CN112952061B - Lithium iron phosphate aqueous anode slurry, preparation method thereof and environment-friendly long-cycle lithium ion battery - Google Patents
Lithium iron phosphate aqueous anode slurry, preparation method thereof and environment-friendly long-cycle lithium ion battery Download PDFInfo
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Abstract
According to the lithium iron phosphate aqueous anode slurry and the preparation method thereof and the environment-friendly long-cycle lithium ion battery provided by the invention, solid powder lithium iron phosphate, CMC and conductive carbon black are dry-mixed firstly, then deionized water, EC and PAA solution are added for kneading, then deionized water and CNTs are added for large-rotation-speed dispersion, and after dispersion is finished, SBR emulsion is added for mixing to obtain uniform and stable aqueous anode slurry; the water-based anode slurry is coated, and the like, so that the environment-friendly long-cycle lithium ion battery can be prepared. The invention adopts deionized water as the solvent of the anode slurry, and firstly, the solvent is environment-friendly, secondly, secondary recovery is not needed, and thirdly, the source is rich, and the preparation cost is low; the water-based lithium iron phosphate core prepared by the invention has the following cycle performance at 25 ℃: the capacity retention rate reaches about 95 percent after 1000 cycles of circulation. In addition, the lithium ion battery provided by the invention has good processing stability.
Description
Technical Field
The invention belongs to the field of batteries, and particularly relates to lithium iron phosphate aqueous anode slurry, a preparation method thereof and an environment-friendly long-cycle lithium ion battery.
Background
Along with the continuous development of lithium ion batteries, the demand for products related to the lithium ion batteries is gradually increased, at present, NMP is still adopted as a solvent for preparing anode slurry of the lithium ion batteries, the solvent needs to be recycled for the second time in the production process, firstly, the solvent is not thoroughly recycled and is volatile, so that the environmental pollution exists, secondly, the energy consumption exists in the recycling process, the cost is increased, and thirdly, NMP as an industrial solvent needs to be additionally purchased, so that the cost is increased.
The chinese patent application publication No. CN105261760A, published in 2016, 1, 20, discloses a composite current collector of a water-based positive electrode of a lithium ion battery, a positive plate, a preparation method thereof, and a lithium ion battery, and indicates that the prepared battery has improved cycle performance, but the capacity retention rate of 500 cycles of actual battery cell cycle is lower than 90%, which cannot meet the requirements of the existing long-cycle lithium iron phosphate battery.
Disclosure of Invention
The invention aims to provide lithium iron phosphate water-based anode slurry which is prepared from lithium iron phosphate, CNTs, conductive carbon black, a binder PAA, SBR, CMC, EC and deionized water, is environment-friendly, does not need secondary recovery and has low cost.
The invention also aims to provide a preparation method of the lithium iron phosphate water-based anode slurry, which designs the sequence of adding raw materials, improves the uniformity of the slurry and improves the performance.
The last purpose of the invention is to provide an environment-friendly long-cycle lithium ion battery, wherein the anode is made of the lithium iron phosphate aqueous anode slurry, and the obtained aqueous lithium iron phosphate core has the following 25 ℃ cycle performance: the capacity retention rate reaches about 95 percent after 1000 cycles of circulation.
The specific technical scheme of the invention is as follows:
the lithium iron phosphate water-based cathode slurry comprises the following raw materials in percentage by mass:
47.0 wt% -49.0 wt% of lithium iron phosphate, 0.34 wt% -0.5 wt% of carbon nanotube dispersion CNTs, 0.15 wt% -0.3 wt% of conductive carbon black, 0.5 wt% -1.0 wt% of PAA polyacrylic acid binder solution, 0.25 wt% -0.5 wt% of styrene-butadiene rubber emulsion SBR, 0.4 wt% -0.6 wt% of carboxymethyl cellulose CMC, 1.0 wt% -2.0 wt% of ethylene carbonate EC, and 47% -50% of deionized water.
The total amount of the above raw materials is 100%.
The SBR solid content of the styrene-butadiene rubber emulsion is 40 percent; the PAA polyacrylic acid binder solution has a solid content of 6.5 percent, type LA 133; the solid content of the carbon nano tube dispersion liquid is 6.7 percent;
based on the fact that the solvent used by the anode slurry is replaced by the deionized water from the NMP, the original oily binder PVDF is replaced by the aqueous binder system of PAA and SBR, and the sufficient bonding strength and the electron conductivity between the slurry coating and the aluminum foil can be ensured; the double-conductive agent system of conductive carbon black SP and carbon nano tubes is adopted, and the purpose of reducing the internal resistance of the pole piece is achieved by increasing the combination mode of point points and point lines between the conductive agent and the main material, so that the slurry coating is ensured to have good electronic conductivity; meanwhile, by adding the ethylene carbonate, the flexibility of the pole piece is improved, and the processing capacity of the processes of slurry coating, cold pressing of the pole piece, winding and the like is optimized.
The invention provides a preparation method of lithium iron phosphate water-based anode slurry, which comprises the following steps:
1) carrying out dry mixing and dispersing on the lithium iron phosphate, the conductive carbon black and the carboxymethyl cellulose according to the formula amount;
2) adding one fifth to one fourth of deionized water, ethylene carbonate and polyacrylic acid binder solution according to the formula amount for soaking powder, and kneading;
3) adding the deionized water and the carbon nano tube dispersion liquid with the rest formula amount, and performing high-speed dispersion to obtain a uniform solution;
4) and finally adding styrene butadiene rubber emulsion and dispersing at low speed to obtain the product.
Furthermore, the equipment model adopted for preparing the lithium iron phosphate aqueous anode slurry is a ROSS 100L double-planet distributed stirring machine.
The dry mixing and dispersing conditions in the step 1) are as follows: revolution is 15-30rmp, rotation is 600-1000rmp, and time is 30-60 min.
The purpose of the dry powder mixing in step 1) is to enable large aggregates in the powder to be dispersed and broken under the action of high-shear force dispersion and simultaneously realize micro uniform mixing of the powder, and dispersed fine SP and CMC are deposited on the surfaces of large main material particles. The deposited SP can form a good conductive network, so that the resistance is reduced and the consistency is improved. The deposited CMC can quickly form a macromolecular chain coating main material after a solvent is added in the later step, and the stability is improved.
In the step 2), the purpose of pre-soaking the powder is to enable the solvent to uniformly disperse and rapidly soak the powder, so that the situation that the powder is directly kneaded without pre-soaking, and the abnormal conditions such as poor consistency and sedimentation of slurry caused by excessive local kneading and insufficient kneading of the other part are avoided. The stirring parameters for soaking the powder are set as follows: revolution is 15-30rmp, rotation is 600-1000rmp, and the time is 1-5 min;
the kneading in step 2) is to separate the agglomerates and ensure a good homogeneity state of the slurry. Setting parameters during kneading: revolution is carried out for 15-30rmp, and the time is 60-120 min.
And 3) performing high-speed dispersion in the step 3), further dispersing small aggregates in the slurry under a high-speed shearing condition, and uniformly dispersing the small aggregates in the solvent, wherein the parameters are as follows: revolution is 15-30rmp, rotation is 800-.
In the step 4), the SBR emulsion is added as the last step, and high shearing force can cause SBR demulsification, so medium and low speed dispersion is adopted. Setting parameters: revolution is 15-30rmp, rotation is 500-800rmp, and time is 30-90 min.
The environment-friendly long-cycle lithium ion battery provided by the invention is prepared by adopting the anode prepared from the lithium iron phosphate aqueous anode slurry.
Further, the environment-friendly long-cycle lithium ion battery comprises a positive plate and a negative plate;
the positive plate is prepared by adopting the lithium iron phosphate water-based positive slurry, and specifically comprises the following steps: the thickness of the aluminum foil is 12-16 mu m, the prepared lithium iron phosphate water-based anode slurry is uniformly coated on two surfaces of the anode current collector aluminum foil through a transfer coater, and is dried in a convection drying mode, a temperature sensor is arranged in each section of drying oven, the temperature in the drying oven can be monitored so as to regulate and control the temperature, single-sided coating is firstly carried out, and then double-sided coating is carried out after drying; specifically, the single-side coating speed is 3-5m/min, and the single-side drying parameters are as follows: adopting four sections of ovens to carry out convection type drying at the temperature of 92-91-89-88 ℃; the double-sided coating speed is 3-5m/min, and the double-sided drying parameters are as follows: the temperature is 100-98-95 ℃; and obtaining the water-based positive pole piece.
Furthermore, the obtained water-based positive pole piece adopts 2.2-2.4g/mm 3 The cold-pressed pole piece is obtained by the cold-pressed density, the pole piece is divided into strips, the strips are baked for 12 to 36 hours at the temperature of 80 to 100 ℃, and then the strips and the corresponding graphite negative pole piece are prepared by a series of procedures such as winding, liquid injection, formation, capacity grading and the likeThe environment-friendly long-cycle lithium ion battery with excellent consistency is obtained.
The homogenizing process of the water-based anode comprises the steps of firstly dry-mixing solid powder (lithium iron phosphate, CMC and conductive carbon black), then adding deionized water, EC and PAA solution for soaking powder, kneading, then adding deionized water and CNTs for high-speed dispersion, and after dispersion is finished, adding SBR emulsion for mixing to obtain uniform and stable water-based anode slurry; the water-based positive electrode slurry is subjected to a series of procedures of coating, cold pressing, stripping, winding with a corresponding negative electrode plate, drying, injecting and the like, so that the environment-friendly long-cycle lithium ion battery can be prepared.
Compared with the prior art, the invention adopts the deionized water as the solvent of the anode slurry, so that the solvent is environment-friendly, secondary recovery is not needed, and the source is rich and the preparation cost is low, thereby effectively avoiding the disadvantages of environmental pollution and high cost caused by using the NMP solvent. Meanwhile, the lithium ion battery prepared by adopting the aqueous anode slurry has excellent consistency, has the same cycle performance as the lithium ion battery prepared by using an oily anode (the coating weight is consistent with the compaction), and can meet the requirement of the existing long-cycle lithium iron phosphate battery. The 25 ℃ cycle performance of the water-based lithium iron phosphate core prepared by the invention is as follows: the capacity retention rate reaches about 95 percent after 1000 cycles of circulation. In addition, in the aspect of processing stability of the lithium ion battery, compared with the conventional NMP slurry, the binder adopted based on the NMP slurry is PVDF, and the phenomenon of physical gel and irreversible chemical gel after meeting water can be generated; the method has the advantages of energy conservation and environmental protection, can also prepare batteries with excellent cycle performance, and is suitable for industrialized popularization and application. Moreover, the provided battery achieves the purposes of energy conservation and environmental protection.
Drawings
FIG. 1 is a schematic flow diagram of slurry agitation according to the present invention;
FIG. 2 is a graph showing the viscosity of slurries of comparative example 1 and example 1 as a function of time;
FIG. 3 is a comparison of cycling performance tests at 25 ℃ for a 30Ah aqueous positive electrode hard shell cell obtained in example 1 of the invention versus a 30Ah oily positive electrode hard shell cell obtained in comparative example 1;
fig. 4 is a comparison of cycling performance tests at 60 ℃ for a 30Ah aqueous positive electrode hard shell cell obtained in example 1 of the invention versus a 30Ah oily positive electrode hard shell cell obtained in comparative example 1.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
The lithium iron phosphate water-based cathode slurry comprises the following raw materials in percentage by mass:
48.0 wt% of lithium iron phosphate, 0.35 wt% of carbon nanotube dispersion liquid CNTs, 0.15 wt% of conductive carbon black, 0.65 wt% of PAA polyacrylic acid binder solution, 0.35 wt% of styrene butadiene rubber emulsion SBR, 0.5 wt% of carboxymethyl cellulose CMC, 2.0 wt% of ethylene carbonate EC, and 48% of deionized water;
wherein the SBR solid content of the styrene butadiene rubber emulsion is 40 percent; the PAA polyacrylic acid binder solution has a solid content of 6.5 percent, type LA 133; the solid content of the carbon nano tube dispersion liquid is 6.7 percent;
the preparation method of the lithium iron phosphate water-based anode slurry comprises the following steps:
1) the preparation method is characterized by adopting a ROSS 100L double-planet dispersed stirring machine, firstly carrying out dry mixing dispersion on lithium iron phosphate, conductive carbon black and CMC powder according to the proportion, and setting parameters: revolution is carried out at 25rmp, rotation is carried out at 800rmp, and the time is 30 min;
2) then, one fifth of the formula amount of deionized water, EC and PAA solution are added for quick soaking of powder, and the parameters are set as follows: revolution is carried out at 20rmp, rotation is carried out at 800rmp, and the time is 1 min; the kneading phase is carried out again in order to separate the agglomerates and to ensure a good homogeneity state of the slurry, with the parameters set: revolution is carried out for 25rmp, and the time is 90 min;
3) and (2) in a high-speed dispersion stage, adding the deionized water and the carbon nano tube dispersion liquid CNTs with the amount of the remaining four fifths of formula into the dispersion stage to obtain a uniform solution, and setting parameters: revolution is carried out at 25rmp, rotation is carried out at 1500rmp, and the time is 240 min;
4) the SBR emulsion is added as the last step, and the high shearing force can cause SBR demulsification, so medium-low speed dispersion is adopted, and the parameters are set as follows: and (4) revolving for 25rmp, rotating for 500rmp, and standing for 60min to obtain the lithium iron phosphate aqueous anode slurry.
The environment-friendly long-circulation lithium ion battery comprises a positive plate and a negative plate, wherein the positive plate is prepared from the lithium iron phosphate water-based positive electrode slurry. The preparation method comprises the following steps:
A. uniformly coating the prepared lithium iron phosphate water-based anode slurry on two surfaces of an anode current collector aluminum foil through a transfer coater with the thickness of the aluminum foil being 12-16 mu m, wherein the coating weight of one surface of the anode current collector aluminum foil is 168.8g/mm 2 Meanwhile, a convection drying mode is adopted for drying, a temperature sensor is arranged in each section of the drying oven, the temperature in the drying oven can be monitored so as to regulate and control the temperature, single-sided coating is firstly carried out, and then double-sided coating is carried out after drying; the single-side coating speed is 3.5m/min, and the single-side drying parameters are as follows: the temperature is 92-91-89-88 ℃, and the fan frequency is as follows: 38Hz-38Hz-38Hz-35 Hz; the double-sided coating speed is 4m/min, and the double-sided drying parameters are as follows: temperature 100 ℃ -98 ℃ -95 ℃ -95 ℃, fan frequency: 38Hz-40Hz-40Hz-38 Hz; and obtaining the water-based positive pole piece.
B. Using a 2.3g/mm 3 The cold-pressed pole piece is obtained by the cold-pressed density, is subjected to stripping, is baked for 24 hours at 85 ℃, and is wound, injected and subjected to,The environment-friendly long-cycle lithium ion (30Ah) hard shell battery cell with excellent consistency is prepared through a series of procedures such as formation, capacity and grading.
Comparative example 1
The lithium iron phosphate oily anode slurry comprises the following raw materials in percentage by mass:
59.52 wt% of lithium iron phosphate, 0.93 wt% of conductive carbon black, 1.55 wt% of PVDF binder and 38% of NMP solvent.
The preparation method of the lithium iron phosphate oily anode slurry comprises the following steps:
1) firstly, carrying out dry mixing dispersion on lithium iron phosphate, conductive carbon black and PVDF powder according to the proportion, and setting parameters: revolution is carried out at 25rmp, rotation is carried out at 800rmp, and the time is 15 min.
2) Then adding NMP with the mass percent of 24% for kneading, and setting the parameters as follows: revolution is carried out for 25rmp, and the time is 60 min.
3) And in the pre-dispersion stage, NMP with the residual mass percentage of 14% is added and then pre-dispersed. Setting parameters: revolution is carried out at 20rmp, rotation is carried out at 600rmp, and the time is 30 min.
4) High-speed dispersion, parameter setting: revolution is carried out at 25rmp, rotation is carried out at 1200rmp, and the time is 210 min.
A lithium ion battery comprises a positive plate and a negative plate, wherein the positive plate is prepared from the lithium iron phosphate oily positive slurry, and the lithium iron phosphate oily positive slurry specifically comprises the following components:
A. uniformly coating the prepared conductive slurry on two surfaces of the aluminum foil of the positive current collector by a transfer coater, wherein the thickness of the aluminum foil is 12-16 mu m, and the single-side coating weight is 168.8g/m 2 And simultaneously drying by adopting a convection drying mode, wherein the single-side coating speed is 4m/min, and the single-side drying parameters are as follows: the temperature is 120-115-110 ℃, and the fan frequency is as follows: 35Hz-32Hz-30Hz-30 Hz; the double-sided coating speed is 4m/min, and the double-sided drying parameters are as follows: the temperature is 120-118-115 ℃, and the frequency of a fan is as follows: 38Hz-38Hz-38Hz-38 Hz; and obtaining the oily positive pole piece.
B. Using a mass of 2.3g/mm 3 The cold-pressed pole piece is obtained by the cold-pressed density, is subjected to strip division, is baked for 24 hours at 85 ℃, and is wound, injected, formed and held with the corresponding graphite negative pole pieceA series of procedures such as quantity, partial volume and the like are carried out to prepare the lithium ion (30Ah) hard shell battery cell with excellent consistency.
The difference between the comparative example 1 and the example 1 is that NMP is used as a solvent, as shown in fig. 2, the change trend of the viscosity of the slurry of the comparative example 1 and the slurry of the example 1 along with the time is shown, it can be seen that the viscosity of the oily slurry of the comparative example 1 rises rapidly within 6h along with the increase of the standing time, which is not beneficial to the coating of the slurry, while the viscosity of the aqueous slurry of the example 1 rises slowly within 6h, which shows that the aqueous slurry of the lithium iron phosphate is beneficial to improving the increase of the viscosity of the oily slurry caused by the gelation.
As shown in fig. 3 and 4, the cycle performance test comparison results of the 30Ah aqueous positive electrode hard shell battery cell obtained in example 1 of the present invention and the 30Ah oily positive electrode hard shell battery cell obtained in comparative example 1 are shown, and the test is performed by using the charge and discharge rate of 1C/1C and the charge and discharge interval of 2.5V to 3.65V, so that the cycle trends at 25 ℃ and 60 ℃ of the battery prepared by the formulation in the example are obviously better than those of the battery prepared by the formulation in the comparative example.
Claims (9)
1. The lithium iron phosphate water-based anode slurry is characterized by comprising the following raw materials in percentage by mass:
47.0 wt% -49.0 wt% of lithium iron phosphate, 0.34 wt% -0.5 wt% of carbon nanotube dispersion CNTs, 0.15 wt% -0.3 wt% of conductive carbon black, 0.5 wt% -1.0 wt% of PAA polyacrylic acid binder solution, 0.25 wt% -0.5 wt% of styrene-butadiene rubber emulsion SBR, 0.4 wt% -0.6 wt% of carboxymethyl cellulose CMC, 1.0 wt% -2.0 wt% of ethylene carbonate EC, and 47% -50% of deionized water;
the total amount of the raw materials is 100 percent;
the preparation method of the lithium iron phosphate aqueous anode slurry comprises the following steps:
1) carrying out dry mixing and dispersing on the lithium iron phosphate, the conductive carbon black and the carboxymethyl cellulose according to the formula amount;
2) adding one fifth to one fourth of deionized water, ethylene carbonate and polyacrylic acid binder solution according to the formula amount for soaking powder, and kneading;
3) adding the deionized water and the carbon nano tube dispersion liquid with the rest formula amount, and performing high-speed dispersion to obtain a uniform solution;
4) and finally adding styrene butadiene rubber emulsion and dispersing at low speed to obtain the product.
2. The lithium iron phosphate aqueous positive electrode slurry according to claim 1, wherein the dry-mixing dispersion conditions in step 1) are as follows: revolution at 15-30rpm, rotation at 600-1000rpm, and time at 30-60 min.
3. The lithium iron phosphate aqueous positive electrode slurry of claim 1, wherein in the step 2), the stirring parameters are set as follows during the powder soaking process: revolution at 15-30rpm, rotation at 600-1000rpm, and time at 1-5 min.
4. The lithium iron phosphate aqueous positive electrode slurry according to claim 1, wherein the kneading in step 2) is performed by setting parameters: revolving at 15-30rpm for 60-120 min.
5. The lithium iron phosphate aqueous positive electrode slurry according to claim 1, wherein high-speed dispersion is performed in step 3), and parameters are set as follows: revolution at 15-30rpm, rotation at 800-.
6. The lithium iron phosphate aqueous positive electrode slurry according to claim 1, wherein parameters in step 4) are set as follows: revolution at 15-30rpm, rotation at 500-800rpm, and time at 30-90 min.
7. The environment-friendly long-cycle lithium ion battery is characterized by being manufactured by adopting the anode prepared from the lithium iron phosphate aqueous anode slurry disclosed by any one of claims 1 to 6.
8. The environment-friendly long-cycle lithium ion battery according to claim 7, wherein the method for manufacturing the positive electrode comprises: the thickness of the aluminum foil is 12-16 mu m, the lithium iron phosphate water-based anode slurry is uniformly coated on two surfaces of the anode current collector aluminum foil through a transfer coater, and meanwhile, a convection drying mode is adopted for drying, wherein single-side coating is firstly carried out, and then double-side coating is carried out after drying; and obtaining the water-based positive pole piece.
9. The environment-friendly long-cycle lithium ion battery according to claim 8, wherein the obtained positive electrode plate is 2.2-2.4g/mm 3 The pole piece after cold pressing is obtained through the cold pressing density, and then the pole piece is manufactured into the environment-friendly long-circulation type lithium ion battery.
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