CN112582577A - Lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process and prepared slurry - Google Patents
Lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process and prepared slurry Download PDFInfo
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- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
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- B01F33/82—Combinations of dissimilar mixers
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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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Abstract
A lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process and a prepared slurry comprise the following steps: s1) putting the dry powder into a stirring cylinder, and controlling the temperature in the stirring process; s2) wetting stage: adding conductive slurry into the uniformly mixed dry powder obtained in the step S1), and adding the conductive slurry for 4-6 times; s3) kneading stage: after the last 1 time of conductive slurry feeding is finished, adding a solvent to adjust the solid content of the slurry in the stirring cylinder to 66% -68% for kneading, and gradually increasing the revolution speed and the dispersion speed; s4) adding the solvent into a stirring cylinder at one time, and continuing stirring. The invention improves the particle agglomeration of the slurry and reduces the fineness of the slurry; the slurry kneaded under the high solid content condition is beneficial to uniformly dispersing the material under the action of high shear force, so that the charge and discharge of the high-rate battery are more uniform, the rate charge and discharge performance of the battery is greatly improved, and the service life of the battery is greatly prolonged. In addition, the invention shortens the homogenizing period to 4.5-5.5 h.
Description
Technical Field
The invention relates to the technical field of lithium batteries, in particular to a dry-process homogenizing process for lithium iron phosphate start-stop battery anode slurry.
Background
Although the lithium battery has the defects of cost, grouping, safety performance and the like in the field of starting batteries, the lithium starting and stopping battery is taken as an important component of an automobile as the starting and stopping technology becomes hot, and the lithium iron phosphate system starting and stopping battery has outstanding advantages in light weight, service life, charging and discharging and safety performance.
The pulping process of the battery anode slurry is used as the first process of lithium battery manufacturing, and is the most important in the whole lithium battery manufacturing process. Under the condition of using a conventional stirrer and ensuring the feeding amount, the current lithium iron phosphate anode slurry dry-method pulping process has the following problems in the manufacturing process: 1. the kneading with high solid content causes rubbing between the stirring paddle and the cylinder wall; 2. the kneading with low solid content causes uneven material dispersion, more particles and incapability of coating in the later process; 3. the kneading time is long and the effect is poor at a low solid content, resulting in a prolonged stirring time at the high-speed dispersion stage. The above problems lead to the following results: 1. metal impurities are introduced into the slurry to influence the safety performance of the battery; 2. the material is not uniformly dispersed, the particle agglomeration can influence the coating production efficiency, and the serious condition influences the multiplying power charge-discharge performance of the battery; 3. the long stirring time seriously affects the production efficiency and increases the manufacturing cost.
Disclosure of Invention
The invention provides a lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process, which can effectively avoid scraping of a stirring paddle and a cylinder wall, improve the dispersion effect of a conductive agent and conductive slurry and shorten the process period by improving the processes of wetting stirring and high solid content kneading under the condition of using a conventional stirrer and ensuring the feeding amount.
The invention also provides the lithium iron phosphate start-stop battery anode slurry prepared by the lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process, which has the characteristics of low slurry fineness, improved slurry particle agglomeration, good fluidity, easiness in sieving and the like.
The technical scheme adopted by the invention for solving the technical problems is as follows: the process comprises the following steps:
s1) putting dry powder into a stirring cylinder with a circulating water cooling function at one time, wherein the revolution speed is 10-15rpm, the dispersion speed is 100-300rpm, the stirring time is 15min, the alarm stopping current of the stirrer is set to be 90-110A before stirring is started, the delay time is 1', the stirring paddle is prevented from being rubbed by the cylinder due to overlarge resistance in the kneading and stirring process, and the temperature in the stirring process is controlled to be 40-50 ℃;
s2) wetting stage: adding conductive slurry into the uniformly mixed dry powder obtained in the step S1), wherein the conductive slurry is added in 4-6 times, the revolution speed is 15-25rpm, the dispersion speed is 300-500rpm, and the stirring time is 5min each time; the process aims at: by controlling revolution and dispersion rotation speed, the CNT is pre-dispersed uniformly, so that the increase of kneading resistance caused by local agglomeration of slurry in a kneading stage is prevented;
s3) kneading stage: in the step S2), after the last 1 time of conductive slurry feeding is finished, adding a solvent to adjust the solid content of the slurry in the stirring cylinder to 66% -68% for kneading, wherein the revolution speed is gradually increased from-5 rpm to 25rpm, the dispersion speed is gradually increased from 100-1000rpm, and the kneading time is 105-155 min; the process aims at: the problem that the stirring paddle or the dispersion disc is scraped with the cylinder wall due to overhigh viscosity of the slurry and overlarge load of the stirrer in the initial kneading stage is solved, and the slurry is rapidly sheared after the viscosity of the slurry is gradually reduced under the shearing action by gradually increasing revolution and dispersion rotating speed, so that the material dispersion is accelerated. The kneading under the condition of the scheme can effectively avoid the scraping and rubbing of the stirring paddle and the cylinder wall, so that the material dispersing effect is optimal, the subsequent stirring time can be shortened, and the purpose of shortening the period of the anode slurry homogenizing process is achieved.
S4) after the step S3) is finished, the solvent is added into the stirring cylinder at one time, the revolution speed is 10-25rpm, the dispersion speed is 1200-1400rpm, and the stirring time is continued for 130 min.
In step S3), after the last 1 time of conductive paste feeding is finished, adding a solvent to adjust the solid content of the paste in the stirring cylinder to 66% -68%, kneading and stirring, and performing the following stirring steps: revolution at-5 rpm for 6-10 min; revolving at 5rpm for 6-10 min; revolving at 8rpm for 6-10 min; revolving at 15rpm for 4-8 min; revolving at 20rpm for 4-8 min; revolving at 25rpm for 5-15 min; revolving at 25rpm, dispersing at 100rpm, and maintaining for 4-8 min; revolving at 25rpm, dispersing at 200rpm, and maintaining for 4-8 min; revolving at 25rpm, dispersing at 300rpm, and maintaining for 2-6 min; revolving at 25rpm, dispersing at 500rpm, and maintaining for 2-6 min; revolution at 25rpm, dispersion at 800rpm, and time 2-6 min; revolving at 25rpm, dispersing at 1000rpm for 20min, and scraping material by opening the cylinder; revolving at 25rpm, dispersing at 1000rpm, and maintaining for 40 min.
The step S4) high-speed dispersion stage is step high-speed dispersion: after the solvent is added into the stirring cylinder at one time, the revolution speed is 10rpm, the time is 10min, and the temperature is controlled to be 40-50 ℃ in the stirring process; the revolution speed is 15-25rpm, the dispersion speed is 1200-1400rpm, the time is 30min, and the temperature in the stirring process is controlled to be 40-50 ℃; revolution speed is 15-25rpm, dispersion speed is 1200-1400rpm, time is 60min, and temperature is controlled at 20-25 ℃ during stirring.
Step S5) defoaming stage: and (4) after the step S4) is finished, continuing stirring, wherein the revolution speed is-15 rpm, the time is 30min, the temperature in the stirring process is controlled to be 20-25 ℃, and the vacuum degree of a stirring cylinder is controlled to be-95 KPa-90 KPa.
The dry powder comprises a lithium iron phosphate active material, a conductive agent (Super P) and a binder (PVDF).
The conductive paste of the present invention is a Carbon Nanotube (CNT) paste and the solvent is NMP (N-methylpyrrolidone).
The material feeding amount in the stirring cylinder is 60-90% of the effective volume of the stirring cylinder.
Compared with the prior art, the invention solves the three problems of uneven dispersion of low-solid content kneading materials, easy cylinder rubbing of high-solid content kneading and long stirring time in the stirring process of the lithium iron phosphate start-stop battery anode slurry using the CNT, and the CNT is added and dispersed uniformly for multiple times by setting the alarm shutdown current of the stirrer, so that the solid content of the kneading is improved, the kneading stirring speed is gradually increased, the stirring paddle cylinder rubbing in the stirring process is effectively avoided, the particle agglomeration of the slurry is improved, and the fineness of the slurry is reduced. The slurry kneaded under the condition of high solid content is beneficial to uniformly dispersing materials, especially CNT (carbon nano tube conductive liquid), by the aid of the materials, gaps among the stirring paddles, a cylinder wall, the stirring paddles and a cylinder bottom under the action of high shear force, and reducing the fineness of the slurry, thereby reducing coating scratches and dark marks, reducing large particles on the surface of a pole piece, increasing the contact area among the materials, especially the contact area between the conductive agent and a main material, enabling the charge and discharge of the high-rate battery to be more uniform, and greatly improving the rate charge and discharge performance and the service life of the battery. In addition, the invention shortens the homogenizing period to 4.5-5.5 h.
Compared with the prior art, the invention has the following improvement effect.
| Stirring method | Time for ingredients (h) | Solid content of kneading | Fineness of pulp (mum) | Viscosity of the slurry (mPa.s) |
| Prior Art | 10-12 | 58%-60% | ＞30 | 6000-8000 |
| The invention | 4.5-5.5 | 66%-68% | ＜20 | 2000-4000 |
Detailed Description
In order to make a person skilled in the art better understand the technical solution of the present invention, the following will clearly and completely describe the technical solution of the present invention in combination with the embodiments, wherein the used lithium iron phosphate, PVDF, conductive agent, conductive paste, and NMP are all common raw materials in the art, and can be purchased from the market directly, and therefore, the description of the three raw materials is omitted in the description process.
Example 1
A lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process comprises the following steps that dry powder feeding amount accounts for 60% of an effective volume of a stirrer:
s1, dry mixing stage: according to the formula requirement of the lithium iron phosphate start-stop battery, dry powder (lithium iron phosphate, PVDF and conductive agent) is put into a stirring cylinder with a circulating water cooling function at one time, the revolution speed is 10rpm, the dispersion speed is 100rpm, the stirring time is 15min, the alarm stop current of the stirrer is set to be 110A before stirring is started, the delay time is 1', and the temperature in the stirring process is controlled to be 40-50 ℃;
s2, wetting stage: adding conductive slurry into the dry powder uniformly mixed in the step S1, adding the conductive slurry into the dry powder by 4 times, revolving at the revolution speed of 15rpm, dispersing at the dispersion speed of 300rpm, stirring for 5min each time, controlling the temperature to be 40-50 ℃ in the stirring process, and then opening a cylinder to scrape the materials after the stirring is finished;
s3, kneading stage: in the step S2, after the last 1 conductive paste feeding is finished, adding the solvent to adjust the solid content of the paste in the stirring cylinder to 68%, kneading and stirring, and performing the following stirring steps: revolution at-5 rpm for 6 min; revolution at 5rpm for 6 min; revolution at 8rpm for 6 min; revolving at 15rpm for 4 min; revolving at 20rpm for 4 min; revolving at 25rpm for 5 min; revolving at 25rpm, dispersing at 100rpm, and maintaining for 4 min; revolving at 25rpm, dispersing at 200rpm, and maintaining for 4 min; revolving at 25rpm, dispersing at 300rpm, and maintaining for 2 min; revolving at 25rpm, dispersing at 500rpm, and maintaining for 2 min; revolution at 25rpm, dispersion at 800rpm, time 2 min; revolving at 25rpm, dispersing at 1000rpm for 20min, and scraping material by opening the cylinder; revolving at 25rpm, dispersing at 1000rpm for 40min, and controlling the temperature at 40-50 deg.C during stirring;
s4, high-speed dispersion stage: after the step S3 is finished, the solvent is added into the stirring cylinder at one time, and the revolution speed is 10rpm for 10 min; revolution speed of 15rpm, dispersion speed of 1200rpm, time of 30min, and temperature control of 40-50 ℃ during stirring; revolution speed 15rpm, dispersion speed 1200rpm, time 60min, and stirring process temperature controlled at 20-25 deg.C.
S5, defoaming: and (4) after the step S4 is finished, continuing stirring, controlling the revolution speed to be 15rpm below zero for 30min, controlling the temperature in the stirring process to be 20-25 ℃, and controlling the vacuum degree of a stirring cylinder to be 95KPa below zero to 90KPa, thus obtaining the lithium iron phosphate start-stop battery anode slurry.
Example 2
A lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process comprises the following steps that dry powder feeding amount accounts for 75% of an effective volume of a stirrer, and the concrete stirring process is as follows:
s1, dry mixing stage: according to the formula requirement of the lithium iron phosphate start-stop battery, dry powder is put into a stirring cylinder with a circulating water cooling function at one time, the revolution speed is 15rpm, the dispersion speed is 200rpm, the stirring time is 15min, the alarm shutdown current of the stirrer is set to be 100A before stirring is started, the delay time is 1', and the temperature in the stirring process is controlled to be 40-50 ℃;
s2, wetting stage: adding conductive slurry into the dry powder uniformly mixed in the step S1, adding the conductive slurry for 5 times, revolving at a revolution speed of 20rpm, dispersing at a dispersion speed of 400rpm, stirring for 5min each time, controlling the temperature at 40-50 ℃ in the stirring process, and then opening a cylinder to scrape the materials after the stirring is finished;
s3, kneading stage: in the step S2, after the last 1 conductive paste feeding is finished, adding the solvent to adjust the solid content of the paste in the stirring cylinder to 67%, kneading and stirring, and performing the following stirring steps: revolution at-5 rpm for 8 min; revolving at 5rpm for 8 min; revolution at 8rpm for 8 min; revolving at 15rpm for 6 min; revolving at 20rpm for 6 min; revolving at 25rpm for 10 min; revolving at 25rpm, dispersing at 100rpm, and standing for 6 min; revolving at 25rpm, dispersing at 200rpm, and standing for 6 min; revolving at 25rpm, dispersing at 300rpm, and maintaining for 4 min; revolving at 25rpm, dispersing at 500rpm, and maintaining for 4 min; revolution at 25rpm, dispersion at 800rpm, time 4 min; revolving at 25rpm, dispersing at 1000rpm for 20min, and scraping material by opening the cylinder; revolving at 25rpm, dispersing at 1000rpm for 40min, and controlling the temperature at 40-50 deg.C during stirring;
s4, high-speed dispersion stage: after the step S3 is finished, the solvent is added into the stirring cylinder at one time, and the revolution speed is 10rpm for 10 min; revolution speed of 20rpm, dispersion speed of 1300rpm, time of 30min, and temperature control of 40-50 ℃ during stirring; revolution speed 20rpm, dispersion speed 1300rpm, time 60min, and stirring process temperature controlled at 20-25 deg.C.
S5, defoaming: and (4) after the step S4 is finished, continuing stirring, controlling the revolution speed to be 15rpm below zero for 30min, controlling the temperature in the stirring process to be 20-25 ℃, and controlling the vacuum degree of a stirring cylinder to be 95KPa below zero to 90KPa, thus obtaining the lithium iron phosphate start-stop battery anode slurry.
Example 3
A lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process comprises the following steps that dry powder feeding amount accounts for 90% of an effective volume of a stirrer, and the concrete stirring process comprises the following steps:
s1, dry mixing stage: according to the formula requirement of the lithium iron phosphate start-stop battery, dry powder is put into a stirring cylinder with a circulating water cooling function at one time, the revolution speed is 15rpm, the dispersion speed is 300rpm, the stirring time is 15min, the alarm shutdown current of a stirrer is set to be 90A before stirring is started, the delay time is 1', and the temperature in the stirring process is controlled to be 40-50 ℃;
s2, wetting stage: adding conductive slurry into the dry powder uniformly mixed in the step S1, adding the conductive slurry for 6 times, revolving at a revolution speed of 25rpm, dispersing at a dispersion speed of 500rpm, stirring for 5min each time, controlling the temperature at 40-50 ℃ in the stirring process, and then opening a cylinder to scrape the materials after the stirring is finished;
s3, kneading stage: in the step S2, after the last 1 conductive paste feeding is finished, adding the solvent to adjust the solid content of the paste in the stirring cylinder to 66%, kneading and stirring, and performing the following stirring steps: revolution at-5 rpm for 10 min; revolving at 5rpm for 10 min; revolution at 8rpm for 10 min; revolving at 15rpm for 8 min; revolving at 20rpm for 8 min; revolving at 25rpm for 15 min; revolving at 25rpm, dispersing at 100rpm, and maintaining for 8 min; revolving at 25rpm, dispersing at 200rpm, and maintaining for 8 min; revolving at 25rpm, dispersing at 300rpm, and standing for 6 min; revolving at 25rpm, dispersing at 500rpm, and standing for 6 min; revolution at 25rpm, dispersion at 800rpm, time 6 min; revolving at 25rpm, dispersing at 1000rpm for 20min, and scraping material by opening the cylinder; revolving at 25rpm, dispersing at 1000rpm for 40min, and controlling the temperature at 40-50 deg.C during stirring;
s4, high-speed dispersion stage: after the step S3 is finished, the solvent is added into the stirring cylinder at one time, and the revolution speed is 10rpm for 10 min; revolution speed of 25rpm, dispersion speed of 1400rpm, time of 30min, and temperature control of 40-50 ℃ during stirring; revolution speed is 25rpm, dispersion speed is 1400rpm, time is 60min, and temperature is controlled to be 20-25 ℃ during stirring.
S5, defoaming: and (4) after the step S4 is finished, continuing stirring, controlling the revolution speed to be 15rpm below zero for 30min, controlling the temperature in the stirring process to be 20-25 ℃, and controlling the vacuum degree of a stirring cylinder to be 95KPa below zero to 90KPa, thus obtaining the lithium iron phosphate start-stop battery anode slurry.
Claims (8)
1. A lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process is characterized by comprising the following steps:
s1) putting dry powder into a stirring cylinder with a circulating water cooling function at one time, wherein the revolution speed is 10-15rpm, the dispersion speed is 100-300rpm, the stirring time is 15min, the alarm stopping current of the stirrer is set to be 90-110A before stirring is started, the delay time is 1', the stirring paddle is prevented from being rubbed by the cylinder due to overlarge resistance in the kneading and stirring process, and the temperature in the stirring process is controlled to be 40-50 ℃;
s2) wetting stage: adding conductive slurry into the dry powder uniformly mixed in the step S1, wherein the conductive slurry is added in 4-6 times, the revolution speed is 15-25rpm, the dispersion speed is 300-500rpm, the stirring time is 5min each time, and the temperature is controlled at 40-50 ℃;
s3) kneading stage: in the step S2, after the last 1 time of conductive slurry feeding is finished, adding a solvent to adjust the solid content of the slurry in the stirring cylinder to 66% -68% for kneading, wherein the revolution speed is gradually increased from-5-25 rpm, the dispersion speed is gradually increased from 100-1000rpm, the kneading time is 105-155min, and the temperature is controlled to be 40-50 ℃;
s4) high-speed dispersion stage: after the step S3 is finished, the solvent is added into the stirring cylinder at one time, the revolution speed is 10-25rpm, the dispersion speed is 1200-1400rpm, and the stirring time is continued for 130 min.
2. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: in the step S3), after the last 1 time of conductive paste feeding is finished, adding a solvent to adjust the solid content of the paste in the stirring cylinder to 66% -68%, kneading and stirring, and performing the following stirring steps: revolution at-5 rpm for 6-10 min; revolving at 5rpm for 6-10 min; revolving at 8rpm for 6-10 min; revolving at 15rpm for 4-8 min; revolving at 20rpm for 4-8 min; revolving at 25rpm for 5-15 min; revolving at 25rpm, dispersing at 100rpm, and maintaining for 4-8 min; revolving at 25rpm, dispersing at 200rpm, and maintaining for 4-8 min; revolving at 25rpm, dispersing at 300rpm, and maintaining for 2-6 min; revolving at 25rpm, dispersing at 500rpm, and maintaining for 2-6 min; revolution at 25rpm, dispersion at 800rpm, and time 2-6 min; revolving at 25rpm, dispersing at 1000rpm for 20min, and scraping material by opening the cylinder; revolving at 25rpm, dispersing at 1000rpm, and maintaining for 40 min.
3. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: the step S4) high-speed dispersion stage is step high-speed dispersion: after the solvent is added into the stirring cylinder at one time, the revolution speed is 10rpm, the time is 10min, and the temperature is controlled to be 40-50 ℃ in the stirring process; the revolution speed is 15-25rpm, the dispersion speed is 1200-1400rpm, the time is 30min, and the temperature in the stirring process is controlled to be 40-50 ℃; revolution speed is 15-25rpm, dispersion speed is 1200-1400rpm, time is 60min, and temperature is controlled at 20-25 ℃ during stirring.
4. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: step S5) defoaming: and (4) after the step S4) is finished, continuing stirring, wherein the revolution speed is-15 rpm, the time is 30min, the temperature in the stirring process is controlled to be 20-25 ℃, and the vacuum degree of a stirring cylinder is controlled to be-95 KPa-90 KPa.
5. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: the dry powder comprises a lithium iron phosphate active material, a conductive agent Super P and a bonding agent PVD.
6. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: the conductive paste is Carbon Nanotube (CNT) paste and the solvent is NMP.
7. The lithium iron phosphate start-stop battery positive electrode slurry dry-process homogenizing process according to claim 1, which is characterized in that: the material feeding amount in the stirring cylinder is 60-90% of the effective volume of the stirring cylinder.
8. The lithium iron phosphate start-stop battery anode slurry prepared by the lithium iron phosphate start-stop battery anode slurry dry-process homogenizing process of claims 1 to 7.
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| CN114441408A (en) * | 2022-01-24 | 2022-05-06 | 蜂巢能源科技(无锡)有限公司 | Method for monitoring degree of fibrosis in dry film making process, dry film making method, and preparation method and application of dry electrode plate |
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