel plate of a testing machine by using double faced adhesive tape, reversely bending the other side of each sample by 180 degrees, fixing the other side of each sample on a pressure probe, and stripping at the speed of 50mm/min to measure the stripping strength.
TABLE 1
As can be seen from table 1, the granularity and fineness of the positive electrode pastes prepared in examples 1 and 2 are small, which indicates that the dispersion performance of the LFP paste is improved by the mixed surfactant, the agglomeration effect between fine particles is reduced, and the positive electrode sheet prepared from the positive electrode paste has strong peel strength and conductivity (the sheet resistance is lowest, which is beneficial to electron transmission), and the peel strength is slightly lower than that of the paste without sodium dodecyl sulfate, but does not reach the degree of affecting the performance; compared with the comparative example 1, when no dispersant is added into the positive electrode slurry, the fineness is larger, and the conductivity is poorer; compared with comparative examples 2 and 3, when the dispersing agent is sodium dodecyl sulfate or AEO-7, the conductivity is poor, the conductivity of the positive pole piece prepared by the positive pole slurry prepared in the embodiment 1 is better than that of the positive pole piece prepared in the comparative examples 2 and 3, and the sodium dodecyl sulfate and the fatty alcohol-polyoxyethylene ether have a synergistic effect and can improve the conductivity of the positive pole piece; from comparative examples 3-5, it can be seen that when PAAS and AEO-7 are compounded, the conductivity of the positive electrode plate is superior to that of comparative example 3, and inferior to that of comparative example 5, which indicates that PAAS and fatty alcohol-polyoxyethylene ether do not have synergistic effect on the conductivity of the positive electrode plate.
As can be seen from fig. 1, the positive electrode slurries prepared in examples 1 and 2 have excellent stability; comparative example 1 no dispersant was added and the prepared slurry had the worst stability; compared with comparative examples 2 and 3, the stability of the positive electrode slurry prepared in example 1 is superior to that of comparative examples 2 and 3, which shows that the sodium dodecyl sulfate and the fatty alcohol-polyoxyethylene ether have synergistic effect and can improve the stability of the positive electrode slurry; from comparative examples 3 to 5, it is understood that when PAAS and AEO-7 were compounded, the stability of the positive electrode slurry was superior to comparative example 5 and inferior to comparative example 3, indicating that PAAS and fatty alcohol polyoxyethylene ether did not have a synergistic effect in the stability of the positive electrode slurry.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. The dispersing agent for the lithium iron phosphate anode slurry is characterized by comprising lauryl sodium sulfate and fatty alcohol-polyoxyethylene ether, wherein the dispersing agent comprises the following components in percentage by weight based on 100% of the total weight of the dispersing agent: 20-40% of sodium dodecyl sulfate and 60-80% of fatty alcohol-polyoxyethylene ether.
2. The dispersing agent for lithium iron phosphate positive electrode slurry according to claim 1, wherein the fatty alcohol-polyoxyethylene ether is at least one of AEO-3, AEO-7 and AEO-9;
and/or the dispersing agent for the lithium iron phosphate anode slurry consists of the sodium dodecyl sulfate and the fatty alcohol-polyoxyethylene ether.
3. A lithium iron phosphate positive electrode slurry characterized by comprising the dispersant for lithium iron phosphate positive electrode slurry according to claim 1 or 2.
4. The lithium iron phosphate positive electrode slurry according to claim 3, wherein the lithium iron phosphate positive electrode slurry comprises lithium iron phosphate, a conductive agent, a binder and the dispersing agent for the lithium iron phosphate positive electrode slurry, and the mass ratio of the lithium iron phosphate to the conductive agent to the binder to the dispersing agent for the lithium iron phosphate positive electrode slurry is (94-96): (1-3): (1-3): (0.5-1).
5. The lithium iron phosphate positive electrode slurry according to claim 4, wherein the conductive agent comprises at least one of acetylene black, super-P, ketjen black, vapor grown carbon fiber, and carbon nanotubes;
and/or the binder comprises at least one of PVDF and PVA.
6. The method for preparing the lithium iron phosphate positive electrode slurry according to any one of claims 3 to 5, comprising the steps of:
s1, mixing and stirring a binder and an organic solvent to obtain a glue solution, and then adding the fatty alcohol-polyoxyethylene ether into the glue solution to obtain a first mixed material;
s2, adding a conductive agent and lithium iron phosphate into a ball mill for ball milling and premixing to obtain a second mixed material, and then adding the sodium dodecyl sulfate into the second mixed material to obtain a third mixed material;
s3, adding the third mixed material into the first mixed material, and performing first stirring dispersion to obtain a fourth mixed material;
and S4, adding the organic solvent into the fourth mixed material, carrying out second stirring and dispersing to obtain a fifth mixed material, and then carrying out viscosity regulation to obtain the lithium iron phosphate anode slurry.
7. The method for preparing lithium iron phosphate positive electrode slurry according to claim 6, wherein the organic solvent includes at least one of NMP solvent, ethanol, and acetone.
8. The method for preparing the lithium iron phosphate positive electrode slurry according to claim 6, wherein in step S1, the mixing and stirring sequentially comprises medium-speed stirring, high-speed stirring and low-speed vacuum reverse defoaming, wherein the revolution speed of the medium-speed stirring is 20-30 rpm, the dispersion speed is 5-8 m/S, and the time is 5-15 min; the revolution speed of the high-speed stirring is 30-40 rpm, the dispersion speed is 8-11 m/s, and the time is 140-160 min; the revolution speed of the low-speed vacuum reverse defoaming is 10-20 rpm, the dispersion speed is 0rpm, and the time is 20-40 min;
And/or the solid content of the glue solution is 5-10%.
9. The method for preparing lithium iron phosphate positive electrode slurry according to claim 6, wherein in step S2, the rotation speed of the ball mill is 100 to 200rpm, the premixing time is 1 to 3 hours, and the ball-to-material ratio is (2;
and/or in step S3, adding the third mixed material into the first mixed material twice to perform first stirring dispersion, wherein the first stirring dispersion comprises stirring dispersion after the third mixed material is added for the first time and stirring dispersion after the third mixed material is added for the second time, and the stirring dispersion after the third mixed material is added for the first time comprises stirring dispersion for 5-15 min at a revolution speed of 10-20 rpm and a dispersion speed of 1-5 m/S and stirring dispersion for 20-40 min at a revolution speed of 20-30 rpm and a dispersion speed of 5-8 m/S; stirring and dispersing for the second time after the third mixed material is added comprises stirring and dispersing for 5-15 min at a revolution speed of 10-20 rpm and a dispersion speed of 1-5 m/s, and stirring and dispersing for 70-90 min at a revolution speed of 20-30 rpm and a dispersion speed of 5-8 m/s;
and/or in step S4, the revolution speed of the second stirring dispersion is 30-40 rpm, the dispersion speed is 8-11 m/S, and the time is 80-100 min;
And/or the solid content of the fifth mixed material is 50-70%.
10. A lithium ion battery comprises a positive pole piece, a negative pole piece, a diaphragm and electrolyte, and is characterized in that the positive pole piece is prepared by adopting the lithium iron phosphate positive slurry of any one of claims 3 to 5 or the positive slurry prepared by the preparation method of the lithium iron phosphate positive slurry of any one of claims 6 to 9.
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